Palladium Alkynyl and Allenylidene Complexes: Very Efficient Precatalysts for C‒C Coupling Reactions
Wuttke, Evelyn; Nägele, Bettina; Weibert, Bernhard; Kessler, Florian; Organometallics 30 (2011) 6270–; doi:10.1021/om200862m

data_4065502
_publ_section_title
;
 Palladium Alkynyl and Allenylidene Complexes: Very Efficient Precatalysts
 for C--C Coupling Reactions
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6270
_journal_paper_doi               10.1021/om200862m
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C32 H60 N2 O2 P2 Pd, 2(B F4)'
_chemical_formula_sum            'C32 H60 B2 F8 N2 O2 P2 Pd'
_chemical_formula_weight         846.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 129.296(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.590(2)
_cell_length_b                   15.586(3)
_cell_length_c                   15.350(5)
_cell_measurement_reflns_used    38405
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.03
_cell_volume                     1960.7(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25256
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.8060
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0311P)^2^+2.7559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                3635
_reflns_number_total             4165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200862m_si_001.cif
_cod_data_source_block           ewbw07a_(10e'-BF4)
_cod_original_cell_volume        1960.7(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4065502