#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:39 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318555.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_4318555
loop_
_publ_author_name
'Zengquan Qin'
'Michael C. Jennings'
'Richard J. Puddephatt'
'Kenneth W. Muir'
_publ_section_title
;
 Self-Assembly of Polymer and Sheet Structures in Palladium(II) Complexes
 Containing Carboxylic Acid Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5174
_journal_page_last               5186
_journal_paper_doi               10.1021/ic020239b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H8 N2 O4 Pd'
_chemical_formula_weight         350.60
_chemical_name_systematic
;
  ?
;
_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                 91.008(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.7077(2)
_cell_length_b                   12.8197(5)
_cell_length_c                   11.5267(6)
_cell_measurement_temperature    200(2)
_cell_volume                     547.80(5)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7363
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.7266
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                893
_reflns_number_total             1254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020239b_04.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318555
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_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
Pd Pd 0.5000 0.5000 0.0000 0.02349(13) Uani 1 2 d S . .
N1 N 0.2995(6) 0.4612(2) -0.1561(2) 0.0237(6) Uani 1 1 d . . .
C2 C 0.1578(8) 0.5260(2) -0.2358(3) 0.0277(7) Uani 1 1 d . . .
H2A H 0.1546 0.5989 -0.2207 0.033 Uiso 1 1 calc R . .
C3 C 0.0161(9) 0.4891(2) -0.3396(3) 0.0297(7) Uani 1 1 d . . .
H3A H -0.0906 0.5356 -0.3945 0.036 Uiso 1 1 calc R . .
C4 C 0.0322(8) 0.3831(2) -0.3623(3) 0.0303(7) Uani 1 1 d . . .
H4A H -0.0642 0.3558 -0.4328 0.036 Uiso 1 1 calc R . .
C5 C 0.1904(8) 0.3177(2) -0.2808(3) 0.0280(7) Uani 1 1 d . . .
H5A H 0.2109 0.2452 -0.2961 0.034 Uiso 1 1 calc R . .
C6 C 0.3174(7) 0.3581(2) -0.1781(2) 0.0240(6) Uani 1 1 d . . .
C7 C 0.4873(8) 0.2934(2) -0.0819(3) 0.0270(7) Uani 1 1 d . . .
O8 O 0.5214(6) 0.19985(16) -0.09298(19) 0.0371(6) Uani 1 1 d . . .
O9 O 0.5929(6) 0.34630(18) 0.00981(16) 0.0307(5) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.02850(19) 0.02093(19) 0.02094(19) -0.00021(14) -0.00200(13) -0.00008(14)
N1 0.0249(13) 0.0225(12) 0.0236(14) 0.0006(11) 0.0000(11) -0.0013(10)
C2 0.0291(16) 0.0272(17) 0.0267(18) 0.0015(13) -0.0009(14) 0.0009(12)
C3 0.0287(16) 0.0356(19) 0.0248(16) 0.0068(14) -0.0003(13) -0.0010(14)
C4 0.0272(16) 0.0397(19) 0.0241(17) -0.0004(15) -0.0006(13) -0.0065(14)
C5 0.0306(16) 0.0259(17) 0.0277(17) -0.0018(13) 0.0025(14) -0.0053(13)
C6 0.0248(15) 0.0232(15) 0.0239(16) -0.0016(13) 0.0016(12) -0.0017(12)
C7 0.0263(16) 0.0287(17) 0.0259(17) -0.0002(14) 0.0011(13) 0.0002(13)
O8 0.0492(14) 0.0229(12) 0.0388(13) -0.0015(10) -0.0084(11) 0.0032(10)
O9 0.0406(13) 0.0252(12) 0.0262(13) 0.0013(9) -0.0045(10) 0.0008(9)
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'
O O 0.0106 0.0060 '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 Pd N1 180.00(15) . 3_665 ?
N1 Pd O9 82.36(9) . . ?
N1 Pd O9 97.64(9) 3_665 . ?
N1 Pd O9 97.64(9) . 3_665 ?
N1 Pd O9 82.36(9) 3_665 3_665 ?
O9 Pd O9 180.0 . 3_665 ?
C2 N1 C6 120.0(3) . . ?
C2 N1 Pd 126.8(2) . . ?
C6 N1 Pd 113.22(19) . . ?
N1 C2 C3 121.3(3) . . ?
C2 C3 C4 118.9(3) . . ?
C5 C4 C3 119.1(3) . . ?
C6 C5 C4 119.6(3) . . ?
N1 C6 C5 121.1(3) . . ?
N1 C6 C7 114.9(3) . . ?
C5 C6 C7 124.0(3) . . ?
O8 C7 O9 124.5(3) . . ?
O8 C7 C6 120.5(3) . . ?
O9 C7 C6 115.0(3) . . ?
C7 O9 Pd 114.53(19) . . ?
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
Pd N1 1.998(2) . ?
Pd N1 1.998(3) 3_665 ?
Pd O9 2.003(2) . ?
Pd O9 2.003(2) 3_665 ?
N1 C2 1.339(4) . ?
N1 C6 1.349(4) . ?
C2 C3 1.382(5) . ?
C3 C4 1.385(4) . ?
C4 C5 1.382(4) . ?
C5 C6 1.368(4) . ?
C6 C7 1.513(4) . ?
C7 O8 1.213(3) . ?
C7 O9 1.310(4) . ?
