Single and Multiple Insertion of Alkynes into Pd−Acyl and Pd−Aryl Bonds in Cationic Palladium Complexes with Phosphine−Imine (Pσim N) Ligands
Reddy, K. Rajender; Surekha, K.; Lee, Gene-Hsiang; Peng, Shie-Ming; Liu, Shiuh-Tzung; Organometallics 20 (2001) 5557–; doi:10.1021/om0106377

data_4077425
_publ_section_title
;
 Single and Multiple Insertion of Alkynes into Pd&#x2212;Acyl and
 Pd&#x2212;Aryl Bonds in Cationic Palladium Complexes with
 Phosphine&#x2212;Imine (P\sim N) Ligands
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5557
_journal_paper_doi               10.1021/om0106377
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C33 H29 B F4 N O5 P Pd'
_chemical_formula_weight         743.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.242(4)
_cell_length_b                   10.257(2)
_cell_length_c                   19.028(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3285.7(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18632
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.677
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             1504
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0016(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_all   0.892
_refine_ls_goodness_of_fit_obs   0.891
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_restrained_S_obs      0.891
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_obs          0.0372
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1296
_refine_ls_wR_factor_obs         0.1106
_reflns_number_observed          4533
_reflns_number_total             5792
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0106377.cif
_cod_data_source_block           ic6067
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3285.7(11)
_cod_database_code               4077425