# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H16 N6 O6 Pd S2'
_chemical_formula_weight         630.93

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'
S S 0.1246 0.1234 '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/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                   8.0530(3)
_cell_length_b                   9.7220(4)
_cell_length_c                   16.0510(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.788(2)
_cell_angle_gamma                90.00
_cell_volume                     1247.84(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7950
_exptl_absorpt_correction_T_max  0.8692
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  ?
_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            10326
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2890
_reflns_number_gt                1945
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2890
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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
O1 O 0.3839(4) 0.1226(4) 0.0267(2) 0.0562(8) Uani 1 1 d . . .
O2 O -0.0680(4) 0.2671(4) 0.1455(2) 0.0705(11) Uani 1 1 d . . .
O3 O 0.0265(5) 0.0622(5) 0.2235(2) 0.0787(12) Uani 1 1 d . . .
N2 N 0.1144(5) -0.1748(4) 0.0413(2) 0.0445(8) Uani 1 1 d . . .
N3 N 0.0186(6) -0.2652(5) 0.0739(3) 0.0687(13) Uani 1 1 d . . .
C11 C 0.2722(6) -0.1998(5) 0.0319(3) 0.0526(11) Uani 1 1 d . . .
H11 H 0.3345 -0.1320 0.0090 0.063 Uiso 1 1 calc R . .
C10 C 0.3467(8) -0.3233(6) 0.0549(4) 0.0750(16) Uani 1 1 d . . .
H10 H 0.4576 -0.3411 0.0478 0.090 Uiso 1 1 calc R . .
C9 C 0.2501(9) -0.4183(7) 0.0888(4) 0.088(2) Uani 1 1 d . . .
H9 H 0.2941 -0.5034 0.1062 0.106 Uiso 1 1 calc R . .
C8 C 0.0860(10) -0.3863(6) 0.0968(4) 0.0833(19) Uani 1 1 d . . .
H8 H 0.0199 -0.4519 0.1192 0.100 Uiso 1 1 calc R . .
Pd1 Pd 0.0000 0.0000 0.0000 0.03572(17) Uani 1 2 d S . .
S1 S 0.06360(14) 0.17205(12) 0.17043(7) 0.0461(3) Uani 1 1 d . . .
N1 N 0.1425(4) 0.1115(4) 0.0882(2) 0.0414(8) Uani 1 1 d . . .
C2 C 0.3678(5) 0.2365(4) 0.1588(3) 0.0405(9) Uani 1 1 d . . .
C7 C 0.2480(5) 0.2586(4) 0.2118(3) 0.0404(9) Uani 1 1 d . . .
C1 C 0.3034(5) 0.1519(4) 0.0837(3) 0.0425(10) Uani 1 1 d . . .
C4 C 0.5551(7) 0.3708(6) 0.2504(3) 0.0642(14) Uani 1 1 d . . .
H4 H 0.6603 0.4093 0.2647 0.077 Uiso 1 1 calc R . .
C3 C 0.5250(6) 0.2929(5) 0.1786(3) 0.0534(12) Uani 1 1 d . . .
H3 H 0.6085 0.2787 0.1441 0.064 Uiso 1 1 calc R . .
C6 C 0.2762(6) 0.3353(5) 0.2843(3) 0.0524(11) Uani 1 1 d . . .
H6 H 0.1941 0.3478 0.3197 0.063 Uiso 1 1 calc R . .
C5 C 0.4325(7) 0.3923(6) 0.3012(3) 0.0635(14) Uani 1 1 d . . .
H5 H 0.4558 0.4472 0.3486 0.076 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
O1 0.0378(17) 0.067(2) 0.0659(19) -0.0164(16) 0.0165(15) -0.0025(15)
O2 0.0376(17) 0.092(3) 0.080(2) -0.035(2) -0.0019(17) 0.0172(19)
O3 0.098(3) 0.080(3) 0.061(2) -0.007(2) 0.023(2) -0.045(3)
N2 0.043(2) 0.041(2) 0.0491(19) -0.0010(17) 0.0047(15) -0.0006(17)
N3 0.082(3) 0.056(3) 0.075(3) 0.018(2) 0.038(2) 0.009(2)
C11 0.041(3) 0.055(3) 0.061(3) 0.002(2) 0.003(2) 0.006(2)
C10 0.064(4) 0.067(4) 0.092(4) 0.013(3) 0.005(3) 0.022(3)
C9 0.100(5) 0.063(4) 0.103(5) 0.025(4) 0.015(4) 0.028(4)
C8 0.117(6) 0.056(4) 0.082(4) 0.024(3) 0.035(4) 0.010(4)
Pd1 0.0303(2) 0.0345(3) 0.0421(3) -0.00412(19) 0.00299(17) 0.0001(2)
S1 0.0358(6) 0.0541(7) 0.0489(6) -0.0125(5) 0.0070(4) -0.0090(5)
N1 0.0345(18) 0.043(2) 0.0467(19) -0.0081(16) 0.0036(14) -0.0008(15)
C2 0.035(2) 0.034(2) 0.051(2) 0.0014(18) -0.0015(18) 0.0007(17)
C7 0.034(2) 0.036(2) 0.049(2) -0.0024(18) -0.0042(17) -0.0007(18)
C1 0.034(2) 0.038(2) 0.055(2) -0.0011(19) 0.0011(19) 0.0038(18)
C4 0.043(3) 0.065(3) 0.080(3) -0.010(3) -0.011(2) -0.013(2)
C3 0.037(2) 0.059(3) 0.063(3) -0.003(2) 0.000(2) -0.002(2)
C6 0.048(3) 0.050(3) 0.057(3) -0.010(2) -0.003(2) 0.001(2)
C5 0.059(3) 0.061(3) 0.067(3) -0.018(2) -0.008(2) -0.008(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
O1 C1 1.215(5) . ?
O2 S1 1.427(4) . ?
O3 S1 1.420(4) . ?
N2 N3 1.318(5) . ?
N2 C11 1.320(6) . ?
N2 Pd1 2.008(4) . ?
N3 C8 1.330(7) . ?
C11 C10 1.373(7) . ?
C10 C9 1.361(8) . ?
C9 C8 1.379(9) . ?
Pd1 N2 2.008(4) 3 ?
Pd1 N1 2.028(3) 3 ?
Pd1 N1 2.028(3) . ?
S1 N1 1.640(3) . ?
S1 C7 1.767(4) . ?
N1 C1 1.365(5) . ?
C2 C3 1.382(6) . ?
C2 C7 1.377(6) . ?
C2 C1 1.500(6) . ?
C7 C6 1.377(6) . ?
C4 C5 1.368(7) . ?
C4 C3 1.377(7) . ?
C6 C5 1.373(7) . ?

