Reactions of 9-Triptyceneselenol with Palladium(0) Complexes: Unexpected Formations of the Dinuclear Palladium(I) Complex [{Pd(PPh3)}2(μ-SeTrip)2] and Five-Membered Selenapalladacycle [Pd(η2(C,Se)-Trip)(dppe)]
Nakata, Norio; Uchiumi, Rei; Yoshino, Tomoharu; Ikeda, Takashige; Kamon, Hitomi; Ishii, Akihiko; Organometallics 28 (2009) 1981–; doi:10.1021/om900077d

data_4069223
_publ_section_title
;
 Reactions of 9-Triptyceneselenol with Palladium(0) Complexes: Unexpected
 Formations of the Dinuclear Palladium(I) Complex
 [{Pd(PPh3)}2(\m-SeTrip)2] and Five-Membered Selenapalladacycle
 [Pd(\h2(C,Se)-Trip)(dppe)]
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1981
_journal_paper_doi               10.1021/om900077d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C76 H58 P2 Pd2 Se2, C2 H2 Cl4'
_chemical_formula_sum            'C78 H60 Cl4 P2 Pd2 Se2'
_chemical_formula_weight         1571.72
_chemical_name_common            '[{Pd(PPh3)}2(SeTrip)2]_2 CH2Cl2'
_chemical_name_systematic
; 
 [{Pd(PPh3)}2(SeTrip)2]_2 CH2Cl2 
;
_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_method           SHELXL-97
_cell_angle_alpha                67.2280(10)
_cell_angle_beta                 72.261(2)
_cell_angle_gamma                89.9150(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2728(7)
_cell_length_b                   12.3538(8)
_cell_length_c                   13.3474(9)
_cell_measurement_temperature    103(2)
_cell_volume                     1617.99(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9842
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.8296
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.808
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0715P)^2^+1.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                4908
_reflns_number_total             5991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900077d_si_001.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069223