# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_12007
_database_code_depnum_ccdc_archive 'CCDC 912611'
#TrackingRef '12007.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C31 H32 N2 O2 Pd,2CH2Cl2'
_chemical_formula_sum            'C33 H36 Cl4 N2 O2 Pd'
_chemical_formula_weight         740.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
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                   16.649(10)
_cell_length_b                   11.043(6)
_cell_length_c                   18.579(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.617(10)
_cell_angle_gamma                90.00
_cell_volume                     3106(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1013
_cell_measurement_theta_min      2.219
_cell_measurement_theta_max      28.138
_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 5387 reflections(SADABS);Rint 0.1382 before
correction and 0.0684 after.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ' Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23875
_diffrn_reflns_av_R_equivalents  0.1476
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6107
_reflns_number_gt                3784
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON.
The solvent accessible voids are 668.8 3 with an estimated 361e/cell to
be added. Eight solvent CH2Cl2 molecules/unit cell accounting for 336e
were included in the formula, FWt, (000) and density calculations.
PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         6107
_refine_ls_number_parameters     331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1514
_refine_ls_wR_factor_gt          0.1406
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.906
_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 0.33541(3) 0.15717(4) 0.76795(2) 0.02604(15) Uani 1 1 d . . .
O1 O 0.3092(3) 0.0253(4) 0.8312(2) 0.0378(10) Uani 1 1 d . . .
O2 O 0.2260(3) 0.1494(5) 0.8665(3) 0.0496(12) Uani 1 1 d . . .
N1 N 0.2307(3) 0.1020(4) 0.6629(3) 0.0281(11) Uani 1 1 d . . .
N2 N 0.3501(3) 0.2748(4) 0.6934(2) 0.0237(10) Uani 1 1 d . . .
C1 C 0.1696(4) 0.0072(5) 0.6574(3) 0.0288(13) Uani 1 1 d . . .
C2 C 0.0835(4) 0.0360(6) 0.6485(3) 0.0296(13) Uani 1 1 d . . .
C3 C 0.0293(4) -0.0562(6) 0.6510(3) 0.0357(15) Uani 1 1 d . . .
H3 H -0.0282 -0.0367 0.6464 0.043 Uiso 1 1 calc R . .
C4 C 0.0548(4) -0.1747(6) 0.6598(3) 0.0406(16) Uani 1 1 d . . .
H4 H 0.0166 -0.2364 0.6628 0.049 Uiso 1 1 calc R . .
C5 C 0.1404(4) -0.2037(6) 0.6642(3) 0.0396(16) Uani 1 1 d . . .
H5 H 0.1580 -0.2862 0.6678 0.048 Uiso 1 1 calc R . .
C6 C 0.1985(4) -0.1140(6) 0.6635(3) 0.0325(14) Uani 1 1 d . . .
C7 C 0.2310(4) 0.1562(5) 0.6016(3) 0.0301(13) Uani 1 1 d . . .
C8 C 0.1680(4) 0.1257(6) 0.5163(3) 0.0412(16) Uani 1 1 d . . .
H8A H 0.1375 0.0495 0.5154 0.062 Uiso 1 1 calc R . .
H8B H 0.2017 0.1173 0.4841 0.062 Uiso 1 1 calc R . .
H8C H 0.1245 0.1908 0.4947 0.062 Uiso 1 1 calc R . .
C9 C 0.2967(4) 0.2515(5) 0.6156(3) 0.0287(13) Uani 1 1 d . . .
C10 C 0.3027(4) 0.3186(5) 0.5557(3) 0.0340(15) Uani 1 1 d . . .
H10 H 0.2630 0.3035 0.5023 0.041 Uiso 1 1 calc R . .
C11 C 0.3647(4) 0.4057(6) 0.5723(4) 0.0385(15) Uani 1 1 d . . .
H11 H 0.3712 0.4489 0.5309 0.046 Uiso 1 1 calc R . .
C12 C 0.4177(4) 0.4310(6) 0.6494(3) 0.0362(15) Uani 1 1 d . . .
H12 H 0.4615 0.4922 0.6614 0.043 Uiso 1 1 calc R . .
C13 C 0.4090(4) 0.3678(5) 0.7124(3) 0.0285(13) Uani 1 1 d . . .
C14 C 0.4574(3) 0.4085(5) 0.7950(3) 0.0273(13) Uani 1 1 d . . .
C15 C 0.4859(4) 0.5267(6) 0.8076(4) 0.0398(15) Uani 1 1 d . . .
H15 H 0.4682 0.5785 0.7628 0.048 Uiso 1 1 calc R . .
C16 C 0.5372(4) 0.5743(6) 0.8789(4) 0.0385(15) Uani 1 1 d . . .
H16 H 0.5517 0.6580 0.8839 0.046 Uiso 1 1 calc R . .
C17 C 0.5687(4) 0.4985(6) 0.9453(4) 0.0477(18) Uani 1 1 d . . .
H17 H 0.6106 0.5282 0.9947 0.057 Uiso 1 1 calc R . .
C18 C 0.5385(4) 0.3796(5) 0.9390(4) 0.0312(14) Uani 1 1 d . . .
C19 C 0.4767(3) 0.3323(5) 0.8624(3) 0.0271(12) Uani 1 1 d . . .
C20 C 0.4394(4) 0.2160(5) 0.8612(3) 0.0254(12) Uani 1 1 d . . .
C21 C 0.4720(4) 0.1472(5) 0.9300(3) 0.0318(13) Uani 1 1 d . . .
H21 H 0.4495 0.0676 0.9283 0.038 Uiso 1 1 calc R . .
C22 C 0.5377(4) 0.1906(5) 1.0030(3) 0.0336(14) Uani 1 1 d . . .
H22 H 0.5606 0.1402 1.0486 0.040 Uiso 1 1 calc R . .
C23 C 0.5664(4) 0.3059(6) 1.0053(4) 0.0416(16) Uani 1 1 d . . .
H23 H 0.6073 0.3376 1.0545 0.050 Uiso 1 1 calc R . .
C24 C 0.2504(4) 0.0495(7) 0.8594(3) 0.0395(16) Uani 1 1 d . . .
C25 C 0.2162(4) -0.0602(7) 0.8846(4) 0.055(2) Uani 1 1 d . . .
H25A H 0.1792 -0.1074 0.8379 0.082 Uiso 1 1 calc R . .
H25B H 0.1810 -0.0352 0.9132 0.082 Uiso 1 1 calc R . .
H25C H 0.2660 -0.1100 0.9194 0.082 Uiso 1 1 calc R . .
C26 C 0.0499(4) 0.1686(6) 0.6390(4) 0.0380(15) Uani 1 1 d . . .
H26 H 0.0974 0.2235 0.6384 0.046 Uiso 1 1 calc R . .
C27 C -0.0317(4) 0.1844(6) 0.5624(4) 0.0491(18) Uani 1 1 d . . .
H27A H -0.0395 0.2704 0.5480 0.074 Uiso 1 1 calc R . .
H27B H -0.0836 0.1551 0.5694 0.074 Uiso 1 1 calc R . .
H27C H -0.0249 0.1381 0.5203 0.074 Uiso 1 1 calc R . .
C28 C 0.0292(4) 0.2024(7) 0.7106(4) 0.0481(18) Uani 1 1 d . . .
H28A H 0.0837 0.1988 0.7594 0.072 Uiso 1 1 calc R . .
H28B H -0.0139 0.1451 0.7141 0.072 Uiso 1 1 calc R . .
H28C H 0.0049 0.2845 0.7034 0.072 Uiso 1 1 calc R . .
C29 C 0.2890(4) -0.1500(6) 0.6672(4) 0.0478(18) Uani 1 1 d . . .
H29 H 0.3205 -0.0743 0.6643 0.057 Uiso 1 1 calc R . .
C30 C 0.3444(5) -0.2134(7) 0.7425(4) 0.059(2) Uani 1 1 d . . .
H30A H 0.4043 -0.2241 0.7460 0.089 Uiso 1 1 calc R . .
H30B H 0.3186 -0.2928 0.7434 0.089 Uiso 1 1 calc R . .
H30C H 0.3466 -0.1650 0.7875 0.089 Uiso 1 1 calc R . .
