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_1556086
_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         'C144 H126 Ag10 N6 P12, 4(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C148 H134 Ag10 B2 Cl8 F8 N6 P12'
_chemical_formula_weight         3904.16
_chemical_name_systematic        '[Ag10H8(dppa)6](BF4)2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1498(7)
_cell_length_b                   17.1737(3)
_cell_length_c                   30.4308(7)
_cell_measurement_reflns_used    15798
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.8480
_cell_measurement_theta_min      2.9000
_cell_volume                     14711.4(6)
_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      100.01(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2045
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            73646
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.298
_diffrn_reflns_theta_min         2.904
_exptl_absorpt_coefficient_mu    13.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16800
_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    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             7728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and pentane'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.195
_refine_diff_density_max         2.726
_refine_diff_density_min         -3.625
_refine_diff_density_rms         0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15461
_refine_ls_number_restraints     1001
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.1210
_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^)+(0.1854P)^2^+224.3415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3062
_refine_ls_wR_factor_ref         0.3495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10180
_reflns_number_total             15461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr08321a2.cif
_cod_data_source_block           shelx
_cod_database_code               1556086
_shelx_shelxl_version_number     2018/3
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C73(H73A,H73B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N2(H2), C42(H42), C56(H56), C11(H11), C12(H12), C2(H2A),
 C28(H28), C41(H41), C48(H48), C10(H10), C35(H35), C6(H6), C36(H36), C54(H54),
 C20(H20), C60(H60), C53(H53), C17(H17), C18(H18), C5(H5), C47(H47), C34(H34),
 C32(H32), C44(H44), C4(H4), C64(H64), C57(H57), C21(H21), C52(H52), C50(H50),
 C59(H59), C38(H38), C3(H3A), C8(H8), C14(H14), C39(H39), C58(H58), C45(H45),
 C9(H9), C46(H46), C30(H30), C68(H68), C15(H15), C22(H22), C26(H26), C24(H24),
 C70(H70), C27(H27), C71(H71), C16(H16), C51(H51), C72(H72), C23(H23), C40(H40),
  C33(H33), C69(H69), C29(H29), C62(H62), C63(H63), C65(H65), C66(H66)
;
_shelx_res_checksum              24070
_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
;