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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
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data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
bis(2,4-pentanedionato)palladium(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C10 H14 O4 Pd'
_chemical_formula_sum     'C10 H14 O4 Pd'
_chemical_formula_iupac     '[Pd (C5 H7 O2)2]'
_chemical_formula_weight     304.61
_chemical_melting_point     ?
_symmetry_cell_setting     Monoclinic
_symmetry_space_group_name_H-M     'P 21/n'
_symmetry_space_group_name_Hall     '-P 2yn'
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'
_cell_length_a     9.9119(10)
_cell_length_b     5.2232(5)
_cell_length_c     10.3877(10)
_cell_angle_alpha     90.00
_cell_angle_beta     95.807(2)
_cell_angle_gamma     90.00
_cell_volume     535.03(9)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     4907
_cell_measurement_theta_min     3.00
_cell_measurement_theta_max     30.16
_cell_measurement_temperature     100(2)
_exptl_crystal_description     block
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.60
_exptl_crystal_size_mid     0.55
_exptl_crystal_size_min     0.25
_exptl_crystal_density_diffrn     1.891
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     304
_exptl_absorpt_coefficient_mu     1.725
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(SADABS in SAINT-Plus; Bruker, 2003)'
_exptl_absorpt_correction_T_min     0.4534
_exptl_absorpt_correction_T_max     0.65
_exptl_special_details
;
;
_diffrn_ambient_temperature     100(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART APEX CCD'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     5832
_diffrn_reflns_av_R_equivalents     0.0331
_diffrn_reflns_av_sigmaI/netI     0.0239
_diffrn_reflns_theta_min     3.94
_diffrn_reflns_theta_max     30.16
_diffrn_reflns_theta_full     30.16
_diffrn_measured_fraction_theta_max     0.996
_diffrn_measured_fraction_theta_full     0.996
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     13
_diffrn_reflns_limit_k_min     -7
_diffrn_reflns_limit_k_max     7
_diffrn_reflns_limit_l_min     -14
_diffrn_reflns_limit_l_max     14
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     1581
_reflns_number_gt     1457
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0256
_refine_ls_R_factor_gt     0.0242
_refine_ls_wR_factor_gt     0.0659
_refine_ls_wR_factor_ref     0.0675
_refine_ls_goodness_of_fit_ref     1.096
_refine_ls_restrained_S_all     1.096
_refine_ls_number_reflns     1581
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
       'calc w = 1/[σ²(Fo²)+(0.0402P)²+0.24P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.231
_refine_diff_density_min     -1.730
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    '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'
_computing_data_collection     'SMART (Bruker, 2002)'
_computing_cell_refinement     'SAINT-Plus (Bruker, 2003)'
_computing_data_reduction     'SAINT-Plus'
_computing_structure_solution     'SHELXTL (Bruker, 2000)'
_computing_structure_refinement     'SHELXTL'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material     'SHELXTL'
loop_
    _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
    _atom_site_type_symbol
    Pd1 0.0000 0.0000 0.0000 0.01332(8) Uani d S 1 . . Pd
    O2 0.16908(10) 0.2016(2) -0.00239(10) 0.0177(2) Uani d . 1 . . O
    O1 -0.06801(10) 0.1940(2) 0.14436(10) 0.0179(2) Uani d . 1 . . O
    C2 -0.00692(14) 0.3901(3) 0.19495(13) 0.0165(3) Uani d . 1 . . C
    C4 0.19486(14) 0.3966(3) 0.06983(13) 0.0165(3) Uani d . 1 . . C
    C3 0.1164(2) 0.4891(2) 0.1640(2) 0.0169(4) Uani d . 1 . . C
    H3 0.1505 0.6343 0.2119 0.020 Uiso calc R 1 . . H
    C1 -0.0787(2) 0.5240(3) 0.2962(2) 0.0206(4) Uani d . 1 . . C
    H1A -0.1572 0.4220 0.3156 0.031 Uiso calc R 1 . . H
    H1B -0.1094 0.6927 0.2641 0.031 Uiso calc R 1 . . H
    H1C -0.0165 0.5445 0.3750 0.031 Uiso calc R 1 . . H
    C5 0.3224(2) 0.5367(4) 0.0475(2) 0.0203(3) Uani d . 1 . . C
    H5A 0.3867 0.5266 0.1255 0.030 Uiso calc R 1 . . H
    H5B 0.3012 0.7165 0.0276 0.030 Uiso calc R 1 . . H
    H5C 0.3629 0.4584 -0.0253 0.030 Uiso calc R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Pd1 0.01223(11) 0.01361(12) 0.01494(12) -0.00067(4) 0.00536(7) -0.00084(4)
    O2 0.0159(4) 0.0172(5) 0.0210(5) -0.0024(4) 0.0066(4) -0.0020(4)
    O1 0.0173(4) 0.0181(5) 0.0195(5) -0.0013(4) 0.0078(4) -0.0029(4)
    C2 0.0175(6) 0.0171(6) 0.0153(6) 0.0019(5) 0.0033(5) 0.0013(5)
    C4 0.0145(6) 0.0176(7) 0.0176(6) -0.0004(5) 0.0024(4) 0.0022(5)
    C3 0.0173(9) 0.0166(9) 0.0172(9) -0.0014(4) 0.0030(7) -0.0016(4)
    C1 0.0212(9) 0.0233(8) 0.0186(8) 0.0004(5) 0.0092(7) -0.0038(5)
    C5 0.0135(7) 0.0236(7) 0.0247(8) -0.0046(6) 0.0057(6) -0.0015(7)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O2 . 1.9815(10) y
    Pd1 O2 3 1.9816(10) n
    Pd1 O1 . 1.9837(10) y
    Pd1 O1 3 1.9837(10) ?