C31 C 0.2795(5) -0.2298(8) 0.5973(5) 0.068(2) Uani 1 1 d . . .
H31A H 0.2481 -0.1852 0.5479 0.103 Uiso 1 1 calc R . .
H31B H 0.2460 -0.3028 0.5974 0.103 Uiso 1 1 calc R . .
H31C H 0.3382 -0.2530 0.6018 0.103 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0272(2) 0.0277(2) 0.0223(2) 0.0008(2) 0.00943(18) -0.0014(2)
O1 0.044(3) 0.035(2) 0.039(2) 0.006(2) 0.022(2) -0.002(2)
O2 0.051(3) 0.062(3) 0.040(3) -0.010(3) 0.023(2) -0.002(3)
N1 0.023(3) 0.032(3) 0.026(3) 0.001(2) 0.007(2) -0.001(2)
N2 0.023(2) 0.020(2) 0.026(2) 0.001(2) 0.008(2) 0.002(2)
C1 0.033(3) 0.035(3) 0.018(3) 0.004(2) 0.010(3) -0.005(3)
C2 0.024(3) 0.042(4) 0.026(3) -0.003(3) 0.014(3) -0.005(3)
C3 0.022(3) 0.043(4) 0.034(3) -0.004(3) 0.005(3) -0.005(3)
C4 0.034(4) 0.054(5) 0.031(3) 0.003(3) 0.011(3) -0.011(3)
C5 0.054(4) 0.028(3) 0.031(3) 0.006(3) 0.011(3) -0.001(3)
C6 0.031(3) 0.034(3) 0.029(3) 0.005(3) 0.010(3) -0.003(3)
C7 0.028(3) 0.035(3) 0.027(3) 0.002(3) 0.012(2) 0.005(3)
C8 0.043(4) 0.050(4) 0.026(3) 0.002(3) 0.010(3) -0.007(3)
C9 0.025(3) 0.032(3) 0.031(3) 0.005(3) 0.013(3) -0.001(3)
C10 0.034(3) 0.044(4) 0.023(3) 0.004(3) 0.010(3) 0.008(3)
C11 0.045(4) 0.031(4) 0.037(4) 0.008(3) 0.016(3) 0.003(3)
C12 0.047(4) 0.035(4) 0.033(3) 0.004(3) 0.022(3) -0.007(3)
C13 0.022(3) 0.028(3) 0.037(3) 0.000(3) 0.015(3) -0.005(3)
C14 0.015(3) 0.031(3) 0.038(3) -0.001(3) 0.012(3) 0.001(2)
C15 0.041(4) 0.029(3) 0.050(4) 0.000(3) 0.020(3) -0.004(3)
C16 0.048(4) 0.029(3) 0.049(4) -0.006(3) 0.031(3) -0.006(3)
C17 0.041(4) 0.046(4) 0.048(4) -0.003(3) 0.011(3) -0.007(3)
C18 0.018(3) 0.031(3) 0.045(4) -0.005(3) 0.014(3) -0.007(3)
C19 0.022(3) 0.031(3) 0.032(3) 0.006(3) 0.016(2) 0.006(3)
C20 0.029(3) 0.024(3) 0.027(3) 0.002(2) 0.016(3) 0.002(3)
C21 0.032(3) 0.026(3) 0.032(3) 0.001(3) 0.008(3) 0.001(3)
C22 0.044(4) 0.031(3) 0.029(3) 0.002(3) 0.018(3) 0.001(3)
C23 0.036(4) 0.054(4) 0.028(3) -0.003(3) 0.006(3) -0.006(3)
C24 0.042(4) 0.056(5) 0.019(3) 0.001(3) 0.011(3) -0.013(4)
C25 0.038(4) 0.087(6) 0.042(4) 0.013(4) 0.019(3) -0.012(4)
C26 0.039(4) 0.037(4) 0.039(3) -0.009(3) 0.017(3) -0.010(3)
C27 0.053(4) 0.042(4) 0.047(4) 0.004(3) 0.015(4) 0.009(3)
C28 0.039(4) 0.063(5) 0.039(4) -0.015(3) 0.013(3) 0.012(4)
C29 0.031(3) 0.035(4) 0.074(5) 0.012(4) 0.018(3) 0.003(3)
C30 0.054(5) 0.051(5) 0.059(5) 0.001(4) 0.010(4) 0.019(4)
C31 0.047(5) 0.087(6) 0.072(6) 0.004(5) 0.027(4) 0.015(5)
_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 C20 1.980(6) . ?
Pd1 N2 1.987(4) . ?
Pd1 O1 2.030(4) . ?
Pd1 N1 2.094(4) . ?
O1 C24 1.315(7) . ?
O2 C24 1.202(8) . ?
N1 C7 1.289(7) . ?
N1 C1 1.434(7) . ?
N2 C13 1.361(6) . ?
N2 C9 1.369(7) . ?
C1 C2 1.409(8) . ?
C1 C6 1.411(8) . ?
C2 C3 1.374(8) . ?
C2 C26 1.551(8) . ?
C3 C4 1.364(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.429(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(8) . ?
C5 H5 0.9500 . ?
C6 C29 1.532(8) . ?
C7 C9 1.461(8) . ?
C7 C8 1.530(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.376(7) . ?
C10 C11 1.349(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.421(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.475(8) . ?
C14 C15 1.376(8) . ?
C14 C19 1.429(8) . ?
C15 C16 1.349(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.400(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(8) . ?
C17 H17 0.9500 . ?
C18 C23 1.386(8) . ?
C18 C19 1.462(8) . ?
C19 C20 1.423(8) . ?
C20 C21 1.387(7) . ?
C21 C22 1.425(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.355(8) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.495(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.514(8) . ?
C26 C28 1.551(8) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.491(9) . ?
C29 C31 1.521(10) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
C20 Pd1 N2 94.5(2) . . ?
C20 Pd1 O1 92.8(2) . . ?
N2 Pd1 O1 172.43(17) . . ?
C20 Pd1 N1 174.8(2) . . ?
N2 Pd1 N1 80.64(18) . . ?
O1 Pd1 N1 91.96(18) . . ?
C24 O1 Pd1 117.4(4) . . ?
C7 N1 C1 122.6(5) . . ?
C7 N1 Pd1 112.4(4) . . ?
C1 N1 Pd1 124.8(3) . . ?
C13 N2 C9 119.8(5) . . ?
C13 N2 Pd1 126.7(4) . . ?
C9 N2 Pd1 113.4(4) . . ?
C2 C1 C6 121.3(5) . . ?
C2 C1 N1 120.1(5) . . ?
C6 C1 N1 118.6(5) . . ?
C3 C2 C1 118.6(6) . . ?
C3 C2 C26 119.5(5) . . ?
C1 C2 C26 121.9(5) . . ?
C4 C3 C2 122.6(6) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 118.4(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 117.5(5) . . ?
C5 C6 C29 119.4(6) . . ?
C1 C6 C29 123.1(5) . . ?
N1 C7 C9 117.0(5) . . ?
N1 C7 C8 124.1(5) . . ?
C9 C7 C8 118.9(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 121.2(5) . . ?
N2 C9 C7 115.7(5) . . ?
C10 C9 C7 123.0(5) . . ?
C11 C10 C9 120.3(6) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 119.1(6) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 121.4(6) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
N2 C13 C12 117.9(5) . . ?
N2 C13 C14 121.4(5) . . ?
C12 C13 C14 120.5(5) . . ?
C15 C14 C19 118.3(5) . . ?
C15 C14 C13 117.8(5) . . ?
C19 C14 C13 123.9(5) . . ?
C16 C15 C14 124.7(6) . . ?
C16 C15 H15 117.7 . . ?
C14 C15 H15 117.7 . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 119.9(6) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C23 C18 C17 120.2(6) . . ?
C23 C18 C19 119.7(5) . . ?
C17 C18 C19 120.1(6) . . ?
C20 C19 C14 125.5(5) . . ?
C20 C19 C18 117.6(5) . . ?
C14 C19 C18 116.9(5) . . ?
C21 C20 C19 118.7(5) . . ?
C21 C20 Pd1 119.4(4) . . ?
C19 C20 Pd1 121.7(4) . . ?
