Bis(tetraphenylphosphonium) bis(tetraselenomolybdato)palladate(II)
Shiffler, Zachary J.; Baldwin, Steven M.; Keane, Joseph M.; Belz, Brian L.; Barr, Matthew L.; Slavin III, Edward R.; Kastner, Margaret E.; Mahler, Charles H.; Acta Crystallographica Section E 60 (2004) m1539–m1541; doi:10.1107/S1600536804023104

data_2204369
_publ_section_title
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 Bis(tetraphenylphosphonium) bis(tetraselenomolybdato)palladate(II)
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_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1539
_journal_page_last               m1541
_journal_paper_doi               10.1107/S1600536804023104
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C24 H20 P)2 [Pd Mo2 Se8]'
_chemical_formula_moiety         '2C24 H20 P +, Mo2 Pd Se8 2-'
_chemical_formula_sum            'C48 H40 Mo2 P2 Pd Se8'
_chemical_formula_weight         1608.70
_chemical_name_systematic
'Bis(tetraphenylphosphonium) bis(tetraselenomolybdato)palladate(II)'
_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                66.096(13)
_cell_angle_beta                 84.511(13)
_cell_angle_gamma                70.047(9)
_cell_formula_units_Z            1
_cell_length_a                   9.4976(9)
_cell_length_b                   12.5798(16)
_cell_length_c                   12.622(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.944
_cell_measurement_theta_min      6.516
_cell_volume                     1294.3(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1991-1996)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6737
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.539
_exptl_absorpt_correction_T_max  0.095
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2000)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake/arrowhead
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0733P)^2^+3.8281P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                3974
_reflns_number_total             5698
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6276.cif
_cod_data_source_block           I
_cod_database_code               2204369
_cod_database_fobs_code          2204369