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
N3 N2 C11 122.6(4) . . ?
N3 N2 Pd1 115.3(3) . . ?
C11 N2 Pd1 121.9(3) . . ?
N2 N3 C8 117.4(5) . . ?
N2 C11 C10 121.8(5) . . ?
C9 C10 C11 116.7(5) . . ?
C10 C9 C8 118.9(6) . . ?
N3 C8 C9 122.6(6) . . ?
N2 Pd1 N2 180.0(3) . 3 ?
N2 Pd1 N1 88.74(14) . 3 ?
N2 Pd1 N1 91.26(14) 3 3 ?
N2 Pd1 N1 91.26(14) . . ?
N2 Pd1 N1 88.74(14) 3 . ?
N1 Pd1 N1 180.0(2) 3 . ?
O3 S1 O2 117.0(3) . . ?
O3 S1 N1 110.0(2) . . ?
O2 S1 N1 110.6(2) . . ?
O3 S1 C7 111.1(2) . . ?
O2 S1 C7 111.1(2) . . ?
N1 S1 C7 94.90(19) . . ?
C1 N1 S1 113.6(3) . . ?
C1 N1 Pd1 125.4(3) . . ?
S1 N1 Pd1 120.84(19) . . ?
C3 C2 C7 119.1(4) . . ?
C3 C2 C1 128.5(4) . . ?
C7 C2 C1 112.5(3) . . ?
C6 C7 C2 123.3(4) . . ?
C6 C7 S1 128.5(3) . . ?
C2 C7 S1 108.2(3) . . ?
O1 C1 N1 124.5(4) . . ?
O1 C1 C2 124.7(4) . . ?
N1 C1 C2 110.8(4) . . ?
C5 C4 C3 121.0(5) . . ?
C4 C3 C2 118.4(4) . . ?
C5 C6 C7 116.2(4) . . ?
C4 C5 C6 122.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         0.572
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.244
_database_code_depnum_ccdc_archive 'CCDC 982563'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_s_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H10 N O3 Pd0.50 S2'
_chemical_formula_weight         297.50

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'
S S 0.1246 0.1234 '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                   8.3977(14)
_cell_length_b                   11.2186(18)
_cell_length_c                   12.207(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.288(5)
_cell_angle_gamma                90.00
_cell_volume                     1091.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6790
_exptl_absorpt_correction_T_max  0.7851
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  ?
_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            28341
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         28.38
_reflns_number_total             2725
_reflns_number_gt                2542
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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)+(0.1017P)²+10.0682P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2725
_refine_ls_number_parameters     142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1752
_refine_ls_wR_factor_gt          0.1692
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_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 0.5000 0.5000 0.5000 0.00807(19) Uani 1 2 d S . .
S1 S 0.50477(15) 0.51786(10) 0.76249(10) 0.0121(3) Uani 1 1 d . . .
N1 N 0.5563(5) 0.5803(3) 0.6569(3) 0.0117(7) Uani 1 1 d . . .
C1 C 0.5968(5) 0.6988(4) 0.6757(4) 0.0125(8) Uani 1 1 d . . .
C2 C 0.5819(5) 0.7397(4) 0.7890(4) 0.0122(8) Uani 1 1 d . . .
C3 C 0.6112(6) 0.8518(4) 0.8362(4) 0.0156(9) Uani 1 1 d . . .
H3 H 0.6432 0.9139 0.7971 0.019 Uiso 1 1 calc R . .
C6 C 0.5113(6) 0.6647(5) 0.9551(4) 0.0181(9) Uani 1 1 d . . .
H6 H 0.4779 0.6028 0.9936 0.022 Uiso 1 1 calc R . .
C7 C 0.5311(6) 0.6481(4) 0.8472(4) 0.0130(8) Uani 1 1 d . . .
C5 C 0.5437(7) 0.7785(5) 1.0027(4) 0.0198(10) Uani 1 1 d . . .
H5 H 0.5329 0.7929 1.0751 0.024 Uiso 1 1 calc R . .
O2 O 0.3328(5) 0.4787(3) 0.7216(3) 0.0194(7) Uani 1 1 d . . .
O1 O 0.6389(5) 0.7626(3) 0.6086(3) 0.0202(7) Uani 1 1 d . . .
O3 O 0.6258(5) 0.4293(3) 0.8203(3) 0.0231(8) Uani 1 1 d . . .
C4 C 0.5916(6) 0.8701(5) 0.9443(4) 0.0185(9) Uani 1 1 d . . .
H4 H 0.6113 0.9454 0.9777 0.022 Uiso 1 1 calc R . .
S2 S 0.2726(6) 0.5869(4) 0.4587(4) 0.1048(12) Uani 1 1 d . . .
C8 C 0.2710(7) 0.6998(5) 0.3945(5) 0.0206(10) Uani 1 1 d . . .
H8A H 0.3646 0.7483 0.4362 0.031 Uiso 1 1 calc R . .
H8B H 0.1685 0.7419 0.3865 0.031 Uiso 1 1 calc R . .
H8C H 0.2790 0.6820 0.3195 0.031 Uiso 1 1 calc R . .
C9 C 0.1276(7) 0.5117(5) 0.3955(6) 0.0258(12) Uani 1 1 d . . .
H9A H 0.1292 0.4391 0.4375 0.039 Uiso 1 1 calc R . .
H9B H 0.1345 0.4934 0.3203 0.039 Uiso 1 1 calc R . .
H9C H 0.0253 0.5540 0.3879 0.039 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 0.0111(3) 0.0079(3) 0.0055(3) -0.00071(13) 0.00321(18) 0.00009(14)
S1 0.0192(6) 0.0103(5) 0.0081(5) 0.0003(4) 0.0060(4) 0.0013(4)
N1 0.0160(18) 0.0119(18) 0.0080(16) -0.0008(13) 0.0051(14) -0.0018(14)
C1 0.0118(19) 0.015(2) 0.0098(18) -0.0034(16) 0.0022(15) -0.0031(15)
C2 0.0113(18) 0.016(2) 0.0084(18) -0.0028(15) 0.0020(15) -0.0005(16)
C3 0.015(2) 0.015(2) 0.015(2) -0.0028(17) 0.0030(16) -0.0005(17)
C6 0.023(2) 0.021(2) 0.012(2) -0.0002(17) 0.0072(17) 0.0008(18)
C7 0.0144(19) 0.014(2) 0.0105(19) -0.0015(16) 0.0036(16) 0.0005(16)
C5 0.022(2) 0.027(3) 0.011(2) -0.0060(18) 0.0067(17) 0.003(2)
O2 0.0242(19) 0.0162(16) 0.0215(18) -0.0050(14) 0.0126(15) -0.0072(14)
O1 0.0309(19) 0.0184(17) 0.0144(16) -0.0021(13) 0.0114(14) -0.0071(15)
O3 0.038(2) 0.0179(18) 0.0126(16) 0.0043(13) 0.0068(15) 0.0117(15)
C4 0.017(2) 0.021(2) 0.016(2) -0.0097(18) 0.0027(17) 0.0006(18)
S2 0.106(3) 0.099(3) 0.108(3) 0.002(2) 0.030(2) 0.005(2)
C8 0.025(2) 0.017(2) 0.022(2) 0.0025(19) 0.0104(19) 0.0075(19)
C9 0.016(2) 0.023(3) 0.036(3) -0.008(2) 0.005(2) 0.0007(18)

