Single-pot template transformations of cyanopyridines on a PdII centre: syntheses of ketoimine and 2,4-dipyridyl-1,3,5-triazapentadiene palladium(II) complexes and their catalytic activity for microwave-assisted Suzuki–Miyaura and Heck reactions
Kopylovich, Maximilian N.; Lasri, Jamal; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; Dalton Transactions  (2009) 3074–3084; doi:10.1039/b820680e

data_7001078
_publ_section_title
;
 Single-pot template transformations of cyanopyridines on a PdII
 centre: syntheses of ketoimine and
 2,4-dipyridyl-1,3,5-triazapentadiene palladium(II) complexes and their
 catalytic activity for microwave-assisted Suzuki--Miyaura and Heck
 reactions
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3074
_journal_page_last               3084
_journal_paper_doi               10.1039/b820680e
_journal_year                    2009
_chemical_formula_moiety         'C24 H20 N10 Pd'
_chemical_formula_sum            'C24 H20 N10 Pd'
_chemical_formula_weight         554.90
_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                 102.660(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1888(7)
_cell_length_b                   15.910(2)
_cell_length_c                   11.4138(13)
_cell_measurement_reflns_used    4278
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.56
_cell_volume                     1096.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'WinGX v.1.70.01 (Farrugia, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10220
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.9068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0290P)^2^+0.3130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                2159
_reflns_number_total             2709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820680e.txt
_cod_data_source_block           max930acet=compound5a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001078