 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-08-25 at 19:10:49
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf017 dreduc struct
 
 
data_ljf017
 
_audit_creation_date            2000-08-25T19:10:49-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FM
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C16 H14 N2 O2 Pd'
_chemical_formula_structural            'C16 H14 N2 O2 Pd'
_chemical_formula_sum                   'C16 H14 N2 O2 Pd'
_chemical_formula_weight                372.69
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/c'
_symmetry_space_group_name_Hall         '-P 2ybc'
_symmetry_Int_Tables_number             14
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'
 
_cell_length_a                          13.7972(4)
_cell_length_b                          7.2708(2)
_cell_length_c                          13.9890(5)
_cell_angle_alpha                       90
_cell_angle_beta                        105.5110(10)
_cell_angle_gamma                       90
_cell_volume                            1352.22(7)
_cell_formula_units_Z                   4
_cell_measurement_temperature           173(2)
_cell_measurement_reflns_used           26678
_cell_measurement_theta_min             3.395
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   yellow
_exptl_crystal_size_max                 0.25
_exptl_crystal_size_mid                 0.1
_exptl_crystal_size_min                 0.1
_exptl_crystal_density_diffrn           1.831
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    744
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           1.378
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_correction_T_min         0.7246
_exptl_absorpt_correction_T_max         0.8745
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             173(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             0.630072E-1
_diffrn_orient_matrix_ub_12             0.69367E-2
_diffrn_orient_matrix_ub_13             0.404913E-1
_diffrn_orient_matrix_ub_21             -0.745127E-1
_diffrn_orient_matrix_ub_22             0.2117E-2
_diffrn_orient_matrix_ub_23             0.115584
_diffrn_orient_matrix_ub_31             0.215679E-1
_diffrn_orient_matrix_ub_32             -0.693408E-1
_diffrn_orient_matrix_ub_33             0.151741E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              CCD
_diffrn_reflns_number                   10260
_diffrn_reflns_av_R_equivalents         0.0473
_diffrn_reflns_av_unetI/netI            0.0506
_diffrn_reflns_limit_h_min              -17
_diffrn_reflns_limit_h_max              15
_diffrn_reflns_limit_k_min              -9
_diffrn_reflns_limit_k_max              9
_diffrn_reflns_limit_l_min              -18
_diffrn_reflns_limit_l_max              18
_diffrn_reflns_theta_min                3.7
_diffrn_reflns_theta_max                27.5
_diffrn_reflns_theta_full               27.5
_diffrn_measured_fraction_theta_full
                                        0.997
_diffrn_measured_fraction_theta_max
                                        0.997
_reflns_number_total                    3103
_reflns_number_gt                       2428
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_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.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0277P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                3103
_refine_ls_number_parameters            190
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0508
_refine_ls_R_factor_gt                  0.0307
_refine_ls_wR_factor_ref                0.0647
_refine_ls_wR_factor_gt                 0.0596
_refine_ls_goodness_of_fit_ref          1.049
_refine_ls_restrained_S_all             1.049
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.912
_refine_diff_density_min                -0.713
_refine_diff_density_rms                0.102
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
 
