A Stable 1,2-Disilacyclohexene and Its 14-Electron Palladium(0) Complex
Takashi Abe; Takeaki Iwamoto; Mitsuo Kira; Journal of the American Chemical Society 132 (2010) 5008–5009; doi:10.1021/ja101654b

data_4102261
_publ_section_title
;
 A Stable 1,2-Disilacyclohexene and Its 14-Electron Palladium(0) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5008
_journal_page_last               5009
_journal_paper_doi               10.1021/ja101654b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C46 H83 P Pd Si6'
_chemical_formula_weight         942.03
_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                 99.409(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.231(2)
_cell_length_b                   20.760(4)
_cell_length_c                   22.617(5)
_cell_measurement_reflns_used    '   8738'
_cell_measurement_temperature    173
_cell_measurement_theta_max      '      27.44'
_cell_measurement_theta_min      '       2.18'
_cell_volume                     5202.3(18)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58283
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_correction_T_min  0.8972
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         11816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0307P)^2^+2.2724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                10052
_reflns_number_total             11816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101654b_si_003.cif
_cod_data_source_block           ta31_(Cy3P)Pd(disilene)_complex
_cod_original_cell_volume        5202.6(18)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4102261