#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:31:00 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179688 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/10/7001080.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_7001080
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 H14 Cl4 N10 Pd'
_chemical_formula_sum            'C24 H14 Cl4 N10 Pd'
_chemical_formula_weight         690.65
_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                 108.20(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.286(2)
_cell_length_b                   8.924(2)
_cell_length_c                   13.858(3)
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.76
_cell_volume                     1325.9(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD are detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31010
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.9552
_exptl_absorpt_correction_T_min  0.8944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0357P)²+0.5656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                2568
_reflns_number_total             3273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820680e.txt
_cod_data_source_block           max935mon=compound5d
_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               7001080
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
C10 C 0.3964(2) 0.2988(3) 0.42664(19) 0.0189(5) Uani 1 1 d . . .
C11 C 0.3846(2) 0.4302(3) 0.3567(2) 0.0202(5) Uani 1 1 d . . .
C12 C 0.3582(2) 0.5730(3) 0.3858(2) 0.0225(5) Uani 1 1 d . . .
H12 H 0.3433 0.5876 0.4490 0.027 Uiso 1 1 calc R . .
C13 C 0.3539(3) 0.6925(3) 0.3220(2) 0.0280(6) Uani 1 1 d . . .
H13 H 0.3364 0.7889 0.3433 0.034 Uiso 1 1 calc R . .
C14 C 0.3960(3) 0.5442(3) 0.2054(2) 0.0259(6) Uani 1 1 d . . .
C15 C 0.4026(2) 0.4159(3) 0.2627(2) 0.0231(6) Uani 1 1 d . . .
H15 H 0.4190 0.3210 0.2385 0.028 Uiso 1 1 calc R . .
C20 C 0.3445(2) 0.2147(3) 0.56833(19) 0.0194(5) Uani 1 1 d . . .
C21 C 0.2738(2) 0.2575(3) 0.6397(2) 0.0201(5) Uani 1 1 d . . .
C22 C 0.3222(3) 0.2325(3) 0.7439(2) 0.0244(6) Uani 1 1 d . A .
H22 H 0.4018 0.1875 0.7720 0.029 Uiso 1 1 calc R . .
C23 C 0.2521(3) 0.2743(3) 0.8059(2) 0.0290(6) Uani 1 1 d . . .
C24 C 0.0951(2) 0.3579(3) 0.6706(2) 0.0239(6) Uani 1 1 d . . .
C25 C 0.1570(3) 0.3233(3) 0.6022(2) 0.0227(6) Uani 1 1 d . A .
H25 H 0.1209 0.3437 0.5318 0.027 Uiso 1 1 calc R . .
N1 N 0.4629(2) 0.1842(2) 0.41632(17) 0.0210(5) Uani 1 1 d . . .
N2 N 0.5984(2) -0.0861(2) 0.41806(18) 0.0217(5) Uani 1 1 d . . .
N3 N 0.3376(2) 0.3184(2) 0.49693(16) 0.0202(5) Uani 1 1 d . . .
N10 N 0.3731(2) 0.6807(3) 0.23125(19) 0.0301(6) Uani 1 1 d . . .
N20 N 0.1383(2) 0.3363(3) 0.76983(18) 0.0270(5) Uani 1 1 d . A .
Cl10 Cl 0.42168(9) 0.52674(9) 0.08784(6) 0.0421(2) Uani 1 1 d . . .
Cl20 Cl -0.05206(7) 0.43756(9) 0.62803(6) 0.0316(2) Uani 0.905(2) 1 d P A 1
Pd1 Pd 0.5000 0.0000 0.5000 0.01741(9) Uani 1 2 d S . .
Cl2B Cl 0.2881(9) 0.2417(11) 0.9166(7) 0.045(3) Uiso 0.095(2) 1 d P A 2
H1 H 0.493(3) 0.194(3) 0.370(2) 0.028(8) Uiso 1 1 d . . .
H2 H 0.610(3) -0.041(3) 0.374(2) 0.022(8) Uiso 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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 127.6(2) . . ?
N1 C10 C11 118.7(2) . . ?
N3 C10 C11 113.6(2) . . ?
C15 C11 C12 117.5(2) . . ?
C15 C11 C10 121.7(2) . . ?
C12 C11 C10 120.7(2) . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
N10 C13 C12 123.8(3) . . ?
N10 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
N10 C14 C15 126.1(3) . . ?
N10 C14 Cl10 116.1(2) . . ?
C15 C14 Cl10 117.8(2) . . ?
C14 C15 C11 117.8(2) . . ?
C14 C15 H15 121.1 . . ?
C11 C15 H15 121.1 . . ?
N2 C20 N3 128.9(2) 3_656 . ?
N2 C20 C21 118.1(2) 3_656 . ?
N3 C20 C21 113.0(2) . . ?
C25 C21 C22 118.3(2) . . ?
C25 C21 C20 120.0(2) . . ?
C22 C21 C20 121.7(2) . . ?
C23 C22 C21 118.9(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
N20 C23 C22 123.0(3) . . ?
N20 C23 Cl2B 112.7(4) . . ?
C22 C23 Cl2B 124.1(4) . . ?
N20 C24 C25 125.6(3) . . ?
N20 C24 Cl20 114.7(2) . . ?
C25 C24 Cl20 119.8(2) . . ?
C24 C25 C21 117.7(3) . . ?
C24 C25 H25 121.1 . . ?
C21 C25 H25 121.1 . . ?
C10 N1 Pd1 127.69(18) . . ?
C10 N1 H1 113(2) . . ?
Pd1 N1 H1 119(2) . . ?
C20 N2 Pd1 127.02(18) 3_656 . ?
C20 N2 H2 112(2) 3_656 . ?
Pd1 N2 H2 121(2) . . ?
C20 N3 C10 121.0(2) . . ?
C14 N10 C13 115.4(2) . . ?
C24 N20 C23 116.5(2) . . ?
N2 Pd1 N2 180.0 . 3_656 ?
N2 Pd1 N1 92.32(9) . . ?
N2 Pd1 N1 87.68(9) 3_656 . ?
N2 Pd1 N1 87.68(9) . 3_656 ?
N2 Pd1 N1 92.32(9) 3_656 3_656 ?
N1 Pd1 N1 180.0 . 3_656 ?
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 1.303(3) . ?
C10 N3 1.350(3) . ?
C10 C11 1.500(3) . ?
C11 C15 1.386(4) . ?
C11 C12 1.397(4) . ?
C12 C13 1.376(4) . ?
C12 H12 0.9500 . ?
C13 N10 1.346(4) . ?
C13 H13 0.9500 . ?
C14 N10 1.318(4) . ?
C14 C15 1.382(4) . ?
C14 Cl10 1.748(3) . ?
C15 H15 0.9500 . ?
C20 N2 1.301(3) 3_656 ?
C20 N3 1.339(3) . ?
C20 C21 1.500(3) . ?
C21 C25 1.387(4) . ?
C21 C22 1.393(4) . ?
C22 C23 1.388(4) . ?
C22 H22 0.9500 . ?
C23 N20 1.343(4) . ?
C23 Cl2B 1.488(10) . ?
C24 N20 1.322(4) . ?
C24 C25 1.376(4) . ?
C24 Cl20 1.732(3) . ?
C25 H25 0.9500 . ?
N1 Pd1 1.980(2) . ?
N1 H1 0.81(3) . ?
N2 C20 1.301(3) 3_656 ?
N2 Pd1 1.975(2) . ?
N2 H2 0.77(3) . ?
Pd1 N2 1.975(2) 3_656 ?
Pd1 N1 1.980(2) 3_656 ?
