#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/62/2236217.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_2236217
loop_
_publ_author_name
'Young, Cyril'
'Roodt, Andreas'
'Bezuidenhoudt, Barend C. B.'
_publ_section_title
;
 μ-(2,2'-Bipyrimidine)-bis[dichloridopalladium(II)] dimethylformamide
 monosolvate
;
_journal_coeditor_code           GG2102
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1374
_journal_paper_doi               10.1107/S1600536812040779
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd2 Cl4 (C8 H6 N4)], C3 H7 N O'
_chemical_formula_moiety         'C8 H6 Cl4 N4 Pd2, C3 H7 N O'
_chemical_formula_sum            'C11 H13 Cl4 N5 O Pd2'
_chemical_formula_weight         578.81
_chemical_name_systematic
;
μ-(2,2'-Bipyrimidine)-bis[dichloridopalladium(II)] dimethylformamide
monosolvate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7299(6)
_cell_length_b                   14.2399(7)
_cell_length_c                   5.9381(3)
_cell_measurement_reflns_used    1958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.86
_cell_volume                     861.76(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6102
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         3.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.786
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0172P)²+2.5414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.059
_reflns_number_gt                975
_reflns_number_total             1108
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg2102.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      ' C 2/m'
_cod_database_code               2236217
_cod_database_fobs_code          2236217
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
C C11 0.5 0.4487(3) 0.5 0.0149(8) Uani d S 1
C C12 0.5694(3) 0.3120(2) 0.6987(6) 0.0270(8) Uani d . 1
H H12 0.6167 0.2793 0.8341 0.032 Uiso calc R 1
C C13 0.5 0.2637(3) 0.5 0.0370(13) Uani d S 1
H H13 0.5 0.1984 0.5 0.044 Uiso calc SR 1
N N1 0.5696(2) 0.40577(17) 0.6995(4) 0.0152(5) Uani d . 1
Cl Cl11 0.72957(8) 0.61422(6) 1.23998(14) 0.0303(2) Uani d . 1
Pd Pd01 0.65034(3) 0.5 0.96630(6) 0.01736(12) Uani d S 1
N N22 0.5 0 0 0.0288(14) Uani d S 1
O O22 0.5 0.1536(5) 0 0.052(2) Uani d SP 0.5
C C21 0.4476(8) 0.0853(5) -0.1298(13) 0.0356(18) Uani d P 0.5
C C22 0.4325(11) 0 -0.2451(19) 0.053(4) Uani d SP 0.5
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 0 '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'
O O 0.0106 0.006 '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
N1 C11 N1 2_656 . 125.5(4)
N1 C11 C11 2_656 5_666 117.24(18)
N1 C11 C11 . 5_666 117.24(18)
N1 C12 C13 . . 120.4(3)
N1 C12 H12 . . 119.8
C13 C12 H12 . . 119.8
C12 C13 C12 . 2_656 119.6(4)
C12 C13 H13 . . 120.2
C12 C13 H13 2_656 . 120.2
C11 N1 C12 . . 117.1(3)
C11 N1 Pd01 . . 111.7(2)
C12 N1 Pd01 . . 131.1(2)
N1 Pd01 N1 . 6_565 81.77(13)
N1 Pd01 Cl11 . . 174.98(7)
N1 Pd01 Cl11 6_565 . 93.29(7)
N1 Pd01 Cl11 . 6_565 93.29(7)
N1 Pd01 Cl11 6_565 6_565 174.98(7)
Cl11 Pd01 Cl11 . 6_565 91.63(5)
C22 N22 C22 . 5_655 180.0000(10)
C22 N22 C21 . 2_655 122.4(3)
C22 N22 C21 5_655 2_655 57.6(3)
C22 N22 C21 . 6 57.6(3)
C22 N22 C21 5_655 6 122.4(3)
C21 N22 C21 2_655 6 180.0(3)
C22 N22 C21 . . 57.6(3)
C22 N22 C21 5_655 . 122.4(3)
C21 N22 C21 2_655 . 66.7(6)
C21 N22 C21 6 . 113.3(6)
C22 N22 C21 . 5_655 122.4(3)
C22 N22 C21 5_655 5_655 57.6(3)
C21 N22 C21 2_655 5_655 113.3(6)
C21 N22 C21 6 5_655 66.7(6)
C21 N22 C21 . 5_655 180.0(6)
C21 O22 C21 . 2_655 78.9(8)
O22 C21 C22 . . 160.9(9)
O22 C21 N22 . . 107.2(6)
C22 C21 N22 . . 59.5(5)
O22 C21 C21 . 2_655 50.6(4)
C22 C21 C21 . 2_655 114.6(6)
N22 C21 C21 . 2_655 56.7(3)
C21 C22 C21 . 6 123.5(10)
C21 C22 N22 . . 62.9(5)
C21 C22 N22 6 . 62.9(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C11 N1 2_656 1.335(3)
C11 N1 . 1.335(3)
C11 C11 5_666 1.462(8)
C12 N1 . 1.336(4)
C12 C13 . 1.368(4)
C12 H12 . 0.93
C13 C12 2_656 1.368(4)
C13 H13 . 0.93
N1 Pd01 . 2.050(2)
Cl11 Pd01 . 2.2682(8)
Pd01 N1 6_565 2.050(2)
Pd01 Cl11 6_565 2.2682(8)
N22 C22 . 1.408(11)
N22 C22 5_655 1.408(11)
N22 C21 2_655 1.454(8)
N22 C21 6 1.454(8)
N22 C21 . 1.454(8)
N22 C21 5_655 1.454(8)
O22 C21 . 1.258(9)
O22 C21 2_655 1.258(9)
C21 C22 . 1.379(9)
C21 C21 2_655 1.598(16)
C22 C21 6 1.379(9)
