Preparation, Structures, and Thermal Reactivity of Alkoxycarbonyl(cyano)palladium(II) Complexestrans-Pd(COOR)(CN)(PPh3)2(R = Me, Et,nPr,iPr,nBu,tBu, and Bn) as Intermediates of the Palladium-Catalyzed Cyanoesterification of Norbornene Derivatives
Nishihara, Yasushi; Miyasaka, Mitsuru; Inoue, Yoshiaki; Yamaguchi, Tomoka; Kojima, Masaaki; Takagi, Kentaro; Organometallics 26 (2007) 4054–; doi:10.1021/om700343y

data_4073459
_publ_section_title
;
 Preparation, Structures, and Thermal Reactivity of
 Alkoxycarbonyl(cyano)palladium(II) Complexestrans-Pd(COOR)(CN)(PPh3)2(R =
 Me, Et,nPr,iPr,nBu,tBu, and Bn) as Intermediates of the
 Palladium-Catalyzed Cyanoesterification of Norbornene Derivatives
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4054
_journal_paper_doi               10.1021/om700343y
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C85 H80 Cl2 N2 O4 P4 Pd2 '
_chemical_formula_sum            'C85 H80 Cl2 N2 O4 P4 Pd2'
_chemical_formula_weight         1601.18
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 115.382(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   16.215(3)
_cell_length_b                   15.318(3)
_cell_length_c                   17.591(3)
_cell_measurement_reflns_used    44401
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.0
_cell_volume                     3947.5(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47549
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         7.77
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     893
_refine_ls_number_reflns         22759
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1239P)^2^+25.3399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2125
_reflns_number_gt                20438
_reflns_number_total             22759
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om700343y-file006.cif
_cod_data_source_block           '_3'
_cod_original_cell_volume        3947.6(11)
_cod_original_formula_sum        'C85 H80 Cl2 N2 O4 P4 Pd2 '
_cod_database_code               4073459