#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:31:00 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179688 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/10/7001078.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7001078
loop_
_publ_author_name
'Kopylovich, Maximilian N.'
'Lasri, Jamal'
'Guedes da Silva, M. Fátima C.'
'Pombeiro, Armando J. L.'
_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
_chemical_name_systematic
;
?
;
_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/[σ²(Fo²)+(0.0290P)²+0.3130P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H2 H 0.108(4) 0.4209(16) -0.172(2) 0.025(6) Uiso 1 1 d . . .
H1 H 0.245(5) 0.4824(15) 0.209(2) 0.030(7) Uiso 1 1 d . . .
C10 C 0.4198(3) 0.42602(13) 0.13603(17) 0.0179(4) Uani 1 1 d . . .
C11 C 0.5863(3) 0.41588(13) 0.25240(17) 0.0192(4) Uani 1 1 d . . .
C12 C 0.8034(3) 0.39290(14) 0.25472(19) 0.0234(4) Uani 1 1 d . . .
H12 H 0.8496 0.3814 0.1823 0.028 Uiso 1 1 calc R . .
C13 C 0.9511(4) 0.38710(15) 0.36419(19) 0.0271(5) Uani 1 1 d . . .
H13 H 1.1016 0.3729 0.3682 0.032 Uiso 1 1 calc R . .
C14 C 0.8768(4) 0.40228(15) 0.46815(19) 0.0288(5) Uani 1 1 d . . .
H14 H 0.9737 0.3974 0.5449 0.035 Uiso 1 1 calc R . .
C15 C 0.6576(4) 0.42473(16) 0.45718(19) 0.0305(5) Uani 1 1 d . . .
H15 H 0.6067 0.4349 0.5286 0.037 Uiso 1 1 calc R . .
C20 C 0.3463(3) 0.39359(13) -0.06893(17) 0.0190(4) Uani 1 1 d . . .
C21 C 0.4366(3) 0.34932(13) -0.16510(18) 0.0202(4) Uani 1 1 d . . .
C22 C 0.6565(3) 0.32391(13) -0.14452(19) 0.0231(4) Uani 1 1 d . . .
H22 H 0.7534 0.3330 -0.0687 0.028 Uiso 1 1 calc R . .
C23 C 0.7321(4) 0.28494(15) -0.2368(2) 0.0279(5) Uani 1 1 d . . .
H23 H 0.8824 0.2680 -0.2260 0.033 Uiso 1 1 calc R . .
C24 C 0.5838(4) 0.27128(15) -0.3449(2) 0.0310(5) Uani 1 1 d . . .
H24 H 0.6292 0.2437 -0.4093 0.037 Uiso 1 1 calc R . .
C25 C 0.3684(4) 0.29872(16) -0.3569(2) 0.0325(5) Uani 1 1 d . . .
H25 H 0.2674 0.2891 -0.4312 0.039 Uiso 1 1 calc R . .
N1 N 0.2399(3) 0.46810(12) 0.13807(16) 0.0202(3) Uani 1 1 d . . .
N2 N 0.1539(3) 0.43036(12) -0.10105(15) 0.0208(4) Uani 1 1 d . . .
N3 N 0.4793(3) 0.39000(11) 0.04107(15) 0.0197(4) Uani 1 1 d . . .
N10 N 0.5134(3) 0.43293(13) 0.35252(15) 0.0260(4) Uani 1 1 d . . .
N20 N 0.2933(3) 0.33796(12) -0.27026(16) 0.0266(4) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.5000 0.0000 0.01700(7) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C10 N3 128.17(19) . . ?
N1 C10 C11 117.56(17) . . ?
N3 C10 C11 114.27(17) . . ?
N10 C11 C12 122.74(19) . . ?
N10 C11 C10 115.94(17) . . ?
C12 C11 C10 121.29(17) . . ?
C13 C12 C11 118.77(19) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 119.07(19) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.1(2) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
N10 C15 C14 123.9(2) . . ?
N10 C15 H15 118.0 . . ?
C14 C15 H15 118.0 . . ?
N2 C20 N3 128.04(19) . . ?
N2 C20 C21 117.72(18) . . ?
N3 C20 C21 114.24(17) . . ?
N20 C21 C22 122.96(19) . . ?
N20 C21 C20 115.86(18) . . ?
C22 C21 C20 121.17(19) . . ?
C23 C22 C21 118.8(2) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C24 C23 C22 118.6(2) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C25 C24 C23 118.4(2) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
N20 C25 C24 124.0(2) . . ?
N20 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
C10 N1 Pd1 127.72(14) . . ?
C10 N1 H1 107.7(19) . . ?
Pd1 N1 H1 124.5(18) . . ?
C20 N2 Pd1 127.66(15) . . ?
C20 N2 H2 107.3(17) . . ?
Pd1 N2 H2 125.1(17) . . ?
C20 N3 C10 120.96(17) . . ?
C15 N10 C11 117.31(18) . . ?
C25 N20 C21 117.18(19) . . ?
N1 Pd1 N1 180.00(11) . 3_565 ?
N1 Pd1 N2 87.01(7) . . ?
N1 Pd1 N2 92.99(7) 3_565 . ?
N1 Pd1 N2 92.99(7) . 3_565 ?
N1 Pd1 N2 87.01(7) 3_565 3_565 ?
N2 Pd1 N2 180.0 . 3_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C10 N1 1.304(3) . ?
C10 N3 1.347(2) . ?
C10 C11 1.500(3) . ?
C11 N10 1.345(2) . ?
C11 C12 1.387(3) . ?
C12 C13 1.380(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C15 N10 1.332(3) . ?
C15 H15 0.9500 . ?
C20 N2 1.305(3) . ?
C20 N3 1.343(3) . ?
C20 C21 1.511(3) . ?
C21 N20 1.339(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.389(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 N20 1.336(3) . ?
C25 H25 0.9500 . ?
N1 Pd1 1.9799(18) . ?
N1 H1 0.84(3) . ?
N2 Pd1 1.9864(17) . ?
N2 H2 0.81(2) . ?
Pd1 N1 1.9799(18) 3_565 ?
Pd1 N2 1.9864(17) 3_565 ?