C20 C21 C22 122.9(5) . . ?
C20 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C23 C22 C21 117.9(6) . . ?
C23 C22 H22 121.1 . . ?
C21 C22 H22 121.1 . . ?
C22 C23 C18 122.7(6) . . ?
C22 C23 H23 118.6 . . ?
C18 C23 H23 118.6 . . ?
O2 C24 O1 124.9(6) . . ?
O2 C24 C25 121.2(6) . . ?
O1 C24 C25 113.9(6) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C28 110.2(5) . . ?
C27 C26 C2 110.8(5) . . ?
C28 C26 C2 109.2(5) . . ?
C27 C26 H26 108.9 . . ?
C28 C26 H26 108.9 . . ?
C2 C26 H26 108.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C31 109.4(6) . . ?
C30 C29 C6 112.1(6) . . ?
C31 C29 C6 111.2(6) . . ?
C30 C29 H29 108.0 . . ?
C31 C29 H29 108.0 . . ?
C6 C29 H29 108.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
C20 Pd1 O1 C24 95.6(4) . . . . ?
N1 Pd1 O1 C24 -86.5(4) . . . . ?
N2 Pd1 N1 C7 7.4(4) . . . . ?
O1 Pd1 N1 C7 -171.1(4) . . . . ?
N2 Pd1 N1 C1 -177.9(4) . . . . ?
O1 Pd1 N1 C1 3.7(4) . . . . ?
C20 Pd1 N2 C13 -6.6(4) . . . . ?
N1 Pd1 N2 C13 175.4(4) . . . . ?
C20 Pd1 N2 C9 170.0(4) . . . . ?
N1 Pd1 N2 C9 -8.1(4) . . . . ?
C7 N1 C1 C2 -82.0(7) . . . . ?
Pd1 N1 C1 C2 103.8(5) . . . . ?
C7 N1 C1 C6 100.0(6) . . . . ?
Pd1 N1 C1 C6 -74.3(6) . . . . ?
C6 C1 C2 C3 4.2(8) . . . . ?
N1 C1 C2 C3 -173.8(5) . . . . ?
C6 C1 C2 C26 -178.0(5) . . . . ?
N1 C1 C2 C26 4.0(8) . . . . ?
C1 C2 C3 C4 -1.7(9) . . . . ?
C26 C2 C3 C4 -179.5(5) . . . . ?
C2 C3 C4 C5 -1.8(9) . . . . ?
C3 C4 C5 C6 3.0(9) . . . . ?
C4 C5 C6 C1 -0.6(8) . . . . ?
C4 C5 C6 C29 -179.1(6) . . . . ?
C2 C1 C6 C5 -3.0(8) . . . . ?
N1 C1 C6 C5 175.0(5) . . . . ?
C2 C1 C6 C29 175.4(5) . . . . ?
N1 C1 C6 C29 -6.6(8) . . . . ?
C1 N1 C7 C9 179.8(5) . . . . ?
Pd1 N1 C7 C9 -5.3(6) . . . . ?
C1 N1 C7 C8 -1.0(8) . . . . ?
Pd1 N1 C7 C8 173.9(4) . . . . ?
C13 N2 C9 C10 1.5(8) . . . . ?
Pd1 N2 C9 C10 -175.3(4) . . . . ?
C13 N2 C9 C7 -175.3(5) . . . . ?
Pd1 N2 C9 C7 7.8(6) . . . . ?
N1 C7 C9 N2 -1.5(7) . . . . ?
C8 C7 C9 N2 179.3(5) . . . . ?
N1 C7 C9 C10 -178.3(5) . . . . ?
C8 C7 C9 C10 2.5(8) . . . . ?
N2 C9 C10 C11 3.1(9) . . . . ?
C7 C9 C10 C11 179.8(5) . . . . ?
C9 C10 C11 C12 -3.7(9) . . . . ?
C10 C11 C12 C13 -0.1(9) . . . . ?
C9 N2 C13 C12 -5.3(7) . . . . ?
Pd1 N2 C13 C12 171.1(4) . . . . ?
C9 N2 C13 C14 170.0(5) . . . . ?
Pd1 N2 C13 C14 -13.6(7) . . . . ?
C11 C12 C13 N2 4.7(8) . . . . ?
C11 C12 C13 C14 -170.6(6) . . . . ?
N2 C13 C14 C15 -153.8(5) . . . . ?
C12 C13 C14 C15 21.3(8) . . . . ?
N2 C13 C14 C19 26.6(8) . . . . ?
C12 C13 C14 C19 -158.2(5) . . . . ?
C19 C14 C15 C16 5.6(9) . . . . ?
C13 C14 C15 C16 -174.0(6) . . . . ?
C14 C15 C16 C17 3.7(10) . . . . ?
C15 C16 C17 C18 -7.7(10) . . . . ?
C16 C17 C18 C23 -177.1(6) . . . . ?
C16 C17 C18 C19 2.5(9) . . . . ?
C15 C14 C19 C20 168.2(5) . . . . ?
C13 C14 C19 C20 -12.3(8) . . . . ?
C15 C14 C19 C18 -10.3(7) . . . . ?
C13 C14 C19 C18 169.2(5) . . . . ?
C23 C18 C19 C20 7.5(8) . . . . ?
C17 C18 C19 C20 -172.1(5) . . . . ?
C23 C18 C19 C14 -173.9(5) . . . . ?
C17 C18 C19 C14 6.5(8) . . . . ?
C14 C19 C20 C21 172.9(5) . . . . ?
C18 C19 C20 C21 -8.6(7) . . . . ?
C14 C19 C20 Pd1 -13.0(7) . . . . ?
C18 C19 C20 Pd1 165.4(4) . . . . ?
N2 Pd1 C20 C21 -166.9(4) . . . . ?
O1 Pd1 C20 C21 11.3(4) . . . . ?
N2 Pd1 C20 C19 19.1(4) . . . . ?
O1 Pd1 C20 C19 -162.7(4) . . . . ?
C19 C20 C21 C22 3.8(8) . . . . ?
Pd1 C20 C21 C22 -170.4(4) . . . . ?
C20 C21 C22 C23 2.7(9) . . . . ?
C21 C22 C23 C18 -4.0(9) . . . . ?
C17 C18 C23 C22 178.5(6) . . . . ?
C19 C18 C23 C22 -1.1(9) . . . . ?
Pd1 O1 C24 O2 -17.8(8) . . . . ?
Pd1 O1 C24 C25 163.6(4) . . . . ?
C3 C2 C26 C27 -60.3(7) . . . . ?
C1 C2 C26 C27 121.9(6) . . . . ?
C3 C2 C26 C28 61.2(7) . . . . ?
C1 C2 C26 C28 -116.5(6) . . . . ?
C5 C6 C29 C30 -62.9(8) . . . . ?
C1 C6 C29 C30 118.7(6) . . . . ?
C5 C6 C29 C31 59.8(8) . . . . ?
C1 C6 C29 C31 -118.5(7) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.139


data_12069
_database_code_depnum_ccdc_archive 'CCDC 912612'
#TrackingRef '12069.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H36 N2 O2 Pd,1.5 H2 O'
_chemical_formula_sum            'C32 H39 N2 O3.50 Pd'
_chemical_formula_weight         614.05
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
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                   8.965(3)
_cell_length_b                   15.135(5)
_cell_length_c                   20.959(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.929(6)
_cell_angle_gamma                90.00
_cell_volume                     2843.6(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    819
_cell_measurement_theta_min      2.363
_cell_measurement_theta_max      28.458
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1276
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 7089 reflections(SADABS);Rint 0.1099 before
correction and 0.0456 after.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21814
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5568
_reflns_number_gt                4031
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Disordered H2O was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 198.2 3 with an estimated 63e/cell to be added.Six
solvent H2O molecules/unit cell accounting for 60e were included in the
formula, FWt, (000) and density calculations. PLATON Reference:
Spek, A.L. (1990), Acta Cryst. A46, C-34.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         5568
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1408
_refine_ls_wR_factor_gt          0.1318
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.003
_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 0.65874(4) 0.22057(2) 0.270652(18) 0.03263(14) Uani 1 1 d . . .
O1 O 0.6180(5) 0.1139(2) 0.32684(19) 0.0548(11) Uani 1 1 d . . .