_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 2.033(4) 3_666 ?
Pd1 N1 2.033(4) . ?
Pd1 S2 2.061(4) 3_666 ?
Pd1 S2 2.061(4) . ?
S1 O3 1.439(4) . ?
S1 O2 1.441(4) . ?
S1 N1 1.640(4) . ?
S1 C7 1.763(5) . ?
N1 C1 1.373(6) . ?
C1 O1 1.221(6) . ?
C1 C2 1.499(6) . ?
C2 C3 1.373(6) . ?
C2 C7 1.390(6) . ?
C3 C4 1.396(7) . ?
C6 C7 1.390(6) . ?
C6 C5 1.393(7) . ?
C5 C4 1.381(8) . ?
S2 C9 1.483(7) . ?
S2 C8 1.487(7) . ?

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 N1 180.000(1) 3_666 . ?
N1 Pd1 S2 86.83(17) 3_666 3_666 ?
N1 Pd1 S2 93.17(17) . 3_666 ?
N1 Pd1 S2 93.17(17) 3_666 . ?
N1 Pd1 S2 86.83(17) . . ?
S2 Pd1 S2 180.000(1) 3_666 . ?
O3 S1 O2 115.9(3) . . ?
O3 S1 N1 111.2(2) . . ?
O2 S1 N1 110.0(2) . . ?
O3 S1 C7 110.2(2) . . ?
O2 S1 C7 112.5(2) . . ?
N1 S1 C7 95.3(2) . . ?
C1 N1 S1 113.2(3) . . ?
C1 N1 Pd1 124.0(3) . . ?
S1 N1 Pd1 120.7(2) . . ?
O1 C1 N1 124.4(4) . . ?
O1 C1 C2 124.4(4) . . ?
N1 C1 C2 111.3(4) . . ?
C3 C2 C7 120.4(4) . . ?
C3 C2 C1 127.7(4) . . ?
C7 C2 C1 111.9(4) . . ?
C2 C3 C4 118.3(5) . . ?
C7 C6 C5 116.9(5) . . ?
C6 C7 C2 122.1(4) . . ?
C6 C7 S1 129.5(4) . . ?
C2 C7 S1 108.3(3) . . ?
C4 C5 C6 121.1(4) . . ?
C5 C4 C3 121.2(5) . . ?
C9 S2 C8 109.9(4) . . ?
C9 S2 Pd1 113.9(3) . . ?
C8 S2 Pd1 112.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.609
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.235
_database_code_depnum_ccdc_archive 'CCDC 982564'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H22 N2 O8 Pd S4'
_chemical_formula_weight         629.02