    O2 C4 . 1.2755(18) n
    O1 C2 . 1.2757(18) n
    C2 C3 . 1.394(3) n
    C2 C1 . 1.501(2) n
    C4 C3 . 1.396(3) n
    C4 C5 . 1.499(2) n
    C3 H3 . 0.9500 ?
    C1 H1A . 0.9800 ?
    C1 H1B . 0.9800 ?
    C1 H1C . 0.9800 ?
    C5 H5A . 0.9800 ?
    C5 H5B . 0.9800 ?
    C5 H5C . 0.9800 ?
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
    O2 Pd1 O2 . 3 180.0 n
    O2 Pd1 O1 . . 95.19(4) y
    O2 Pd1 O1 3 . 84.81(4) n
    O2 Pd1 O1 . 3 84.81(4) y
    O2 Pd1 O1 3 3 95.19(4) ?
    O1 Pd1 O1 . 3 180.0 n
    C4 O2 Pd1 . . 122.44(9) n
    C2 O1 Pd1 . . 122.56(9) n
    O1 C2 C3 . . 126.41(14) n
    O1 C2 C1 . . 115.06(13) n
    C3 C2 C1 . . 118.53(15) n
    O2 C4 C3 . . 126.58(14) n
    O2 C4 C5 . . 114.87(13) n
    C3 C4 C5 . . 118.55(15) n
    C2 C3 C4 . . 126.62(15) n
    C2 C3 H3 . . 116.7 ?
    C4 C3 H3 . . 116.7 ?
    C2 C1 H1A . . 109.5 ?
    C2 C1 H1B . . 109.5 ?
    H1A C1 H1B . . 109.5 ?
    C2 C1 H1C . . 109.5 ?
    H1A C1 H1C . . 109.5 ?
    H1B C1 H1C . . 109.5 ?
    C4 C5 H5A . . 109.5 ?
    C4 C5 H5B . . 109.5 ?
    H5A C5 H5B . . 109.5 ?
    C4 C5 H5C . . 109.5 ?
    H5A C5 H5C . . 109.5 ?
    H5B C5 H5C . . 109.5 ?
data_global
_journal_date_recd_electronic     2005-09-19
_journal_date_accepted     2005-09-26
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2005
_journal_volume     61
_journal_issue     11
_journal_page_first     m2181
_journal_page_last     m2183
_journal_paper_category     EM
_journal_coeditor_code     HB6271
_publ_contact_author_name     'Prof. Dr Muhammad Mazhar'
_publ_contact_author_address
; Department of Chemistry
  Quaid-i-Azam University
  Islamabad 45320
  Pakistan
;
_publ_contact_author_email     mazhar42pk@yahoo.com
_publ_contact_author_fax     +92-051-9219888
_publ_contact_author_phone
                    92000000000000E294
_publ_section_title
;
Redetermination of bis(2,4-pentanedionato)palladium(II)
;
loop_
    _publ_author_name
    _publ_author_address
    'Hamid, Mazhar'
; Department of Chemistry
  Quaid-i-Azam University
  Islamabad 45320
  Pakistan
;
    'Zeller, Matthias'
; Department of Chemistry
  Youngstown State University
  1 University Plaza
  Youngstown, OH 44555-3663
  USA
;
    'Hunter, Allen D.'
; Department of Chemistry
  Youngstown State University
  1 University Plaza
  Youngstown, OH 44555-3663
  USA
;
    'Mazhar, Muhammad'
; Department of Chemistry
  Quaid-i-Azam University
  Islamabad 45320
  Pakistan
;
    'Tahir, Asif Ali'
; Department of Chemistry
  Quaid-i-Azam University
  Islamabad 45320
  Pakistan
;
