
data_global


data_bi
#TrackingRef 'bidentate.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H24 B F4 N4 Na O6 Pd2'
_chemical_formula_weight         811.09

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.894(4)
_cell_length_b                   10.276(6)
_cell_length_c                   18.762(11)
_cell_angle_alpha                89.999(13)
_cell_angle_beta                 86.530(16)
_cell_angle_gamma                86.072(14)
_cell_volume                     1323.6(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    3307
_cell_measurement_theta_min      3.0977
_cell_measurement_theta_max      25.3415

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7594
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Saturn724 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18004
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4651
_reflns_number_gt                3953
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  ?

_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)+(0.0561P)²+3.7021P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4651
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Pd1 Pd -0.40635(6) 0.72248(4) 0.35784(2) 0.02247(14) Uani 1 1 d . . .
O1 O -0.3535(6) 0.6600(3) 0.46166(19) 0.0268(8) Uani 1 1 d . . .
O2 O -0.4495(5) 0.8642(3) 0.43969(19) 0.0261(8) Uani 1 1 d . . .
C1 C -0.3839(8) 0.7784(5) 0.4870(3) 0.0257(12) Uani 1 1 d . . .
O3 O -0.3510(6) 0.8103(4) 0.5481(2) 0.0305(9) Uani 1 1 d . . .
Na1 Na -0.2552(3) 1.0192(2) 0.51283(11) 0.0282(5) Uani 1 1 d . . .
C2 C -0.3636(7) 0.5688(5) 0.2937(3) 0.0260(12) Uani 1 1 d . . .
N1 N -0.3211(7) 0.4425(4) 0.3141(3) 0.0277(10) Uani 1 1 d . . .
C3 C -0.2859(9) 0.3434(6) 0.2677(3) 0.0361(14) Uani 1 1 d . . .
H1 H -0.2507 0.2583 0.2845 0.043 Uiso 1 1 calc R . .
C4 C -0.3008(9) 0.3644(6) 0.1955(3) 0.0393(15) Uani 1 1 d . . .
H2 H -0.2788 0.2937 0.1628 0.047 Uiso 1 1 calc R . .
C5 C -0.3476(9) 0.4887(6) 0.1712(3) 0.0332(13) Uani 1 1 d . . .
H3 H -0.3591 0.5044 0.1217 0.040 Uiso 1 1 calc R . .
C6 C -0.3773(8) 0.5894(6) 0.2199(3) 0.0303(13) Uani 1 1 d . . .
C7 C -0.3105(9) 0.4108(5) 0.3903(3) 0.0330(13) Uani 1 1 d . . .
H4 H -0.4423 0.4150 0.4133 0.050 Uiso 1 1 calc R . .
H5 H -0.2332 0.4737 0.4131 0.050 Uiso 1 1 calc R . .
H6 H -0.2491 0.3227 0.3952 0.050 Uiso 1 1 calc R . .
C8 C -0.4530(8) 0.8067(5) 0.2648(3) 0.0263(12) Uani 1 1 d . . .
N2 N -0.5013(6) 0.9367(4) 0.2528(2) 0.0214(9) Uani 1 1 d . . .
C9 C -0.5219(8) 0.9850(6) 0.1868(3) 0.0330(13) Uani 1 1 d . . .
H7 H -0.5551 1.0756 0.1814 0.040 Uiso 1 1 calc R . .
C10 C -0.4963(9) 0.9072(6) 0.1271(3) 0.0352(14) Uani 1 1 d . . .
H8 H -0.5120 0.9430 0.0809 0.042 Uiso 1 1 calc R . .
C11 C -0.4474(9) 0.7762(6) 0.1353(3) 0.0339(14) Uani 1 1 d . . .
H9 H -0.4290 0.7204 0.0948 0.041 Uiso 1 1 calc R . .
C12 C -0.4254(8) 0.7264(5) 0.2027(3) 0.0261(12) Uani 1 1 d . . .
C13 C -0.5349(8) 1.0262(5) 0.3135(3) 0.0284(12) Uani 1 1 d . . .
H10 H -0.6571 1.0085 0.3399 0.043 Uiso 1 1 calc R . .
H11 H -0.5431 1.1163 0.2962 0.043 Uiso 1 1 calc R . .
H12 H -0.4270 1.0139 0.3450 0.043 Uiso 1 1 calc R . .
Pd2 Pd 0.03543(6) 0.83917(4) 0.30448(2) 0.02477(15) Uani 1 1 d . . .
O4 O -0.0546(6) 1.0385(4) 0.3078(2) 0.0343(9) Uani 1 1 d . . .
C14 C -0.0568(8) 1.0403(6) 0.3771(3) 0.0307(13) Uani 1 1 d . . .
O5 O 0.0159(6) 0.9306(4) 0.4050(2) 0.0310(9) Uani 1 1 d . . .
O6 O -0.1259(7) 1.1316(4) 0.4151(2) 0.0397(10) Uani 1 1 d . . .
C15 C 0.1096(8) 0.6514(5) 0.3176(3) 0.0268(12) Uani 1 1 d . . .
N3 N 0.1389(6) 0.5903(4) 0.3819(3) 0.0293(11) Uani 1 1 d . . .
C16 C 0.1803(8) 0.4583(6) 0.3849(4) 0.0369(14) Uani 1 1 d . . .
H13 H 0.2005 0.4192 0.4299 0.044 Uiso 1 1 calc R . .
C17 C 0.1936(10) 0.3823(6) 0.3265(4) 0.0436(16) Uani 1 1 d . . .
H14 H 0.2187 0.2906 0.3305 0.052 Uiso 1 1 calc R . .
C18 C 0.1702(9) 0.4389(6) 0.2601(4) 0.0429(16) Uani 1 1 d . . .
H15 H 0.1826 0.3868 0.2180 0.051 Uiso 1 1 calc R . .
C19 C 0.1287(8) 0.5722(6) 0.2560(3) 0.0305(13) Uani 1 1 d . . .
C20 C 0.1295(9) 0.6628(6) 0.4480(3) 0.0336(13) Uani 1 1 d . . .
H16 H 0.2374 0.7201 0.4475 0.050 Uiso 1 1 calc R . .
H17 H 0.1392 0.6019 0.4881 0.050 Uiso 1 1 calc R . .
H18 H 0.0055 0.7154 0.4533 0.050 Uiso 1 1 calc R . .
C21 C 0.0562(8) 0.7813(6) 0.2037(3) 0.0298(13) Uani 1 1 d . . .
N4 N 0.0336(8) 0.8571(5) 0.1439(3) 0.0384(12) Uani 1 1 d . . .
C22 C 0.0588(11) 0.8074(8) 0.0768(3) 0.0524(19) Uani 1 1 d . . .
H19 H 0.0420 0.8640 0.0372 0.063 Uiso 1 1 calc R . .
C23 C 0.1076(12) 0.6785(9) 0.0648(4) 0.059(2) Uani 1 1 d . . .
H20 H 0.1272 0.6456 0.0174 0.070 Uiso 1 1 calc R . .
C24 C 0.1283(10) 0.5954(7) 0.1227(3) 0.0462(17) Uani 1 1 d . . .
H21 H 0.1585 0.5046 0.1156 0.055 Uiso 1 1 calc R . .
C25 C 0.1040(9) 0.6477(6) 0.1906(3) 0.0357(14) Uani 1 1 d . . .
C26 C -0.0167(10) 0.9975(7) 0.1506(3) 0.0467(17) Uani 1 1 d . . .
H22 H 0.0997 1.0450 0.1392 0.070 Uiso 1 1 calc R . .
H23 H -0.0666 1.0180 0.1996 0.070 Uiso 1 1 calc R . .
H24 H -0.1167 1.0234 0.1174 0.070 Uiso 1 1 calc R . .
B1 B 0.3614(15) 0.2408(8) 0.0574(4) 0.050(2) Uani 1 1 d . . .
F1 F 0.2970(7) 0.2544(4) 0.12784(19) 0.0570(11) Uani 1 1 d . . .
F2 F 0.2768(6) 0.1413(4) 0.02593(19) 0.0491(10) Uani 1 1 d . . .
F3 F 0.3275(8) 0.3565(4) 0.0209(2) 0.0680(14) Uani 1 1 d . . .
F4 F 0.5653(7) 0.2078(5) 0.0562(2) 0.0678(13) Uani 1 1 d . . .


_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
Pd1 C2 1.980(6) . ?
Pd1 C8 1.983(6) . ?
Pd1 O1 2.096(4) . ?
Pd1 O2 2.110(4) . ?
Pd1 C1 2.507(6) . ?
O1 C1 1.305(7) . ?
O2 C1 1.328(6) . ?
O2 Na1 2.412(4) 2_476 ?
O2 Na1 2.594(4) . ?
C1 O3 1.231(7) . ?
C1 Na1 2.739(6) . ?
O3 Na1 2.372(4) . ?
Na1 O6 2.330(5) . ?
Na1 O5 2.406(4) 2_576 ?
Na1 O2 2.412(4) 2_476 ?
Na1 O5 2.780(5) . ?
Na1 C14 2.833(6) . ?
Na1 C14 3.103(6) 2_576 ?
Na1 Na1 3.487(5) 2_476 ?
Na1 Na1 3.518(5) 2_576 ?
C2 N1 1.371(7) . ?
C2 C6 1.409(8) . ?
N1 C3 1.340(7) . ?
N1 C7 1.471(7) . ?
C3 C4 1.379(9) . ?
C3 H1 0.9500 . ?
C4 C5 1.380(9) . ?
C4 H2 0.9500 . ?
C5 C6 1.377(8) . ?
C5 H3 0.9500 . ?
C6 C12 1.465(8) . ?
C7 H4 0.9800 . ?
C7 H5 0.9800 . ?
C7 H6 0.9800 . ?
C8 N2 1.376(7) . ?
C8 C12 1.422(8) . ?
N2 C9 1.346(7) . ?
N2 C13 1.461(7) . ?
C9 C10 1.372(8) . ?
C9 H7 0.9500 . ?
C10 C11 1.376(9) . ?
C10 H8 0.9500 . ?
C11 C12 1.377(8) . ?
C11 H9 0.9500 . ?
C13 H10 0.9800 . ?
C13 H11 0.9800 . ?
C13 H12 0.9800 . ?
Pd2 C21 1.976(6) . ?
Pd2 C15 1.981(6) . ?
Pd2 O4 2.099(4) . ?
Pd2 O5 2.099(4) . ?
Pd2 C14 2.499(6) . ?
O4 C14 1.299(7) . ?
C14 O6 1.231(7) . ?
C14 O5 1.322(7) . ?
C14 Na1 3.103(6) 2_576 ?
O5 Na1 2.406(4) 2_576 ?
C15 N3 1.379(7) . ?
C15 C19 1.408(8) . ?
N3 C16 1.369(7) . ?
N3 C20 1.442(8) . ?
C16 C17 1.340(9) . ?
C16 H13 0.9500 . ?
C17 C18 1.389(10) . ?
C17 H14 0.9500 . ?
C18 C19 1.383(9) . ?
C18 H15 0.9500 . ?
C19 C25 1.463(8) . ?
C20 H16 0.9800 . ?
C20 H17 0.9800 . ?
C20 H18 0.9800 . ?
C21 N4 1.376(7) . ?
C21 C25 1.408(9) . ?
N4 C22 1.355(8) . ?
N4 C26 1.465(9) . ?
C22 C23 1.360(11) . ?
C22 H19 0.9500 . ?
C23 C24 1.390(10) . ?
C23 H20 0.9500 . ?
C24 C25 1.380(9) . ?
C24 H21 0.9500 . ?
C26 H22 0.9800 . ?
C26 H23 0.9800 . ?
C26 H24 0.9800 . ?
B1 F2 1.364(9) . ?
B1 F1 1.372(8) . ?
B1 F3 1.385(8) . ?
B1 F4 1.422(11) . ?

