# Electronic Supplementary Material (ESI) for ChemComm.
# 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_global
#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Fe N12 Pd S2, (H2O, C2H6O)'
_chemical_formula_sum            'C20 H20 Fe N12 Pd S2 O2'
_chemical_formula_weight         685.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  'P -1'

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

_cell_length_a                   7.0850(14)
_cell_length_b                   13.334(3)
_cell_length_c                   14.383(3)
_cell_angle_alpha                69.66(3)
_cell_angle_beta                 90.02(3)
_cell_angle_gamma                74.60(3)
_cell_volume                     1221.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5899
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_T_max  0.9268
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Australian synchrotron MX2'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'scan in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22271
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         31.42
_reflns_number_total             5819
_reflns_number_gt                5339
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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)+(0.1215P)²+36.3338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.050(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5819
_refine_ls_number_parameters     367
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.1000
_refine_ls_wR_factor_ref         0.2738
_refine_ls_wR_factor_gt          0.2702
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.105
_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 -0.51864(10) 1.03734(5) 0.73828(4) 0.0138(3) Uani 1 1 d . . .
Fe2 Fe 0.0000 1.0000 0.5000 0.0135(4) Uani 1 2 d S . .
C2 C -0.3212(14) 1.0392(8) 0.8362(7) 0.0193(17) Uani 1 1 d . . .
N4 N -0.8182(12) 1.0190(6) 0.5881(6) 0.0175(14) Uani 1 1 d . . .
N2 N -0.2080(12) 1.0324(7) 0.8965(6) 0.0184(14) Uani 1 1 d . . .
C4 C -0.7133(14) 1.0285(7) 0.6433(7) 0.0185(16) Uani 1 1 d . . .
C3 C -0.3156(14) 1.0285(7) 0.6434(7) 0.0185(17) Uani 1 1 d . . .
N3 N -0.2010(12) 1.0190(6) 0.5887(6) 0.0167(14) Uani 1 1 d . . .
Fe1 Fe 0.0000 1.0000 1.0000 0.0141(4) Uani 1 2 d S . .
N5 N -0.0786(13) 1.1573(7) 0.9887(7) 0.0256(17) Uani 1 1 d . . .
N9 N -0.0812(13) 1.1618(7) 0.4250(7) 0.0227(16) Uani 1 1 d . . .
C1 C -0.7164(14) 1.0393(8) 0.8361(7) 0.0183(16) Uani 1 1 d . . .
N10 N -0.1185(18) 1.2368(8) 0.4738(9) 0.041(3) Uani 1 1 d . . .
C14 C -0.2558(17) 1.5108(9) 0.2167(8) 0.028(2) Uani 1 1 d . B .
H14 H -0.2622 1.5203 0.2792 0.034 Uiso 1 1 calc R . .
N11 N -0.1646(15) 1.3288(7) 0.3154(7) 0.0282(19) Uani 1 1 d . . .
C13 C -0.169(2) 1.3370(9) 0.4056(8) 0.034(3) Uani 1 1 d . . .
H13 H -0.2031 1.4047 0.4181 0.041 Uiso 1 1 calc R . .
C5 C -0.1198(18) 1.2430(10) 0.9095(11) 0.036(3) Uani 1 1 d . . .
H5 H -0.1179 1.2415 0.8439 0.043 Uiso 1 1 calc R . .
C12 C -0.1105(18) 1.2201(8) 0.3300(7) 0.028(2) Uani 1 1 d . . .
H12 H -0.0955 1.1900 0.2786 0.033 Uiso 1 1 calc R . .
N12 N -0.206(2) 1.4114(8) 0.2172(7) 0.045(3) Uani 1 1 d . B .
N7 N -0.167(2) 1.3366(9) 0.9313(10) 0.059(4) Uani 1 1 d . . .
N6 N -0.100(3) 1.1949(10) 1.0703(9) 0.059(4) Uani 1 1 d . . .
N1 N -0.8245(12) 1.0323(6) 0.8965(6) 0.0185(15) Uani 1 1 d . . .
C16 C -0.3604(19) 1.7172(9) 0.1258(8) 0.032(2) Uani 1 1 d . B .
H16 H -0.3738 1.7368 0.1834 0.039 Uiso 1 1 calc R . .
C15 C -0.3024(18) 1.6089(8) 0.1286(8) 0.030(2) Uani 1 1 d . . .
C17 C -0.3974(17) 1.7952(8) 0.0279(8) 0.027(2) Uani 1 1 d . . .
H17 H -0.3994 1.8711 0.0096 0.032 Uiso 1 1 calc R A 1
C7 C -0.2371(17) 1.4735(8) 0.7831(9) 0.029(2) Uani 1 1 d . . .
H7 H -0.2086 1.4136 0.7592 0.034 Uiso 1 1 calc R . .
C18A C -0.316(3) 1.7463(17) -0.0369(16) 0.026(4) Uiso 0.50 1 d PU B 2
H18A H -0.3071 1.7873 -0.1047 0.032 Uiso 0.50 1 calc PR B 2
N8 N -0.223(3) 1.4511(10) 0.8690(10) 0.087(7) Uani 1 1 d . . .
C8 C -0.2944(16) 1.5854(9) 0.7101(8) 0.027(2) Uani 1 1 d . . .
C9 C -0.308(5) 1.6131(13) 0.6146(11) 0.117(12) Uani 1 1 d . . .
H9 H -0.2804 1.5592 0.5836 0.140 Uiso 1 1 calc R . .
C6 C -0.151(5) 1.2984(14) 1.0343(14) 0.101(10) Uani 1 1 d . . .
H6 H -0.1753 1.3452 1.0725 0.122 Uiso 1 1 calc R . .
C11 C -0.3922(19) 1.7865(10) 0.6137(8) 0.032(2) Uani 1 1 d . . .
H11 H -0.4037 1.8640 0.5916 0.038 Uiso 1 1 calc R C 1
C10 C -0.364(3) 1.7270(11) 0.5598(10) 0.064(5) Uani 1 1 d . . .
H10 H -0.3795 1.7573 0.4890 0.077 Uiso 1 1 calc R . .
S2B S -0.3742(12) 1.6069(4) 0.0142(4) 0.0330(13) Uani 0.50 1 d PU B 1
S2A S -0.2334(12) 1.6068(4) 0.0145(4) 0.0333(13) Uani 0.50 1 d PU B 2
C18B C -0.431(4) 1.7457(18) -0.0378(17) 0.028(4) Uiso 0.50 1 d PU B 1
H18B H -0.4804 1.7864 -0.1057 0.034 Uiso 0.50 1 calc PR B 1
O1 O -0.1187(18) 1.2373(8) 0.6687(7) 0.049(3) Uani 1 1 d . . .
O2A O -0.497(2) 1.5916(10) 0.4044(11) 0.025(3) Uani 0.50 1 d P . .
O2B O -0.096(2) 1.5919(10) 0.4049(11) 0.023(3) Uani 0.50 1 d P . .
Pd1A Pd -0.481(4) 0.962(2) 0.6154(19) 0.100 Uiso 0.10 1 d P . 4
Fe2A Fe -0.002(7) 1.003(4) 0.648(4) 0.100 Uiso 0.10 1 d P . 4
Fe1A Fe 0.001(7) 1.002(4) 0.848(3) 0.100 Uiso 0.10 1 d P . 4
Pd1B Pd -0.479(4) 0.960(2) 0.9147(19) 0.100 Uiso 0.10 1 d P . 4
S1B S -0.2955(13) 1.7016(5) 0.7352(5) 0.0331(13) Uani 0.50 1 d P . 2
S1A S -0.4066(13) 1.7015(5) 0.7351(5) 0.0325(13) Uani 0.50 1 d P . 1


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.988(10) . ?
