#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/89/2228936.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2228936
loop_
_publ_author_name
'Mao, Pu'
'Liu, Xiujun'
'Yang, Liangru'
'Yuan, Jinwei'
'Song, Maoping'
_publ_section_title
;
 Dibromidobis[1-(2,4,6-trimethylphenyl)-1,4,5,6-tetrahydropyrimidine-κN³]palladium(II)
;
_journal_coeditor_code           SU2226
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m62
_journal_paper_doi               10.1107/S1600536810050968
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pd Br2 (C13 H18 N2)2]'
_chemical_formula_moiety         'C26 H36 Br2 N4 Pd'
_chemical_formula_sum            'C26 H36 Br2 N4 Pd'
_chemical_formula_weight         670.81
_chemical_name_systematic
;
Dibromidobis[1-(2,4,6-trimethylphenyl)-1,4,5,6-tetrahydropyrimidine-
κN³]palladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1348(14)
_cell_length_b                   21.308(4)
_cell_length_c                   8.9704(18)
_cell_measurement_reflns_used    3263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8644
_cell_measurement_theta_min      2.4701
_cell_volume                     1359.4(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6809
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    3.643
_exptl_absorpt_correction_T_max  0.5295
_exptl_absorpt_correction_T_min  0.5295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0553P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                1931
_reflns_number_total             2393
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su2226.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228936
_cod_database_fobs_code          2228936
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.5000 0.5000 0.0000 0.0445(2) Uani d S 1 . .
Br Br1 0.27385(9) 0.45987(3) -0.19525(7) 0.0700(2) Uani d . 1 . .
N N1 0.3804(6) 0.44800(17) 0.1532(5) 0.0502(11) Uani d . 1 . .
N N2 0.4027(6) 0.36304(16) 0.3218(5) 0.0513(11) Uani d . 1 . .
C C1 0.2139(8) 0.4701(2) 0.2167(6) 0.0595(16) Uani d . 1 . .
H H1A 0.1044 0.4545 0.1570 0.071 Uiso calc R 1 . .
H H1B 0.2111 0.5156 0.2118 0.071 Uiso calc R 1 . .
C C2 0.2026(10) 0.4506(2) 0.3718(7) 0.0722(19) Uani d . 1 . .
H H2A 0.0783 0.4607 0.4015 0.087 Uiso calc R 1 . .
H H2B 0.2929 0.4747 0.4348 0.087 Uiso calc R 1 . .
C C3 0.2385(8) 0.3831(2) 0.3997(7) 0.0659(17) Uani d . 1 . .
H H3A 0.2622 0.3757 0.5062 0.079 Uiso calc R 1 . .
H H3B 0.1290 0.3589 0.3638 0.079 Uiso calc R 1 . .
C C4 0.4604(8) 0.3983(2) 0.2102(6) 0.0534(14) Uani d . 1 . .
H H4 0.5700 0.3855 0.1695 0.064 Uiso calc R 1 . .
C C5 0.5155(7) 0.3102(2) 0.3749(6) 0.0461(12) Uani d . 1 . .
C C6 0.4605(8) 0.2496(2) 0.3291(6) 0.0541(14) Uani d . 1 . .
C C7 0.5759(8) 0.1998(2) 0.3757(6) 0.0586(15) Uani d . 1 . .
H H7 0.5389 0.1592 0.3491 0.070 Uiso calc R 1 . .
C C8 0.7456(8) 0.2088(3) 0.4614(7) 0.0631(16) Uani d . 1 . .
C C9 0.7929(8) 0.2699(2) 0.5081(7) 0.0628(15) Uani d . 1 . .
H H9 0.9027 0.2766 0.5691 0.075 Uiso calc R 1 . .
C C10 0.6784(8) 0.3208(2) 0.4650(7) 0.0561(14) Uani d . 1 . .
C C11 0.2792(9) 0.2376(3) 0.2354(7) 0.0757(18) Uani d . 1 . .
H H11A 0.1756 0.2527 0.2871 0.114 Uiso calc R 1 . .
H H11B 0.2649 0.1933 0.2180 0.114 Uiso calc R 1 . .
H H11C 0.2817 0.2590 0.1415 0.114 Uiso calc R 1 . .
C C12 0.8751(9) 0.1538(3) 0.5026(9) 0.087(2) Uani d . 1 . .
H H12A 0.9802 0.1548 0.4423 0.130 Uiso calc R 1 . .
H H12B 0.8074 0.1152 0.4855 0.130 Uiso calc R 1 . .
H H12C 0.9194 0.1567 0.6063 0.130 Uiso calc R 1 . .
C C13 0.7335(9) 0.3853(3) 0.5220(8) 0.081(2) Uani d . 1 . .
H H13A 0.7528 0.4123 0.4390 0.122 Uiso calc R 1 . .
H H13B 0.8477 0.3826 0.5861 0.122 Uiso calc R 1 . .
H H13C 0.6352 0.4021 0.5773 0.122 Uiso calc R 1 . .
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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pd1 N1 3_665 . 180.0000(10) ?
N1 Pd1 Br1 3_665 3_665 90.30(14) ?
N1 Pd1 Br1 . 3_665 89.70(14) ?
N1 Pd1 Br1 3_665 . 89.70(13) ?
N1 Pd1 Br1 . . 90.30(14) ?
Br1 Pd1 Br1 3_665 . 180.0 ?
C4 N1 C1 . . 117.8(4) ?