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
C2 Pd1 C8 80.0(2) . . ?
C2 Pd1 O1 107.78(19) . . ?
C8 Pd1 O1 171.94(19) . . ?
C2 Pd1 O2 170.76(19) . . ?
C8 Pd1 O2 109.2(2) . . ?
O1 Pd1 O2 63.17(14) . . ?
C2 Pd1 C1 139.1(2) . . ?
C8 Pd1 C1 140.8(2) . . ?
O1 Pd1 C1 31.35(16) . . ?
O2 Pd1 C1 31.99(15) . . ?
C1 O1 Pd1 92.0(3) . . ?
C1 O2 Pd1 90.7(3) . . ?
C1 O2 Na1 110.3(3) . 2_476 ?
Pd1 O2 Na1 130.19(18) . 2_476 ?
C1 O2 Na1 81.7(3) . . ?
Pd1 O2 Na1 140.60(18) . . ?
Na1 O2 Na1 88.22(14) 2_476 . ?
O3 C1 O1 124.2(5) . . ?
O3 C1 O2 122.2(5) . . ?
O1 C1 O2 113.6(5) . . ?
O3 C1 Pd1 172.4(4) . . ?
O1 C1 Pd1 56.7(3) . . ?
O2 C1 Pd1 57.3(3) . . ?
O3 C1 Na1 59.8(3) . . ?
O1 C1 Na1 150.6(4) . . ?
O2 C1 Na1 69.6(3) . . ?
Pd1 C1 Na1 115.3(2) . . ?
C1 O3 Na1 93.5(3) . . ?
O6 Na1 O3 141.99(16) . . ?
O6 Na1 O5 97.16(17) . 2_576 ?
O3 Na1 O5 104.57(15) . 2_576 ?
O6 Na1 O2 109.54(16) . 2_476 ?
O3 Na1 O2 95.10(15) . 2_476 ?
O5 Na1 O2 104.01(15) 2_576 2_476 ?
O6 Na1 O2 96.14(16) . . ?
O3 Na1 O2 53.42(13) . . ?
O5 Na1 O2 154.54(15) 2_576 . ?
O2 Na1 O2 91.78(14) 2_476 . ?
O6 Na1 C1 117.12(17) . . ?
O3 Na1 C1 26.65(14) . . ?
O5 Na1 C1 126.59(17) 2_576 . ?
O2 Na1 C1 101.39(16) 2_476 . ?
O2 Na1 C1 28.68(14) . . ?
O6 Na1 O5 50.72(14) . . ?
O3 Na1 O5 96.07(14) . . ?
O5 Na1 O5 94.90(14) 2_576 . ?
O2 Na1 O5 154.82(15) 2_476 . ?
O2 Na1 O5 77.08(13) . . ?
C1 Na1 O5 79.66(15) . . ?
O6 Na1 C14 25.26(15) . . ?
O3 Na1 C14 117.55(17) . . ?
O5 Na1 C14 103.71(17) 2_576 . ?
O2 Na1 C14 129.27(17) 2_476 . ?
O2 Na1 C14 80.26(16) . . ?
C1 Na1 C14 94.90(17) . . ?
O5 Na1 C14 27.23(14) . . ?
O6 Na1 C14 110.80(17) . 2_576 ?
O3 Na1 C14 82.40(15) . 2_576 ?
O5 Na1 C14 23.74(14) 2_576 2_576 ?
O2 Na1 C14 114.87(17) 2_476 2_576 ?
O2 Na1 C14 130.87(16) . 2_576 ?
C1 Na1 C14 102.91(17) . 2_576 ?
O5 Na1 C14 88.98(15) . 2_576 ?
C14 Na1 C14 107.47(15) . 2_576 ?
O6 Na1 Na1 108.12(15) . 2_476 ?
O3 Na1 Na1 67.55(12) . 2_476 ?
O5 Na1 Na1 147.05(15) 2_576 2_476 ?
O2 Na1 Na1 48.03(10) 2_476 2_476 ?
O2 Na1 Na1 43.75(9) . 2_476 ?
C1 Na1 Na1 58.94(13) . 2_476 ?
O5 Na1 Na1 117.37(13) . 2_476 ?
C14 Na1 Na1 108.19(15) . 2_476 ?
C14 Na1 Na1 141.05(14) 2_576 2_476 ?
O6 Na1 Na1 65.48(13) . 2_576 ?
O3 Na1 Na1 104.82(14) . 2_576 ?
O5 Na1 Na1 51.94(11) 2_576 2_576 ?
O2 Na1 Na1 151.72(14) 2_476 2_576 ?
O2 Na1 Na1 116.16(13) . 2_576 ?
C1 Na1 Na1 105.41(14) . 2_576 ?
O5 Na1 Na1 42.96(9) . 2_576 ?
C14 Na1 Na1 57.28(13) . 2_576 ?
C14 Na1 Na1 50.19(12) 2_576 2_576 ?
Na1 Na1 Na1 159.60(13) 2_476 2_576 ?
N1 C2 C6 116.0(5) . . ?
N1 C2 Pd1 126.2(4) . . ?
C6 C2 Pd1 117.8(4) . . ?
C3 N1 C2 123.2(5) . . ?
C3 N1 C7 116.8(5) . . ?
C2 N1 C7 119.9(5) . . ?
N1 C3 C4 120.2(6) . . ?
N1 C3 H1 119.9 . . ?
C4 C3 H1 119.9 . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H2 120.2 . . ?
C5 C4 H2 120.2 . . ?
C6 C5 C4 118.9(6) . . ?
C6 C5 H3 120.6 . . ?
C4 C5 H3 120.6 . . ?
C5 C6 C2 121.9(6) . . ?
C5 C6 C12 125.6(5) . . ?
C2 C6 C12 112.5(5) . . ?
N1 C7 H4 109.5 . . ?
N1 C7 H5 109.5 . . ?
H4 C7 H5 109.5 . . ?
N1 C7 H6 109.5 . . ?
H4 C7 H6 109.5 . . ?
H5 C7 H6 109.5 . . ?
N2 C8 C12 115.6(5) . . ?
N2 C8 Pd1 127.1(4) . . ?
C12 C8 Pd1 117.2(4) . . ?
C9 N2 C8 122.3(5) . . ?
C9 N2 C13 118.2(5) . . ?
C8 N2 C13 119.4(4) . . ?
N2 C9 C10 121.9(5) . . ?
N2 C9 H7 119.0 . . ?
C10 C9 H7 119.0 . . ?
C9 C10 C11 118.7(5) . . ?
C9 C10 H8 120.7 . . ?
C11 C10 H8 120.7 . . ?
C10 C11 C12 119.6(6) . . ?
C10 C11 H9 120.2 . . ?
C12 C11 H9 120.2 . . ?
C11 C12 C8 121.8(5) . . ?
C11 C12 C6 125.8(5) . . ?
C8 C12 C6 112.4(5) . . ?
N2 C13 H10 109.5 . . ?
N2 C13 H11 109.5 . . ?
H10 C13 H11 109.5 . . ?
N2 C13 H12 109.5 . . ?
H10 C13 H12 109.5 . . ?
H11 C13 H12 109.5 . . ?
C21 Pd2 C15 80.3(2) . . ?
C21 Pd2 O4 108.4(2) . . ?
C15 Pd2 O4 171.03(19) . . ?
C21 Pd2 O5 170.9(2) . . ?
C15 Pd2 O5 108.36(19) . . ?
O4 Pd2 O5 63.07(15) . . ?
C21 Pd2 C14 139.7(2) . . ?
C15 Pd2 C14 139.9(2) . . ?
O4 Pd2 C14 31.30(16) . . ?
O5 Pd2 C14 31.95(16) . . ?
C14 O4 Pd2 91.6(3) . . ?
O6 C14 O4 124.9(5) . . ?
O6 C14 O5 121.3(5) . . ?
O4 C14 O5 113.8(5) . . ?
O6 C14 Pd2 171.2(4) . . ?
O4 C14 Pd2 57.1(3) . . ?
O5 C14 Pd2 57.2(3) . . ?
O6 C14 Na1 53.9(3) . . ?
O4 C14 Na1 150.9(4) . . ?
O5 C14 Na1 74.2(3) . . ?
Pd2 C14 Na1 119.6(2) . . ?
O6 C14 Na1 88.9(4) . 2_576 ?
O4 C14 Na1 134.2(4) . 2_576 ?
O5 C14 Na1 47.1(3) . 2_576 ?
Pd2 C14 Na1 94.52(19) . 2_576 ?
Na1 C14 Na1 72.53(15) . 2_576 ?
C14 O5 Pd2 90.9(3) . . ?
C14 O5 Na1 109.2(3) . 2_576 ?
Pd2 O5 Na1 133.03(19) . 2_576 ?
C14 O5 Na1 78.6(3) . . ?
Pd2 O5 Na1 141.44(18) . . ?
Na1 O5 Na1 85.10(14) 2_576 . ?
C14 O6 Na1 100.9(3) . . ?
N3 C15 C19 116.9(5) . . ?
N3 C15 Pd2 125.9(4) . . ?
C19 C15 Pd2 117.1(4) . . ?
C16 N3 C15 120.8(5) . . ?
C16 N3 C20 117.7(5) . . ?
C15 N3 C20 121.5(5) . . ?
C17 C16 N3 122.4(6) . . ?
C17 C16 H13 118.8 . . ?
N3 C16 H13 118.8 . . ?
C16 C17 C18 119.3(6) . . ?
C16 C17 H14 120.3 . . ?
C18 C17 H14 120.3 . . ?
C19 C18 C17 119.1(6) . . ?
C19 C18 H15 120.4 . . ?
C17 C18 H15 120.4 . . ?
C18 C19 C15 121.4(6) . . ?
C18 C19 C25 126.2(6) . . ?
C15 C19 C25 112.3(5) . . ?
N3 C20 H16 109.5 . . ?
N3 C20 H17 109.5 . . ?
H16 C20 H17 109.5 . . ?
N3 C20 H18 109.5 . . ?
H16 C20 H18 109.5 . . ?
H17 C20 H18 109.5 . . ?
N4 C21 C25 115.5(5) . . ?
N4 C21 Pd2 127.6(4) . . ?
C25 C21 Pd2 116.9(4) . . ?
C22 N4 C21 122.6(6) . . ?
C22 N4 C26 116.9(6) . . ?
C21 N4 C26 120.5(5) . . ?
N4 C22 C23 121.5(7) . . ?
N4 C22 H19 119.3 . . ?
C23 C22 H19 119.3 . . ?
C22 C23 C24 119.2(7) . . ?
C22 C23 H20 120.4 . . ?
C24 C23 H20 120.4 . . ?
C25 C24 C23 118.6(7) . . ?
C25 C24 H21 120.7 . . ?
C23 C24 H21 120.7 . . ?
C24 C25 C21 122.7(6) . . ?
C24 C25 C19 124.1(6) . . ?
C21 C25 C19 113.2(5) . . ?
N4 C26 H22 109.5 . . ?
N4 C26 H23 109.5 . . ?
H22 C26 H23 109.5 . . ?
N4 C26 H24 109.5 . . ?
H22 C26 H24 109.5 . . ?
H23 C26 H24 109.5 . . ?
F2 B1 F1 111.0(7) . . ?
F2 B1 F3 110.9(6) . . ?
