Synthesis of the First Stable Palladium Allenylidene Complexes
Kessler, Florian; Szesni, Normen; Põhako, Kaija; Weibert, Bernhard; Fischer, Helmut; Organometallics 28 (2009) 348–; doi:10.1021/om800843e

data_4068436
_publ_section_title
;
 Synthesis of the First Stable Palladium Allenylidene Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              348
_journal_paper_doi               10.1021/om800843e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C44 H39 F3 N O3 P2 Pd, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C46 H43 B Cl4 F7 N O3 P2 Pd'
_chemical_formula_weight         1111.76
_chemical_name_systematic
; 
 ? 
;
_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                 90.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.612(2)
_cell_length_b                   23.143(5)
_cell_length_c                   18.136(4)
_cell_measurement_reflns_used    69877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      1.51
_cell_volume                     4873.4(17)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70118
_diffrn_reflns_theta_full        26.84
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.7878
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0477P)^2^+7.2460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                8828
_reflns_number_total             10300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800843e_si_003.cif
_cod_data_source_block           fkbw13
_cod_original_cell_volume        4873.5(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4068436