C4 N1 Pd1 . . 121.7(3) ?
C1 N1 Pd1 . . 120.0(3) ?
C4 N2 C5 . . 119.1(4) ?
C4 N2 C3 . . 119.6(4) ?
C5 N2 C3 . . 120.9(4) ?
N1 C1 C2 . . 113.2(4) ?
N1 C1 H1A . . 108.9 ?
C2 C1 H1A . . 108.9 ?
N1 C1 H1B . . 108.9 ?
C2 C1 H1B . . 108.9 ?
H1A C1 H1B . . 107.7 ?
C1 C2 C3 . . 114.5(5) ?
C1 C2 H2A . . 108.6 ?
C3 C2 H2A . . 108.6 ?
C1 C2 H2B . . 108.6 ?
C3 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
N2 C3 C2 . . 109.6(4) ?
N2 C3 H3A . . 109.7 ?
C2 C3 H3A . . 109.7 ?
N2 C3 H3B . . 109.7 ?
C2 C3 H3B . . 109.7 ?
H3A C3 H3B . . 108.2 ?
N1 C4 N2 . . 127.1(5) ?
N1 C4 H4 . . 116.5 ?
N2 C4 H4 . . 116.5 ?
C10 C5 C6 . . 121.6(4) ?
C10 C5 N2 . . 119.2(4) ?
C6 C5 N2 . . 119.1(5) ?
C7 C6 C5 . . 118.1(5) ?
C7 C6 C11 . . 120.0(5) ?
C5 C6 C11 . . 121.8(5) ?
C6 C7 C8 . . 122.0(5) ?
C6 C7 H7 . . 119.0 ?
C8 C7 H7 . . 119.0 ?
C7 C8 C9 . . 118.0(5) ?
C7 C8 C12 . . 120.9(5) ?
C9 C8 C12 . . 121.1(6) ?
C10 C9 C8 . . 121.2(6) ?
C10 C9 H9 . . 119.4 ?
C8 C9 H9 . . 119.4 ?
C5 C10 C9 . . 118.9(4) ?
C5 C10 C13 . . 122.1(5) ?
C9 C10 C13 . . 118.9(5) ?
C6 C11 H11A . . 109.5 ?
C6 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C6 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C8 C12 H12A . . 109.5 ?
C8 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C8 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 3_665 2.008(4) ?
Pd1 N1 . 2.008(4) ?
Pd1 Br1 3_665 2.4391(9) ?
Pd1 Br1 . 2.4391(9) ?
N1 C4 . 1.289(6) ?
N1 C1 . 1.437(6) ?
N2 C4 . 1.343(6) ?
N2 C5 . 1.442(6) ?
N2 C3 . 1.474(6) ?
C1 C2 . 1.461(8) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C3 . 1.478(7) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4 . 0.9300 ?
C5 C10 . 1.380(7) ?
C5 C6 . 1.402(7) ?
C6 C7 . 1.386(7) ?
C6 C11 . 1.507(8) ?
C7 C8 . 1.394(8) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.401(8) ?
C8 C12 . 1.519(7) ?
C9 C10 . 1.394(7) ?
C9 H9 . 0.9300 ?
C10 C13 . 1.508(7) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Br1 Pd1 N1 C4 3_665 . . . -73.6(4) ?
Br1 Pd1 N1 C4 . . . . 106.4(4) ?
Br1 Pd1 N1 C1 3_665 . . . 98.2(4) ?
Br1 Pd1 N1 C1 . . . . -81.8(4) ?
C4 N1 C1 C2 . . . . 24.7(8) ?
Pd1 N1 C1 C2 . . . . -147.4(4) ?
N1 C1 C2 C3 . . . . -48.5(8) ?
C4 N2 C3 C2 . . . . -18.5(8) ?
C5 N2 C3 C2 . . . . 154.1(5) ?
C1 C2 C3 N2 . . . . 44.1(8) ?
C1 N1 C4 N2 . . . . 1.8(9) ?
Pd1 N1 C4 N2 . . . . 173.8(4) ?
C5 N2 C4 N1 . . . . -177.5(5) ?
C3 N2 C4 N1 . . . . -4.7(9) ?
C4 N2 C5 C10 . . . . 75.9(7) ?
C3 N2 C5 C10 . . . . -96.7(6) ?
C4 N2 C5 C6 . . . . -101.8(6) ?
C3 N2 C5 C6 . . . . 85.6(7) ?
C10 C5 C6 C7 . . . . -0.7(8) ?
N2 C5 C6 C7 . . . . 177.0(4) ?
C10 C5 C6 C11 . . . . 177.7(5) ?
N2 C5 C6 C11 . . . . -4.7(8) ?
C5 C6 C7 C8 . . . . -2.2(8) ?
C11 C6 C7 C8 . . . . 179.4(5) ?
C6 C7 C8 C9 . . . . 3.9(8) ?
C6 C7 C8 C12 . . . . -176.1(5) ?
C7 C8 C9 C10 . . . . -2.9(9) ?
C12 C8 C9 C10 . . . . 177.2(5) ?
C6 C5 C10 C9 . . . . 1.7(8) ?
N2 C5 C10 C9 . . . . -176.0(5) ?
C6 C5 C10 C13 . . . . -176.5(5) ?
N2 C5 C10 C13 . . . . 5.8(8) ?
C8 C9 C10 C5 . . . . 0.1(8) ?
C8 C9 C10 C13 . . . . 178.4(6) ?