F1 B1 F3 110.8(6) . . ?
F2 B1 F4 107.9(6) . . ?
F1 B1 F4 106.8(6) . . ?
F3 B1 F4 109.4(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Pd1 O1 C1 177.3(3) . . . . ?
O2 Pd1 O1 C1 -4.7(3) . . . . ?
C8 Pd1 O2 C1 -172.7(3) . . . . ?
O1 Pd1 O2 C1 4.6(3) . . . . ?
C8 Pd1 O2 Na1 69.7(3) . . . 2_476 ?
O1 Pd1 O2 Na1 -113.0(3) . . . 2_476 ?
C1 Pd1 O2 Na1 -117.6(4) . . . 2_476 ?
C8 Pd1 O2 Na1 -95.0(3) . . . . ?
O1 Pd1 O2 Na1 82.3(3) . . . . ?
C1 Pd1 O2 Na1 77.7(4) . . . . ?
Pd1 O1 C1 O3 -170.9(5) . . . . ?
Pd1 O1 C1 O2 7.2(4) . . . . ?
Pd1 O1 C1 Na1 -82.8(7) . . . . ?
Pd1 O2 C1 O3 171.0(5) . . . . ?
Na1 O2 C1 O3 -55.2(6) 2_476 . . . ?
Na1 O2 C1 O3 29.8(5) . . . . ?
Pd1 O2 C1 O1 -7.2(4) . . . . ?
Na1 O2 C1 O1 126.6(4) 2_476 . . . ?
Na1 O2 C1 O1 -148.4(4) . . . . ?
Na1 O2 C1 Pd1 133.8(3) 2_476 . . . ?
Na1 O2 C1 Pd1 -141.19(17) . . . . ?
Pd1 O2 C1 Na1 141.19(17) . . . . ?
Na1 O2 C1 Na1 -85.0(2) 2_476 . . . ?
C2 Pd1 C1 O1 -3.9(5) . . . . ?
C8 Pd1 C1 O1 -177.0(3) . . . . ?
O2 Pd1 C1 O1 172.1(5) . . . . ?
C2 Pd1 C1 O2 -176.0(3) . . . . ?
C8 Pd1 C1 O2 10.9(5) . . . . ?
O1 Pd1 C1 O2 -172.1(5) . . . . ?
C2 Pd1 C1 Na1 143.5(3) . . . . ?
C8 Pd1 C1 Na1 -29.6(4) . . . . ?
O1 Pd1 C1 Na1 147.4(4) . . . . ?
O2 Pd1 C1 Na1 -40.5(2) . . . . ?
O1 C1 O3 Na1 145.4(5) . . . . ?
O2 C1 O3 Na1 -32.6(5) . . . . ?
C1 O3 Na1 O6 -25.9(5) . . . . ?
C1 O3 Na1 O5 -148.8(3) . . . 2_576 ?
C1 O3 Na1 O2 105.3(3) . . . 2_476 ?
C1 O3 Na1 O2 16.9(3) . . . . ?
C1 O3 Na1 O5 -52.1(3) . . . . ?
C1 O3 Na1 C14 -34.4(4) . . . . ?
C1 O3 Na1 C14 -140.2(3) . . . 2_576 ?
C1 O3 Na1 Na1 65.1(3) . . . 2_476 ?
C1 O3 Na1 Na1 -94.9(3) . . . 2_576 ?
C1 O2 Na1 O6 139.3(3) . . . . ?
Pd1 O2 Na1 O6 58.4(3) . . . . ?
Na1 O2 Na1 O6 -109.87(16) 2_476 . . . ?
C1 O2 Na1 O3 -15.8(3) . . . . ?
Pd1 O2 Na1 O3 -96.7(3) . . . . ?
Na1 O2 Na1 O3 95.03(18) 2_476 . . . ?
C1 O2 Na1 O5 18.2(5) . . . 2_576 ?
Pd1 O2 Na1 O5 -62.7(5) . . . 2_576 ?
Na1 O2 Na1 O5 128.9(4) 2_476 . . 2_576 ?
C1 O2 Na1 O2 -110.8(3) . . . 2_476 ?
Pd1 O2 Na1 O2 168.3(3) . . . 2_476 ?
Na1 O2 Na1 O2 0.0 2_476 . . 2_476 ?
Pd1 O2 Na1 C1 -80.9(4) . . . . ?
Na1 O2 Na1 C1 110.8(3) 2_476 . . . ?
C1 O2 Na1 O5 92.0(3) . . . . ?
Pd1 O2 Na1 O5 11.1(3) . . . . ?
Na1 O2 Na1 O5 -157.18(15) 2_476 . . . ?
C1 O2 Na1 C14 119.6(3) . . . . ?
Pd1 O2 Na1 C14 38.7(3) . . . . ?
Na1 O2 Na1 C14 -129.59(17) 2_476 . . . ?
C1 O2 Na1 C14 14.9(4) . . . 2_576 ?
Pd1 O2 Na1 C14 -66.0(3) . . . 2_576 ?
Na1 O2 Na1 C14 125.7(2) 2_476 . . 2_576 ?
C1 O2 Na1 Na1 -110.8(3) . . . 2_476 ?
Pd1 O2 Na1 Na1 168.3(3) . . . 2_476 ?
C1 O2 Na1 Na1 73.7(3) . . . 2_576 ?
Pd1 O2 Na1 Na1 -7.2(3) . . . 2_576 ?
Na1 O2 Na1 Na1 -175.53(16) 2_476 . . 2_576 ?
O3 C1 Na1 O6 162.4(3) . . . . ?
O1 C1 Na1 O6 55.4(8) . . . . ?
O2 C1 Na1 O6 -46.7(3) . . . . ?
Pd1 C1 Na1 O6 -11.0(3) . . . . ?
O1 C1 Na1 O3 -107.0(9) . . . . ?
O2 C1 Na1 O3 150.9(5) . . . . ?
Pd1 C1 Na1 O3 -173.4(5) . . . . ?
O3 C1 Na1 O5 38.7(4) . . . 2_576 ?
O1 C1 Na1 O5 -68.3(8) . . . 2_576 ?
O2 C1 Na1 O5 -170.4(3) . . . 2_576 ?
Pd1 C1 Na1 O5 -134.7(2) . . . 2_576 ?
O3 C1 Na1 O2 -78.5(3) . . . 2_476 ?
O1 C1 Na1 O2 174.5(7) . . . 2_476 ?
O2 C1 Na1 O2 72.4(3) . . . 2_476 ?
Pd1 C1 Na1 O2 108.1(2) . . . 2_476 ?
O3 C1 Na1 O2 -150.9(5) . . . . ?
O1 C1 Na1 O2 102.1(9) . . . . ?
Pd1 C1 Na1 O2 35.7(2) . . . . ?
O3 C1 Na1 O5 127.1(3) . . . . ?
O1 C1 Na1 O5 20.1(8) . . . . ?
O2 C1 Na1 O5 -82.0(3) . . . . ?
Pd1 C1 Na1 O5 -46.3(2) . . . . ?
O3 C1 Na1 C14 149.8(3) . . . . ?
O1 C1 Na1 C14 42.8(8) . . . . ?
O2 C1 Na1 C14 -59.3(3) . . . . ?
Pd1 C1 Na1 C14 -23.6(2) . . . . ?
O3 C1 Na1 C14 40.6(4) . . . 2_576 ?
O1 C1 Na1 C14 -66.4(8) . . . 2_576 ?
O2 C1 Na1 C14 -168.5(3) . . . 2_576 ?
Pd1 C1 Na1 C14 -132.8(2) . . . 2_576 ?
O3 C1 Na1 Na1 -101.9(3) . . . 2_476 ?
O1 C1 Na1 Na1 151.1(8) . . . 2_476 ?
O2 C1 Na1 Na1 49.0(2) . . . 2_476 ?
Pd1 C1 Na1 Na1 84.7(2) . . . 2_476 ?
O3 C1 Na1 Na1 92.4(3) . . . 2_576 ?
O1 C1 Na1 Na1 -14.6(8) . . . 2_576 ?
O2 C1 Na1 Na1 -116.7(3) . . . 2_576 ?
Pd1 C1 Na1 Na1 -81.0(2) . . . 2_576 ?
C8 Pd1 C2 N1 -178.0(5) . . . . ?
O1 Pd1 C2 N1 4.3(5) . . . . ?
C1 Pd1 C2 N1 6.5(6) . . . . ?
C8 Pd1 C2 C6 2.2(4) . . . . ?
O1 Pd1 C2 C6 -175.5(4) . . . . ?
C1 Pd1 C2 C6 -173.4(3) . . . . ?
C6 C2 N1 C3 2.7(8) . . . . ?
Pd1 C2 N1 C3 -177.2(4) . . . . ?
C6 C2 N1 C7 -177.9(5) . . . . ?
Pd1 C2 N1 C7 2.2(7) . . . . ?
C2 N1 C3 C4 -3.2(9) . . . . ?
C7 N1 C3 C4 177.4(5) . . . . ?
N1 C3 C4 C5 1.5(9) . . . . ?
C3 C4 C5 C6 0.4(9) . . . . ?
C4 C5 C6 C2 -0.8(9) . . . . ?
C4 C5 C6 C12 179.2(6) . . . . ?
N1 C2 C6 C5 -0.7(8) . . . . ?
Pd1 C2 C6 C5 179.2(4) . . . . ?
N1 C2 C6 C12 179.3(5) . . . . ?
Pd1 C2 C6 C12 -0.8(6) . . . . ?
C2 Pd1 C8 N2 179.9(5) . . . . ?
O2 Pd1 C8 N2 1.4(5) . . . . ?
C1 Pd1 C8 N2 -4.7(6) . . . . ?
C2 Pd1 C8 C12 -3.2(4) . . . . ?
O2 Pd1 C8 C12 178.3(4) . . . . ?
C1 Pd1 C8 C12 172.2(3) . . . . ?
C12 C8 N2 C9 0.2(7) . . . . ?
Pd1 C8 N2 C9 177.1(4) . . . . ?
C12 C8 N2 C13 179.2(4) . . . . ?
Pd1 C8 N2 C13 -3.9(7) . . . . ?
C8 N2 C9 C10 0.2(8) . . . . ?
C13 N2 C9 C10 -178.9(5) . . . . ?
N2 C9 C10 C11 -0.3(9) . . . . ?
C9 C10 C11 C12 0.0(9) . . . . ?
C10 C11 C12 C8 0.4(9) . . . . ?
C10 C11 C12 C6 178.9(5) . . . . ?
N2 C8 C12 C11 -0.5(8) . . . . ?
Pd1 C8 C12 C11 -177.7(4) . . . . ?
N2 C8 C12 C6 -179.2(4) . . . . ?
Pd1 C8 C12 C6 3.6(6) . . . . ?
C5 C6 C12 C11 -0.4(9) . . . . ?
C2 C6 C12 C11 179.6(5) . . . . ?
C5 C6 C12 C8 178.2(5) . . . . ?
C2 C6 C12 C8 -1.7(7) . . . . ?
C21 Pd2 O4 C14 178.5(3) . . . . ?
O5 Pd2 O4 C14 -4.9(3) . . . . ?
Pd2 O4 C14 O6 -169.6(5) . . . . ?
Pd2 O4 C14 O5 7.6(5) . . . . ?
Pd2 O4 C14 Na1 -92.7(8) . . . . ?
Pd2 O4 C14 Na1 60.1(5) . . . 2_576 ?
C21 Pd2 C14 O4 -2.2(5) . . . . ?
C15 Pd2 C14 O4 -176.9(3) . . . . ?
O5 Pd2 C14 O4 171.7(5) . . . . ?
C21 Pd2 C14 O5 -174.0(3) . . . . ?
C15 Pd2 C14 O5 11.4(5) . . . . ?
O4 Pd2 C14 O5 -171.7(5) . . . . ?