Pd1 C3 1.992(10) . ?
Pd1 C4 1.995(10) . ?
Pd1 C2 1.996(10) . ?
Pd1 Pd1A 2.30(3) . ?
Pd1 Pd1B 2.37(3) . ?
Fe2 N4 1.930(8) 2_476 ?
Fe2 N4 1.930(8) 1_655 ?
Fe2 N3 1.937(8) . ?
Fe2 N3 1.937(8) 2_576 ?
Fe2 N9 1.967(8) . ?
Fe2 N9 1.967(8) 2_576 ?
Fe2 Fe2A 2.15(5) 2_576 ?
Fe2 Fe2A 2.15(5) . ?
C2 N2 1.144(13) . ?
C2 Pd1B 1.85(3) . ?
C2 Fe1A 2.20(5) . ?
N4 C4 1.148(13) . ?
N4 Fe2A 1.58(5) 1_455 ?
N4 Fe2 1.930(8) 1_455 ?
N4 Pd1A 2.29(3) . ?
N2 Fe1A 1.65(5) . ?
N2 Fe1 1.946(8) . ?
N2 Pd1B 2.34(3) . ?
C4 Pd1A 1.77(3) . ?
C4 Fe2A 2.16(5) 1_455 ?
C3 N3 1.144(13) . ?
C3 Pd1A 1.77(3) . ?
C3 Fe2A 2.16(5) . ?
N3 Fe2A 1.58(5) . ?
N3 Pd1A 2.30(3) . ?
Fe1 N2 1.946(8) 2_577 ?
Fe1 N1 1.947(9) 2_477 ?
Fe1 N1 1.947(9) 1_655 ?
Fe1 N5 1.969(9) . ?
Fe1 N5 1.969(9) 2_577 ?
Fe1 Fe1A 2.18(5) . ?
Fe1 Fe1A 2.18(5) 2_577 ?
N5 C5 1.268(16) . ?
N5 N6 1.420(15) . ?
N9 C12 1.301(12) . ?
N9 N10 1.382(13) . ?
C1 N1 1.153(13) . ?
C1 Pd1B 1.86(3) . ?
C1 Fe1A 2.18(5) 1_455 ?
N10 C13 1.307(14) . ?
C14 N12 1.274(15) . ?
C14 C15 1.430(14) . ?
C14 H14 0.9500 . ?
N11 C12 1.336(13) . ?
N11 C13 1.339(14) . ?
N11 N12 1.428(12) . ?
C13 H13 0.9500 . ?
C5 N7 1.348(18) . ?
C5 H5 0.9500 . ?
C12 H12 0.9500 . ?
N7 C6 1.38(2) . ?
N7 N8 1.420(16) . ?
N6 C6 1.24(2) . ?
N6 Fe1A 2.37(5) 2_577 ?
N1 Fe1A 1.63(5) 1_455 ?
N1 Fe1 1.947(8) 1_455 ?
N1 Pd1B 2.36(3) . ?
C16 C15 1.379(15) . ?
C16 C17 1.403(15) . ?
C16 H16 0.9500 . ?
C15 S2A 1.720(13) . ?
C15 S2B 1.733(12) . ?
C17 C18A 1.36(2) . ?
C17 C18B 1.38(2) . ?
C17 Pd1B 2.16(3) 1_564 ?
C17 H17 0.9500 . ?
C7 N8 1.163(18) . ?
C7 C8 1.443(14) . ?
C7 H7 0.9500 . ?
C18A S2A 1.68(2) . ?
C18A H18A 0.9500 . ?
C8 C9 1.288(18) . ?
C8 S1A 1.701(12) . ?
C8 S1B 1.707(12) . ?
C9 C10 1.39(2) . ?
C9 H9 0.9500 . ?
C6 H6 0.9500 . ?
C11 C10 1.270(16) . ?
C11 S1B 1.737(13) . ?
C11 S1A 1.741(13) . ?
C11 Pd1A 2.26(3) 1_565 ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
S2B C18B 1.67(2) . ?
C18B H18B 0.9500 . ?
Pd1A C11 2.26(3) 1_545 ?
Pd1A Pd1A 3.10(5) 2_476 ?
Fe2A N4 1.58(5) 1_655 ?
Fe2A C4 2.16(5) 1_655 ?
Fe2A Fe1A 2.87(7) . ?
Fe1A N1 1.63(5) 1_655 ?
Fe1A C1 2.18(5) 1_655 ?
Fe1A N6 2.37(5) 2_577 ?
Pd1B C17 2.16(3) 1_546 ?
Pd1B Pd1B 2.98(5) 2_477 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 C3 177.6(4) . . ?
C1 Pd1 C4 90.4(4) . . ?
C3 Pd1 C4 89.9(4) . . ?
C1 Pd1 C2 89.3(4) . . ?
C3 Pd1 C2 90.3(4) . . ?
C4 Pd1 C2 177.6(4) . . ?
C1 Pd1 Pd1A 131.3(7) . . ?
C3 Pd1 Pd1A 48.0(7) . . ?
C4 Pd1 Pd1A 47.9(7) . . ?
C2 Pd1 Pd1A 131.1(7) . . ?
C1 Pd1 Pd1B 49.5(7) . . ?
C3 Pd1 Pd1B 128.8(7) . . ?
C4 Pd1 Pd1B 129.1(7) . . ?
C2 Pd1 Pd1B 49.3(7) . . ?
Pd1A Pd1 Pd1B 133.8(8) . . ?
N4 Fe2 N4 179.998(2) 2_476 1_655 ?
N4 Fe2 N3 91.0(3) 2_476 . ?
N4 Fe2 N3 89.0(3) 1_655 . ?
N4 Fe2 N3 89.0(3) 2_476 2_576 ?
N4 Fe2 N3 91.0(3) 1_655 2_576 ?
N3 Fe2 N3 179.999(2) . 2_576 ?
N4 Fe2 N9 89.9(3) 2_476 . ?
N4 Fe2 N9 90.1(3) 1_655 . ?
N3 Fe2 N9 90.0(3) . . ?
N3 Fe2 N9 90.0(3) 2_576 . ?
N4 Fe2 N9 90.1(3) 2_476 2_576 ?
N4 Fe2 N9 89.9(3) 1_655 2_576 ?
N3 Fe2 N9 90.0(3) . 2_576 ?
N3 Fe2 N9 90.0(3) 2_576 2_576 ?
N9 Fe2 N9 179.999(3) . 2_576 ?
N4 Fe2 Fe2A 45.3(13) 2_476 2_576 ?
N4 Fe2 Fe2A 134.7(13) 1_655 2_576 ?
N3 Fe2 Fe2A 135.0(13) . 2_576 ?
N3 Fe2 Fe2A 45.0(13) 2_576 2_576 ?
N9 Fe2 Fe2A 81.3(12) . 2_576 ?
N9 Fe2 Fe2A 98.7(12) 2_576 2_576 ?
N4 Fe2 Fe2A 134.7(13) 2_476 . ?
N4 Fe2 Fe2A 45.3(13) 1_655 . ?
N3 Fe2 Fe2A 45.0(12) . . ?
N3 Fe2 Fe2A 135.0(13) 2_576 . ?
N9 Fe2 Fe2A 98.7(12) . . ?
N9 Fe2 Fe2A 81.3(12) 2_576 . ?
Fe2A Fe2 Fe2A 180(2) 2_576 . ?