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmc21

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

_cell_length_a                   22.245(2)
_cell_length_b                   13.6954(14)
_cell_length_c                   7.5899(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2312.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7355
_exptl_absorpt_correction_T_max  0.9419
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  ?
_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            13931
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         28.77
_reflns_number_total             2885
_reflns_number_gt                2777
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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)+(0.0623P)²+4.9696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_number_reflns         2885
_refine_ls_number_parameters     161
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.064
_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
C2 C 0.31167(17) 0.0692(3) 0.0423(6) 0.0185(8) Uani 1 1 d . . .
C1 C 0.37772(19) 0.0576(3) 0.0115(5) 0.0193(9) Uani 1 1 d . . .
C4 C 0.2084(2) 0.0275(4) 0.0478(10) 0.0308(10) Uani 1 1 d . . .
H4 H 0.1775 -0.0165 0.0256 0.037 Uiso 1 1 calc R . .
C7 C 0.2975(2) 0.1605(3) 0.1127(6) 0.0211(9) Uani 1 1 d . . .
C6 C 0.2396(2) 0.1870(4) 0.1516(6) 0.0264(10) Uani 1 1 d . . .
H6 H 0.2306 0.2480 0.1985 0.032 Uiso 1 1 calc R . .
C3 C 0.26714(19) 0.0004(4) 0.0100(6) 0.0236(9) Uani 1 1 d . . .
H3 H 0.2762 -0.0610 -0.0350 0.028 Uiso 1 1 calc R . .
C5 C 0.1946(2) 0.1180(4) 0.1176(7) 0.0306(11) Uani 1 1 d . . .
H5 H 0.1548 0.1333 0.1423 0.037 Uiso 1 1 calc R . .
Pd1 Pd 0.5000 0.14412(3) 0.06088(6) 0.01604(12) Uani 1 2 d S . .
S2 S 0.5000 0.23937(11) -0.1780(2) 0.0206(3) Uani 1 2 d S . .
S1 S 0.36465(5) 0.22686(8) 0.13703(14) 0.0197(2) Uani 1 1 d . . .
N1 N 0.40904(14) 0.1380(2) 0.0646(9) 0.0194(6) Uani 1 1 d . . .
O5 O 0.5000 0.0512(4) 0.2732(7) 0.0330(13) Uani 1 2 d S . .
S4 S 0.5000 0.3980(2) -0.7165(4) 0.0587(7) Uani 1 2 d S . .
O3 O 0.36602(15) 0.3073(2) 0.0150(4) 0.0275(8) Uani 1 1 d . . .
O1 O 0.39916(13) -0.0155(2) -0.0552(4) 0.0246(7) Uani 1 1 d . . .
O2 O 0.37646(15) 0.2496(3) 0.3173(5) 0.0282(7) Uani 1 1 d . . .
C8 C 0.4396(2) 0.2007(4) -0.3162(6) 0.0254(10) Uani 1 1 d . . .
H8A H 0.4020 0.2159 -0.2606 0.038 Uiso 1 1 calc R . .
H8B H 0.4423 0.1315 -0.3348 0.038 Uiso 1 1 calc R . .
H8C H 0.4421 0.2338 -0.4274 0.038 Uiso 1 1 calc R . .
O6 O 0.5000 0.3737(6) -0.5222(14) 0.081(3) Uani 1 2 d S . .
C9 C 0.5605(3) 0.4829(9) -0.728(2) 0.118(6) Uani 1 1 d . . .
H9A H 0.5980 0.4483 -0.7242 0.177 Uiso 1 1 calc R . .
H9B H 0.5582 0.5271 -0.6304 0.177 Uiso 1 1 calc R . .
H9C H 0.5579 0.5189 -0.8364 0.177 Uiso 1 1 calc R . .
H50 H 0.467(2) 0.049(4) 0.322(10) 0.031(15) Uiso 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
C2 0.0174(17) 0.0267(19) 0.012(2) 0.0005(18) -0.0006(17) 0.0043(14)
C1 0.0169(19) 0.025(2) 0.016(2) 0.0046(15) -0.0004(13) 0.0002(16)
C4 0.0211(19) 0.043(2) 0.029(3) -0.005(3) -0.001(2) -0.0050(17)
C7 0.018(2) 0.029(2) 0.016(2) 0.0006(15) -0.0036(14) 0.0028(16)
C6 0.026(2) 0.030(2) 0.023(2) -0.0005(19) 0.0020(18) 0.0093(19)
C3 0.021(2) 0.027(2) 0.022(2) -0.0026(16) 0.0028(15) -0.0023(17)
C5 0.012(2) 0.044(3) 0.036(3) 0.004(2) 0.0001(17) 0.0044(18)
Pd1 0.01317(18) 0.0213(2) 0.01364(18) 0.0016(2) 0.000 0.000
S2 0.0225(7) 0.0233(7) 0.0160(7) 0.0027(6) 0.000 0.000
S1 0.0173(5) 0.0233(5) 0.0186(5) -0.0024(4) -0.0008(4) 0.0029(4)
N1 0.0170(14) 0.0213(14) 0.0198(14) 0.0037(17) 0.001(2) 0.0021(12)
O5 0.018(3) 0.056(4) 0.026(3) 0.019(2) 0.000 0.000
S4 0.0312(11) 0.0703(17) 0.0745(19) 0.0177(15) 0.000 0.000
O3 0.0302(17) 0.0247(17) 0.028(2) 0.0029(13) 0.0038(12) 0.0014(13)
O1 0.0172(15) 0.0271(17) 0.0296(17) -0.0059(13) 0.0061(12) 0.0006(13)
O2 0.0297(17) 0.0327(18) 0.0222(16) -0.0074(14) -0.0074(14) 0.0012(15)
C8 0.025(2) 0.034(3) 0.017(2) 0.0017(18) -0.0045(16) -0.0040(19)
O6 0.084(6) 0.075(5) 0.084(6) 0.023(5) 0.000 0.000
C9 0.038(4) 0.125(9) 0.190(16) 0.092(10) 0.001(6) -0.013(6)

_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
C2 C3 1.388(6) . ?
C2 C7 1.396(6) . ?
C2 C1 1.496(5) . ?
C1 O1 1.220(5) . ?
C1 N1 1.363(6) . ?
C4 C5 1.382(7) . ?
C4 C3 1.388(6) . ?
C7 C6 1.370(6) . ?
C7 S1 1.759(5) . ?
C6 C5 1.400(7) . ?
Pd1 N1 2.025(3) 3_655 ?
Pd1 N1 2.025(3) . ?
Pd1 O5 2.053(5) . ?
Pd1 S2 2.2339(16) . ?
S2 C8 1.785(5) 3_655 ?
S2 C8 1.785(5) . ?
S1 O2 1.428(3) . ?
S1 O3 1.440(3) . ?
S1 N1 1.661(4) . ?
S4 O6 1.511(10) . ?
S4 C9 1.781(9) . ?
S4 C9 1.781(9) 3_655 ?

