Oxidative Reactions of Tetrametal Pd(0)...Mo(II)-Mo(II)...Pd(0) Clusters: Electrochemical Communication of Two Pd(0) Centers through the Mo2 Moiety and Oxidative Formation of a Pd(I)-Mo(II)-Mo(II)-Pd(I) Array
Kazushi Mashima; Asuka Shima; Keisuke Nakao; Atsushi Fukumoto; Yutaka Kaneda; Inorganic Chemistry 48 (2009) 1879–1886; doi:10.1021/ic801398f

data_4301530
_publ_contact_author_address
;
                   Department of Chemistry
                   Graduate School of Engineering Science
                   Osaka University
                   Machikaneyama, 1-3
                   Toyonaka
                   Osaka, 560-8531
                   Japan
;
_publ_contact_author_email       mashima@chem.es.osaka-u.ac.jp
_publ_contact_author_fax         ' +81 6 6850 6249'
_publ_contact_author_name        ' Prof. Kazushi Mashima '
_publ_contact_author_phone       ' +81 6 6850 6248'
_publ_section_title
;
Oxidative Reactions of Tetrametal Pd(0)...Mo(II)-Mo(II)...Pd(0)
Clusters: Electrochemical Communication of Two Pd(0) Centers through the
Mo2 Moiety and Oxidative Formation of a Pd(I)-Mo(II)-Mo(II)-Pd(I) Array
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1879
_journal_page_last               1886
_journal_paper_doi               10.1021/ic801398f
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'(C76 H56 Mo2 N8 O4 P4 Pd2), 2(C4 H8 O), 1(C4 H10 O) '
_chemical_formula_sum            'C88 H82 Mo2 N8 O7 P4 Pd2'
_chemical_formula_weight         1892.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             ' 1997-Sep 12nd '
_audit_creation_method
'from SHELXL97 CIF and IUCr SHELXL97-template'
_audit_update_record
;
Wed Jun 25th T20:05:08 2008
Thu Jun 26th T19:18 2008 # Formatted by EnCIFer
Thu Jun 26th T19:20 2008 # Formatted by EnCIFer
Thu Jul  2nd T18:20 2008 # Formatted by EnCIFer
Thu Jul  4nd T15:14 2008 # Formatted by publCIF
;
_cell_angle_alpha                96.42(14)
_cell_angle_beta                 108.60(11)
_cell_angle_gamma                102.00(16)
_cell_formula_units_Z            2
_cell_length_a                   18.53(2)
_cell_length_b                   20.23(5)
_cell_length_c                   12.242(14)
_cell_measurement_reflns_used    11
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.89
_cell_measurement_theta_min      14.77
_cell_volume                     4175(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'CrystalStructure (Rigaku/RMC, 2007)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) and modified'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY & DIRDIF-99'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_type       'TEXSAN conversion (MSC, 1989)'
_diffrn_orient_matrix_UB_11      -0.04175
_diffrn_orient_matrix_UB_12      -0.03677
_diffrn_orient_matrix_UB_13      0.00924
_diffrn_orient_matrix_UB_21      0.02927
_diffrn_orient_matrix_UB_22      0.00952
_diffrn_orient_matrix_UB_23      0.08664
_diffrn_orient_matrix_UB_31      -0.02960
_diffrn_orient_matrix_UB_32      0.03476
_diffrn_orient_matrix_UB_33      0.01104
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_sigmaI/netI    0.3054
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19718
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.54
_diffrn_source_current           200.0000
_diffrn_source_power             12.0000
_diffrn_source_voltage           60.0000
_diffrn_standards_decay_%        0.95
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.7274
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'( North, Phillips, & Mathews (1968), Acta Cryst. A24, 351-359. ) '
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.445
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         19126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2712
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                6893
_reflns_number_total             19126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801398f_si_002.cif
_cod_data_source_block           global
_cod_original_cell_volume        4175(12)
_cod_original_sg_symbol_Hall     ' -P 1 '
_cod_database_code               4301530