O2 O 0.6930(5) 0.1887(3) 0.41263(19) 0.0611(12) Uani 1 1 d . . .
N1 N 0.5177(4) 0.3078(3) 0.3256(2) 0.0323(9) Uani 1 1 d . . .
H1 H 0.5337 0.2877 0.3652 0.09(3) Uiso 1 1 d R . .
N2 N 0.6829(4) 0.3274(3) 0.21648(19) 0.0333(9) Uani 1 1 d . . .
C1 C 0.3579(5) 0.2928(3) 0.3357(2) 0.0353(12) Uani 1 1 d . . .
C2 C 0.3042(6) 0.2902(3) 0.3990(3) 0.0415(13) Uani 1 1 d . . .
C3 C 0.1536(6) 0.2708(4) 0.4067(3) 0.0472(14) Uani 1 1 d . . .
H3 H 0.1156 0.2678 0.4487 0.057 Uiso 1 1 calc R . .
C4 C 0.0587(6) 0.2559(4) 0.3564(3) 0.0502(15) Uani 1 1 d . . .
H4 H -0.0432 0.2425 0.3635 0.060 Uiso 1 1 calc R . .
C5 C 0.1117(6) 0.2603(3) 0.2954(3) 0.0411(13) Uani 1 1 d . . .
H5 H 0.0449 0.2499 0.2605 0.049 Uiso 1 1 calc R . .
C6 C 0.2613(5) 0.2798(3) 0.2829(2) 0.0354(11) Uani 1 1 d . . .
C7 C 0.5710(5) 0.4007(3) 0.3102(2) 0.0348(12) Uani 1 1 d . . .
C8 C 0.4451(6) 0.4676(4) 0.3178(3) 0.0592(17) Uani 1 1 d . . .
H8A H 0.3667 0.4560 0.2857 0.089 Uiso 1 1 calc R . .
H8B H 0.4843 0.5275 0.3119 0.089 Uiso 1 1 calc R . .
H8C H 0.4035 0.4624 0.3606 0.089 Uiso 1 1 calc R . .
C9 C 0.6966(6) 0.4219(4) 0.3585(2) 0.0435(14) Uani 1 1 d . . .
H9A H 0.7432 0.4782 0.3472 0.065 Uiso 1 1 calc R . .
H9B H 0.7715 0.3748 0.3578 0.065 Uiso 1 1 calc R . .
H9C H 0.6551 0.4262 0.4014 0.065 Uiso 1 1 calc R . .
C10 C 0.6361(6) 0.4029(4) 0.2441(3) 0.0417(13) Uani 1 1 d . . .
C11 C 0.6577(9) 0.4830(4) 0.2145(3) 0.075(2) Uani 1 1 d . . .
H11 H 0.6234 0.5359 0.2337 0.090 Uiso 1 1 calc R . .
C12 C 0.7299(11) 0.4861(5) 0.1564(3) 0.101(3) Uani 1 1 d . . .
H12 H 0.7480 0.5411 0.1361 0.121 Uiso 1 1 calc R . .
C13 C 0.7749(9) 0.4083(4) 0.1288(3) 0.075(2) Uani 1 1 d . . .
H13 H 0.8273 0.4096 0.0898 0.090 Uiso 1 1 calc R . .
C14 C 0.7443(6) 0.3284(4) 0.1573(2) 0.0462(14) Uani 1 1 d . . .
C15 C 0.7783(6) 0.2460(4) 0.1232(3) 0.0416(13) Uani 1 1 d . . .
C16 C 0.7839(6) 0.2513(4) 0.0565(3) 0.0512(15) Uani 1 1 d . . .
H16 H 0.7535 0.3047 0.0364 0.061 Uiso 1 1 calc R . .
C17 C 0.8321(6) 0.1815(4) 0.0184(3) 0.0545(16) Uani 1 1 d . . .
H17 H 0.8296 0.1865 -0.0267 0.065 Uiso 1 1 calc R . .
C18 C 0.8829(6) 0.1058(4) 0.0471(3) 0.0569(17) Uani 1 1 d . . .
H18 H 0.9189 0.0586 0.0218 0.068 Uiso 1 1 calc R . .
C19 C 0.8819(5) 0.0975(4) 0.1146(3) 0.0428(13) Uani 1 1 d . . .
C20 C 0.8181(5) 0.1661(4) 0.1535(2) 0.0366(12) Uani 1 1 d . . .
C21 C 0.7996(5) 0.1497(3) 0.2198(2) 0.0360(12) Uani 1 1 d . . .
C22 C 0.8669(6) 0.0760(3) 0.2461(3) 0.0414(13) Uani 1 1 d . . .
H22 H 0.8608 0.0671 0.2908 0.050 Uiso 1 1 calc R . .
C23 C 0.9441(6) 0.0133(4) 0.2097(3) 0.0536(16) Uani 1 1 d . . .
H23 H 0.9964 -0.0340 0.2297 0.064 Uiso 1 1 calc R . .
C24 C 0.9420(6) 0.0223(4) 0.1448(3) 0.0555(16) Uani 1 1 d . . .
H24 H 0.9824 -0.0235 0.1193 0.067 Uiso 1 1 calc R . .
C25 C 0.3993(6) 0.3065(4) 0.4595(3) 0.0558(16) Uani 1 1 d . . .
H25 H 0.4864 0.3113 0.4464 0.067 Uiso 1 1 d R . .
C26 C 0.3921(8) 0.2291(5) 0.5052(3) 0.068(2) Uani 1 1 d . . .
H26A H 0.2893 0.2214 0.5193 0.102 Uiso 1 1 calc R . .
H26B H 0.4574 0.2405 0.5422 0.102 Uiso 1 1 calc R . .
H26C H 0.4251 0.1753 0.4835 0.102 Uiso 1 1 calc R . .
C27 C 0.3519(7) 0.3908(5) 0.4920(3) 0.071(2) Uani 1 1 d . . .
H27A H 0.3467 0.4388 0.4607 0.106 Uiso 1 1 calc R . .
H27B H 0.4247 0.4060 0.5257 0.106 Uiso 1 1 calc R . .
H27C H 0.2536 0.3824 0.5108 0.106 Uiso 1 1 calc R . .
C28 C 0.3094(6) 0.2816(4) 0.2142(2) 0.0421(13) Uani 1 1 d . . .
H28 H 0.4154 0.3021 0.2133 0.051 Uiso 1 1 calc R . .
C29 C 0.3022(10) 0.1922(4) 0.1844(3) 0.080(2) Uani 1 1 d . . .
H29A H 0.3693 0.1520 0.2077 0.121 Uiso 1 1 calc R . .
H29B H 0.3328 0.1961 0.1398 0.121 Uiso 1 1 calc R . .
H29C H 0.1999 0.1697 0.1862 0.121 Uiso 1 1 calc R . .
C30 C 0.2150(8) 0.3454(4) 0.1728(3) 0.068(2) Uani 1 1 d . . .
H30A H 0.1115 0.3246 0.1708 0.101 Uiso 1 1 calc R . .
H30B H 0.2553 0.3476 0.1296 0.101 Uiso 1 1 calc R . .
H30C H 0.2182 0.4046 0.1917 0.101 Uiso 1 1 calc R . .
C31 C 0.6453(7) 0.1228(4) 0.3838(3) 0.0467(14) Uani 1 1 d . . .
C32 C 0.6202(13) 0.0384(5) 0.4247(4) 0.133(4) Uani 1 1 d . . .
H32A H 0.7159 0.0183 0.4426 0.200 Uiso 1 1 calc R . .
H32B H 0.5771 -0.0082 0.3977 0.200 Uiso 1 1 calc R . .