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 C2 C7 120.9(4) . . ?
C3 C2 C1 127.0(4) . . ?
C7 C2 C1 112.1(4) . . ?
O1 C1 N1 125.9(4) . . ?
O1 C1 C2 122.4(4) . . ?
N1 C1 C2 111.8(4) . . ?
C5 C4 C3 121.8(4) . . ?
C6 C7 C2 122.2(4) . . ?
C6 C7 S1 129.7(4) . . ?
C2 C7 S1 108.1(3) . . ?
C7 C6 C5 116.9(5) . . ?
C2 C3 C4 117.0(4) . . ?
C4 C5 C6 121.2(4) . . ?
N1 Pd1 N1 175.0(2) 3_655 . ?
N1 Pd1 O5 87.89(16) 3_655 . ?
N1 Pd1 O5 87.89(16) . . ?
N1 Pd1 S2 92.04(16) 3_655 . ?
N1 Pd1 S2 92.04(16) . . ?
O5 Pd1 S2 177.44(17) . . ?
C8 S2 C8 97.7(3) 3_655 . ?
C8 S2 Pd1 107.67(16) 3_655 . ?
C8 S2 Pd1 107.67(16) . . ?
O2 S1 O3 116.4(2) . . ?
O2 S1 N1 111.6(3) . . ?
O3 S1 N1 109.6(2) . . ?
O2 S1 C7 111.7(2) . . ?
O3 S1 C7 110.2(2) . . ?
N1 S1 C7 95.25(19) . . ?
C1 N1 S1 112.7(3) . . ?
C1 N1 Pd1 122.7(3) . . ?
S1 N1 Pd1 124.6(2) . . ?
O6 S4 C9 101.1(6) . . ?
O6 S4 C9 101.1(6) . 3_655 ?
C9 S4 C9 98.2(7) . 3_655 ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.133
_database_code_depnum_ccdc_archive 'CCDC 982565'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_J35

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C26 H20 N6 O8 Pd S2'
_chemical_formula_weight         715.02

_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
pd 19.33190 0.69866 15.50170 7.98929 5.29537 25.20520 0.60584 76.89860 5.26593
-1.17700 1.00700
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.00800 0.00600
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.00400 0.00300
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.00200 0.00200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
s 6.90530 1.46790 5.20340 22.21510 1.43790 0.25360 1.58630 56.17200 0.86690
0.11000 0.12400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y+1/2,-z+1/2
-x,-y,-z
x,-y+1/2,z+1/2

_cell_length_a                   12.03223(12)
_cell_length_b                   14.00604(15)
_cell_length_c                   9.78155(10)
_cell_angle_alpha                90.00000
_cell_angle_beta                 110.8723(13)
_cell_angle_gamma                90.00000
_cell_volume                     1540.25(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_exptl_crystal_density_diffrn    1.542
_cell_special_details            
; ?
;

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                'borosilicate capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; SpLine - BM25, Spanish Beamline at the ESRF (Grenoble, France)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_type           synchrotron
_diffrn_source                   Synchrotron
_diffrn_measurement_device_type  'SpLine-BM25 Powder Diffractometer'
_diffrn_radiation_wavelength     0.82690
_diffrn_radiation_monochromator  Si(111)
_diffrn_measurement_method       '2θ scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'scintillation counter'
_diffrn_detector_type            Cyberstar
_pd_meas_scan_method             step
_pd_meas_special_details         
;  ?
;
#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        3133
_pd_meas_2theta_range_min        2.99931
_pd_meas_2theta_range_max        49.98557
_pd_meas_2theta_range_inc        0.015002


_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_refine_ls_hydrogen_treatment    mixed
_pd_proc_ls_profile_function     'Thompson-Cox-Hasting Pseudo-Voigt'
_pd_proc_ls_background_function  'Interpolation of points'
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        6.5382
_pd_proc_ls_prof_wR_factor       8.6666
_pd_proc_ls_prof_wR_expected     3.2776

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       10.0764
_pd_proc_ls_prof_cwR_factor      11.9037
_pd_proc_ls_prof_cwR_expected    4.5019

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            6.9917
_pd_proc_ls_prof_echi2           7.1172
_refine_ls_goodness_of_fit_all   2.6442

#  Items related to LS refinement

_refine_ls_R_I_factor            3.7832
_refine_ls_number_reflns         1881
_refine_ls_number_parameters     94
_refine_ls_number_restraints     1

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.9991
_pd_proc_2theta_range_max        49.9854
_pd_proc_2theta_range_inc        0.015002
_pd_proc_wavelength              0.826900