C21 Pd2 C14 Na1 143.8(3) . . . . ?
C15 Pd2 C14 Na1 -30.8(4) . . . . ?
O4 Pd2 C14 Na1 146.1(5) . . . . ?
O5 Pd2 C14 Na1 -42.2(3) . . . . ?
C21 Pd2 C14 Na1 -143.7(3) . . . 2_576 ?
C15 Pd2 C14 Na1 41.6(3) . . . 2_576 ?
O4 Pd2 C14 Na1 -141.5(4) . . . 2_576 ?
O5 Pd2 C14 Na1 30.3(2) . . . 2_576 ?
O3 Na1 C14 O6 167.7(4) . . . . ?
O5 Na1 C14 O6 -77.5(4) 2_576 . . . ?
O2 Na1 C14 O6 43.9(4) 2_476 . . . ?
O2 Na1 C14 O6 128.2(4) . . . . ?
C1 Na1 C14 O6 152.9(4) . . . . ?
O5 Na1 C14 O6 -151.1(6) . . . . ?
C14 Na1 C14 O6 -101.9(4) 2_576 . . . ?
Na1 Na1 C14 O6 94.1(4) 2_476 . . . ?
Na1 Na1 C14 O6 -101.9(4) 2_576 . . . ?
O6 Na1 C14 O4 -98.2(9) . . . . ?
O3 Na1 C14 O4 69.5(9) . . . . ?
O5 Na1 C14 O4 -175.7(8) 2_576 . . . ?
O2 Na1 C14 O4 -54.3(9) 2_476 . . . ?
O2 Na1 C14 O4 30.0(8) . . . . ?
C1 Na1 C14 O4 54.7(9) . . . . ?
O5 Na1 C14 O4 110.6(9) . . . . ?
C14 Na1 C14 O4 159.9(9) 2_576 . . . ?
Na1 Na1 C14 O4 -4.2(9) 2_476 . . . ?
Na1 Na1 C14 O4 159.9(9) 2_576 . . . ?
O6 Na1 C14 O5 151.1(6) . . . . ?
O3 Na1 C14 O5 -41.2(4) . . . . ?
O5 Na1 C14 O5 73.6(3) 2_576 . . . ?
O2 Na1 C14 O5 -165.0(3) 2_476 . . . ?
O2 Na1 C14 O5 -80.7(3) . . . . ?
C1 Na1 C14 O5 -55.9(3) . . . . ?
C14 Na1 C14 O5 49.3(3) 2_576 . . . ?
Na1 Na1 C14 O5 -114.8(3) 2_476 . . . ?
Na1 Na1 C14 O5 49.3(3) 2_576 . . . ?
O6 Na1 C14 Pd2 -172.9(5) . . . . ?
O3 Na1 C14 Pd2 -5.2(3) . . . . ?
O5 Na1 C14 Pd2 109.6(2) 2_576 . . . ?
O2 Na1 C14 Pd2 -129.0(2) 2_476 . . . ?
O2 Na1 C14 Pd2 -44.7(2) . . . . ?
C1 Na1 C14 Pd2 -20.0(3) . . . . ?
O5 Na1 C14 Pd2 35.9(2) . . . . ?
C14 Na1 C14 Pd2 85.2(2) 2_576 . . . ?
Na1 Na1 C14 Pd2 -78.9(2) 2_476 . . . ?
Na1 Na1 C14 Pd2 85.2(2) 2_576 . . . ?
O6 Na1 C14 Na1 101.9(4) . . . 2_576 ?
O3 Na1 C14 Na1 -90.44(17) . . . 2_576 ?
O5 Na1 C14 Na1 24.35(14) 2_576 . . 2_576 ?
O2 Na1 C14 Na1 145.77(19) 2_476 . . 2_576 ?
O2 Na1 C14 Na1 -129.94(15) . . . 2_576 ?
C1 Na1 C14 Na1 -105.19(16) . . . 2_576 ?
O5 Na1 C14 Na1 -49.3(3) . . . 2_576 ?
C14 Na1 C14 Na1 0.0 2_576 . . 2_576 ?
Na1 Na1 C14 Na1 -164.06(14) 2_476 . . 2_576 ?
O6 C14 O5 Pd2 169.8(5) . . . . ?
O4 C14 O5 Pd2 -7.6(5) . . . . ?
Na1 C14 O5 Pd2 142.61(16) . . . . ?
Na1 C14 O5 Pd2 -136.7(3) 2_576 . . . ?
O6 C14 O5 Na1 -53.5(6) . . . 2_576 ?
O4 C14 O5 Na1 129.1(4) . . . 2_576 ?
Pd2 C14 O5 Na1 136.7(3) . . . 2_576 ?
Na1 C14 O5 Na1 -80.7(2) . . . 2_576 ?
O6 C14 O5 Na1 27.1(5) . . . . ?
O4 C14 O5 Na1 -150.2(5) . . . . ?
Pd2 C14 O5 Na1 -142.61(16) . . . . ?
Na1 C14 O5 Na1 80.7(2) 2_576 . . . ?
C15 Pd2 O5 C14 -172.3(3) . . . . ?
O4 Pd2 O5 C14 4.8(3) . . . . ?
C15 Pd2 O5 Na1 70.1(3) . . . 2_576 ?
O4 Pd2 O5 Na1 -112.8(3) . . . 2_576 ?
C14 Pd2 O5 Na1 -117.6(4) . . . 2_576 ?
C15 Pd2 O5 Na1 -99.6(3) . . . . ?
O4 Pd2 O5 Na1 77.5(3) . . . . ?
C14 Pd2 O5 Na1 72.7(4) . . . . ?
O6 Na1 O5 C14 -15.4(3) . . . . ?
O3 Na1 O5 C14 144.1(3) . . . . ?
O5 Na1 O5 C14 -110.7(3) 2_576 . . . ?
O2 Na1 O5 C14 28.2(5) 2_476 . . . ?
O2 Na1 O5 C14 93.8(3) . . . . ?
C1 Na1 O5 C14 123.0(3) . . . . ?
C14 Na1 O5 C14 -133.7(3) 2_576 . . . ?
Na1 Na1 O5 C14 76.2(3) 2_476 . . . ?
Na1 Na1 O5 C14 -110.7(3) 2_576 . . . ?
O6 Na1 O5 Pd2 -92.3(3) . . . . ?
O3 Na1 O5 Pd2 67.2(3) . . . . ?
O5 Na1 O5 Pd2 172.4(3) 2_576 . . . ?
O2 Na1 O5 Pd2 -48.7(5) 2_476 . . . ?
O2 Na1 O5 Pd2 16.9(3) . . . . ?
C1 Na1 O5 Pd2 46.1(3) . . . . ?
C14 Na1 O5 Pd2 -76.9(4) . . . . ?
C14 Na1 O5 Pd2 149.4(3) 2_576 . . . ?
Na1 Na1 O5 Pd2 -0.7(3) 2_476 . . . ?
Na1 Na1 O5 Pd2 172.4(3) 2_576 . . . ?
O6 Na1 O5 Na1 95.25(19) . . . 2_576 ?
O3 Na1 O5 Na1 -105.25(15) . . . 2_576 ?
O5 Na1 O5 Na1 0.0 2_576 . . 2_576 ?
O2 Na1 O5 Na1 138.9(3) 2_476 . . 2_576 ?
O2 Na1 O5 Na1 -155.51(16) . . . 2_576 ?
C1 Na1 O5 Na1 -126.33(17) . . . 2_576 ?
C14 Na1 O5 Na1 110.7(3) . . . 2_576 ?
C14 Na1 O5 Na1 -23.01(13) 2_576 . . 2_576 ?
Na1 Na1 O5 Na1 -173.09(15) 2_476 . . 2_576 ?
O4 C14 O6 Na1 144.1(5) . . . . ?
O5 C14 O6 Na1 -32.9(6) . . . . ?
Na1 C14 O6 Na1 -69.0(2) 2_576 . . . ?
O3 Na1 O6 C14 -17.9(5) . . . . ?
O5 Na1 O6 C14 107.1(4) 2_576 . . . ?
O2 Na1 O6 C14 -145.3(4) 2_476 . . . ?
O2 Na1 O6 C14 -51.2(4) . . . . ?
C1 Na1 O6 C14 -30.6(4) . . . . ?
O5 Na1 O6 C14 16.6(3) . . . . ?
C14 Na1 O6 C14 87.0(4) 2_576 . . . ?
Na1 Na1 O6 C14 -94.4(4) 2_476 . . . ?
Na1 Na1 O6 C14 64.8(4) 2_576 . . . ?
C21 Pd2 C15 N3 178.7(5) . . . . ?
O5 Pd2 C15 N3 1.5(5) . . . . ?
C14 Pd2 C15 N3 -4.8(6) . . . . ?
C21 Pd2 C15 C19 -3.3(4) . . . . ?
O5 Pd2 C15 C19 179.5(4) . . . . ?
C14 Pd2 C15 C19 173.2(3) . . . . ?
C19 C15 N3 C16 -1.3(7) . . . . ?
Pd2 C15 N3 C16 176.7(4) . . . . ?
C19 C15 N3 C20 177.8(5) . . . . ?
Pd2 C15 N3 C20 -4.2(7) . . . . ?
C15 N3 C16 C17 -0.4(9) . . . . ?
C20 N3 C16 C17 -179.6(6) . . . . ?
N3 C16 C17 C18 1.9(10) . . . . ?
C16 C17 C18 C19 -1.7(9) . . . . ?
C17 C18 C19 C15 0.0(9) . . . . ?
C17 C18 C19 C25 178.6(6) . . . . ?
N3 C15 C19 C18 1.5(8) . . . . ?
Pd2 C15 C19 C18 -176.7(4) . . . . ?
N3 C15 C19 C25 -177.3(5) . . . . ?
Pd2 C15 C19 C25 4.6(6) . . . . ?
C15 Pd2 C21 N4 -177.0(5) . . . . ?
O4 Pd2 C21 N4 5.3(5) . . . . ?
C14 Pd2 C21 N4 6.5(7) . . . . ?
C15 Pd2 C21 C25 1.4(4) . . . . ?
O4 Pd2 C21 C25 -176.4(4) . . . . ?
C14 Pd2 C21 C25 -175.1(4) . . . . ?
C25 C21 N4 C22 -1.1(8) . . . . ?
Pd2 C21 N4 C22 177.3(5) . . . . ?
C25 C21 N4 C26 179.9(6) . . . . ?
Pd2 C21 N4 C26 -1.7(8) . . . . ?
C21 N4 C22 C23 0.3(11) . . . . ?
C26 N4 C22 C23 179.3(7) . . . . ?
N4 C22 C23 C24 1.3(12) . . . . ?
C22 C23 C24 C25 -1.9(11) . . . . ?
C23 C24 C25 C21 1.0(10) . . . . ?
C23 C24 C25 C19 -177.7(6) . . . . ?
N4 C21 C25 C24 0.4(9) . . . . ?
Pd2 C21 C25 C24 -178.1(5) . . . . ?
N4 C21 C25 C19 179.2(5) . . . . ?
Pd2 C21 C25 C19 0.7(7) . . . . ?
C18 C19 C25 C24 -3.2(10) . . . . ?
C15 C19 C25 C24 175.5(6) . . . . ?
C18 C19 C25 C21 178.0(6) . . . . ?
C15 C19 C25 C21 -3.3(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.864
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.136

