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_4114824
_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            'C82 H184 As14 K4 N18 O24 Pd2'
_chemical_formula_weight         3224.55
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9132(10)
_cell_length_b                   23.7330(14)
_cell_length_c                   34.141(2)
_cell_measurement_temperature    193(2)
_cell_volume                     12892.7(13)
_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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            100115
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.039
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             6496
_exptl_crystal_size_max          0.573
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.277
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         14810
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0502P)^2^+34.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                10255
_reflns_number_total             14810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025627r_2.cif
_cod_data_source_block           '[Pd2As14][K(2,2,2-crypt)]4*5en'
_cod_original_cell_volume        12892.8(14)
_cod_database_code               4114824