Long-Range Spin Coupling: A Tetraphosphine-Bridged Palladium Dimer
Kuppuswamy Arumugam; Mohammed C. Shaw; Joel T. Mague; Eckhard Bill; Stephen Sproules; James P. Donahue; Inorganic Chemistry 50 (2011) 2995–3002; doi:10.1021/ic102493g

data_4324775
_publ_contact_author_address
; Department of Chemistry
  Tulane University
  6400 Freret Street
  New Orleans, Louisiana 70118-5698
  U.S.A.
;
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_name        'Dr. James P. Donahue'
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
 Long-Range Spin Coupling: A Tetraphosphine-Bridged Palladium Dimer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2995
_journal_page_last               3002
_journal_paper_doi               10.1021/ic102493g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C86 H70 O4 P4 Pd2 S4'
_chemical_formula_weight         1632.34
_chemical_name_systematic
; 
 (\m-1,2,4,5-tetrakis(diphenylphosphino)benzene)bis[(1,2- 
bis(4-methoxyphenyl)ethene-1,2-dithiolato)palladium(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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.994(4)
_cell_angle_beta                 76.492(2)
_cell_angle_gamma                76.029(3)
_cell_formula_units_Z            8
_cell_length_a                   20.988(4)
_cell_length_b                   28.799(5)
_cell_length_c                   31.661(7)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.17
_cell_volume                     17955(6)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w 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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.1440
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            147328
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.9535
_exptl_absorpt_correction_T_min  0.9125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008b)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       Block
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2841
_refine_ls_number_reflns         69710
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+28.2417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                35644
_reflns_number_total             69710
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic102493g_si_002_2.cif
_cod_data_source_block           jpd271_0m
_cod_database_code               4324775