#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/70/2237044.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_2237044
loop_
_publ_author_name
'Imhof, Wolfgang'
_publ_section_title
;
 Bis{2-[(phenylimino)methyl]-1H-pyrrol-1-ido}palladium(II)
;
_journal_coeditor_code           SU2533
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1567
_journal_paper_doi               10.1107/S1600536812048143
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd (C11 H9 N2)2]'
_chemical_formula_moiety         'C22 H18 N4 Pd'
_chemical_formula_sum            'C22 H18 N4 Pd'
_chemical_formula_weight         444.80
_chemical_name_systematic
;
Bis{2-[(phenylimino)methyl]-1H-pyrrol-1-ido}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                 93.044(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5634(4)
_cell_length_b                   10.6480(6)
_cell_length_c                   8.0560(7)
_cell_measurement_reflns_used    3903
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.72
_cell_volume                     904.85(10)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi-scan, 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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3903
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.753
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0317
_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)+(0.0376P)²+] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                1464
_reflns_number_total             2018
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2533.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237044
_cod_database_fobs_code          2237044
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_symmetry_multiplicity
Pd Pd1 0.5000 0.5000 0.0000 0.02321(12) Uani d S 1 2
N N1 0.6789(2) 0.5646(2) 0.0414(3) 0.0262(6) Uani d . 1 1
C C1 0.7967(3) 0.5447(3) -0.0074(4) 0.0312(7) Uani d . 1 1
H H1 0.8188 0.4863 -0.0902 0.037 Uiso calc R 1 1
C C2 0.8824(3) 0.6229(3) 0.0821(4) 0.0315(7) Uani d . 1 1
H H2 0.9714 0.6268 0.0707 0.038 Uiso calc R 1 1
C C3 0.8136(3) 0.6933(3) 0.1901(4) 0.0321(7) Uani d . 1 1
H H3 0.8457 0.7552 0.2662 0.038 Uiso calc R 1 1
C C4 0.6880(3) 0.6555(3) 0.1652(3) 0.0285(7) Uani d . 1 1
C C5 0.5768(3) 0.6762(3) 0.2483(3) 0.0299(7) Uani d . 1 1
H H5 0.5744 0.7365 0.3349 0.036 Uiso calc R 1 1
N N2 0.4762(2) 0.6101(2) 0.2034(3) 0.0270(6) Uani d . 1 1
C C6 0.3624(3) 0.6222(3) 0.2888(3) 0.0280(7) Uani d . 1 1
C C7 0.3223(3) 0.5215(3) 0.3841(4) 0.0339(8) Uani d . 1 1
H H7 0.3735 0.4486 0.3975 0.041 Uiso calc R 1 1
C C8 0.2079(4) 0.5286(3) 0.4586(4) 0.0385(8) Uani d . 1 1
H H8 0.1811 0.4606 0.5245 0.046 Uiso calc R 1 1
C C9 0.1314(3) 0.6348(3) 0.4379(4) 0.0395(8) Uani d . 1 1
H H9 0.0511 0.6382 0.4858 0.047 Uiso calc R 1 1
C C10 0.1739(3) 0.7353(3) 0.3466(4) 0.0363(8) Uani d . 1 1
H H10 0.1232 0.8088 0.3350 0.044 Uiso calc R 1 1
C C11 0.2885(3) 0.7303(3) 0.2724(3) 0.0300(7) Uani d . 1 1
H H11 0.3168 0.8000 0.2107 0.036 Uiso calc R 1 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'
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
N1 Pd1 N1 . 3_665 180.0
N1 Pd1 N2 . . 80.00(9)
N1 Pd1 N2 3_665 . 100.00(9)
N1 Pd1 N2 . 3_665 100.00(9)
N1 Pd1 N2 3_665 3_665 80.00(9)
N2 Pd1 N2 . 3_665 180.0
C1 N1 C4 . . 106.9(3)
C1 N1 Pd1 . . 140.5(2)
C4 N1 Pd1 . . 112.6(2)
N1 C1 C2 . . 109.8(3)
N1 C1 H1 . . 125.1
C2 C1 H1 . . 125.1
C3 C2 C1 . . 107.4(3)
C3 C2 H2 . . 126.3
C1 C2 H2 . . 126.3
C2 C3 C4 . . 106.3(3)
C2 C3 H3 . . 126.8
C4 C3 H3 . . 126.8
N1 C4 C3 . . 109.5(3)
N1 C4 C5 . . 115.2(3)
C3 C4 C5 . . 134.7(3)
N2 C5 C4 . . 118.2(3)
N2 C5 H5 . . 120.9
C4 C5 H5 . . 120.9
C5 N2 C6 . . 120.8(2)
C5 N2 Pd1 . . 113.4(2)
C6 N2 Pd1 . . 125.75(18)
C11 C6 C7 . . 120.1(3)
C11 C6 N2 . . 120.9(3)
C7 C6 N2 . . 119.0(3)
C8 C7 C6 . . 119.7(3)
C8 C7 H7 . . 120.1
C6 C7 H7 . . 120.1
C9 C8 C7 . . 120.5(3)
C9 C8 H8 . . 119.7
C7 C8 H8 . . 119.7
C10 C9 C8 . . 119.1(3)
C10 C9 H9 . . 120.4
C8 C9 H9 . . 120.4
C9 C10 C11 . . 121.1(3)
C9 C10 H10 . . 119.4
C11 C10 H10 . . 119.4
C6 C11 C10 . . 119.4(3)
C6 C11 H11 . . 120.3
C10 C11 H11 . . 120.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 N1 . 2.022(2)
Pd1 N1 3_665 2.022(2)
Pd1 N2 . 2.041(2)
Pd1 N2 3_665 2.041(2)
N1 C1 . 1.342(4)
N1 C4 . 1.389(3)
C1 C2 . 1.401(4)
C1 H1 . 0.9500
C2 C3 . 1.384(4)
C2 H2 . 0.9500
C3 C4 . 1.391(4)
C3 H3 . 0.9500
C4 C5 . 1.400(4)
C5 N2 . 1.310(4)
C5 H5 . 0.9500
N2 C6 . 1.422(4)
C6 C11 . 1.393(4)
C6 C7 . 1.398(4)
C7 C8 . 1.379(5)
C7 H7 . 0.9500
C8 C9 . 1.395(5)
C8 H8 . 0.9500
C9 C10 . 1.387(5)
C9 H9 . 0.9500
C10 C11 . 1.379(4)
C10 H10 . 0.9500
C11 H11 . 0.9500