data_global
# Attachment 'monodentate.cif'


data_mono
#TrackingRef 'monodentate.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H49 B2 Cl F8 N4 P2 Pd'
_chemical_formula_weight         1107.36

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   11.8013(7)
_cell_length_b                   9.4307(6)
_cell_length_c                   44.208(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.807(3)
_cell_angle_gamma                90
_cell_volume                     4914.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    103.1500
_cell_measurement_reflns_used    8826
_cell_measurement_theta_min      3.0552
_cell_measurement_theta_max      25.3476

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_T_max  0.8947
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50454
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8608
_reflns_number_gt                8159
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  ?

_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)+(0.0398P)²+8.6869P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8608
_refine_ls_number_parameters     663
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Pd1 Pd 0.072117(16) 0.17846(2) 0.383936(4) 0.01276(8) Uani 1 1 d . . .
Cl1 Cl 0.11561(6) -0.06054(7) 0.374147(16) 0.02018(15) Uani 1 1 d . . .
C1 C 0.0292(2) 0.3788(3) 0.39515(6) 0.0137(5) Uani 1 1 d . . .
N1 N 0.01914(19) 0.4120(2) 0.42496(5) 0.0161(5) Uani 1 1 d . . .
C2 C -0.0282(2) 0.5342(3) 0.43483(7) 0.0210(6) Uani 1 1 d . . .
H1 H -0.0320 0.5516 0.4559 0.025 Uiso 1 1 calc R . .
C3 C -0.0702(2) 0.6318(3) 0.41444(7) 0.0217(6) Uani 1 1 d . . .
H2 H -0.1097 0.7130 0.4211 0.026 Uiso 1 1 calc R . .
C4 C -0.0546(2) 0.6108(3) 0.38396(7) 0.0193(6) Uani 1 1 d . . .
H3 H -0.0793 0.6806 0.3696 0.023 Uiso 1 1 calc R . .
C5 C -0.0027(2) 0.4876(3) 0.37436(6) 0.0148(5) Uani 1 1 d . . .
C6 C 0.0625(3) 0.3133(3) 0.44893(6) 0.0216(6) Uani 1 1 d . . .
H4 H 0.0016 0.2490 0.4544 0.032 Uiso 1 1 calc R . .
H5 H 0.0889 0.3677 0.4668 0.032 Uiso 1 1 calc R . .
H6 H 0.1257 0.2581 0.4414 0.032 Uiso 1 1 calc R . .
C7 C 0.0270(2) 0.4777(3) 0.34216(6) 0.0157(6) Uani 1 1 d . . .
C8 C 0.0726(2) 0.5975(3) 0.32924(6) 0.0194(6) Uani 1 1 d . . .
H7 H 0.0785 0.6829 0.3406 0.023 Uiso 1 1 calc R . .
N2 N 0.1084(2) 0.5945(3) 0.30083(5) 0.0228(5) Uani 1 1 d . . .
C9 C 0.1035(3) 0.4750(4) 0.28454(7) 0.0272(7) Uani 1 1 d . . .
H8 H 0.1328 0.4741 0.2649 0.033 Uiso 1 1 calc R . .
C10 C 0.0571(3) 0.3541(3) 0.29566(7) 0.0265(7) Uani 1 1 d . . .
H9 H 0.0522 0.2703 0.2837 0.032 Uiso 1 1 calc R . .
C11 C 0.0174(2) 0.3559(3) 0.32461(6) 0.0206(6) Uani 1 1 d . . .
H10 H -0.0167 0.2734 0.3325 0.025 Uiso 1 1 calc R . .
C12 C 0.1535(3) 0.7258(4) 0.28729(8) 0.0351(8) Uani 1 1 d . . .
H11 H 0.1563 0.8017 0.3025 0.053 Uiso 1 1 calc R . .
H12 H 0.1039 0.7545 0.2699 0.053 Uiso 1 1 calc R . .
H13 H 0.2301 0.7080 0.2805 0.053 Uiso 1 1 calc R . .
P1 P -0.11513(6) 0.10350(7) 0.390108(15) 0.01429(15) Uani 1 1 d . . .
C13 C -0.1694(2) -0.0232(3) 0.36159(6) 0.0166(6) Uani 1 1 d . . .
C14 C -0.1217(2) -0.0308(3) 0.33329(6) 0.0212(6) Uani 1 1 d . . .
H14 H -0.0587 0.0275 0.3291 0.025 Uiso 1 1 calc R . .
C15 C -0.1662(3) -0.1235(3) 0.31128(7) 0.0269(7) Uani 1 1 d . . .
H15 H -0.1335 -0.1280 0.2921 0.032 Uiso 1 1 calc R . .
C16 C -0.2575(3) -0.2089(3) 0.31715(7) 0.0271(7) Uani 1 1 d . . .
H16 H -0.2869 -0.2731 0.3022 0.033 Uiso 1 1 calc R . .
C17 C -0.3059(3) -0.2004(3) 0.34499(7) 0.0245(7) Uani 1 1 d . . .
H17 H -0.3697 -0.2578 0.3489 0.029 Uiso 1 1 calc R . .
C18 C -0.2622(2) -0.1092(3) 0.36722(7) 0.0208(6) Uani 1 1 d . . .
H18 H -0.2956 -0.1052 0.3863 0.025 Uiso 1 1 calc R . .
C19 C -0.2199(2) 0.2459(3) 0.38816(7) 0.0178(6) Uani 1 1 d . . .
C20 C -0.2711(2) 0.2839(3) 0.36021(7) 0.0219(6) Uani 1 1 d . . .
H19 H -0.2565 0.2301 0.3426 0.026 Uiso 1 1 calc R . .
C21 C -0.3433(3) 0.4000(3) 0.35798(7) 0.0270(7) Uani 1 1 d . . .
H20 H -0.3782 0.4250 0.3389 0.032 Uiso 1 1 calc R . .
C22 C -0.3648(3) 0.4798(3) 0.38346(8) 0.0270(7) Uani 1 1 d . . .
H21 H -0.4149 0.5585 0.3820 0.032 Uiso 1 1 calc R . .
C23 C -0.3123(3) 0.4433(3) 0.41116(8) 0.0262(7) Uani 1 1 d . . .
H22 H -0.3251 0.4991 0.4286 0.031 Uiso 1 1 calc R . .
C24 C -0.2413(2) 0.3261(3) 0.41368(7) 0.0204(6) Uani 1 1 d . . .
H23 H -0.2074 0.3006 0.4328 0.024 Uiso 1 1 calc R . .
C25 C -0.1296(2) 0.0188(3) 0.42679(6) 0.0183(6) Uani 1 1 d . . .
C26 C -0.2354(3) 0.0057(3) 0.43949(7) 0.0230(6) Uani 1 1 d . . .
H24 H -0.3012 0.0449 0.4295 0.028 Uiso 1 1 calc R . .
C27 C -0.2436(3) -0.0646(4) 0.46667(7) 0.0323(8) Uani 1 1 d . . .
H25 H -0.3157 -0.0750 0.4751 0.039 Uiso 1 1 calc R . .
C28 C -0.1491(3) -0.1199(4) 0.48173(7) 0.0342(8) Uani 1 1 d . . .
H26 H -0.1561 -0.1679 0.5004 0.041 Uiso 1 1 calc R . .
C29 C -0.0437(3) -0.1057(3) 0.46974(7) 0.0283(7) Uani 1 1 d . . .
H27 H 0.0218 -0.1433 0.4802 0.034 Uiso 1 1 calc R . .
C30 C -0.0339(3) -0.0364(3) 0.44237(7) 0.0214(6) Uani 1 1 d . . .
H28 H 0.0385 -0.0265 0.4342 0.026 Uiso 1 1 calc R . .
P2 P 0.26222(6) 0.23838(7) 0.379306(15) 0.01391(15) Uani 1 1 d . . .
C31 C 0.3422(2) 0.1924(3) 0.41421(6) 0.0155(6) Uani 1 1 d . . .
C32 C 0.4354(2) 0.2733(3) 0.42459(7) 0.0216(6) Uani 1 1 d . . .
H29 H 0.4581 0.3532 0.4133 0.026 Uiso 1 1 calc R . .
C33 C 0.4950(3) 0.2371(4) 0.45140(7) 0.0266(7) Uani 1 1 d . . .
H30 H 0.5583 0.2923 0.4585 0.032 Uiso 1 1 calc R . .
C34 C 0.4619(3) 0.1210(4) 0.46770(7) 0.0271(7) Uani 1 1 d . . .
H31 H 0.5026 0.0965 0.4860 0.032 Uiso 1 1 calc R . .
C35 C 0.3698(3) 0.0394(3) 0.45761(7) 0.0273(7) Uani 1 1 d . . .
H32 H 0.3475 -0.0404 0.4690 0.033 Uiso 1 1 calc R . .
C36 C 0.3105(2) 0.0747(3) 0.43085(7) 0.0210(6) Uani 1 1 d . . .
H33 H 0.2478 0.0184 0.4238 0.025 Uiso 1 1 calc R . .
C37 C 0.2966(2) 0.4236(3) 0.37234(6) 0.0159(6) Uani 1 1 d . . .
C38 C 0.2761(2) 0.5243(3) 0.39467(6) 0.0182(6) Uani 1 1 d . . .
H34 H 0.2455 0.4950 0.4131 0.022 Uiso 1 1 calc R . .
C39 C 0.3000(2) 0.6660(3) 0.39009(7) 0.0217(6) Uani 1 1 d . . .
H35 H 0.2854 0.7337 0.4053 0.026 Uiso 1 1 calc R . .
C40 C 0.3456(2) 0.7093(3) 0.36316(7) 0.0240(7) Uani 1 1 d . . .
H36 H 0.3618 0.8067 0.3600 0.029 Uiso 1 1 calc R . .
C41 C 0.3672(2) 0.6106(3) 0.34098(7) 0.0222(6) Uani 1 1 d . . .
H37 H 0.3992 0.6401 0.3227 0.027 Uiso 1 1 calc R . .
C42 C 0.3423(2) 0.4685(3) 0.34546(6) 0.0188(6) Uani 1 1 d . . .
H38 H 0.3565 0.4013 0.3301 0.023 Uiso 1 1 calc R . .
C43 C 0.3295(2) 0.1435(3) 0.34906(6) 0.0164(6) Uani 1 1 d . . .
C44 C 0.4459(2) 0.1206(3) 0.35067(6) 0.0204(6) Uani 1 1 d . . .
H39 H 0.4900 0.1477 0.3683 0.025 Uiso 1 1 calc R . .
C45 C 0.4976(3) 0.0582(3) 0.32649(7) 0.0253(7) Uani 1 1 d . . .
H40 H 0.5774 0.0438 0.3275 0.030 Uiso 1 1 calc R . .
C46 C 0.4334(3) 0.0167(3) 0.30084(7) 0.0272(7) Uani 1 1 d . . .
H41 H 0.4688 -0.0273 0.2844 0.033 Uiso 1 1 calc R . .
C47 C 0.3176(3) 0.0396(3) 0.29930(7) 0.0246(7) Uani 1 1 d . . .
H42 H 0.2734 0.0116 0.2818 0.030 Uiso 1 1 calc R . .
C48 C 0.2658(2) 0.1033(3) 0.32325(6) 0.0203(6) Uani 1 1 d . . .
H43 H 0.1862 0.1196 0.3220 0.024 Uiso 1 1 calc R . .
C49 C 0.4978(4) 0.6438(5) 0.46450(10) 0.0555(11) Uani 1 1 d . . .
H44 H 0.4552 0.5602 0.4573 0.083 Uiso 1 1 calc R . .
H45 H 0.4515 0.6989 0.4781 0.083 Uiso 1 1 calc R . .
H46 H 0.5678 0.6135 0.4755 0.083 Uiso 1 1 calc R . .
C50 C 0.5255(3) 0.7298(5) 0.43912(11) 0.0499(11) Uani 1 1 d . . .
N3 N 0.5509(3) 0.7978(5) 0.41852(9) 0.0620(11) Uani 1 1 d . . .
C51 C -0.2326(4) 0.2562(5) 0.27075(9) 0.0493(10) Uani 1 1 d . . .
H47 H -0.1828 0.2965 0.2559 0.074 Uiso 1 1 calc R . .
H48 H -0.1873 0.2007 0.2857 0.074 Uiso 1 1 calc R . .
H49 H -0.2713 0.3330 0.2811 0.074 Uiso 1 1 calc R . .
C52 C -0.3162(3) 0.1651(4) 0.25545(8) 0.0372(8) Uani 1 1 d . . .
N4 N -0.3806(3) 0.0950(4) 0.24296(9) 0.0569(10) Uani 1 1 d . . .
B1 B 0.0394(3) 0.0452(4) 0.23918(9) 0.0293(8) Uani 1 1 d . . .
F1 F -0.0496(2) -0.0071(4) 0.22173(7) 0.0850(10) Uani 1 1 d . . .
F2 F 0.0538(3) 0.1877(2) 0.23269(5) 0.0578(7) Uani 1 1 d . . .
F3 F 0.13757(18) -0.0264(3) 0.23289(5) 0.0467(5) Uani 1 1 d . . .
F4 F 0.02065(19) 0.0317(2) 0.26995(5) 0.0452(5) Uani 1 1 d . . .
B2 B 0.2173(3) 0.6162(4) 0.49367(9) 0.0313(8) Uani 1 1 d . . .
F5 F 0.10625(19) 0.6087(3) 0.50235(6) 0.0627(7) Uani 1 1 d . A .
F6 F 0.2287(7) 0.5602(11) 0.4665(2) 0.0637(18) Uani 0.501(12) 1 d PU A 1
F7 F 0.2506(9) 0.7568(10) 0.4956(2) 0.0763(19) Uani 0.501(12) 1 d PU A 1
F8 F 0.2840(6) 0.5438(10) 0.51493(18) 0.0717(18) Uani 0.501(12) 1 d PU A 1
F9 F 0.2053(7) 0.6230(11) 0.46286(17) 0.0580(17) Uani 0.499(12) 1 d PU A 2
F10 F 0.2694(7) 0.4938(10) 0.5024(3) 0.0868(19) Uani 0.499(12) 1 d PU A 2
F11 F 0.2766(8) 0.7276(12) 0.5050(2) 0.0735(19) Uani 0.499(12) 1 d PU A 2