N2 C2 Pd1B 100.2(11) . . ?
N2 C2 Pd1 175.0(8) . . ?
Pd1B C2 Pd1 75.8(9) . . ?
N2 C2 Fe1A 47.3(14) . . ?
Pd1B C2 Fe1A 129.4(15) . . ?
Pd1 C2 Fe1A 133.3(13) . . ?
C4 N4 Fe2A 103.2(19) . 1_455 ?
C4 N4 Fe2 177.6(8) . 1_455 ?
Fe2A N4 Fe2 74.6(17) 1_455 1_455 ?
C4 N4 Pd1A 49.1(9) . . ?
Fe2A N4 Pd1A 138.8(18) 1_455 . ?
Fe2 N4 Pd1A 132.2(8) 1_455 . ?
C2 N2 Fe1A 102.1(18) . . ?
C2 N2 Fe1 172.1(8) . . ?
Fe1A N2 Fe1 74.0(16) . . ?
C2 N2 Pd1B 51.1(8) . . ?
Fe1A N2 Pd1B 132.4(17) . . ?
Fe1 N2 Pd1B 126.6(7) . . ?
N4 C4 Pd1A 101.6(11) . . ?
N4 C4 Pd1 176.5(8) . . ?
Pd1A C4 Pd1 75.2(9) . . ?
N4 C4 Fe2A 45.6(14) . 1_455 ?
Pd1A C4 Fe2A 135.6(15) . 1_455 ?
Pd1 C4 Fe2A 136.3(13) . 1_455 ?
N3 C3 Pd1A 101.8(11) . . ?
N3 C3 Pd1 176.7(8) . . ?
Pd1A C3 Pd1 75.2(9) . . ?
N3 C3 Fe2A 45.2(14) . . ?
Pd1A C3 Fe2A 135.6(15) . . ?
Pd1 C3 Fe2A 136.3(13) . . ?
C3 N3 Fe2A 103.7(19) . . ?
C3 N3 Fe2 178.0(8) . . ?
Fe2A N3 Fe2 74.5(18) . . ?
C3 N3 Pd1A 49.0(8) . . ?
Fe2A N3 Pd1A 139.1(18) . . ?
Fe2 N3 Pd1A 132.0(7) . . ?
N2 Fe1 N2 179.999(3) 2_577 . ?
N2 Fe1 N1 88.5(3) 2_577 2_477 ?
N2 Fe1 N1 91.5(3) . 2_477 ?
N2 Fe1 N1 91.5(3) 2_577 1_655 ?
N2 Fe1 N1 88.5(3) . 1_655 ?
N1 Fe1 N1 180.0(4) 2_477 1_655 ?
N2 Fe1 N5 89.6(4) 2_577 . ?
N2 Fe1 N5 90.4(3) . . ?
N1 Fe1 N5 89.6(4) 2_477 . ?
N1 Fe1 N5 90.4(4) 1_655 . ?
N2 Fe1 N5 90.4(3) 2_577 2_577 ?
N2 Fe1 N5 89.6(4) . 2_577 ?
N1 Fe1 N5 90.4(4) 2_477 2_577 ?
N1 Fe1 N5 89.6(4) 1_655 2_577 ?
N5 Fe1 N5 180.0(5) . 2_577 ?
N2 Fe1 Fe1A 133.2(12) 2_577 . ?
N2 Fe1 Fe1A 46.8(12) . . ?
N1 Fe1 Fe1A 134.0(12) 2_477 . ?
N1 Fe1 Fe1A 46.0(12) 1_655 . ?
N5 Fe1 Fe1A 106.2(12) . . ?
N5 Fe1 Fe1A 73.8(12) 2_577 . ?
N2 Fe1 Fe1A 46.8(12) 2_577 2_577 ?
N2 Fe1 Fe1A 133.2(12) . 2_577 ?
N1 Fe1 Fe1A 46.0(12) 2_477 2_577 ?
N1 Fe1 Fe1A 134.0(13) 1_655 2_577 ?
N5 Fe1 Fe1A 73.8(12) . 2_577 ?
N5 Fe1 Fe1A 106.2(12) 2_577 2_577 ?
Fe1A Fe1 Fe1A 179.999(18) . 2_577 ?
C5 N5 N6 107.4(10) . . ?
C5 N5 Fe1 127.4(9) . . ?
N6 N5 Fe1 125.2(7) . . ?
C12 N9 N10 106.8(9) . . ?
C12 N9 Fe2 132.2(7) . . ?
N10 N9 Fe2 121.0(7) . . ?
N1 C1 Pd1B 100.6(11) . . ?
N1 C1 Pd1 175.0(8) . . ?
Pd1B C1 Pd1 75.9(9) . . ?
N1 C1 Fe1A 46.7(14) . 1_455 ?
Pd1B C1 Fe1A 129.3(15) . 1_455 ?
Pd1 C1 Fe1A 133.1(13) . 1_455 ?
C13 N10 N9 107.4(11) . . ?
N12 C14 C15 124.5(11) . . ?
N12 C14 H14 117.7 . . ?
C15 C14 H14 117.7 . . ?
C12 N11 C13 106.9(9) . . ?
C12 N11 N12 121.2(9) . . ?
C13 N11 N12 131.9(9) . . ?
N10 C13 N11 109.0(10) . . ?
N10 C13 H13 125.5 . . ?
N11 C13 H13 125.5 . . ?
N5 C5 N7 110.5(13) . . ?
N5 C5 H5 124.7 . . ?
N7 C5 H5 124.7 . . ?
N9 C12 N11 109.8(9) . . ?
N9 C12 H12 125.1 . . ?
N11 C12 H12 125.1 . . ?
C14 N12 N11 113.1(10) . . ?
C5 N7 C6 104.3(11) . . ?
C5 N7 N8 131.5(14) . . ?
C6 N7 N8 124.2(13) . . ?
C6 N6 N5 106.8(12) . . ?
C6 N6 Fe1A 175.3(17) . 2_577 ?
N5 N6 Fe1A 77.9(13) . 2_577 ?
C1 N1 Fe1A 102.1(18) . 1_455 ?
C1 N1 Fe1 172.5(8) . 1_455 ?
Fe1A N1 Fe1 74.5(17) 1_455 1_455 ?
C1 N1 Pd1B 50.7(8) . . ?
Fe1A N1 Pd1B 132.1(17) 1_455 . ?
Fe1 N1 Pd1B 126.7(7) 1_455 . ?
C15 C16 C17 112.2(9) . . ?
C15 C16 H16 123.9 . . ?
C17 C16 H16 123.9 . . ?
C16 C15 C14 125.8(11) . . ?
C16 C15 S2A 109.9(8) . . ?
C14 C15 S2A 122.5(9) . . ?
C16 C15 S2B 109.0(8) . . ?
C14 C15 S2B 121.8(8) . . ?
S2A C15 S2B 33.6(4) . . ?
C18A C17 C18B 34.6(12) . . ?
C18A C17 C16 110.6(12) . . ?
C18B C17 C16 110.3(12) . . ?
C18A C17 Pd1B 93.0(13) . 1_564 ?
C18B C17 Pd1B 93.1(13) . 1_564 ?
C16 C17 Pd1B 155.4(10) . 1_564 ?
C18A C17 H17 114.4 . . ?
C18B C17 H17 124.9 . . ?
C16 C17 H17 124.9 . . ?
Pd1B C17 H17 32.6 1_564 . ?
N8 C7 C8 125.1(11) . . ?
N8 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
C17 C18A S2A 113.5(15) . . ?
