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_4077428
_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            'C59 H45 B F4 N P Pd'
_chemical_formula_weight         992.14
_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                100.8630(10)
_cell_angle_beta                 100.3790(10)
_cell_angle_gamma                90.2920(10)
_cell_formula_units_Z            2
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_cell_length_b                   13.2332(4)
_cell_length_c                   17.7982(6)
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_cell_measurement_temperature    150(2)
_cell_volume                     2322.30(13)
_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      150(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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26317
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_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   Multiscan(SADABS)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.726
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0000(3)
_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   1.064
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7939
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0386
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_refine_ls_shift/esd_max         -4.885
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+2.1758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0854
_refine_ls_wR_factor_obs         0.0792
_reflns_number_observed          7185
_reflns_number_total             8172
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0106377.cif
_cod_data_source_block           ic7736
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+2.1758P] 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^)+(0.0434P)^2^+2.1758P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077428