_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
Pd1 C1 2.024(3) . ?
Pd1 P2 2.3322(7) . ?
Pd1 P1 2.3487(7) . ?
Pd1 Cl1 2.3564(7) . ?
C1 N1 1.365(3) . ?
C1 C5 1.416(4) . ?
N1 C2 1.362(4) . ?
N1 C6 1.482(3) . ?
C2 C3 1.365(4) . ?
C2 H1 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H2 0.9500 . ?
C4 C5 1.390(4) . ?
C4 H3 0.9500 . ?
C5 C7 1.486(4) . ?
C6 H4 0.9800 . ?
C6 H5 0.9800 . ?
C6 H6 0.9800 . ?
C7 C8 1.386(4) . ?
C7 C11 1.387(4) . ?
C8 N2 1.346(4) . ?
C8 H7 0.9500 . ?
N2 C9 1.337(4) . ?
N2 C12 1.485(4) . ?
C9 C10 1.367(5) . ?
C9 H8 0.9500 . ?
C10 C11 1.385(4) . ?
C10 H9 0.9500 . ?
C11 H10 0.9500 . ?
C12 H11 0.9800 . ?
C12 H12 0.9800 . ?
C12 H13 0.9800 . ?
P1 C25 1.823(3) . ?
P1 C19 1.825(3) . ?
P1 C13 1.830(3) . ?
C13 C18 1.395(4) . ?
C13 C14 1.399(4) . ?
C14 C15 1.392(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.381(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.392(4) . ?
C19 C20 1.396(4) . ?
C20 C21 1.388(4) . ?
C20 H19 0.9500 . ?
C21 C22 1.388(5) . ?
C21 H20 0.9500 . ?
C22 C23 1.388(5) . ?
C22 H21 0.9500 . ?
C23 C24 1.388(4) . ?
C23 H22 0.9500 . ?
C24 H23 0.9500 . ?
C25 C30 1.394(4) . ?
C25 C26 1.400(4) . ?
C26 C27 1.380(4) . ?
C26 H24 0.9500 . ?
C27 C28 1.374(5) . ?
C27 H25 0.9500 . ?
C28 C29 1.382(5) . ?
C28 H26 0.9500 . ?
C29 C30 1.385(4) . ?
C29 H27 0.9500 . ?
C30 H28 0.9500 . ?
P2 C31 1.821(3) . ?
P2 C37 1.823(3) . ?
P2 C43 1.823(3) . ?
C31 C36 1.393(4) . ?
C31 C32 1.397(4) . ?
C32 C33 1.391(4) . ?
C32 H29 0.9500 . ?
C33 C34 1.378(5) . ?
C33 H30 0.9500 . ?
C34 C35 1.387(4) . ?
C34 H31 0.9500 . ?
C35 C36 1.386(4) . ?
C35 H32 0.9500 . ?
C36 H33 0.9500 . ?
C37 C42 1.395(4) . ?
C37 C38 1.399(4) . ?
C38 C39 1.383(4) . ?
C38 H34 0.9500 . ?
C39 C40 1.391(4) . ?
C39 H35 0.9500 . ?
C40 C41 1.385(4) . ?
C40 H36 0.9500 . ?
C41 C42 1.388(4) . ?
C41 H37 0.9500 . ?
C42 H38 0.9500 . ?
C43 C48 1.388(4) . ?
C43 C44 1.389(4) . ?
C44 C45 1.388(4) . ?
C44 H39 0.9500 . ?
C45 C46 1.390(4) . ?
C45 H40 0.9500 . ?
C46 C47 1.381(4) . ?
C46 H41 0.9500 . ?
C47 C48 1.386(4) . ?
C47 H42 0.9500 . ?
C48 H43 0.9500 . ?
C49 C50 1.435(7) . ?
C49 H44 0.9800 . ?
C49 H45 0.9800 . ?
C49 H46 0.9800 . ?
C50 N3 1.165(6) . ?
C51 C52 1.450(5) . ?
C51 H47 0.9800 . ?
C51 H48 0.9800 . ?
C51 H49 0.9800 . ?
C52 N4 1.131(5) . ?
B1 F1 1.365(4) . ?
B1 F3 1.381(4) . ?
B1 F2 1.386(4) . ?
B1 F4 1.394(4) . ?
B2 F6 1.325(8) . ?
B2 F11 1.345(10) . ?
B2 F10 1.355(8) . ?
B2 F9 1.364(8) . ?
B2 F8 1.377(7) . ?
B2 F7 1.384(10) . ?
B2 F5 1.385(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
C1 Pd1 P2 92.80(7) . . ?
C1 Pd1 P1 90.24(7) . . ?
P2 Pd1 P1 176.10(3) . . ?
C1 Pd1 Cl1 175.73(8) . . ?
P2 Pd1 Cl1 89.80(2) . . ?
P1 Pd1 Cl1 87.02(2) . . ?
N1 C1 C5 115.3(2) . . ?
N1 C1 Pd1 119.03(19) . . ?
C5 C1 Pd1 125.38(19) . . ?
C2 N1 C1 124.0(2) . . ?
C2 N1 C6 115.8(2) . . ?
C1 N1 C6 120.2(2) . . ?
N1 C2 C3 120.1(3) . . ?
N1 C2 H1 120.0 . . ?
C3 C2 H1 120.0 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H2 120.5 . . ?
C4 C3 H2 120.5 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H3 120.0 . . ?
C5 C4 H3 120.0 . . ?
C4 C5 C1 121.0(2) . . ?
C4 C5 C7 118.3(2) . . ?
C1 C5 C7 120.6(2) . . ?
N1 C6 H4 109.5 . . ?
N1 C6 H5 109.5 . . ?
H4 C6 H5 109.5 . . ?
N1 C6 H6 109.5 . . ?
H4 C6 H6 109.5 . . ?
H5 C6 H6 109.5 . . ?
C8 C7 C11 117.9(3) . . ?
C8 C7 C5 117.3(3) . . ?
C11 C7 C5 124.8(3) . . ?
N2 C8 C7 120.9(3) . . ?
N2 C8 H7 119.6 . . ?
C7 C8 H7 119.6 . . ?
C9 N2 C8 120.9(3) . . ?
C9 N2 C12 119.5(3) . . ?
C8 N2 C12 119.6(3) . . ?
N2 C9 C10 121.1(3) . . ?
N2 C9 H8 119.4 . . ?
C10 C9 H8 119.4 . . ?
C9 C10 C11 118.8(3) . . ?
C9 C10 H9 120.6 . . ?
C11 C10 H9 120.6 . . ?
C10 C11 C7 120.3(3) . . ?
C10 C11 H10 119.8 . . ?
C7 C11 H10 119.8 . . ?
N2 C12 H11 109.5 . . ?
N2 C12 H12 109.5 . . ?
H11 C12 H12 109.5 . . ?
N2 C12 H13 109.5 . . ?
H11 C12 H13 109.5 . . ?
H12 C12 H13 109.5 . . ?
C25 P1 C19 105.78(13) . . ?
C25 P1 C13 106.37(13) . . ?
C19 P1 C13 103.58(13) . . ?
C25 P1 Pd1 111.38(10) . . ?
C19 P1 Pd1 114.34(9) . . ?
C13 P1 Pd1 114.59(9) . . ?
C18 C13 C14 119.0(3) . . ?
C18 C13 P1 120.5(2) . . ?
C14 C13 P1 120.4(2) . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.5(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 120.8(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 120.1(3) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C24 C19 C20 119.4(3) . . ?
C24 C19 P1 120.8(2) . . ?
C20 C19 P1 119.6(2) . . ?
C21 C20 C19 120.2(3) . . ?
C21 C20 H19 119.9 . . ?
C19 C20 H19 119.9 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H20 119.8 . . ?
C20 C21 H20 119.8 . . ?
C21 C22 C23 119.4(3) . . ?
C21 C22 H21 120.3 . . ?
C23 C22 H21 120.3 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H22 119.7 . . ?
C22 C23 H22 119.7 . . ?
C23 C24 C19 120.0(3) . . ?
C23 C24 H23 120.0 . . ?
C19 C24 H23 120.0 . . ?
C30 C25 C26 119.0(3) . . ?
C30 C25 P1 119.6(2) . . ?
C26 C25 P1 121.3(2) . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H24 120.2 . . ?
C25 C26 H24 120.2 . . ?
C28 C27 C26 120.9(3) . . ?
C28 C27 H25 119.5 . . ?
C26 C27 H25 119.5 . . ?
C27 C28 C29 120.2(3) . . ?
C27 C28 H26 119.9 . . ?
C29 C28 H26 119.9 . . ?
C28 C29 C30 119.7(3) . . ?
C28 C29 H27 120.1 . . ?
C30 C29 H27 120.1 . . ?
C29 C30 C25 120.5(3) . . ?
C29 C30 H28 119.7 . . ?
C25 C30 H28 119.7 . . ?
C31 P2 C37 105.11(12) . . ?
C31 P2 C43 106.17(12) . . ?
C37 P2 C43 103.77(13) . . ?
C31 P2 Pd1 109.19(9) . . ?
C37 P2 Pd1 118.04(9) . . ?
C43 P2 Pd1 113.63(9) . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 P2 119.7(2) . . ?
C32 C31 P2 121.0(2) . . ?
C33 C32 C31 120.2(3) . . ?
C33 C32 H29 119.9 . . ?
C31 C32 H29 119.9 . . ?
C34 C33 C32 119.7(3) . . ?
C34 C33 H30 120.1 . . ?
C32 C33 H30 120.1 . . ?
C33 C34 C35 120.7(3) . . ?
C33 C34 H31 119.7 . . ?
C35 C34 H31 119.7 . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H32 120.1 . . ?
C34 C35 H32 120.1 . . ?
C35 C36 C31 120.3(3) . . ?
C35 C36 H33 119.8 . . ?
C31 C36 H33 119.8 . . ?
C42 C37 C38 118.8(3) . . ?
C42 C37 P2 122.2(2) . . ?
C38 C37 P2 118.9(2) . . ?
C39 C38 C37 120.6(3) . . ?
C39 C38 H34 119.7 . . ?
C37 C38 H34 119.7 . . ?
C38 C39 C40 119.9(3) . . ?
