Charged Molecular Alloys: Synthesis and Characterization of the Binary Anions Pd7As164- and Pd2As144-
Melanie J. Moses; James Fettinger; Bryan Eichhorn; Journal of the American Chemical Society 124 (2002) 5944–5945; doi:10.1021/ja025627r

data_4114823
_publ_section_title
;
 Charged Molecular Alloys: Synthesis and Characterization of the Binary
 Anions Pd7As164- and Pd2As144-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5944
_journal_page_last               5945
_journal_paper_doi               10.1021/ja025627r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C75.5 H158 As16 K4 N11.5 O24 Pd7'
_chemical_formula_weight         3711.05
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.4360(10)
_cell_angle_beta                 99.2890(10)
_cell_angle_gamma                99.6560(10)
_cell_formula_units_Z            4
_cell_length_a                   17.2784(9)
_cell_length_b                   27.2637(15)
_cell_length_c                   28.9377(16)
_cell_measurement_temperature    193(2)
_cell_volume                     11931.4(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            143867
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.84
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.639
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      0
_exptl_crystal_description       Plate
_exptl_crystal_F_000             7238
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2465
_refine_ls_number_reflns         42004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                23829
_reflns_number_total             42004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025627r_1.cif
_cod_data_source_block           '[Pd7As16]2[K(2,2,2-crypt)]8*3.5en'
_cod_original_formula_sum        'C75.50 H158 As16 K4 N11.50 O24 Pd7'
_cod_database_code               4114823