Electrochemical Reduction of CO2to CO Catalyzed by a Bimetallic Palladium Complex
Raebiger, James W.; Turner, Jeffrey W.; Noll, Bruce C.; Curtis, Calvin J.; Miedaner, Alex; Cox, Brian; DuBois, Daniel L.; Organometallics 25 (2006) 3345–; doi:10.1021/om060228g

data_4075337
_publ_section_title
;
 Electrochemical Reduction of CO2to CO Catalyzed by a Bimetallic Palladium
 Complex
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3345
_journal_paper_doi               10.1021/om060228g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety
'C66 H114 N2 P6 Pd2, 0.78(C H2 Cl2), 3(C2 H3 N)'
_chemical_formula_sum            'C72.78 H124.56 B4 Cl1.56 F16 N5 P6 Pd2'
_chemical_formula_weight         1870.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.821(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.125(6)
_cell_length_b                   12.386(3)
_cell_length_c                   27.917(6)
_cell_measurement_reflns_used    8483
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      23.102
_cell_measurement_theta_min      2.234
_cell_volume                     8677(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      135(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42928
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.8389
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3875
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         11339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1325P)^2^+9.6648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2383
_reflns_number_gt                6892
_reflns_number_total             11339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060228gsi20060312_121627.cif
_cod_data_source_block           rfcjt1s
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075337