C38 C39 H35 120.0 . . ?
C40 C39 H35 120.0 . . ?
C41 C40 C39 120.1(3) . . ?
C41 C40 H36 120.0 . . ?
C39 C40 H36 120.0 . . ?
C40 C41 C42 120.0(3) . . ?
C40 C41 H37 120.0 . . ?
C42 C41 H37 120.0 . . ?
C41 C42 C37 120.5(3) . . ?
C41 C42 H38 119.7 . . ?
C37 C42 H38 119.7 . . ?
C48 C43 C44 119.6(3) . . ?
C48 C43 P2 119.9(2) . . ?
C44 C43 P2 120.3(2) . . ?
C45 C44 C43 119.9(3) . . ?
C45 C44 H39 120.1 . . ?
C43 C44 H39 120.1 . . ?
C44 C45 C46 120.3(3) . . ?
C44 C45 H40 119.8 . . ?
C46 C45 H40 119.8 . . ?
C47 C46 C45 119.7(3) . . ?
C47 C46 H41 120.2 . . ?
C45 C46 H41 120.2 . . ?
C46 C47 C48 120.2(3) . . ?
C46 C47 H42 119.9 . . ?
C48 C47 H42 119.9 . . ?
C47 C48 C43 120.3(3) . . ?
C47 C48 H43 119.8 . . ?
C43 C48 H43 119.8 . . ?
C50 C49 H44 109.5 . . ?
C50 C49 H45 109.5 . . ?
H44 C49 H45 109.5 . . ?
C50 C49 H46 109.5 . . ?
H44 C49 H46 109.5 . . ?
H45 C49 H46 109.5 . . ?
N3 C50 C49 178.1(5) . . ?
C52 C51 H47 109.5 . . ?
C52 C51 H48 109.5 . . ?
H47 C51 H48 109.5 . . ?
C52 C51 H49 109.5 . . ?
H47 C51 H49 109.5 . . ?
H48 C51 H49 109.5 . . ?
N4 C52 C51 178.6(4) . . ?
F1 B1 F3 109.8(3) . . ?
F1 B1 F2 109.4(3) . . ?
F3 B1 F2 108.6(3) . . ?
F1 B1 F4 111.4(3) . . ?
F3 B1 F4 109.1(3) . . ?
F2 B1 F4 108.5(3) . . ?
F6 B2 F11 125.0(6) . . ?
F6 B2 F10 81.6(5) . . ?
F11 B2 F10 109.8(5) . . ?
F6 B2 F9 28.8(4) . . ?
F11 B2 F9 111.1(6) . . ?
F10 B2 F9 110.3(6) . . ?
F6 B2 F8 109.9(6) . . ?
F11 B2 F8 82.2(5) . . ?
F10 B2 F8 31.5(4) . . ?
F9 B2 F8 137.1(5) . . ?
F6 B2 F7 113.4(6) . . ?
F11 B2 F7 24.2(4) . . ?
F10 B2 F7 132.4(6) . . ?
F9 B2 F7 91.9(6) . . ?
F8 B2 F7 106.3(5) . . ?
F6 B2 F5 111.7(5) . . ?
F11 B2 F5 114.8(5) . . ?
F10 B2 F5 107.5(5) . . ?
F9 B2 F5 103.1(4) . . ?
F8 B2 F5 107.6(4) . . ?
F7 B2 F5 107.5(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P2 Pd1 C1 N1 -98.88(19) . . . . ?
P1 Pd1 C1 N1 78.67(19) . . . . ?
P2 Pd1 C1 C5 87.6(2) . . . . ?
P1 Pd1 C1 C5 -94.9(2) . . . . ?
C5 C1 N1 C2 6.3(4) . . . . ?
Pd1 C1 N1 C2 -167.9(2) . . . . ?
C5 C1 N1 C6 -172.8(2) . . . . ?
Pd1 C1 N1 C6 13.0(3) . . . . ?
C1 N1 C2 C3 0.7(4) . . . . ?
C6 N1 C2 C3 179.8(3) . . . . ?
N1 C2 C3 C4 -5.9(4) . . . . ?
C2 C3 C4 C5 3.8(4) . . . . ?
C3 C4 C5 C1 3.5(4) . . . . ?
C3 C4 C5 C7 -171.6(3) . . . . ?
N1 C1 C5 C4 -8.2(4) . . . . ?
Pd1 C1 C5 C4 165.5(2) . . . . ?
N1 C1 C5 C7 166.7(2) . . . . ?
Pd1 C1 C5 C7 -19.5(4) . . . . ?
C4 C5 C7 C8 41.4(3) . . . . ?
C1 C5 C7 C8 -133.7(3) . . . . ?
C4 C5 C7 C11 -141.7(3) . . . . ?
C1 C5 C7 C11 43.2(4) . . . . ?
C11 C7 C8 N2 -1.4(4) . . . . ?
C5 C7 C8 N2 175.7(2) . . . . ?
C7 C8 N2 C9 -1.5(4) . . . . ?
C7 C8 N2 C12 178.1(3) . . . . ?
C8 N2 C9 C10 3.1(4) . . . . ?
C12 N2 C9 C10 -176.5(3) . . . . ?
N2 C9 C10 C11 -1.6(5) . . . . ?
C9 C10 C11 C7 -1.4(4) . . . . ?
C8 C7 C11 C10 2.9(4) . . . . ?
C5 C7 C11 C10 -174.0(3) . . . . ?
C1 Pd1 P1 C25 -99.53(12) . . . . ?
Cl1 Pd1 P1 C25 77.19(10) . . . . ?
C1 Pd1 P1 C19 20.31(13) . . . . ?
Cl1 Pd1 P1 C19 -162.97(11) . . . . ?
C1 Pd1 P1 C13 139.67(12) . . . . ?
Cl1 Pd1 P1 C13 -43.61(10) . . . . ?
C25 P1 C13 C18 36.4(3) . . . . ?
C19 P1 C13 C18 -74.8(2) . . . . ?
Pd1 P1 C13 C18 159.9(2) . . . . ?
C25 P1 C13 C14 -146.5(2) . . . . ?
C19 P1 C13 C14 102.3(2) . . . . ?
Pd1 P1 C13 C14 -22.9(3) . . . . ?
C18 C13 C14 C15 -0.4(4) . . . . ?
P1 C13 C14 C15 -177.5(2) . . . . ?
C13 C14 C15 C16 -0.1(5) . . . . ?
C14 C15 C16 C17 1.0(5) . . . . ?
C15 C16 C17 C18 -1.3(5) . . . . ?
C16 C17 C18 C13 0.8(4) . . . . ?
C14 C13 C18 C17 0.0(4) . . . . ?
P1 C13 C18 C17 177.2(2) . . . . ?
C25 P1 C19 C24 38.1(3) . . . . ?
C13 P1 C19 C24 149.8(2) . . . . ?
Pd1 P1 C19 C24 -84.8(2) . . . . ?
C25 P1 C19 C20 -148.1(2) . . . . ?
C13 P1 C19 C20 -36.4(3) . . . . ?
Pd1 P1 C19 C20 89.0(2) . . . . ?
C24 C19 C20 C21 -0.4(4) . . . . ?
P1 C19 C20 C21 -174.3(2) . . . . ?
C19 C20 C21 C22 0.3(4) . . . . ?
C20 C21 C22 C23 0.7(5) . . . . ?
C21 C22 C23 C24 -1.7(5) . . . . ?
C22 C23 C24 C19 1.6(4) . . . . ?
C20 C19 C24 C23 -0.5(4) . . . . ?
P1 C19 C24 C23 173.3(2) . . . . ?
C19 P1 C25 C30 -146.1(2) . . . . ?
C13 P1 C25 C30 104.2(2) . . . . ?
Pd1 P1 C25 C30 -21.3(3) . . . . ?
C19 P1 C25 C26 35.1(3) . . . . ?
C13 P1 C25 C26 -74.7(3) . . . . ?
Pd1 P1 C25 C26 159.8(2) . . . . ?
C30 C25 C26 C27 -1.7(4) . . . . ?
P1 C25 C26 C27 177.2(2) . . . . ?
C25 C26 C27 C28 1.1(5) . . . . ?
C26 C27 C28 C29 -0.1(5) . . . . ?
C27 C28 C29 C30 -0.5(5) . . . . ?
C28 C29 C30 C25 -0.1(5) . . . . ?
C26 C25 C30 C29 1.2(4) . . . . ?
P1 C25 C30 C29 -177.7(2) . . . . ?
C1 Pd1 P2 C31 97.55(12) . . . . ?
Cl1 Pd1 P2 C31 -79.06(10) . . . . ?
C1 Pd1 P2 C37 -22.33(13) . . . . ?
Cl1 Pd1 P2 C37 161.07(10) . . . . ?
C1 Pd1 P2 C43 -144.15(12) . . . . ?
Cl1 Pd1 P2 C43 39.24(10) . . . . ?
C37 P2 C31 C36 160.7(2) . . . . ?
C43 P2 C31 C36 -89.7(2) . . . . ?
Pd1 P2 C31 C36 33.1(2) . . . . ?
C37 P2 C31 C32 -19.5(3) . . . . ?
C43 P2 C31 C32 90.1(3) . . . . ?
Pd1 P2 C31 C32 -147.0(2) . . . . ?
C36 C31 C32 C33 -0.6(4) . . . . ?
P2 C31 C32 C33 179.6(2) . . . . ?
C31 C32 C33 C34 0.1(5) . . . . ?
C32 C33 C34 C35 0.1(5) . . . . ?
C33 C34 C35 C36 0.1(5) . . . . ?
C34 C35 C36 C31 -0.6(5) . . . . ?
C32 C31 C36 C35 0.8(4) . . . . ?
P2 C31 C36 C35 -179.3(2) . . . . ?
C31 P2 C37 C42 123.4(2) . . . . ?
C43 P2 C37 C42 12.1(3) . . . . ?
Pd1 P2 C37 C42 -114.6(2) . . . . ?
C31 P2 C37 C38 -56.8(2) . . . . ?
C43 P2 C37 C38 -168.1(2) . . . . ?
Pd1 P2 C37 C38 65.1(2) . . . . ?
C42 C37 C38 C39 0.4(4) . . . . ?
P2 C37 C38 C39 -179.3(2) . . . . ?
C37 C38 C39 C40 -0.4(4) . . . . ?
C38 C39 C40 C41 -0.2(4) . . . . ?
C39 C40 C41 C42 0.7(4) . . . . ?
C40 C41 C42 C37 -0.7(4) . . . . ?
C38 C37 C42 C41 0.1(4) . . . . ?
P2 C37 C42 C41 179.9(2) . . . . ?
C31 P2 C43 C48 151.3(2) . . . . ?
C37 P2 C43 C48 -98.2(2) . . . . ?
Pd1 P2 C43 C48 31.3(3) . . . . ?
C31 P2 C43 C44 -33.6(3) . . . . ?
C37 P2 C43 C44 76.9(3) . . . . ?
Pd1 P2 C43 C44 -153.7(2) . . . . ?
C48 C43 C44 C45 0.1(4) . . . . ?
P2 C43 C44 C45 -174.9(2) . . . . ?
C43 C44 C45 C46 -0.9(5) . . . . ?
C44 C45 C46 C47 0.9(5) . . . . ?
C45 C46 C47 C48 -0.2(5) . . . . ?
C46 C47 C48 C43 -0.5(5) . . . . ?
C44 C43 C48 C47 0.6(4) . . . . ?
P2 C43 C48 C47 175.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.075