H32C H 0.5519 0.0520 0.4593 0.200 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0285(2) 0.0303(2) 0.0390(2) 0.00041(19) 0.00016(15) -0.00315(17)
O1 0.072(3) 0.039(2) 0.055(3) 0.003(2) 0.020(2) -0.009(2)
O2 0.057(3) 0.079(3) 0.047(2) 0.009(2) 0.002(2) -0.001(2)
N1 0.027(2) 0.034(2) 0.036(2) -0.0003(18) -0.0021(17) -0.0040(17)
N2 0.032(2) 0.025(2) 0.043(2) -0.0018(19) -0.0009(18) -0.0004(18)
C1 0.027(3) 0.034(3) 0.045(3) -0.004(2) -0.002(2) -0.004(2)
C2 0.034(3) 0.044(3) 0.046(3) 0.000(3) 0.003(2) -0.008(2)
C3 0.038(3) 0.066(4) 0.037(3) 0.001(3) 0.009(2) -0.008(3)
C4 0.030(3) 0.059(4) 0.062(4) 0.009(3) 0.000(3) -0.011(3)
C5 0.034(3) 0.043(3) 0.046(3) 0.002(3) -0.005(2) -0.008(2)
C6 0.037(3) 0.032(3) 0.038(3) -0.003(2) -0.002(2) -0.005(2)
C7 0.027(3) 0.035(3) 0.042(3) -0.001(2) -0.004(2) -0.003(2)
C8 0.041(3) 0.038(3) 0.099(5) -0.009(3) 0.011(3) 0.000(3)
C9 0.039(3) 0.053(4) 0.038(3) -0.008(3) -0.001(2) -0.015(3)
C10 0.046(3) 0.040(3) 0.038(3) -0.001(3) -0.002(2) -0.002(3)
C11 0.135(7) 0.032(3) 0.058(4) 0.009(3) 0.027(4) 0.012(4)
C12 0.200(10) 0.041(4) 0.063(5) 0.019(4) 0.040(6) 0.010(5)
C13 0.124(7) 0.057(4) 0.045(4) 0.011(3) 0.025(4) -0.004(4)
C14 0.056(4) 0.051(4) 0.032(3) -0.006(3) 0.000(3) 0.003(3)
C15 0.033(3) 0.049(3) 0.042(3) -0.002(3) -0.002(2) 0.004(2)
C16 0.047(3) 0.068(4) 0.040(3) -0.004(3) 0.004(3) -0.003(3)
C17 0.048(4) 0.075(4) 0.041(3) -0.013(3) 0.005(3) 0.005(3)
C18 0.039(3) 0.076(5) 0.057(4) -0.019(3) 0.013(3) 0.006(3)
C19 0.023(3) 0.042(3) 0.064(4) -0.009(3) 0.007(2) 0.001(2)
C20 0.018(2) 0.045(3) 0.046(3) -0.002(3) -0.002(2) -0.004(2)
C21 0.026(3) 0.034(3) 0.047(3) -0.004(2) -0.006(2) -0.005(2)
C22 0.034(3) 0.039(3) 0.052(3) 0.000(3) 0.000(2) -0.006(2)
C23 0.034(3) 0.043(3) 0.083(5) 0.001(3) 0.001(3) -0.002(3)
C24 0.037(3) 0.050(4) 0.080(5) -0.011(3) 0.010(3) 0.001(3)
C25 0.039(3) 0.087(5) 0.042(3) -0.004(3) 0.002(3) -0.013(3)
C26 0.060(4) 0.105(6) 0.038(3) 0.012(4) 0.000(3) 0.000(4)
C27 0.071(5) 0.092(5) 0.050(4) -0.026(4) 0.005(3) -0.011(4)
C28 0.031(3) 0.052(3) 0.043(3) -0.011(3) -0.005(2) -0.004(3)
C29 0.153(8) 0.049(4) 0.040(4) -0.008(3) 0.002(4) 0.032(4)
C30 0.108(6) 0.046(4) 0.049(4) 0.006(3) 0.013(4) 0.020(4)
C31 0.056(4) 0.036(3) 0.049(4) -0.001(3) 0.016(3) 0.002(3)
C32 0.254(13) 0.066(6) 0.082(6) 0.022(5) 0.067(7) 0.020(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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C21 1.980(5) . ?
Pd1 N2 1.990(4) . ?
Pd1 O1 2.034(4) . ?
Pd1 N1 2.171(4) . ?
O1 C31 1.223(7) . ?
O2 C31 1.239(7) . ?
N1 C1 1.469(6) . ?
N1 C7 1.520(6) . ?
N1 H1 0.8949 . ?
N2 C10 1.350(6) . ?
N2 C14 1.365(6) . ?
C1 C6 1.407(7) . ?
C1 C2 1.420(7) . ?
C2 C3 1.394(7) . ?
C2 C25 1.536(7) . ?
C3 C4 1.362(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(7) . ?
C5 H5 0.9500 . ?
C6 C28 1.511(7) . ?
C7 C10 1.513(7) . ?
C7 C8 1.527(7) . ?
C7 C9 1.536(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.378(8) . ?
C11 C12 1.389(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.472(8) . ?
C15 C16 1.401(8) . ?
C15 C20 1.409(7) . ?
C16 C17 1.397(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.368(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.421(8) . ?
C18 H18 0.9500 . ?
C19 C24 1.405(8) . ?
C19 C20 1.443(7) . ?
C20 C21 1.425(7) . ?
C21 C22 1.379(7) . ?
C22 C23 1.407(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.367(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C27 1.511(8) . ?
C25 C26 1.516(8) . ?
C25 H25 0.8346 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.490(8) . ?
C28 C30 1.542(8) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.556(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
C21 Pd1 N2 93.25(19) . . ?
C21 Pd1 O1 90.23(18) . . ?
N2 Pd1 O1 175.76(16) . . ?
C21 Pd1 N1 174.99(17) . . ?
N2 Pd1 N1 82.98(16) . . ?
O1 Pd1 N1 93.68(16) . . ?
C31 O1 Pd1 116.3(4) . . ?
C1 N1 C7 119.0(4) . . ?
C1 N1 Pd1 124.0(3) . . ?
C7 N1 Pd1 105.2(3) . . ?
C1 N1 H1 87.4 . . ?
C7 N1 H1 117.7 . . ?
Pd1 N1 H1 101.5 . . ?
C10 N2 C14 120.9(5) . . ?
C10 N2 Pd1 113.9(3) . . ?
C14 N2 Pd1 125.2(4) . . ?
C6 C1 C2 121.1(4) . . ?
C6 C1 N1 119.8(4) . . ?
C2 C1 N1 119.1(4) . . ?
C3 C2 C1 117.2(5) . . ?
C3 C2 C25 117.7(5) . . ?
C1 C2 C25 125.1(5) . . ?
C4 C3 C2 122.7(5) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 122.0(5) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 117.5(5) . . ?
C5 C6 C28 118.0(4) . . ?
C1 C6 C28 124.4(4) . . ?
C10 C7 N1 110.0(4) . . ?
C10 C7 C8 112.2(5) . . ?
N1 C7 C8 110.9(4) . . ?
C10 C7 C9 108.0(4) . . ?
N1 C7 C9 106.4(4) . . ?
C8 C7 C9 109.2(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 120.3(5) . . ?
N2 C10 C7 120.1(5) . . ?
C11 C10 C7 119.4(5) . . ?
C10 C11 C12 119.7(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 120.4(6) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
N2 C14 C13 119.3(5) . . ?
N2 C14 C15 121.5(5) . . ?
C13 C14 C15 119.2(5) . . ?
C16 C15 C20 119.0(5) . . ?
C16 C15 C14 116.6(5) . . ?
C20 C15 C14 124.1(5) . . ?
C17 C16 C15 122.9(6) . . ?
C17 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C18 C17 C16 119.0(6) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 120.3(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C24 C19 C18 120.7(5) . . ?
C24 C19 C20 118.8(5) . . ?
C18 C19 C20 120.5(5) . . ?
C15 C20 C21 123.8(5) . . ?
C15 C20 C19 117.5(5) . . ?
C21 C20 C19 118.7(5) . . ?
C22 C21 C20 118.2(5) . . ?
C22 C21 Pd1 120.2(4) . . ?
C20 C21 Pd1 121.1(4) . . ?
C21 C22 C23 123.1(5) . . ?
C21 C22 H22 118.5 . . ?
C23 C22 H22 118.5 . . ?
C24 C23 C22 118.3(6) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C23 C24 C19 121.8(6) . . ?
C23 C24 H24 119.1 . . ?
C19 C24 H24 119.1 . . ?
C27 C25 C26 110.6(5) . . ?
C27 C25 C2 110.6(5) . . ?