C17 C18A H18A 123.3 . . ?
S2A C18A H18A 123.3 . . ?
C7 N8 N7 118.3(13) . . ?
C9 C8 C7 126.6(12) . . ?
C9 C8 S1A 107.5(10) . . ?
C7 C8 S1A 124.6(9) . . ?
C9 C8 S1B 107.3(10) . . ?
C7 C8 S1B 124.2(9) . . ?
S1A C8 S1B 26.7(3) . . ?
C8 C9 C10 115.8(13) . . ?
C8 C9 H9 122.1 . . ?
C10 C9 H9 122.1 . . ?
N6 C6 N7 111.0(13) . . ?
N6 C6 H6 124.5 . . ?
N7 C6 H6 124.5 . . ?
C10 C11 S1B 108.5(10) . . ?
C10 C11 S1A 108.2(10) . . ?
S1B C11 S1A 26.2(3) . . ?
C10 C11 Pd1A 145.9(12) . 1_565 ?
S1B C11 Pd1A 104.9(9) . 1_565 ?
S1A C11 Pd1A 104.8(9) . 1_565 ?
C10 C11 H11 125.9 . . ?
S1B C11 H11 119.7 . . ?
S1A C11 H11 125.9 . . ?
Pd1A C11 H11 22.5 1_565 . ?
C11 C10 C9 113.4(13) . . ?
C11 C10 H10 123.3 . . ?
C9 C10 H10 123.3 . . ?
C18B S2B C15 91.7(9) . . ?
C18A S2A C15 91.3(9) . . ?
C17 C18B S2B 113.0(15) . . ?
C17 C18B H18B 123.5 . . ?
S2B C18B H18B 123.5 . . ?
C4 Pd1A C3 105.5(14) . . ?
C4 Pd1A C11 124.9(14) . 1_545 ?
C3 Pd1A C11 124.4(14) . 1_545 ?
C4 Pd1A N4 29.4(6) . . ?
C3 Pd1A N4 130.2(13) . . ?
C11 Pd1A N4 105.2(11) 1_545 . ?
C4 Pd1A N3 130.1(13) . . ?
C3 Pd1A N3 29.2(6) . . ?
C11 Pd1A N3 104.7(11) 1_545 . ?
N4 Pd1A N3 144.6(12) . . ?
C4 Pd1A Pd1 56.8(8) . . ?
C3 Pd1A Pd1 56.8(8) . . ?
C11 Pd1A Pd1 134.9(12) 1_545 . ?
N4 Pd1A Pd1 86.2(9) . . ?
N3 Pd1A Pd1 85.9(9) . . ?
C4 Pd1A Pd1A 104.6(14) . 2_476 ?
C3 Pd1A Pd1A 104.4(14) . 2_476 ?
C11 Pd1A Pd1A 85.5(11) 1_545 2_476 ?
N4 Pd1A Pd1A 82.0(11) . 2_476 ?
N3 Pd1A Pd1A 82.0(11) . 2_476 ?
Pd1 Pd1A Pd1A 139.7(14) . 2_476 ?
N3 Fe2A N4 118(3) . 1_655 ?
N3 Fe2A Fe2 60.5(16) . . ?
N4 Fe2A Fe2 60.1(16) 1_655 . ?
N3 Fe2A C3 31.1(10) . . ?
N4 Fe2A C3 147(3) 1_655 . ?
Fe2 Fe2A C3 91.5(18) . . ?
N3 Fe2A C4 148(3) . 1_655 ?
N4 Fe2A C4 31.2(10) 1_655 1_655 ?
Fe2 Fe2A C4 91.3(18) . 1_655 ?
C3 Fe2A C4 163(2) . 1_655 ?
N3 Fe2A Fe1A 120(3) . . ?
N4 Fe2A Fe1A 120(3) 1_655 . ?
Fe2 Fe2A Fe1A 179(2) . . ?
C3 Fe2A Fe1A 89.1(19) . . ?
C4 Fe2A Fe1A 88.5(18) 1_655 . ?
N1 Fe1A N2 112(3) 1_655 . ?
N1 Fe1A C1 31.1(9) 1_655 1_655 ?
N2 Fe1A C1 140(3) . 1_655 ?
N1 Fe1A Fe1 59.5(15) 1_655 . ?
N2 Fe1A Fe1 59.2(15) . . ?
C1 Fe1A Fe1 90.4(17) 1_655 . ?
N1 Fe1A C2 140(3) 1_655 . ?
N2 Fe1A C2 30.6(9) . . ?
C1 Fe1A C2 156(2) 1_655 . ?
Fe1 Fe1A C2 89.6(18) . . ?
N1 Fe1A N6 99(2) 1_655 2_577 ?
N2 Fe1A N6 100(2) . 2_577 ?
C1 Fe1A N6 101.7(18) 1_655 2_577 ?
Fe1 Fe1A N6 83.0(16) . 2_577 ?
C2 Fe1A N6 101.8(18) . 2_577 ?
N1 Fe1A Fe2A 121(3) 1_655 . ?
N2 Fe1A Fe2A 120(2) . . ?
C1 Fe1A Fe2A 90.4(19) 1_655 . ?
Fe1 Fe1A Fe2A 179(2) . . ?
C2 Fe1A Fe2A 89.8(18) . . ?
N6 Fe1A Fe2A 96.6(18) 2_577 . ?
C2 Pd1B C1 98.0(12) . . ?
C2 Pd1B C17 129.5(14) . 1_546 ?
C1 Pd1B C17 129.1(14) . 1_546 ?
C2 Pd1B N2 28.7(5) . . ?
C1 Pd1B N2 121.6(13) . . ?
C17 Pd1B N2 109.3(11) 1_546 . ?
C2 Pd1B N1 121.8(12) . . ?
C1 Pd1B N1 28.7(5) . . ?
C17 Pd1B N1 108.7(11) 1_546 . ?
N2 Pd1B N1 136.6(11) . . ?
C2 Pd1B Pd1 54.8(7) . . ?
C1 Pd1B Pd1 54.5(7) . . ?
C17 Pd1B Pd1 136.6(12) 1_546 . ?
N2 Pd1B Pd1 83.5(9) . . ?
N1 Pd1B Pd1 83.2(8) . . ?
C2 Pd1B Pd1B 103.3(14) . 2_477 ?
C1 Pd1B Pd1B 102.7(14) . 2_477 ?
C17 Pd1B Pd1B 85.1(12) 1_546 2_477 ?
N2 Pd1B Pd1B 81.8(11) . 2_477 ?
N1 Pd1B Pd1B 81.2(11) . 2_477 ?
Pd1 Pd1B Pd1B 138.3(14) . 2_477 ?
C8 S1B C11 90.9(6) . . ?
C8 S1A C11 91.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        31.42
_diffrn_measured_fraction_theta_full 0.927
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.906
_refine_diff_density_rms         0.336

# start Validation Reply Form
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: all authors contributed
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.927       
RESPONSE: synchtrotron data, full sphere collected
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 963504'
#######################################################################
#
#                 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_global
#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Fe N12 Pd S2, (H2O, C2H6O)'
_chemical_formula_sum            'C20 H20 Fe N12 Pd S2 O2'
_chemical_formula_weight         685.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  'P -1'

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

_cell_length_a                   7.2333(15)
_cell_length_b                   13.404(3)
_cell_length_c                   14.527(3)
_cell_angle_alpha                69.130(3)
_cell_angle_beta                 90.027(3)
_cell_angle_gamma                74.359(3)
_cell_volume                     1260.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    600
_cell_measurement_theta_min      2.601
_cell_measurement_theta_max      27.225

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8648
_exptl_absorpt_correction_T_max  0.9289
_exptl_absorpt_process_details   'SADABS - Bruker- V2.05'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6095
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         28.40
_reflns_number_total             6095
_reflns_number_gt                4926
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997), X-SEED'
_computing_molecular_graphics    POV_RAY
_computing_publication_material  CHECKCIF

_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)+(0.1105P)²+16.1934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0078(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6095
_refine_ls_number_parameters     331
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.2249
_refine_ls_wR_factor_gt          0.2065
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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 -0.51874(7) 1.03738(4) 0.73127(4) 0.0136(2) Uani 1 1 d . . .