data_global


data_free
#TrackingRef 'di_free.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H12 N2 O5 Pd'
_chemical_formula_weight         382.65

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   6.8562(12)
_cell_length_b                   20.450(4)
_cell_length_c                   9.9565(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.657(2)
_cell_angle_gamma                90.00
_cell_volume                     1362.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    3328
_cell_measurement_theta_min      3.2039
_cell_measurement_theta_max      25.3295

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7691
_exptl_absorpt_correction_T_max  0.9339
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8946
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2374
_reflns_number_gt                2176
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  ?

_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)+(0.0368P)²+2.7424P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2374
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Pd1 Pd 0.81395(4) 0.199486(12) 0.68739(2) 0.01370(11) Uani 1 1 d . . .
C1 C 0.7883(5) 0.11855(18) 0.4961(4) 0.0208(8) Uani 1 1 d . . .
O1 O 0.7831(4) 0.18185(12) 0.4769(2) 0.0211(6) Uani 1 1 d . . .
O2 O 0.8091(4) 0.10141(12) 0.6251(2) 0.0224(6) Uani 1 1 d . . .
O3 O 0.7739(4) 0.07806(13) 0.4002(3) 0.0264(6) Uani 1 1 d . . .
C2 C 0.8377(5) 0.20232(16) 0.8899(4) 0.0137(7) Uani 1 1 d . . .
C3 C 0.8128(5) 0.29563(16) 0.7152(4) 0.0142(7) Uani 1 1 d . . .
N1 N 0.8488(4) 0.15018(14) 0.9768(3) 0.0167(6) Uani 1 1 d . . .
C4 C 0.8524(5) 0.15685(18) 1.1132(4) 0.0203(8) Uani 1 1 d . . .
H1 H 0.8574 0.1189 1.1687 0.024 Uiso 1 1 calc R . .
C5 C 0.8490(5) 0.21739(19) 1.1721(4) 0.0202(8) Uani 1 1 d . . .
H2 H 0.8491 0.2216 1.2672 0.024 Uiso 1 1 calc R . .
C6 C 0.8454(5) 0.27243(18) 1.0898(3) 0.0175(7) Uani 1 1 d . . .
H3 H 0.8469 0.3150 1.1284 0.021 Uiso 1 1 calc R . .
C7 C 0.8396(5) 0.26453(16) 0.9519(3) 0.0147(7) Uani 1 1 d . . .
C8 C 0.8552(6) 0.08261(17) 0.9244(4) 0.0249(9) Uani 1 1 d . . .
H4 H 0.8778 0.0519 1.0018 0.037 Uiso 1 1 calc R . .
H5 H 0.9642 0.0788 0.8755 0.037 Uiso 1 1 calc R . .
H6 H 0.7279 0.0724 0.8612 0.037 Uiso 1 1 calc R . .
C9 C 0.8316(5) 0.31809(17) 0.8517(4) 0.0159(7) Uani 1 1 d . . .
C10 C 0.8422(5) 0.38383(17) 0.8837(4) 0.0191(8) Uani 1 1 d . . .
H7 H 0.8577 0.3978 0.9764 0.023 Uiso 1 1 calc R . .
C11 C 0.8300(6) 0.42932(18) 0.7784(4) 0.0235(8) Uani 1 1 d . . .
H8 H 0.8370 0.4749 0.7976 0.028 Uiso 1 1 calc R . .
C12 C 0.8078(5) 0.40714(17) 0.6477(4) 0.0197(8) Uani 1 1 d . . .
H9 H 0.7979 0.4380 0.5752 0.024 Uiso 1 1 calc R . .
N2 N 0.7993(4) 0.34257(14) 0.6166(3) 0.0167(6) Uani 1 1 d . . .
C13 C 0.7783(6) 0.32340(19) 0.4710(4) 0.0216(8) Uani 1 1 d . . .
H10 H 0.7425 0.3618 0.4119 0.032 Uiso 1 1 calc R . .
H11 H 0.6732 0.2903 0.4467 0.032 Uiso 1 1 calc R . .
H12 H 0.9052 0.3054 0.4577 0.032 Uiso 1 1 calc R . .
O4 O 0.4106(4) 0.07427(13) 0.2054(3) 0.0285(6) Uani 1 1 d . . .
O5 O 0.0972(4) 0.02628(12) 0.3139(3) 0.0291(6) Uani 1 1 d . . .


_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
Pd1 C3 1.986(3) . ?
Pd1 C2 1.988(3) . ?
Pd1 O1 2.091(2) . ?
Pd1 O2 2.097(2) . ?
Pd1 C1 2.500(4) . ?
C1 O3 1.252(4) . ?
C1 O1 1.308(4) . ?
C1 O2 1.309(4) . ?
C2 N1 1.365(4) . ?
C2 C7 1.413(5) . ?
C3 N2 1.361(4) . ?
C3 C9 1.414(5) . ?
N1 C4 1.359(5) . ?
N1 C8 1.481(4) . ?
C4 C5 1.373(5) . ?
C4 H1 0.9500 . ?
C5 C6 1.389(5) . ?
C5 H2 0.9500 . ?
C6 C7 1.375(5) . ?
C6 H3 0.9500 . ?
C7 C9 1.474(5) . ?
C8 H4 0.9800 . ?
C8 H5 0.9800 . ?
C8 H6 0.9800 . ?
C9 C10 1.380(5) . ?
C10 C11 1.390(5) . ?
C10 H7 0.9500 . ?
C11 C12 1.355(5) . ?
C11 H8 0.9500 . ?
C12 N2 1.354(4) . ?
C12 H9 0.9500 . ?
N2 C13 1.479(4) . ?
C13 H10 0.9800 . ?
C13 H11 0.9800 . ?
C13 H12 0.9800 . ?

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
C3 Pd1 C2 80.32(14) . . ?
C3 Pd1 O1 107.92(12) . . ?
C2 Pd1 O1 171.66(12) . . ?
C3 Pd1 O2 171.00(12) . . ?
C2 Pd1 O2 108.67(12) . . ?
O1 Pd1 O2 63.08(10) . . ?
C3 Pd1 C1 139.45(13) . . ?
C2 Pd1 C1 140.20(13) . . ?
O1 Pd1 C1 31.53(11) . . ?
O2 Pd1 C1 31.55(11) . . ?
O3 C1 O1 123.2(3) . . ?
O3 C1 O2 123.0(3) . . ?
O1 C1 O2 113.7(3) . . ?
O3 C1 Pd1 179.6(3) . . ?
O1 C1 Pd1 56.71(17) . . ?
O2 C1 Pd1 57.01(17) . . ?
C1 O1 Pd1 91.8(2) . . ?
C1 O2 Pd1 91.4(2) . . ?
N1 C2 C7 115.6(3) . . ?
N1 C2 Pd1 127.0(2) . . ?
C7 C2 Pd1 117.4(2) . . ?
N2 C3 C9 116.2(3) . . ?
N2 C3 Pd1 126.9(3) . . ?
C9 C3 Pd1 117.0(2) . . ?
C4 N1 C2 122.8(3) . . ?
C4 N1 C8 116.8(3) . . ?
C2 N1 C8 120.5(3) . . ?
N1 C4 C5 121.3(3) . . ?
N1 C4 H1 119.4 . . ?
C5 C4 H1 119.4 . . ?
C4 C5 C6 118.6(3) . . ?
C4 C5 H2 120.7 . . ?
C6 C5 H2 120.7 . . ?
C7 C6 C5 119.1(3) . . ?
C7 C6 H3 120.4 . . ?
C5 C6 H3 120.4 . . ?
C6 C7 C2 122.5(3) . . ?
C6 C7 C9 125.3(3) . . ?
C2 C7 C9 112.2(3) . . ?
N1 C8 H4 109.5 . . ?
N1 C8 H5 109.5 . . ?
H4 C8 H5 109.5 . . ?
N1 C8 H6 109.5 . . ?
H4 C8 H6 109.5 . . ?
H5 C8 H6 109.5 . . ?
C10 C9 C3 121.9(3) . . ?
C10 C9 C7 125.1(3) . . ?
C3 C9 C7 113.0(3) . . ?
C9 C10 C11 119.1(3) . . ?
C9 C10 H7 120.5 . . ?
C11 C10 H7 120.5 . . ?
C12 C11 C10 118.4(3) . . ?
C12 C11 H8 120.8 . . ?
C10 C11 H8 120.8 . . ?
N2 C12 C11 122.4(3) . . ?
N2 C12 H9 118.8 . . ?
C11 C12 H9 118.8 . . ?
C12 N2 C3 122.0(3) . . ?
C12 N2 C13 118.2(3) . . ?
C3 N2 C13 119.8(3) . . ?
N2 C13 H10 109.5 . . ?
N2 C13 H11 109.5 . . ?
H10 C13 H11 109.5 . . ?
N2 C13 H12 109.5 . . ?
H10 C13 H12 109.5 . . ?
H11 C13 H12 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 Pd1 C1 O1 0.5(3) . . . . ?
C2 Pd1 C1 O1 178.0(2) . . . . ?
O2 Pd1 C1 O1 -179.7(3) . . . . ?
C3 Pd1 C1 O2 -179.8(2) . . . . ?
C2 Pd1 C1 O2 -2.3(3) . . . . ?
O1 Pd1 C1 O2 179.7(3) . . . . ?
O3 C1 O1 Pd1 179.5(3) . . . . ?
O2 C1 O1 Pd1 -0.3(3) . . . . ?
C3 Pd1 O1 C1 -179.6(2) . . . . ?
O2 Pd1 O1 C1 0.2(2) . . . . ?
O3 C1 O2 Pd1 -179.5(3) . . . . ?
O1 C1 O2 Pd1 0.3(3) . . . . ?
C2 Pd1 O2 C1 178.4(2) . . . . ?
O1 Pd1 O2 C1 -0.2(2) . . . . ?
C3 Pd1 C2 N1 179.4(3) . . . . ?
O2 Pd1 C2 N1 -0.2(3) . . . . ?
C1 Pd1 C2 N1 1.1(4) . . . . ?
C3 Pd1 C2 C7 0.8(3) . . . . ?
O2 Pd1 C2 C7 -178.8(2) . . . . ?
C1 Pd1 C2 C7 -177.5(2) . . . . ?
C2 Pd1 C3 N2 179.9(3) . . . . ?
O1 Pd1 C3 N2 -1.4(3) . . . . ?
C1 Pd1 C3 N2 -1.7(4) . . . . ?
C2 Pd1 C3 C9 1.1(3) . . . . ?
O1 Pd1 C3 C9 179.8(2) . . . . ?
C1 Pd1 C3 C9 179.5(2) . . . . ?
C7 C2 N1 C4 2.8(5) . . . . ?
Pd1 C2 N1 C4 -175.8(3) . . . . ?
C7 C2 N1 C8 -177.8(3) . . . . ?
Pd1 C2 N1 C8 3.5(5) . . . . ?
C2 N1 C4 C5 -1.3(5) . . . . ?
C8 N1 C4 C5 179.4(3) . . . . ?
N1 C4 C5 C6 -1.2(5) . . . . ?
C4 C5 C6 C7 1.8(5) . . . . ?
C5 C6 C7 C2 -0.2(5) . . . . ?
C5 C6 C7 C9 178.9(3) . . . . ?
N1 C2 C7 C6 -2.1(5) . . . . ?
Pd1 C2 C7 C6 176.7(3) . . . . ?
N1 C2 C7 C9 178.8(3) . . . . ?
Pd1 C2 C7 C9 -2.5(4) . . . . ?
N2 C3 C9 C10 -2.0(5) . . . . ?
Pd1 C3 C9 C10 176.9(3) . . . . ?
N2 C3 C9 C7 178.3(3) . . . . ?
Pd1 C3 C9 C7 -2.8(4) . . . . ?
C6 C7 C9 C10 4.5(6) . . . . ?
C2 C7 C9 C10 -176.3(3) . . . . ?
C6 C7 C9 C3 -175.9(3) . . . . ?
C2 C7 C9 C3 3.3(4) . . . . ?
C3 C9 C10 C11 1.3(5) . . . . ?
C7 C9 C10 C11 -179.1(3) . . . . ?
C9 C10 C11 C12 0.1(6) . . . . ?
C10 C11 C12 N2 -0.7(6) . . . . ?
C11 C12 N2 C3 -0.1(5) . . . . ?
C11 C12 N2 C13 -179.0(3) . . . . ?
C9 C3 N2 C12 1.4(5) . . . . ?
Pd1 C3 N2 C12 -177.4(3) . . . . ?
C9 C3 N2 C13 -179.7(3) . . . . ?
Pd1 C3 N2 C13 1.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.097

