Synthesis, Structural Characterization, and Gas-Phase Unimolecular Reactivity of the Silver Hydride Nanocluster [Ag3((PPh2)2CH2)3(μ3-H)](BF4)2.
Zavras, Athanasios; Khairallah, George N.; Connell, Timothy U.; White, Jonathan M.; Edwards, Alison J.; Mulder, Roger J.; Donnelly, Paul S.; O'Hair, Richard A J; Inorganic chemistry 53 (2014) 7429–7437; doi:10.1021/ic5007499

data_4340347
_publ_section_title
;
 Synthesis, Structural Characterization, and Gas-Phase Unimolecular
 Reactivity of the Silver Hydride Nanocluster
 [Ag3((PPh2)2CH2)3(\m3-H)](BF4)2.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7429
_journal_page_last               7437
_journal_paper_doi               10.1021/ic5007499
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '(C75 H66 D Ag3 B2 F8 P6, 0.5(C H4 O)'
_chemical_formula_sum            'C75.5 H68 Ag3 B2 D F8 O0.5 P6'
_chemical_formula_weight         1668.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 96.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.9665(10)
_cell_length_b                   13.2190(4)
_cell_length_c                   39.5373(8)
_cell_measurement_reflns_used    35760
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      34.1190
_cell_measurement_theta_min      3.2750
_cell_volume                     14000.8(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      130.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            73424
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.328
_diffrn_reflns_theta_min         2.848
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             6712
_exptl_crystal_size_max          0.5500
_exptl_crystal_size_mid          0.3647
_exptl_crystal_size_min          0.2479
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         27244
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+22.0535P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21917
_reflns_number_total             27244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5007499_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4340347--4340348.cif.'
_cod_original_formula_sum        'C75.50 H68 Ag3 B2 D F8 O0.50 P6'
_cod_database_code               4340347
_shelxl_version_number           2012-9