Fe2 Fe 0.0000 1.0000 0.5000 0.0118(3) Uani 1 2 d S . .
C2 C -0.3329(10) 1.0452(6) 0.8262(5) 0.0164(13) Uani 1 1 d . . .
N4 N -0.8195(8) 1.0164(5) 0.5879(4) 0.0167(11) Uani 1 1 d . . .
N2 N -0.2262(9) 1.0454(6) 0.8849(5) 0.0237(13) Uani 1 1 d . . .
C4 C -0.7081(10) 1.0239(6) 0.6409(5) 0.0166(13) Uani 1 1 d . . .
C3 C -0.3141(10) 1.0251(6) 0.6401(5) 0.0166(13) Uani 1 1 d . . .
N3 N -0.1983(8) 1.0166(5) 0.5880(4) 0.0162(11) Uani 1 1 d . . .
Fe1 Fe 0.0000 1.0000 1.0000 0.0126(3) Uani 1 2 d S . .
N5 N -0.0850(11) 1.1682(6) 1.0011(5) 0.0281(15) Uani 1 1 d . . .
N9 N -0.0822(9) 1.1629(5) 0.4267(4) 0.0184(12) Uani 1 1 d . . .
C1 C -0.7132(10) 1.0450(6) 0.8264(5) 0.0172(13) Uani 1 1 d . . .
N10 N -0.1188(10) 1.2377(5) 0.4742(5) 0.0244(14) Uani 1 1 d . . .
C14 C -0.2567(12) 1.5127(7) 0.2184(6) 0.0263(16) Uani 1 1 d . . .
H14 H -0.2620 1.5235 0.2796 0.032 Uiso 1 1 calc R . .
N11 N -0.1659(11) 1.3310(5) 0.3157(5) 0.0282(15) Uani 1 1 d . . .
C13 C -0.1686(13) 1.3366(7) 0.4057(6) 0.0278(17) Uani 1 1 d . . .
H13 H -0.2024 1.4041 0.4179 0.033 Uiso 1 1 calc R . .
C5 C -0.1278(14) 1.2532(7) 0.9183(6) 0.0304(18) Uani 1 1 d . . .
H5 H -0.1266 1.2491 0.8543 0.037 Uiso 1 1 calc R . .
C12 C -0.1106(15) 1.2203(7) 0.3314(6) 0.035(2) Uani 1 1 d . . .
H12 H -0.0952 1.1897 0.2811 0.042 Uiso 1 1 calc R . .
N12 N -0.2078(18) 1.4140(6) 0.2219(6) 0.056(3) Uani 1 1 d . . .
N7 N -0.174(2) 1.3477(7) 0.9361(7) 0.085(5) Uani 1 1 d . . .
N6 N -0.104(3) 1.2048(7) 1.0783(7) 0.105(6) Uani 1 1 d . . .
N1 N -0.8186(9) 1.0454(6) 0.8850(5) 0.0226(13) Uani 1 1 d . . .
C16 C -0.3593(15) 1.7174(7) 0.1222(7) 0.036(2) Uani 1 1 d . B .
H16 H -0.3702 1.7379 0.1787 0.043 Uiso 1 1 calc R . .
C15 C -0.3052(13) 1.6098(7) 0.1296(6) 0.0285(17) Uani 1 1 d . . .
C17 C -0.3979(13) 1.7962(7) 0.0255(7) 0.0311(18) Uani 1 1 d . . .
H17 H -0.3958 1.8714 0.0067 0.037 Uiso 1 1 calc R A 1
C7 C -0.2394(12) 1.4800(7) 0.7863(7) 0.0276(17) Uani 1 1 d . . .
H7 H -0.2072 1.4184 0.7655 0.033 Uiso 1 1 calc R . .
C18A C -0.310(3) 1.7491(16) -0.0387(15) 0.036(4) Uiso 0.50 1 d PU B 2
H18A H -0.3001 1.7903 -0.1060 0.044 Uiso 0.50 1 calc PR B 2
N8 N -0.230(3) 1.4600(8) 0.8720(7) 0.127(8) Uani 1 1 d . . .
S1 S -0.3546(13) 1.7089(3) 0.7297(3) 0.154(3) Uani 1 1 d . . .
C8 C -0.2952(11) 1.5896(7) 0.7101(6) 0.0252(16) Uani 1 1 d . . .
C9 C -0.309(3) 1.6147(17) 0.6147(14) 0.090(5) Uiso 1 1 d . . .
H9 H -0.2822 1.5591 0.5864 0.109 Uiso 1 1 calc R . .
C6 C -0.157(5) 1.3121(11) 1.0374(10) 0.176(15) Uani 1 1 d . . .
H6 H -0.1823 1.3606 1.0731 0.211 Uiso 1 1 calc R . .
C11 C -0.3953(16) 1.7888(8) 0.6076(7) 0.041(2) Uani 1 1 d . . .
H11 H -0.4357 1.8680 0.5812 0.050 Uiso 1 1 calc R . .
C10 C -0.364(2) 1.7283(9) 0.5565(9) 0.070(4) Uani 1 1 d . . .
H10 H -0.3776 1.7569 0.4861 0.084 Uiso 1 1 calc R . .
S2B S -0.3882(8) 1.6063(4) 0.0171(3) 0.0346(10) Uani 0.50 1 d PU B 1
S2A S -0.2177(7) 1.6064(4) 0.0168(3) 0.0341(10) Uani 0.50 1 d PU B 2
C18B C -0.439(3) 1.7487(15) -0.0377(14) 0.034(4) Uiso 0.50 1 d PU B 1
H18B H -0.4909 1.7900 -0.1050 0.040 Uiso 0.50 1 calc PR B 1
O1 O -0.1214(12) 1.2430(6) 0.6642(5) 0.0480(18) Uani 1 1 d . . .
O2A O -0.4945(13) 1.5909(7) 0.4050(7) 0.0131(17) Uiso 0.50 1 d P . .
O2B O -0.0966(13) 1.5905(7) 0.4051(7) 0.0125(17) Uiso 0.50 1 d P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C2 1.974(7) . ?
Pd1 C1 1.981(7) . ?
Pd1 C4 1.983(7) . ?
Pd1 C3 2.000(7) . ?
Fe2 N4 1.933(6) 1_655 ?
Fe2 N4 1.933(6) 2_476 ?
Fe2 N3 1.943(6) . ?
Fe2 N3 1.943(6) 2_576 ?
Fe2 N9 1.975(6) 2_576 ?
Fe2 N9 1.975(6) . ?
C2 N2 1.151(10) . ?
N4 C4 1.162(10) . ?
N4 Fe2 1.933(6) 1_455 ?
N2 Fe1 2.140(6) . ?
C3 N3 1.139(10) . ?
Fe1 N2 2.140(6) 2_577 ?
Fe1 N1 2.142(6) 2_477 ?
Fe1 N1 2.142(6) 1_655 ?
