Palladium-Assisted Formation of Carbon−Carbon Bonds. 7.1Reactions of (2,3,4-Trimethoxy-6-X-phenyl)palladium Complexes with Alkynes (X = C(O)NHBut) and Isocyanides (X = C(O)NHBut, C(O)Me, CHO): Crystal and Molecular Structures of [Pd{C6H{C(O)NHBut}-6-(OMe)3-2,3,4}(bpy)](CF3SO3), [Pd{C(CO2Me)C(CO2Me)C6H{C(O)NHBut}-6-(OMe)3-2,3,4)}- Cl(PPh3)], [Pd{C(NXy)C6H{C(O)NHBut}-6-(OMe)3-2,3,4}- (bpy)](CF3SO3), and the Ketenimine 2-(2,6-Dimethylphenyl)-1-(((2,6-dimethylphenyl)imino)- methylene)-5,6,7-trimethoxy-3-oxoisoindoline
Vicente, José; Abad, José-Antonio; Shaw, Kenneth F.; Gil-Rubio, Juan; Ramírez de Arellano, M. Carmen; Jones, Peter G.; Organometallics 16 (1997) 4557–; doi:10.1021/om970426v

data_4078382
_publ_section_title
;
 Palladium-Assisted Formation of Carbon&#x2212;Carbon Bonds. 7.1Reactions
 of (2,3,4-Trimethoxy-6-X-phenyl)palladium Complexes with Alkynes (X =
 C(O)NHBut) and Isocyanides (X = C(O)NHBut, C(O)Me, CHO):&#x00A0; Crystal
 and Molecular Structures of
 [Pd{C6H{C(O)NHBut}-6-(OMe)3-2,3,4}(bpy)](CF3SO3),
 [Pd{C(CO2Me)C(CO2Me)C6H{C(O)NHBut}-6-(OMe)3-2,3,4)}- Cl(PPh3)],
 [Pd{C(NXy)C6H{C(O)NHBut}-6-(OMe)3-2,3,4}- (bpy)](CF3SO3), and the
 Ketenimine 2-(2,6-Dimethylphenyl)-1-(((2,6-dimethylphenyl)imino)-
 methylene)-5,6,7-trimethoxy-3-oxoisoindoline
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4557
_journal_paper_doi               10.1021/om970426v
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C35 H39 F3 N4 O7.33 Pd S'
_chemical_formula_weight         828.50
_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                72.406(8)
_cell_angle_beta                 89.433(8)
_cell_angle_gamma                88.567(10)
_cell_formula_units_Z            6
_cell_length_a                   13.241(2)
_cell_length_b                   18.728(2)
_cell_length_c                   23.258(3)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      10.11
_cell_volume                     5495.9(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_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    0.1335
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20560
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2546
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.810
_refine_ls_goodness_of_fit_obs   1.008
_refine_ls_hydrogen_treatment    'Rigid methyls, others riding'
_refine_ls_matrix_type           blocked,fullcycle
_refine_ls_number_parameters     1407
_refine_ls_number_reflns         19073
_refine_ls_number_restraints     1320
_refine_ls_restrained_S_all      0.810
_refine_ls_restrained_S_obs      0.971
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_obs          0.0464
_refine_ls_shift/esd_max         -0.019
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0940
_refine_ls_wR_factor_obs         0.0822
_reflns_number_observed          10263
_reflns_number_total             19075
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om970426v.cif
_cod_data_source_block           bigsel
_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 2.4.1 from 2010-06-29.

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^)+(0.0349P)^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^)+(0.0349P)^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        5495.8(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078382