14-Electron Disilene Palladium Complex Having Strong π-Complex Character
Mitsuo Kira; Yumiko Sekiguchi; Takeaki Iwamoto; Chizuko Kabuto; Journal of the American Chemical Society 126 (2004) 12778–12779; doi:10.1021/ja046354y

data_4113026
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
Tohoku University
;
_publ_contact_author_email       ' mkira@si.chem.tohoku.ac.jp '
_publ_contact_author_fax         ' +81-22-217-6589 '
_publ_contact_author_name        ' Mitsuo Kira'
_publ_contact_author_phone       ' +81-22-217-6585 '
_publ_section_title
;
 14-Electron Disilene Palladium Complex Having Strong \p-Complex Character
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12778
_journal_page_last               12779
_journal_paper_doi               10.1021/ja046354y
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C49 H100 P Pd Si6'
_chemical_formula_sum            'C49 H100 P Pd Si6'
_chemical_formula_weight         995.23
_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_method           SHELXL-97
_cell_angle_alpha                76.653(8)
_cell_angle_beta                 71.024(7)
_cell_angle_gamma                85.812(9)
_cell_formula_units_Z            2
_cell_length_a                   12.0473(2)
_cell_length_b                   12.7355(4)
_cell_length_c                   20.39520(10)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      3.1
_cell_volume                     2879.21(19)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20760
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.8844
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0270P)^2^+4.6513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                9338
_reflns_number_total             10965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046354ysi20040818_110557.cif
_cod_data_source_block           (Cy3P)Pd(disilene)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113026