Fe1 N5 2.177(7) 2_577 ?
Fe1 N5 2.177(7) . ?
N5 C5 1.294(11) . ?
N5 N6 1.370(11) . ?
N9 C12 1.306(10) . ?
N9 N10 1.379(8) . ?
C1 N1 1.143(10) . ?
N10 C13 1.296(10) . ?
C14 N12 1.256(11) . ?
C14 C15 1.428(11) . ?
C14 H14 0.9500 . ?
N11 C13 1.336(10) . ?
N11 C12 1.361(10) . ?
N11 N12 1.387(10) . ?
C13 H13 0.9500 . ?
C5 N7 1.337(11) . ?
C5 H5 0.9500 . ?
C12 H12 0.9500 . ?
N7 C6 1.370(15) . ?
N7 N8 1.403(13) . ?
N6 C6 1.289(16) . ?
N1 Fe1 2.142(6) 1_455 ?
C16 C15 1.353(11) . ?
C16 C17 1.397(12) . ?
C16 H16 0.9500 . ?
C15 S2B 1.762(10) . ?
C15 S2A 1.768(10) . ?
C17 C18B 1.36(2) . ?
C17 C18A 1.37(2) . ?
C17 H17 0.9500 . ?
C7 N8 1.175(13) . ?
C7 C8 1.438(11) . ?
C7 H7 0.9500 . ?
C18A S2A 1.72(2) . ?
C18A H18A 0.9500 . ?
S1 C8 1.667(9) . ?
S1 C11 1.691(10) . ?
C8 C9 1.30(2) . ?
C9 C10 1.40(2) . ?
C9 H9 0.9500 . ?
C6 H6 0.9500 . ?
C11 C10 1.261(15) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
S2B C18B 1.718(19) . ?
C18B H18B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 C1 88.2(3) . . ?
C2 Pd1 C4 177.4(3) . . ?
C1 Pd1 C4 90.2(3) . . ?
C2 Pd1 C3 90.0(3) . . ?
C1 Pd1 C3 177.5(3) . . ?
C4 Pd1 C3 91.5(3) . . ?
N4 Fe2 N4 180.0(3) 1_655 2_476 ?
N4 Fe2 N3 90.0(2) 1_655 . ?
N4 Fe2 N3 90.0(2) 2_476 . ?
N4 Fe2 N3 90.0(2) 1_655 2_576 ?
N4 Fe2 N3 90.0(2) 2_476 2_576 ?
N3 Fe2 N3 179.999(1) . 2_576 ?
N4 Fe2 N9 89.8(3) 1_655 2_576 ?
N4 Fe2 N9 90.2(3) 2_476 2_576 ?
N3 Fe2 N9 90.1(2) . 2_576 ?
N3 Fe2 N9 89.9(2) 2_576 2_576 ?
N4 Fe2 N9 90.2(3) 1_655 . ?
N4 Fe2 N9 89.8(3) 2_476 . ?
N3 Fe2 N9 89.9(2) . . ?
N3 Fe2 N9 90.1(2) 2_576 . ?
N9 Fe2 N9 180.000(2) 2_576 . ?
N2 C2 Pd1 176.8(6) . . ?
C4 N4 Fe2 178.4(6) . 1_455 ?
C2 N2 Fe1 164.8(6) . . ?
N4 C4 Pd1 179.7(6) . . ?
N3 C3 Pd1 178.8(6) . . ?
C3 N3 Fe2 179.3(6) . . ?
N2 Fe1 N2 180.000(4) . 2_577 ?
N2 Fe1 N1 93.0(3) . 2_477 ?
N2 Fe1 N1 87.0(3) 2_577 2_477 ?
N2 Fe1 N1 87.0(3) . 1_655 ?
N2 Fe1 N1 93.0(3) 2_577 1_655 ?
N1 Fe1 N1 179.998(3) 2_477 1_655 ?
N2 Fe1 N5 89.0(3) . 2_577 ?
N2 Fe1 N5 91.0(3) 2_577 2_577 ?
N1 Fe1 N5 91.3(3) 2_477 2_577 ?
N1 Fe1 N5 88.7(3) 1_655 2_577 ?
N2 Fe1 N5 91.0(3) . . ?
N2 Fe1 N5 89.0(3) 2_577 . ?
N1 Fe1 N5 88.7(3) 2_477 . ?
N1 Fe1 N5 91.3(3) 1_655 . ?
N5 Fe1 N5 179.999(3) 2_577 . ?
C5 N5 N6 109.3(7) . . ?
C5 N5 Fe1 119.9(6) . . ?
N6 N5 Fe1 130.8(6) . . ?
C12 N9 N10 107.6(6) . . ?
C12 N9 Fe2 130.2(5) . . ?
N10 N9 Fe2 122.2(5) . . ?
N1 C1 Pd1 176.5(7) . . ?
C13 N10 N9 106.8(6) . . ?
N12 C14 C15 125.1(8) . . ?
N12 C14 H14 117.5 . . ?
C15 C14 H14 117.5 . . ?
C13 N11 C12 105.7(7) . . ?
C13 N11 N12 131.3(7) . . ?
C12 N11 N12 123.0(7) . . ?
N10 C13 N11 110.8(7) . . ?
N10 C13 H13 124.6 . . ?
N11 C13 H13 124.6 . . ?
N5 C5 N7 109.9(8) . . ?
N5 C5 H5 125.0 . . ?
N7 C5 H5 125.0 . . ?
N9 C12 N11 109.0(7) . . ?
N9 C12 H12 125.5 . . ?
N11 C12 H12 125.5 . . ?
C14 N12 N11 116.2(8) . . ?
C5 N7 C6 103.9(9) . . ?
C5 N7 N8 131.6(9) . . ?
C6 N7 N8 124.5(9) . . ?
C6 N6 N5 105.0(9) . . ?
C1 N1 Fe1 164.6(6) . 1_455 ?
C15 C16 C17 115.1(8) . . ?
C15 C16 H16 122.4 . . ?
C17 C16 H16 122.4 . . ?
C16 C15 C14 127.2(8) . . ?
C16 C15 S2B 107.7(7) . . ?
C14 C15 S2B 121.5(6) . . ?
C16 C15 S2A 107.7(7) . . ?
C14 C15 S2A 121.5(6) . . ?
S2B C15 S2A 40.9(3) . . ?
C18B C17 C18A 40.2(10) . . ?
C18B C17 C16 109.5(11) . . ?
C18A C17 C16 110.1(11) . . ?
C18B C17 H17 125.2 . . ?
C18A C17 H17 111.3 . . ?
C16 C17 H17 125.2 . . ?
N8 C7 C8 125.7(9) . . ?
N8 C7 H7 117.1 . . ?
C8 C7 H7 117.1 . . ?
C17 C18A S2A 112.2(13) . . ?
C17 C18A H18A 123.9 . . ?
S2A C18A H18A 123.9 . . ?
C7 N8 N7 118.1(10) . . ?
C8 S1 C11 93.6(5) . . ?
C9 C8 C7 127.3(11) . . ?
C9 C8 S1 107.5(10) . . ?
C7 C8 S1 125.2(7) . . ?
C8 C9 C10 115.9(16) . . ?
C8 C9 H9 122.0 . . ?
C10 C9 H9 122.0 . . ?
N6 C6 N7 111.8(11) . . ?
N6 C6 H6 124.1 . . ?
N7 C6 H6 124.1 . . ?
C10 C11 S1 110.4(8) . . ?
C10 C11 H11 124.8 . . ?
S1 C11 H11 124.8 . . ?
C11 C10 C9 112.6(13) . . ?
