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_4340348
_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 D1 Ag3 P6, 2 (B 1 F 4), 0.5(C 1 H 4 O)'
_chemical_formula_sum            'C75.5 H68 Ag3 B2 D F8 O0.5 P6'
_chemical_formula_weight         1668.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     geom
_atom_sites_solution_secondary   geom
_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    0
_cell_measurement_temperature    123
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     14000.8(7)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003) + LaueG'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
;
;
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 1.619
_diffrn_measured_fraction_theta_max 1.619
_diffrn_measurement_details      '26 images, exposure time 167 minutes'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.2398
_diffrn_reflns_av_unetI/netI     0.2185
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64498
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.00
_diffrn_reflns_theta_full        57.98
_diffrn_reflns_theta_max         58.08
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          2.0
_exptl_crystal_size_mid          1.0
_exptl_crystal_size_min          0.8
_refine_diff_density_max         1.71
_refine_diff_density_min         -1.37
_refine_ls_extinction_coef       30(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.1280
_refine_ls_shift/su_max          0.0012035
_refine_ls_shift/su_mean         0.0000249
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 15.5 -8.44 3.47 4.16 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1491
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                4647
_reflns_number_total             5994
_reflns_threshold_expression     >2sigma(I)
_oxford_refine_ls_r_factor_ref   0.1153
_oxford_refine_ls_scale          0.3190(19)
_oxford_reflns_number_all        5803
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic5007499_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4340347--4340348.cif.'
_cod_original_sg_symbol_H-M      'I 1 2/a 1 '
_cod_original_formula_sum        'C75.50 H68 Ag3 B2 D1 F8 O0.50 P6'
_cod_database_code               4340348
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE EXTPARAM 
CONT P  (    11 ,X'S,U[ISO])  UNTIL D(1) 
CONT B(1,X'S,U'S) UNTIL F(24) 
CONT AG(1,X'S,U'S) UNTIL AG(3) C(4,X'S,U'S) O(1,X'S,U[ISO]) 
RIDE C(4,X'S) H(41,X'S) UNTIL H(43) 
EQUIV H(41,U[ISO]) H(42,U[ISO]) H(43,U[ISO]) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;