Bi- and Trinuclear Complexes of Group 4 Metal and Palladium Bridged by OPPh2Groups: Synthesis and High Catalytic Activities in Double Hydrophosphinylation of 1-Octyne
Mizuta, Tsutomu; Miyaji, Chihiro; Katayama, Takafumi; Ushio, Jun-ichi; Kubo, Kazuyuki; Miyoshi, Katsuhiko; Organometallics 28 (2009) 539–; doi:10.1021/om8008298

data_4068422
_publ_section_title
;
 Bi- and Trinuclear Complexes of Group 4 Metal and Palladium Bridged by
 OPPh2Groups: Synthesis and High Catalytic Activities in Double
 Hydrophosphinylation of 1-Octyne
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              539
_journal_paper_doi               10.1021/om8008298
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C105 H96 O6 P8 Pd2 Ti'
_chemical_formula_weight         1962.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                95.0290(10)
_cell_angle_beta                 102.0540(10)
_cell_angle_gamma                107.525(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4700(2)
_cell_length_b                   15.2910(3)
_cell_length_c                   24.5460(7)
_cell_measurement_temperature    200(2)
_cell_volume                     4652.94(19)
_computing_cell_refinement       'HKL (Otwinowski, 1997)'
_computing_data_collection       'HKL (Otwinowski, 1997)'
_computing_data_reduction        'HKL (Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Mac Science DIP2030 Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19971
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8774
_exptl_absorpt_correction_T_min  0.8003
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0068(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         19971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+6.2869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                14723
_reflns_number_total             19971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008298_si_002.cif
_cod_data_source_block           mizuta-6
_cod_original_cell_volume        4652.93(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068422