C11 C10 H10 123.7 . . ?
C9 C10 H10 123.7 . . ?
C18B S2B C15 90.6(7) . . ?
C18A S2A C15 90.9(7) . . ?
C17 C18B S2B 112.8(13) . . ?
C17 C18B H18B 123.6 . . ?
S2B C18B H18B 123.6 . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        28.40
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         4.574
_refine_diff_density_min         -4.423
_refine_diff_density_rms         0.289

# start Validation Reply Form
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: all authors contributed
;
_vrf_PLAT113_I                   
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group.       I2/m       
RESPONSE: space group tested, results in significant disorder
 not present in P-1. PXRD data confirms assigned SG.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 963505'
#######################################################################
#
#                 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_global
#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Fe N12 Pd S2, (H2O, C2H6O)'
_chemical_formula_sum            'C20 H20 Fe N12 Pd S2 O2'
_chemical_formula_weight         685.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  'P -1'

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

_cell_length_a                   7.4566(11)
_cell_length_b                   13.554(3)
_cell_length_c                   14.747(3)
_cell_angle_alpha                69.852(9)
_cell_angle_beta                 90.053(8)
_cell_angle_gamma                74.024(9)
_cell_volume                     1337.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    211
_cell_measurement_theta_min      3.140
_cell_measurement_theta_max      23.313

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_process_details   'SADABS - Bruker- V2.05'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5016
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.03
_reflns_number_total             5016
_reflns_number_gt                3830
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997), X-SEED'
_computing_molecular_graphics    POV_RAY
_computing_publication_material  CHECKCIF

_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)+(0.1228P)²+1.1214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5016
_refine_ls_number_parameters     355
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.2035
_refine_ls_wR_factor_gt          0.1684
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.066
_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 -0.51970(7) 1.03920(5) 0.73928(5) 0.0224(3) Uani 1 1 d . . .
Fe2 Fe 0.0000 1.0000 0.5000 0.0208(5) Uani 1 2 d S . .
C2 C -0.3309(14) 1.0444(8) 0.8334(7) 0.027(2) Uani 1 1 d . . .
N4 N -0.8072(12) 1.0217(8) 0.5956(6) 0.033(2) Uani 1 1 d . . .
N2 N -0.2224(11) 1.0421(8) 0.8886(6) 0.032(2) Uani 1 1 d . . .
C4 C -0.7050(14) 1.0285(9) 0.6478(8) 0.029(2) Uani 1 1 d . . .
C3 C -0.3252(14) 1.0281(9) 0.6494(7) 0.026(2) Uani 1 1 d . . .
N3 N -0.2135(12) 1.0224(8) 0.5950(6) 0.032(2) Uani 1 1 d . . .
Fe1 Fe 0.0000 1.0000 1.0000 0.0229(5) Uani 1 2 d S . .
N5 N -0.0862(12) 1.1670(7) 0.9983(6) 0.039(2) Uani 1 1 d . C .
N9 N -0.0880(11) 1.1777(7) 0.4189(6) 0.0293(19) Uani 1 1 d . . .
C1 C -0.7125(14) 1.0446(8) 0.8318(7) 0.025(2) Uani 1 1 d . . .
N10 N -0.1295(15) 1.2517(7) 0.4653(7) 0.048(3) Uani 1 1 d . . .
C14 C -0.2606(14) 1.5195(9) 0.2131(8) 0.043(3) Uani 1 1 d . . .
H14 H -0.2668 1.5309 0.2718 0.051 Uiso 1 1 calc R . .
N11 N -0.1718(13) 1.3420(7) 0.3096(7) 0.043(2) Uani 1 1 d . . .
C13 C -0.1761(17) 1.3493(10) 0.3993(9) 0.049(3) Uani 1 1 d . . .
H13 H -0.2079 1.4146 0.4114 0.059 Uiso 1 1 calc R . .
C5 C -0.1290(18) 1.2521(10) 0.9178(8) 0.044(3) Uani 1 1 d . C .
H5 H -0.1269 1.2483 0.8561 0.052 Uiso 1 1 calc R . .
C12 C -0.1188(19) 1.2334(10) 0.3256(9) 0.051(3) Uani 1 1 d . . .
H12 H -0.1061 1.2028 0.2775 0.061 Uiso 1 1 calc R . .
N12 N -0.2136(18) 1.4223(8) 0.2168(7) 0.066(3) Uani 1 1 d . . .
N7 N -0.176(2) 1.3446(9) 0.9356(8) 0.082(4) Uani 1 1 d . . .
N6 N -0.106(2) 1.2079(10) 1.0737(8) 0.095(5) Uani 1 1 d . . .
N1 N -0.8210(12) 1.0413(8) 0.8892(6) 0.031(2) Uani 1 1 d . . .
C16 C -0.3582(19) 1.7224(10) 0.1167(10) 0.055(4) Uani 1 1 d . B .
H16 H -0.3672 1.7447 0.1700 0.067 Uiso 1 1 calc R . .
C15 C -0.3054(19) 1.6138(10) 0.1270(9) 0.046(3) Uani 1 1 d . . .
C17 C -0.3972(16) 1.7969(9) 0.0226(8) 0.047(3) Uani 1 1 d . . .
H17 H -0.3952 1.8694 0.0035 0.056 Uiso 1 1 calc R A 1
C7 C -0.2387(16) 1.4785(9) 0.7837(9) 0.049(3) Uani 1 1 d . . .
H7 H -0.2053 1.4202 0.7615 0.059 Uiso 1 1 calc R C .
C18A C -0.308(4) 1.748(2) -0.0393(19) 0.052(7) Uiso 0.50 1 d PU B 2
H18A H -0.2359 1.7715 -0.0893 0.062 Uiso 0.50 1 calc PR B 2
N8 N -0.231(3) 1.4550(10) 0.8709(9) 0.109(6) Uani 1 1 d . C .
C8 C -0.2932(17) 1.5855(10) 0.7120(9) 0.049(3) Uani 1 1 d . C .
C9 C -0.298(4) 1.6128(15) 0.6192(12) 0.145(11) Uani 1 1 d . . .
H9 H -0.2630 1.5600 0.5904 0.174 Uiso 1 1 calc R C .
C6B C -0.097(4) 1.310(2) 1.0344(19) 0.049(6) Uiso 0.50 1 d PU C 2
H6B H -0.0507 1.3494 1.0639 0.059 Uiso 0.50 1 calc PR C 2
O1 O -0.1235(16) 1.2408(9) 0.6595(8) 0.088(3) Uani 1 1 d . . .
C11 C -0.387(2) 1.7784(11) 0.6153(12) 0.077(5) Uani 1 1 d . . .
H11 H -0.3956 1.8527 0.5930 0.093 Uiso 1 1 calc R C 1
C10 C -0.355(4) 1.7203(14) 0.5657(14) 0.131(10) Uani 1 1 d . C .
H10 H -0.3694 1.7480 0.4981 0.157 Uiso 1 1 calc R . .
