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_4068419
_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            'C43.7 H45.1 Cl0.3 O2 P2 Pd Ti'
_chemical_formula_weight         829.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 102.708(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8889(12)
_cell_length_b                   10.1284(6)
_cell_length_c                   20.0295(12)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3661
_cell_measurement_theta_min      2.2836
_cell_volume                     3936.0(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8987
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             1706
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00000(16)
_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   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1741
_refine_ls_R_factor_gt           0.0975
_refine_ls_shift/su_max          3.781
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+18.1773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                5180
_reflns_number_total             8987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008298_si_002.cif
_cod_data_source_block           mizuta-1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/a
_cod_original_formula_sum        'C43.70 H45.10 Cl0.30 O2 P2 Pd Ti'
_cod_database_code               4068419