C26 C25 C2 111.6(5) . . ?
C27 C25 H25 110.2 . . ?
C26 C25 H25 108.8 . . ?
C2 C25 H25 104.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C6 111.8(5) . . ?
C29 C28 C30 108.3(5) . . ?
C6 C28 C30 112.6(4) . . ?
C29 C28 H28 108.0 . . ?
C6 C28 H28 108.0 . . ?
C30 C28 H28 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 O2 128.8(5) . . ?
O1 C31 C32 114.8(6) . . ?
O2 C31 C32 116.4(6) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
C21 Pd1 O1 C31 121.1(4) . . . . ?
N1 Pd1 O1 C31 -55.7(4) . . . . ?
N2 Pd1 N1 C1 118.5(4) . . . . ?
O1 Pd1 N1 C1 -58.9(4) . . . . ?
N2 Pd1 N1 C7 -23.6(3) . . . . ?
O1 Pd1 N1 C7 159.0(3) . . . . ?
C21 Pd1 N2 C10 -162.5(4) . . . . ?
N1 Pd1 N2 C10 14.2(4) . . . . ?
C21 Pd1 N2 C14 15.7(4) . . . . ?
N1 Pd1 N2 C14 -167.6(4) . . . . ?
C7 N1 C1 C6 83.4(6) . . . . ?
Pd1 N1 C1 C6 -54.0(6) . . . . ?
C7 N1 C1 C2 -97.5(5) . . . . ?
Pd1 N1 C1 C2 125.1(4) . . . . ?
C6 C1 C2 C3 2.6(8) . . . . ?
N1 C1 C2 C3 -176.4(5) . . . . ?
C6 C1 C2 C25 -177.9(5) . . . . ?
N1 C1 C2 C25 3.1(8) . . . . ?
C1 C2 C3 C4 -1.0(9) . . . . ?
C25 C2 C3 C4 179.4(6) . . . . ?
C2 C3 C4 C5 -0.3(9) . . . . ?
C3 C4 C5 C6 0.0(9) . . . . ?
C4 C5 C6 C1 1.6(8) . . . . ?
C4 C5 C6 C28 178.9(5) . . . . ?
C2 C1 C6 C5 -2.9(7) . . . . ?
N1 C1 C6 C5 176.2(4) . . . . ?
C2 C1 C6 C28 179.9(5) . . . . ?
N1 C1 C6 C28 -1.0(7) . . . . ?
C1 N1 C7 C10 -116.1(5) . . . . ?
Pd1 N1 C7 C10 28.3(4) . . . . ?
C1 N1 C7 C8 8.5(6) . . . . ?
Pd1 N1 C7 C8 152.9(4) . . . . ?
C1 N1 C7 C9 127.1(4) . . . . ?
Pd1 N1 C7 C9 -88.5(4) . . . . ?
C14 N2 C10 C11 -3.9(8) . . . . ?
Pd1 N2 C10 C11 174.4(5) . . . . ?
C14 N2 C10 C7 -178.9(5) . . . . ?
Pd1 N2 C10 C7 -0.6(6) . . . . ?
N1 C7 C10 N2 -20.6(6) . . . . ?
C8 C7 C10 N2 -144.5(5) . . . . ?
C9 C7 C10 N2 95.2(6) . . . . ?
N1 C7 C10 C11 164.4(5) . . . . ?
C8 C7 C10 C11 40.5(7) . . . . ?
C9 C7 C10 C11 -79.9(7) . . . . ?
N2 C10 C11 C12 -0.9(11) . . . . ?
C7 C10 C11 C12 174.1(7) . . . . ?
C10 C11 C12 C13 1.8(13) . . . . ?
C11 C12 C13 C14 2.1(13) . . . . ?
C10 N2 C14 C13 7.7(8) . . . . ?
Pd1 N2 C14 C13 -170.4(5) . . . . ?
C10 N2 C14 C15 -172.2(5) . . . . ?
Pd1 N2 C14 C15 9.7(7) . . . . ?
C12 C13 C14 N2 -6.8(11) . . . . ?
C12 C13 C14 C15 173.1(7) . . . . ?
N2 C14 C15 C16 155.6(5) . . . . ?
C13 C14 C15 C16 -24.3(8) . . . . ?
N2 C14 C15 C20 -30.4(8) . . . . ?
C13 C14 C15 C20 149.7(6) . . . . ?
C20 C15 C16 C17 -2.2(8) . . . . ?
C14 C15 C16 C17 172.1(5) . . . . ?
C15 C16 C17 C18 -3.2(9) . . . . ?
C16 C17 C18 C19 2.0(9) . . . . ?
C17 C18 C19 C24 -176.2(5) . . . . ?
C17 C18 C19 C20 4.3(8) . . . . ?
C16 C15 C20 C21 -172.2(5) . . . . ?
C14 C15 C20 C21 14.0(8) . . . . ?
C16 C15 C20 C19 8.2(7) . . . . ?
C14 C15 C20 C19 -165.7(5) . . . . ?
C24 C19 C20 C15 171.0(5) . . . . ?
C18 C19 C20 C15 -9.4(7) . . . . ?
C24 C19 C20 C21 -8.6(7) . . . . ?
C18 C19 C20 C21 171.0(5) . . . . ?
C15 C20 C21 C22 -168.4(5) . . . . ?
C19 C20 C21 C22 11.2(7) . . . . ?
C15 C20 C21 Pd1 20.1(7) . . . . ?
C19 C20 C21 Pd1 -160.2(4) . . . . ?
N2 Pd1 C21 C22 159.0(4) . . . . ?
O1 Pd1 C21 C22 -23.4(4) . . . . ?
N2 Pd1 C21 C20 -29.7(4) . . . . ?
O1 Pd1 C21 C20 147.9(4) . . . . ?
C20 C21 C22 C23 -4.4(8) . . . . ?
Pd1 C21 C22 C23 167.1(4) . . . . ?
C21 C22 C23 C24 -5.4(8) . . . . ?
C22 C23 C24 C19 8.2(8) . . . . ?
C18 C19 C24 C23 179.2(5) . . . . ?
C20 C19 C24 C23 -1.2(8) . . . . ?
C3 C2 C25 C27 -67.5(7) . . . . ?
C1 C2 C25 C27 113.0(6) . . . . ?
C3 C2 C25 C26 56.2(7) . . . . ?
C1 C2 C25 C26 -123.4(6) . . . . ?
C5 C6 C28 C29 -66.8(7) . . . . ?
C1 C6 C28 C29 110.4(6) . . . . ?
C5 C6 C28 C30 55.4(7) . . . . ?
C1 C6 C28 C30 -127.4(5) . . . . ?
Pd1 O1 C31 O2 1.0(8) . . . . ?
Pd1 O1 C31 C32 -177.1(5) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O2 0.89 2.29 2.993(6) 135.8 .
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.115


data_12074
_database_code_depnum_ccdc_archive 'CCDC 912613'
#TrackingRef '12074.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H19 N O3 Pd, C H2 Cl2'
_chemical_formula_sum            'C21 H21 Cl2 N O3 Pd'
_chemical_formula_weight         512.69
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   30.215(10)
_cell_length_b                   11.882(4)
_cell_length_c                   12.283(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.179(5)
_cell_angle_gamma                90.00
_cell_volume                     4235(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    882
_cell_measurement_theta_min      2.395
_cell_measurement_theta_max      23.096
_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 3861 reflections(SADABS);Rint 0.1180 before
correction and 0.0640 after.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16176
_diffrn_reflns_av_R_equivalents  0.1214
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4145
_reflns_number_gt                2491
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         4145
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.1864
_refine_ls_wR_factor_gt          0.1648
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_restrained_S_all      0.951
_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 0.386718(19) 0.69094(5) 0.20608(5) 0.0508(2) Uani 1 1 d . . .
O1 O 0.42731(19) 0.6308(6) 0.1007(5) 0.0760(18) Uani 1 1 d . . .
H1 H 0.4575 0.6338 0.1181 0.091 Uiso 1 1 d R . .
O2 O 0.4309(2) 0.7848(5) 0.3283(5) 0.0687(16) Uani 1 1 d . . .
O3 O 0.48444(18) 0.6523(5) 0.3612(4) 0.0606(14) Uani 1 1 d . . .