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Pd 0.50000 0.50000 0.50000 0.111(2) 1.00000 Uiso Pd
O1 0.590(1) 0.723(1) 0.594(2) 0.176(5) 1.00000 Uiso O
O2 0.764(2) 0.524(2) 0.375(3) 0.176(5) 1.00000 Uiso O
O3 0.794(2) 0.460(1) 0.623(2) 0.176(5) 1.00000 Uiso O
O4 0.315(2) 0.713(1) -0.139(3) 0.176(5) 1.00000 Uiso O
N3 0.282(2) 0.776(1) 0.059(3) 0.176(5) 1.00000 Uiso N
H1A 0.290(2) 0.766(1) 0.164(3) 0.176(5) 1.00000 Uiso H
H1B 0.251(2) 0.839(1) 0.009(3) 0.176(5) 1.00000 Uiso H
C1 0.661(3) 0.672(4) 0.573(5) 0.137(4) 1.00000 Uiso C
N1 0.652(3) 0.577(4) 0.538(5) 0.137(4) 1.00000 Uiso N
S1 0.769(3) 0.528(4) 0.519(5) 0.137(4) 1.00000 Uiso S
C7 0.853(3) 0.631(4) 0.590(5) 0.137(4) 1.00000 Uiso C
C2 0.786(3) 0.704(4) 0.608(5) 0.137(4) 1.00000 Uiso C
C3 0.838(3) 0.786(4) 0.669(5) 0.137(4) 1.00000 Uiso C
C4 0.958(3) 0.796(4) 0.711(5) 0.137(4) 1.00000 Uiso C
C5 1.024(3) 0.724(4) 0.691(5) 0.137(4) 1.00000 Uiso C
C6 0.972(3) 0.641(4) 0.630(5) 0.137(4) 1.00000 Uiso C
H3 0.785(3) 0.845(4) 0.685(5) 0.137(4) 1.00000 Uiso H
H4 1.000(3) 0.862(4) 0.760(5) 0.137(4) 1.00000 Uiso H
H5 1.120(3) 0.732(4) 0.724(5) 0.137(4) 1.00000 Uiso H
H6 1.025(3) 0.583(4) 0.614(5) 0.137(4) 1.00000 Uiso H
N2 0.442(5) 0.516(5) 0.286(4) 0.175(6) 1.00000 Uiso N
C8 0.403(5) 0.602(5) 0.217(4) 0.175(6) 1.00000 Uiso C
C9 0.358(5) 0.615(5) 0.063(4) 0.175(6) 1.00000 Uiso C
C10 0.354(5) 0.534(5) -0.026(4) 0.175(6) 1.00000 Uiso C
C11 0.394(5) 0.444(5) 0.041(4) 0.175(6) 1.00000 Uiso C
C12 0.436(5) 0.439(5) 0.196(4) 0.175(6) 1.00000 Uiso C
C13 0.317(5) 0.707(5) -0.007(4) 0.175(6) 1.00000 Uiso C
H8 0.406(5) 0.664(5) 0.284(4) 0.175(6) 1.00000 Uiso H
H10 0.320(5) 0.540(5) -0.144(4) 0.175(6) 1.00000 Uiso H
H11 0.391(5) 0.381(5) -0.024(4) 0.175(6) 1.00000 Uiso H
H12 0.466(5) 0.370(5) 0.246(4) 0.175(6) 1.00000 Uiso H



# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#=============================================================================

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd N1 2.04(5) 1_555 ?
Pd N2 1.97(4) 1_555 ?
Pd N1 2.04(4) 3_666 ?
Pd N2 1.97(4) 3_666 ?
S1 O2 1.39(5) 1_555 ?
S1 O3 1.35(5) 1_555 ?
S1 N1 1.64(6) 1_555 ?
S1 C7 1.76(7) 1_555 ?
O1 C1 1.19(5) 1_555 ?
O4 C13 1.29(5) 1_555 ?
N1 C1 1.37(8) 1_555 ?
N2 C8 1.38(9) 1_555 ?
N2 C12 1.38(8) 1_555 ?
N3 C13 1.31(7) 1_555 ?
N3 H1B 1.01(3) 1_555 ?
N3 H1A 1.01(4) 1_555 ?
C1 C2 1.49(6) 1_555 ?
C2 C3 1.34(7) 1_555 ?
C2 C7 1.35(7) 1_555 ?
C3 C4 1.36(6) 1_555 ?
C4 C5 1.34(7) 1_555 ?
C5 C6 1.35(8) 1_555 ?
C6 C7 1.35(6) 1_555 ?
C8 C9 1.42(5) 1_555 ?
C9 C10 1.42(9) 1_555 ?
C9 C13 1.46(9) 1_555 ?
C10 C11 1.42(9) 1_555 ?
C11 C12 1.42(5) 1_555 ?
C3 H3 1.09(7) 1_555 ?
C4 H4 1.08(7) 1_555 ?
C5 H5 1.09(6) 1_555 ?
C6 H6 1.08(7) 1_555 ?
C8 H8 1.08(9) 1_555 ?
C10 H10 1.08(5) 1_555 ?
C11 H11 1.08(9) 1_555 ?
C12 H12 1.09(9) 1_555 ?


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd N2 95(2) 1_555 1_555 ?
N1 Pd N1_a 180.00 1_555 3_666 ?
N1 Pd N2_a 85(2) 1_555 3_666 ?
N1_a Pd N2 85(2) 3_666 1_555 ?
N2 Pd N2_a 180.00 1_555 3_666 ?
N1_a Pd N2_a 95(2) 3_666 3_666 ?
O2 S1 O3 131(4) 1_555 1_555 ?
O2 S1 N1 114(3) 1_555 1_555 ?
O2 S1 C7 104(3) 1_555 1_555 ?
O3 S1 N1 100(3) 1_555 1_555 ?
O3 S1 C7 110(3) 1_555 1_555 ?
N1 S1 C7 90(3) 1_555 1_555 ?
Pd N1 S1 121(4) 1_555 1_555 ?
Pd N1 C1 123(3) 1_555 1_555 ?
S1 N1 C1 116(4) 1_555 1_555 ?
Pd N2 C8 123(4) 1_555 1_555 ?
Pd N2 C12 121(4) 1_555 1_555 ?
C8 N2 C12 116(4) 1_555 1_555 ?
H1A N3 H1B 120(3) 1_555 1_555 ?
C13 N3 H1A 118(3) 1_555 1_555 ?
C13 N3 H1B 122(4) 1_555 1_555 ?
O1 C1 N1 129(4) 1_555 1_555 ?
O1 C1 C2 121(5) 1_555 1_555 ?
N1 C1 C2 110(4) 1_555 1_555 ?
C1 C2 C7 110(5) 1_555 1_555 ?
C1 C2 C3 129(4) 1_555 1_555 ?
C3 C2 C7 120(4) 1_555 1_555 ?
C2 C3 C4 120(5) 1_555 1_555 ?
C3 C4 C5 120(5) 1_555 1_555 ?
C4 C5 C6 120(4) 1_555 1_555 ?
C5 C6 C7 120(5) 1_555 1_555 ?
C2 C7 C6 120(5) 1_555 1_555 ?
S1 C7 C6 127(4) 1_555 1_555 ?
S1 C7 C2 113(4) 1_555 1_555 ?
N2 C8 C9 125(6) 1_555 1_555 ?
C8 C9 C10 118(6) 1_555 1_555 ?
C8 C9 C13 123(5) 1_555 1_555 ?
C10 C9 C13 119(4) 1_555 1_555 ?
C9 C10 C11 120(4) 1_555 1_555 ?
C10 C11 C12 118(5) 1_555 1_555 ?
N2 C12 C11 124(6) 1_555 1_555 ?
O4 C13 N3 124(5) 1_555 1_555 ?
O4 C13 C9 114(5) 1_555 1_555 ?
N3 C13 C9 122(4) 1_555 1_555 ?
C2 C3 H3 121(5) 1_555 1_555 ?
C4 C3 H3 119(5) 1_555 1_555 ?
C3 C4 H4 120(5) 1_555 1_555 ?
C5 C4 H4 120(5) 1_555 1_555 ?
C4 C5 H5 120(6) 1_555 1_555 ?
C6 C5 H5 120(5) 1_555 1_555 ?
C5 C6 H6 120(5) 1_555 1_555 ?
C7 C6 H6 120(6) 1_555 1_555 ?
N2 C8 H8 118(4) 1_555 1_555 ?
C9 C8 H8 117(6) 1_555 1_555 ?
C9 C10 H10 121(7) 1_555 1_555 ?
C11 C10 H10 120(7) 1_555 1_555 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?