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
C1 C 0.9232(2) 0.3732(4) 1.10760(19) 0.0266(7) Uani 1 1 d . . .
H1A H 0.882 0.3457 1.1539 0.032 Uiso 1 1 calc R . .
H1B H 0.9261 0.5084 1.1004 0.032 Uiso 1 1 calc R . .
C2 C 1.0284(2) 0.2977(4) 1.14866(19) 0.0261(7) Uani 1 1 d . . .
H2A H 1.0698 0.3864 1.1961 0.031 Uiso 1 1 calc R . .
H2B H 1.0257 0.1808 1.1842 0.031 Uiso 1 1 calc R . .
C3 C 0.7808(2) 0.2906(3) 0.9734(2) 0.0245(6) Uani 1 1 d . . .
H3 H 0.7422 0.3441 1.0132 0.029 Uiso 1 1 calc R . .
C4 C 1.1693(2) 0.2707(4) 1.0790(2) 0.0259(7) Uani 1 1 d . . .
H4 H 1.2085 0.3161 1.1409 0.031 Uiso 1 1 calc R . .
C101 C 0.7719(2) 0.1325(4) 0.81021(19) 0.0217(6) Uani 1 1 d . . .
C102 C 0.7068(2) 0.0533(4) 0.72417(19) 0.0279(7) Uani 1 1 d . . .
H102 H 0.7349 -0.0133 0.6797 0.033 Uiso 1 1 calc R . .
C103 C 0.6040(2) 0.0701(5) 0.7033(2) 0.0371(8) Uani 1 1 d . . .
H103 H 0.5626 0.0179 0.6441 0.044 Uiso 1 1 calc R . .
C104 C 0.5597(2) 0.1629(5) 0.7682(2) 0.0400(8) Uani 1 1 d . . .
H104 H 0.4888 0.1767 0.7529 0.048 Uiso 1 1 calc R . .
C105 C 0.6202(2) 0.2334(4) 0.8540(2) 0.0346(7) Uani 1 1 d . . .
H105 H 0.5901 0.2939 0.899 0.042 Uiso 1 1 calc R . .
C106 C 0.7262(2) 0.2195(4) 0.8781(2) 0.0240(6) Uani 1 1 d . . .
C202 C 1.2410(2) 0.0472(4) 0.8641(2) 0.0298(7) Uani 1 1 d . . .
H202 H 1.2128 -0.0199 0.8049 0.036 Uiso 1 1 calc R . .
C203 C 1.3433(2) 0.0683(4) 0.8955(2) 0.0362(7) Uani 1 1 d . . .
H203 H 1.3843 0.0163 0.8576 0.043 Uiso 1 1 calc R . .
C204 C 1.3885(2) 0.1649(4) 0.9821(2) 0.0375(8) Uani 1 1 d . . .
H204 H 1.4593 0.1828 1.0022 0.045 Uiso 1 1 calc R . .
C205 C 1.3286(2) 0.2333(4) 1.0376(2) 0.0347(8) Uani 1 1 d . . .
H205 H 1.3591 0.2961 1.0976 0.042 Uiso 1 1 calc R . .
C206 C 1.2226(2) 0.2134(4) 1.0083(2) 0.0247(6) Uani 1 1 d . . .
C210 C 1.1762(2) 0.1220(4) 0.9170(2) 0.0237(6) Uani 1 1 d . . .
N1 N 0.87684(18) 0.2885(3) 1.00989(16) 0.0220(5) Uani 1 1 d . . .
N2 N 1.07365(18) 0.2658(3) 1.06577(16) 0.0226(5) Uani 1 1 d . . .
O1 O 0.86884(14) 0.1178(3) 0.82133(12) 0.0244(4) Uani 1 1 d . . .
O2 O 1.07885(13) 0.1004(3) 0.87992(12) 0.0233(4) Uani 1 1 d . . .
Pd1 Pd 0.974362(15) 0.19340(3) 0.943422(14) 0.01981(8) Uani 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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_distance
    _geom_bond_site_symmetry_2
    _geom_bond_publ_flag
C1 N1 1.480(3) . ?
C1 C2 1.514(4) . ?
C2 N2 1.475(4) . ?
C3 N1 1.287(4) . ?
C3 C106 1.441(4) . ?
C4 N2 1.283(4) . ?
C4 C206 1.443(4) . ?
C101 O1 1.309(3) . ?
C101 C102 1.418(4) . ?
C101 C106 1.421(4) . ?
C102 C103 1.375(4) . ?
C103 C104 1.395(4) . ?
C104 C105 1.365(4) . ?
C105 C106 1.413(4) . ?
C202 C203 1.371(4) . ?
C202 C210 1.414(4) . ?
C203 C204 1.395(4) . ?
C204 C205 1.369(5) . ?
C205 C206 1.417(4) . ?
C206 C210 1.430(4) . ?
C210 O2 1.313(3) . ?
N1 Pd1 1.955(2) . ?
N2 Pd1 1.957(2) . ?
O1 Pd1 2.0022(17) . ?
O2 Pd1 2.0025(18) . ?
Pd1 Pd1 3.2119(4) 3_757 ?
 
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 C1 C2 109.5(2) . . ?
N2 C2 C1 108.9(2) . . ?
N1 C3 C106 126.2(3) . . ?
N2 C4 C206 125.9(3) . . ?
O1 C101 C102 117.6(2) . . ?
O1 C101 C106 125.4(2) . . ?
C102 C101 C106 117.0(3) . . ?
C103 C102 C101 121.9(3) . . ?
C102 C103 C104 120.7(3) . . ?
C105 C104 C103 118.8(3) . . ?
C104 C105 C106 122.2(3) . . ?
C105 C106 C101 119.2(3) . . ?
C105 C106 C3 116.5(3) . . ?
C101 C106 C3 124.2(3) . . ?
C203 C202 C210 122.0(3) . . ?
C202 C203 C204 121.2(3) . . ?
C205 C204 C203 118.5(3) . . ?
C204 C205 C206 122.1(3) . . ?
C205 C206 C210 119.1(3) . . ?
C205 C206 C4 116.6(3) . . ?
C210 C206 C4 123.9(3) . . ?
O2 C210 C202 118.0(2) . . ?
O2 C210 C206 125.1(3) . . ?
C202 C210 C206 116.9(3) . . ?
C3 N1 C1 120.4(2) . . ?
C3 N1 Pd1 125.64(19) . . ?
C1 N1 Pd1 113.84(18) . . ?
C4 N2 C2 121.2(2) . . ?
C4 N2 Pd1 125.9(2) . . ?
C2 N2 Pd1 112.67(18) . . ?
C101 O1 Pd1 124.47(16) . . ?
C210 O2 Pd1 124.45(17) . . ?
N1 Pd1 N2 84.19(10) . . ?
N1 Pd1 O1 93.83(8) . . ?
N2 Pd1 O1 177.74(9) . . ?
N1 Pd1 O2 177.61(8) . . ?
N2 Pd1 O2 93.45(9) . . ?
O1 Pd1 O2 88.54(7) . . ?
N1 Pd1 Pd1 99.45(6) . 3_757 ?
N2 Pd1 Pd1 78.11(7) . 3_757 ?
O1 Pd1 Pd1 101.20(5) . 3_757 ?
O2 Pd1 Pd1 80.40(5) . 3_757 ?
 
