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_4077424
_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            'C31.5 H28 B Cl F4 N O3 P Pd'
_chemical_formula_weight         728.18
_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
_cell_angle_alpha                114.151(1)
_cell_angle_beta                 116.522(1)
_cell_angle_gamma                94.510(1)
_cell_formula_units_Z            2
_cell_length_a                   12.5765(1)
_cell_length_b                   12.7653(2)
_cell_length_c                   12.7816(1)
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    295(2)
_cell_volume                     1587.20(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19497
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0001(6)
_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   1.026
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1132
_refine_ls_wR_factor_obs         0.1081
_reflns_number_observed          5713
_reflns_number_total             6486
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0106377.cif
_cod_data_source_block           ic5967
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.5601P] 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^)+(0.0625P)^2^+1.5601P] 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        1587.20(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31.50 H28 B Cl F4 N O3 P Pd'
_cod_database_code               4077424