N1 N 0.3406(2) 0.6125(5) 0.0872(5) 0.0469(15) Uani 1 1 d . . .
C1 C 0.4058(3) 0.5448(8) 0.0236(6) 0.057(2) Uani 1 1 d . . .
C2 C 0.3533(2) 0.5587(6) 0.0056(6) 0.0480(18) Uani 1 1 d . . .
C3 C 0.3206(3) 0.5136(7) -0.0866(6) 0.057(2) Uani 1 1 d . . .
H3 H 0.3295 0.4724 -0.1435 0.068 Uiso 1 1 calc R . .
C4 C 0.2751(3) 0.5306(8) -0.0929(6) 0.061(2) Uani 1 1 d . . .
H4 H 0.2519 0.5038 -0.1568 0.073 Uiso 1 1 calc R . .
C5 C 0.2625(3) 0.5863(6) -0.0073(6) 0.0534(19) Uani 1 1 d . . .
H5 H 0.2299 0.6037 -0.0227 0.064 Uiso 1 1 d R . .
C6 C 0.2952(3) 0.6279(6) 0.0852(6) 0.0481(18) Uani 1 1 d . . .
C7 C 0.2913(2) 0.6914(6) 0.1864(6) 0.0469(17) Uani 1 1 d . . .
C8 C 0.2501(3) 0.7119(6) 0.2178(6) 0.0517(19) Uani 1 1 d . . .
C9 C 0.2053(3) 0.6690(8) 0.1609(8) 0.075(3) Uani 1 1 d . . .
H9 H 0.2003 0.6261 0.1053 0.090 Uiso 1 1 d R . .
C10 C 0.1682(3) 0.6932(10) 0.1960(10) 0.099(4) Uani 1 1 d . . .
H10 H 0.1390 0.6652 0.1537 0.119 Uiso 1 1 calc R . .
C11 C 0.1710(3) 0.7591(9) 0.2941(8) 0.080(3) Uani 1 1 d . . .
H11 H 0.1443 0.7738 0.3182 0.095 Uiso 1 1 calc R . .
C12 C 0.2125(3) 0.8004(8) 0.3523(8) 0.074(3) Uani 1 1 d . . .
H12 H 0.2151 0.8453 0.4179 0.089 Uiso 1 1 calc R . .
C13 C 0.2527(3) 0.7769(7) 0.3157(6) 0.055(2) Uani 1 1 d . . .
C14 C 0.2964(3) 0.8213(7) 0.3807(7) 0.060(2) Uani 1 1 d . . .
H14 H 0.2981 0.8674 0.4449 0.073 Uiso 1 1 calc R . .
C15 C 0.3346(3) 0.7972(6) 0.3501(7) 0.055(2) Uani 1 1 d . . .
H15 H 0.3635 0.8252 0.3943 0.066 Uiso 1 1 calc R . .
C16 C 0.3328(3) 0.7325(6) 0.2557(6) 0.0487(18) Uani 1 1 d . . .
C17 C 0.4185(3) 0.5630(8) -0.0868(7) 0.070(2) Uani 1 1 d . . .
H17A H 0.4058 0.6351 -0.1204 0.105 Uiso 1 1 calc R . .
H17B H 0.4056 0.5018 -0.1397 0.105 Uiso 1 1 calc R . .
H17C H 0.4521 0.5638 -0.0714 0.105 Uiso 1 1 calc R . .
C18 C 0.4211(3) 0.4304(8) 0.0740(7) 0.072(3) Uani 1 1 d . . .
H18A H 0.4548 0.4263 0.0962 0.108 Uiso 1 1 calc R . .
H18B H 0.4084 0.3719 0.0177 0.108 Uiso 1 1 calc R . .
H18C H 0.4099 0.4188 0.1409 0.108 Uiso 1 1 calc R . .
C19 C 0.4710(3) 0.7483(9) 0.3765(7) 0.064(2) Uani 1 1 d . . .
C20 C 0.5011(3) 0.8268(9) 0.4595(10) 0.110(4) Uani 1 1 d . . .
H20A H 0.5316 0.8302 0.4459 0.165 Uiso 1 1 calc R . .
H20B H 0.5043 0.7998 0.5367 0.165 Uiso 1 1 calc R . .
H20C H 0.4873 0.9021 0.4504 0.165 Uiso 1 1 calc R . .
C21 C 0.0987(7) 0.4996(13) 0.8113(11) 0.191(9) Uani 1 1 d . . .
H21A H 0.1253 0.4870 0.7806 0.230 Uiso 1 1 calc R . .
H21B H 0.0822 0.5672 0.7734 0.230 Uiso 1 1 calc R . .
Cl1 Cl 0.11762(13) 0.5247(3) 0.9436(3) 0.1371(13) Uani 1 1 d . . .
Cl2 Cl 0.06085(11) 0.3811(5) 0.7751(4) 0.178(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0390(4) 0.0619(4) 0.0490(4) -0.0106(3) 0.0083(2) -0.0003(3)
O1 0.039(3) 0.115(5) 0.079(4) -0.032(4) 0.024(3) -0.011(3)
O2 0.048(4) 0.072(4) 0.078(4) -0.021(3) 0.002(3) 0.001(3)
O3 0.043(3) 0.082(4) 0.056(3) -0.008(3) 0.013(3) 0.001(3)
N1 0.045(4) 0.058(4) 0.039(3) -0.002(3) 0.015(3) 0.000(3)
C1 0.044(5) 0.078(6) 0.049(4) -0.012(4) 0.013(4) -0.002(4)
C2 0.038(4) 0.061(5) 0.043(4) -0.004(4) 0.007(3) 0.002(3)
C3 0.056(5) 0.070(6) 0.046(4) -0.013(4) 0.015(4) -0.005(4)
C4 0.049(5) 0.084(6) 0.041(4) -0.009(4) -0.003(4) -0.010(4)
C5 0.040(4) 0.068(5) 0.049(4) -0.004(4) 0.007(3) -0.002(4)
C6 0.045(4) 0.055(5) 0.042(4) 0.003(4) 0.009(3) 0.004(3)
C7 0.046(4) 0.049(4) 0.045(4) 0.005(4) 0.011(3) 0.008(4)
C8 0.054(5) 0.054(5) 0.045(4) 0.006(4) 0.010(4) 0.010(4)
C9 0.049(5) 0.107(8) 0.075(6) -0.026(5) 0.025(4) -0.005(5)
C10 0.045(6) 0.143(10) 0.113(9) -0.023(8) 0.030(6) -0.014(6)
C11 0.060(6) 0.108(8) 0.081(7) -0.010(6) 0.038(5) 0.002(6)
C12 0.059(6) 0.094(7) 0.071(6) 0.000(5) 0.022(5) 0.015(5)
C13 0.055(5) 0.066(5) 0.045(4) 0.009(4) 0.015(4) 0.015(4)
C14 0.057(5) 0.072(6) 0.050(5) -0.005(4) 0.011(4) 0.015(4)
C15 0.047(5) 0.056(5) 0.061(5) -0.013(4) 0.012(4) 0.001(4)
C16 0.047(5) 0.050(5) 0.044(4) -0.003(3) 0.004(3) 0.003(3)
C17 0.045(5) 0.096(7) 0.073(6) -0.013(5) 0.022(4) -0.002(5)
C18 0.044(5) 0.099(7) 0.076(6) 0.003(5) 0.022(4) 0.006(5)
C19 0.048(5) 0.080(7) 0.063(5) -0.018(5) 0.012(4) -0.007(5)
C20 0.063(7) 0.101(9) 0.134(10) -0.052(7) -0.025(6) -0.005(6)
C21 0.35(3) 0.091(10) 0.101(10) -0.014(8) 0.001(13) 0.012(13)
Cl1 0.129(3) 0.145(3) 0.108(2) 0.016(2) -0.016(2) 0.005(2)
Cl2 0.0546(19) 0.272(6) 0.192(4) -0.091(4) 0.011(2) -0.011(3)
_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 N1 1.952(6) . ?
Pd1 C16 1.957(7) . ?
Pd1 O2 2.040(5) . ?
Pd1 O1 2.139(5) . ?
O1 C1 1.422(9) . ?