#=============================================================================

#=============================================================================
# Additional structures (last six sections and associated data_? identifiers) 
# may be added at this point.                                                 
#=============================================================================

# The following lines are used to test the character set of files sent by     
# network email or other means. They are not part of the CIF data set.        
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789              
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 
_database_code_depnum_ccdc_archive 'CCDC 982566'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_J31

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C20 H20 N6 O6 Pd'
_chemical_formula_weight         546.82
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
pd 19.33190 0.69866 15.50170 7.98929 5.29537 25.20520 0.60584 76.89860 5.26593
-1.17700 1.00700
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.00800 0.00600
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.00400 0.00300
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.00200 0.00200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_space_group_name_Hall  '-P 2yab'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x+1/2,y+1/2,-z
-x,-y,-z
x+1/2,-y+1/2,z

_cell_length_a                   9.67234(10)
_cell_length_b                   14.37138(15)
_cell_length_c                   8.18547(10)
_cell_angle_alpha                90.00000
_cell_angle_beta                 92.73275(10)
_cell_angle_gamma                90.00000
_cell_volume                     1136.52637(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_exptl_crystal_density_diffrn    1.598
_cell_special_details            
; ?
;

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                'borosilicate capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; SpLine - BM25, Spanish Beamline at the ESRF (Grenoble, France)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_type           synchrotron
_diffrn_source                   Synchrotron
_diffrn_measurement_device_type  'SpLine-BM25 Powder Diffractometer'
_diffrn_radiation_wavelength     0.82690
_diffrn_radiation_monochromator  Si(111)
_diffrn_measurement_method       '2θ scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'scintillation counter'
_diffrn_detector_type            Cyberstar
_pd_meas_scan_method             step
_pd_meas_special_details         
;  ?
;
#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        3067
_pd_meas_2theta_range_min        3.99869
_pd_meas_2theta_range_max        49.98563
_pd_meas_2theta_range_inc        0.014999


_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_refine_ls_hydrogen_treatment    mixed
_pd_proc_ls_profile_function     'Thompson-Cox-Hasting Pseudo-Voigt'
_pd_proc_ls_background_function  'Interpolation of points'
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        6.1296
_pd_proc_ls_prof_wR_factor       8.6217
_pd_proc_ls_prof_wR_expected     3.3474

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       9.6272
_pd_proc_ls_prof_cwR_factor      12.0242
_pd_proc_ls_prof_cwR_expected    4.6684

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            6.6339
_pd_proc_ls_prof_echi2           6.7556
_refine_ls_goodness_of_fit_all   2.5756

#  Items related to LS refinement

_refine_ls_R_I_factor            4.3496
_refine_ls_number_reflns         1670
_refine_ls_number_parameters     68
_refine_ls_number_restraints     7

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        4.0021
_pd_proc_2theta_range_max        49.9890
_pd_proc_2theta_range_inc        0.014999
_pd_proc_wavelength              0.826900

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Pd 0.50000 0.50000 0.50000 0.153(3) 1.00000 Uiso Pd
O1 0.4591(14) 0.2929(6) 0.3904(16) 0.202(8) 1.00000 Uiso O
O2 0.6561(13) 0.5338(6) 0.1358(12) 0.202(8) 1.00000 Uiso O
O3 0.8684(17) 0.2208(7) 0.762(2) 0.18(1) 1.00000 Uiso O
N3 1.0649(10) 0.2807(8) 0.7586(20) 0.15(1) 1.00000 Uiso N
H1A 1.1353(10) 0.3310(8) 0.7412(20) 0.15(1) 1.00000 Uiso H
H1B 1.0963(10) 0.2164(8) 0.7938(20) 0.15(1) 1.00000 Uiso H
C9 0.738(7) 0.401(5) 0.633(7) 0.241(5) 1.00000 Uiso C
N2 0.682(7) 0.486(5) 0.582(7) 0.241(5) 1.00000 Uiso N
C5 0.767(7) 0.559(5) 0.598(7) 0.241(5) 1.00000 Uiso C
C6 0.903(7) 0.556(5) 0.659(7) 0.241(5) 1.00000 Uiso C
C7 0.958(7) 0.469(5) 0.708(7) 0.241(5) 1.00000 Uiso C
C8 0.875(7) 0.390(5) 0.697(7) 0.241(5) 1.00000 Uiso C
C10 0.931(7) 0.295(5) 0.751(7) 0.241(5) 1.00000 Uiso C
H9 0.673(7) 0.340(5) 0.623(7) 0.241(5) 1.00000 Uiso H
H5 0.726(7) 0.627(5) 0.560(7) 0.241(5) 1.00000 Uiso H
H6 0.966(7) 0.618(5) 0.668(7) 0.241(5) 1.00000 Uiso H
H7 1.064(7) 0.464(5) 0.755(7) 0.241(5) 1.00000 Uiso H
C4 0.617(9) 0.453(3) 0.16(2) 0.174(6) 1.00000 Uiso C
N1 0.554(9) 0.426(3) 0.30(2) 0.174(6) 1.00000 Uiso N
C1 0.536(9) 0.332(3) 0.30(2) 0.174(6) 1.00000 Uiso C
C2 0.593(9) 0.289(3) 0.15(2) 0.174(6) 1.00000 Uiso C
C3 0.649(9) 0.370(3) 0.06(2) 0.174(6) 1.00000 Uiso C
H2A 0.512(9) 0.253(3) 0.08(2) 0.174(6) 1.00000 Uiso H
H2B 0.675(9) 0.240(3) 0.19(2) 0.174(6) 1.00000 Uiso H
H3A 0.760(9) 0.363(3) 0.05(2) 0.174(6) 1.00000 Uiso H
H3B 0.597(9) 0.376(3) -0.06(2) 0.174(6) 1.00000 Uiso H


# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#=============================================================================

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd N1 2.04(13) 1_555 ?
Pd N2 1.87(7) 1_555 ?
Pd N1 2.04(14) 3_666 ?
Pd N2 1.87(7) 3_666 ?
O1 C1 1.21(11) 1_555 ?
O2 C4 1.24(6) 1_555 ?
O3 C10 1.23(7) 1_555 ?
N1 C1 1.36(6) 1_555 ?
N1 C4 1.4(2) 1_555 ?
N2 C5 1.34(10) 1_555 ?
N2 C9 1.39(10) 1_555 ?
N3 C10 1.31(7) 1_555 ?
N3 H1A 1.009(15) 1_555 ?
N3 H1B 1.010(17) 1_555 ?
C1 C2 1.5(2) 1_555 ?
C2 C3 1.49(13) 1_555 ?
C3 C4 1.49(14) 1_555 ?
C5 C6 1.39(9) 1_555 ?
C6 C7 1.41(10) 1_555 ?
C7 C8 1.39(10) 1_555 ?
C8 C10 1.53(10) 1_555 ?
C8 C9 1.41(9) 1_555 ?
C2 H2A 1.08(15) 1_555 ?
C2 H2B 1.10(12) 1_555 ?
C3 H3A 1.09(13) 1_555 ?
C3 H3B 1.1(2) 1_555 ?
C5 H5 1.09(10) 1_555 ?
C6 H6 1.08(10) 1_555 ?
C7 H7 1.08(9) 1_555 ?
C9 H9 1.08(10) 1_555 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd N2 88(3) 1_555 1_555 ?
N1 Pd N1 180.00 1_555 3_666 ?
N1 Pd N2 92(4) 1_555 3_666 ?
N1 Pd N2 92(3) 3_666 1_555 ?
N2 Pd N2 180.00 1_555 3_666 ?
N1 Pd N2 88(3) 3_666 3_666 ?
Pd N1 C1 119(11) 1_555 1_555 ?
Pd N1 C4 131(4) 1_555 1_555 ?
C1 N1 C4 110(11) 1_555 1_555 ?
Pd N2 C5 121(5) 1_555 1_555 ?
Pd N2 C9 123(5) 1_555 1_555 ?
C5 N2 C9 116(6) 1_555 1_555 ?
C10 N3 H1A 124(3) 1_555 1_555 ?
C10 N3 H1B 116(3) 1_555 1_555 ?
H1A N3 H1B 120.1(13) 1_555 1_555 ?
O1 C1 N1 123(10) 1_555 1_555 ?
O1 C1 C2 125(6) 1_555 1_555 ?
N1 C1 C2 111(11) 1_555 1_555 ?
C1 C2 C3 104(6) 1_555 1_555 ?
C2 C3 C4 105(11) 1_555 1_555 ?
N1 C4 C3 110(6) 1_555 1_555 ?
O2 C4 C3 126(11) 1_555 1_555 ?
O2 C4 N1 123(10) 1_555 1_555 ?
N2 C5 C6 126(7) 1_555 1_555 ?
C5 C6 C7 118(6) 1_555 1_555 ?
C6 C7 C8 120(6) 1_555 1_555 ?
C9 C8 C10 122(6) 1_555 1_555 ?
C7 C8 C9 118(6) 1_555 1_555 ?
C7 C8 C10 121(6) 1_555 1_555 ?
N2 C9 C8 124(6) 1_555 1_555 ?
O3 C10 N3 110(5) 1_555 1_555 ?
O3 C10 C8 129(6) 1_555 1_555 ?
N3 C10 C8 119(6) 1_555 1_555 ?
C1 C2 H2A 110(10) 1_555 1_555 ?
C1 C2 H2B 108(15) 1_555 1_555 ?
C3 C2 H2A 113(14) 1_555 1_555 ?
C3 C2 H2B 112(9) 1_555 1_555 ?
H2A C2 H2B 110(8) 1_555 1_555 ?
C2 C3 H3A 110(8) 1_555 1_555 ?
C2 C3 H3B 110(9) 1_555 1_555 ?
C4 C3 H3A 110(9) 1_555 1_555 ?
C4 C3 H3B 110(8) 1_555 1_555 ?
H3A C3 H3B 111(16) 1_555 1_555 ?
N2 C5 H5 117(7) 1_555 1_555 ?
C6 C5 H5 117(7) 1_555 1_555 ?
C5 C6 H6 122(7) 1_555 1_555 ?
C7 C6 H6 121(7) 1_555 1_555 ?
C6 C7 H7 120(7) 1_555 1_555 ?
C8 C7 H7 120(7) 1_555 1_555 ?
N2 C9 H9 118(7) 1_555 1_555 ?
C8 C9 H9 118(7) 1_555 1_555 ?

#=============================================================================

#=============================================================================
# Additional structures (last six sections and associated data_? identifiers) 
# may be added at this point.                                                 
#=============================================================================

# The following lines are used to test the character set of files sent by     
# network email or other means. They are not part of the CIF data set.        
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789              
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 







_database_code_depnum_ccdc_archive 'CCDC 982567'