O1 H1 0.8790 . ?
O2 C19 1.267(10) . ?
O3 C19 1.243(10) . ?
N1 C2 1.332(9) . ?
N1 C6 1.375(9) . ?
C1 C18 1.512(12) . ?
C1 C17 1.524(10) . ?
C1 C2 1.549(10) . ?
C2 C3 1.386(10) . ?
C3 C4 1.373(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(10) . ?
C5 H5 0.9724 . ?
C6 C7 1.487(10) . ?
C7 C16 1.393(10) . ?
C7 C8 1.423(10) . ?
C8 C13 1.413(10) . ?
C8 C9 1.434(11) . ?
C9 C10 1.337(12) . ?
C9 H9 0.8324 . ?
C10 C11 1.421(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.351(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.435(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.439(11) . ?
C14 C15 1.343(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(10) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.490(12) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 Cl1 1.594(12) . ?
C21 Cl2 1.790(17) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
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 Pd1 C16 82.5(3) . . ?
N1 Pd1 O2 174.8(2) . . ?
C16 Pd1 O2 93.6(3) . . ?
N1 Pd1 O1 78.4(2) . . ?
C16 Pd1 O1 160.2(3) . . ?
O2 Pd1 O1 105.1(2) . . ?
C1 O1 Pd1 114.3(4) . . ?
C1 O1 H1 116.2 . . ?
Pd1 O1 H1 124.9 . . ?
C19 O2 Pd1 120.0(6) . . ?
C2 N1 C6 123.0(6) . . ?
C2 N1 Pd1 119.7(5) . . ?
C6 N1 Pd1 116.8(5) . . ?
O1 C1 C18 110.0(7) . . ?
O1 C1 C17 108.0(7) . . ?
C18 C1 C17 111.7(7) . . ?
O1 C1 C2 106.2(6) . . ?
C18 C1 C2 109.7(7) . . ?
C17 C1 C2 111.1(6) . . ?
N1 C2 C3 120.7(7) . . ?
N1 C2 C1 116.3(6) . . ?
C3 C2 C1 122.9(7) . . ?
C4 C3 C2 117.6(7) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 120.8(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 121.0(7) . . ?
C6 C5 H5 122.8 . . ?
C4 C5 H5 115.6 . . ?
C5 C6 N1 116.8(6) . . ?
C5 C6 C7 131.9(7) . . ?
N1 C6 C7 111.3(6) . . ?
C16 C7 C8 118.7(7) . . ?
C16 C7 C6 114.9(6) . . ?
C8 C7 C6 126.4(7) . . ?
C13 C8 C7 118.7(7) . . ?
C13 C8 C9 115.4(7) . . ?
C7 C8 C9 125.9(7) . . ?
C10 C9 C8 121.9(9) . . ?
C10 C9 H9 114.9 . . ?
C8 C9 H9 123.2 . . ?
C9 C10 C11 122.4(9) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 118.4(9) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C11 C12 C13 120.4(9) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 121.5(8) . . ?
C8 C13 C14 119.7(7) . . ?
C12 C13 C14 118.7(8) . . ?
C15 C14 C13 119.7(7) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 121.1(8) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C7 122.0(7) . . ?
C15 C16 Pd1 124.1(6) . . ?
C7 C16 Pd1 114.0(5) . . ?
C1 C17 H17A 109.5 . . ?
C1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C18 H18A 109.5 . . ?
C1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 O2 123.6(8) . . ?
O3 C19 C20 120.9(9) . . ?
O2 C19 C20 115.4(9) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cl1 C21 Cl2 115.0(10) . . ?
Cl1 C21 H21A 108.5 . . ?
Cl2 C21 H21A 108.5 . . ?
Cl1 C21 H21B 108.5 . . ?
Cl2 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
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
N1 Pd1 O1 C1 -16.2(5) . . . . ?
C16 Pd1 O1 C1 -31.4(11) . . . . ?
O2 Pd1 O1 C1 167.8(5) . . . . ?
C16 Pd1 O2 C19 141.9(7) . . . . ?
O1 Pd1 O2 C19 -44.5(7) . . . . ?
C16 Pd1 N1 C2 177.4(6) . . . . ?
O1 Pd1 N1 C2 2.5(6) . . . . ?
C16 Pd1 N1 C6 5.1(5) . . . . ?
O1 Pd1 N1 C6 -169.7(6) . . . . ?
Pd1 O1 C1 C18 -94.9(6) . . . . ?
Pd1 O1 C1 C17 143.0(5) . . . . ?
Pd1 O1 C1 C2 23.8(7) . . . . ?
C6 N1 C2 C3 -0.7(11) . . . . ?
Pd1 N1 C2 C3 -172.5(6) . . . . ?
C6 N1 C2 C1 -177.7(7) . . . . ?
Pd1 N1 C2 C1 10.6(9) . . . . ?
O1 C1 C2 N1 -22.6(9) . . . . ?
C18 C1 C2 N1 96.3(8) . . . . ?
C17 C1 C2 N1 -139.8(7) . . . . ?
O1 C1 C2 C3 160.6(7) . . . . ?
C18 C1 C2 C3 -80.6(9) . . . . ?
C17 C1 C2 C3 43.4(11) . . . . ?
N1 C2 C3 C4 2.7(12) . . . . ?
C1 C2 C3 C4 179.4(8) . . . . ?
C2 C3 C4 C5 -2.9(12) . . . . ?
C3 C4 C5 C6 1.2(13) . . . . ?
C4 C5 C6 N1 0.8(11) . . . . ?
C4 C5 C6 C7 178.9(8) . . . . ?
C2 N1 C6 C5 -1.1(11) . . . . ?
Pd1 N1 C6 C5 170.9(5) . . . . ?
C2 N1 C6 C7 -179.5(6) . . . . ?
Pd1 N1 C6 C7 -7.5(8) . . . . ?
C5 C6 C7 C16 -171.8(8) . . . . ?
N1 C6 C7 C16 6.4(9) . . . . ?
C5 C6 C7 C8 8.9(13) . . . . ?
N1 C6 C7 C8 -172.9(7) . . . . ?
C16 C7 C8 C13 2.4(11) . . . . ?
C6 C7 C8 C13 -178.3(7) . . . . ?
C16 C7 C8 C9 -175.2(8) . . . . ?
C6 C7 C8 C9 4.1(13) . . . . ?
C13 C8 C9 C10 2.7(14) . . . . ?
C7 C8 C9 C10 -179.6(9) . . . . ?
C8 C9 C10 C11 -2.6(17) . . . . ?
C9 C10 C11 C12 1.4(18) . . . . ?
C10 C11 C12 C13 -0.5(15) . . . . ?
C7 C8 C13 C12 -179.8(7) . . . . ?
C9 C8 C13 C12 -1.9(12) . . . . ?
C7 C8 C13 C14 0.4(11) . . . . ?
C9 C8 C13 C14 178.3(7) . . . . ?
C11 C12 C13 C8 0.9(13) . . . . ?
C11 C12 C13 C14 -179.3(9) . . . . ?
C8 C13 C14 C15 -2.4(12) . . . . ?
C12 C13 C14 C15 177.8(8) . . . . ?
C13 C14 C15 C16 1.5(12) . . . . ?
C14 C15 C16 C7 1.5(12) . . . . ?
C14 C15 C16 Pd1 -178.9(6) . . . . ?
C8 C7 C16 C15 -3.5(11) . . . . ?
C6 C7 C16 C15 177.2(7) . . . . ?
C8 C7 C16 Pd1 176.9(5) . . . . ?
C6 C7 C16 Pd1 -2.4(8) . . . . ?
N1 Pd1 C16 C15 179.1(7) . . . . ?
O2 Pd1 C16 C15 -4.4(7) . . . . ?
O1 Pd1 C16 C15 -165.9(7) . . . . ?
N1 Pd1 C16 C7 -1.3(5) . . . . ?
O2 Pd1 C16 C7 175.2(6) . . . . ?
O1 Pd1 C16 C7 13.7(12) . . . . ?
Pd1 O2 C19 O3 -6.6(12) . . . . ?
Pd1 O2 C19 C20 176.6(7) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O3 0.88 1.71 2.588(7) 172.7 2_655
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.126