S2B S -0.3868(13) 1.6091(6) 0.0153(5) 0.062(2) Uani 0.50 1 d PU B 2
S2A S -0.2194(12) 1.6092(6) 0.0157(5) 0.0607(19) Uani 0.50 1 d PU B 1
O2A O -0.1000(17) 1.5919(11) 0.4054(11) 0.042(4) Uani 0.50 1 d P D 1
O2B O -0.4947(18) 1.5923(11) 0.4054(10) 0.040(4) Uani 0.50 1 d P E 2
C18B C -0.440(4) 1.748(2) -0.0393(19) 0.050(6) Uiso 0.50 1 d PU B 1
H18B H -0.5361 1.7699 -0.0888 0.060 Uiso 0.50 1 calc PR B 1
S1B S -0.2835(12) 1.7014(7) 0.7334(6) 0.0613(19) Uani 0.50 1 d PU C 2
S1A S -0.4153(13) 1.7018(6) 0.7335(6) 0.0621(19) Uani 0.50 1 d PU C 1
C6A C -0.227(4) 1.315(2) 1.0292(18) 0.047(6) Uiso 0.50 1 d PU C 1
H6A H -0.3179 1.3559 1.0558 0.057 Uiso 0.50 1 calc PR C 1


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C3 1.976(11) . ?
Pd1 C1 1.987(10) . ?
Pd1 C4 1.998(11) . ?
Pd1 C2 2.009(10) . ?
Fe2 N3 2.150(9) 2_576 ?
Fe2 N3 2.150(9) . ?
Fe2 N4 2.157(8) 2_476 ?
Fe2 N4 2.157(8) 1_655 ?
Fe2 N9 2.192(8) 2_576 ?
Fe2 N9 2.192(8) . ?
C2 N2 1.133(13) . ?
N4 C4 1.127(14) . ?
N4 Fe2 2.157(8) 1_455 ?
N2 Fe1 2.146(8) . ?
C3 N3 1.162(14) . ?
Fe1 N1 2.134(9) 1_655 ?
Fe1 N1 2.134(9) 2_477 ?
Fe1 N2 2.146(8) 2_577 ?
Fe1 N5 2.167(9) . ?
Fe1 N5 2.167(9) 2_577 ?
N5 C5 1.302(14) . ?
N5 N6 1.395(13) . ?
N9 C12 1.305(14) . ?
N9 N10 1.369(12) . ?
C1 N1 1.170(13) . ?
N10 C13 1.295(14) . ?
C14 N12 1.248(15) . ?
C14 C15 1.415(16) . ?
C14 H14 0.9300 . ?
N11 C12 1.350(15) . ?
N11 C13 1.359(14) . ?
N11 N12 1.394(13) . ?
C13 H13 0.9300 . ?
C5 N7 1.322(15) . ?
C5 H5 0.9300 . ?
C12 H12 0.9300 . ?
N7 C6A 1.38(3) . ?
N7 N8 1.412(16) . ?
N7 C6B 1.44(3) . ?
N6 C6B 1.32(3) . ?
N6 C6A 1.41(3) . ?
N1 Fe1 2.134(8) 1_455 ?
C16 C15 1.368(17) . ?
C16 C17 1.379(16) . ?
C16 H16 0.9300 . ?
C15 S2A 1.778(15) . ?
C15 S2B 1.783(14) . ?
C17 C18A 1.37(3) . ?
C17 C18B 1.39(3) . ?
C17 H17 0.9300 . ?
C7 N8 1.211(16) . ?
C7 C8 1.415(16) . ?
C7 H7 0.9300 . ?
C18A S2B 2.03(3) . ?
C18A H18A 0.9300 . ?
C8 C9 1.29(2) . ?
C8 S1B 1.726(14) . ?
C8 S1A 1.723(14) . ?
C9 C10 1.34(2) . ?
C9 H9 0.9300 . ?
C6B H6B 0.9300 . ?
C11 C10 1.23(2) . ?
C11 S1B 1.738(17) . ?
C11 S1A 1.741(18) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?
S2A C18B 2.03(3) . ?
C18B H18B 0.9300 . ?
C6A H6A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Pd1 C1 178.0(4) . . ?
C3 Pd1 C4 90.8(4) . . ?
C1 Pd1 C4 89.1(3) . . ?
C3 Pd1 C2 89.2(3) . . ?
C1 Pd1 C2 90.8(4) . . ?
C4 Pd1 C2 178.1(4) . . ?
N3 Fe2 N3 179.999(2) 2_576 . ?
N3 Fe2 N4 89.3(3) 2_576 2_476 ?
N3 Fe2 N4 90.7(3) . 2_476 ?
N3 Fe2 N4 90.7(3) 2_576 1_655 ?
N3 Fe2 N4 89.3(3) . 1_655 ?
N4 Fe2 N4 180.0(5) 2_476 1_655 ?
N3 Fe2 N9 89.7(3) 2_576 2_576 ?
N3 Fe2 N9 90.3(3) . 2_576 ?
N4 Fe2 N9 89.6(3) 2_476 2_576 ?
N4 Fe2 N9 90.4(3) 1_655 2_576 ?
N3 Fe2 N9 90.3(3) 2_576 . ?
N3 Fe2 N9 89.7(3) . . ?
N4 Fe2 N9 90.3(3) 2_476 . ?
N4 Fe2 N9 89.7(3) 1_655 . ?
N9 Fe2 N9 180.0(4) 2_576 . ?
N2 C2 Pd1 176.7(10) . . ?
C4 N4 Fe2 177.2(10) . 1_455 ?
C2 N2 Fe1 167.6(9) . . ?
N4 C4 Pd1 178.9(10) . . ?
N3 C3 Pd1 178.7(8) . . ?
C3 N3 Fe2 176.1(10) . . ?
N1 Fe1 N1 179.999(2) 1_655 2_477 ?
N1 Fe1 N2 91.3(3) 1_655 2_577 ?
N1 Fe1 N2 88.7(3) 2_477 2_577 ?
N1 Fe1 N2 88.7(3) 1_655 . ?
N1 Fe1 N2 91.4(3) 2_477 . ?
N2 Fe1 N2 179.999(3) 2_577 . ?
N1 Fe1 N5 91.2(3) 1_655 . ?
N1 Fe1 N5 88.8(3) 2_477 . ?
N2 Fe1 N5 89.7(3) 2_577 . ?
N2 Fe1 N5 90.3(3) . . ?
N1 Fe1 N5 88.8(3) 1_655 2_577 ?
N1 Fe1 N5 91.2(3) 2_477 2_577 ?
N2 Fe1 N5 90.3(3) 2_577 2_577 ?
N2 Fe1 N5 89.7(3) . 2_577 ?
N5 Fe1 N5 180.000(3) . 2_577 ?
C5 N5 N6 106.4(10) . . ?
C5 N5 Fe1 122.3(7) . . ?
N6 N5 Fe1 131.3(8) . . ?
C12 N9 N10 107.6(8) . . ?
C12 N9 Fe2 130.9(7) . . ?
N10 N9 Fe2 121.5(6) . . ?
N1 C1 Pd1 176.0(9) . . ?
C13 N10 N9 107.5(9) . . ?
N12 C14 C15 125.5(11) . . ?
N12 C14 H14 117.3 . . ?
C15 C14 H14 117.3 . . ?
C12 N11 C13 105.3(10) . . ?
C12 N11 N12 122.8(10) . . ?
C13 N11 N12 131.8(10) . . ?
N10 C13 N11 109.9(10) . . ?
N10 C13 H13 125.1 . . ?
N11 C13 H13 125.1 . . ?
N5 C5 N7 111.0(10) . . ?
N5 C5 H5 124.5 . . ?
N7 C5 H5 124.5 . . ?
N9 C12 N11 109.6(10) . . ?
N9 C12 H12 125.2 . . ?
N11 C12 H12 125.2 . . ?
C14 N12 N11 115.8(10) . . ?
C5 N7 C6A 104.5(14) . . ?
C5 N7 N8 130.3(11) . . ?
C6A N7 N8 121.7(15) . . ?
C5 N7 C6B 102.7(14) . . ?
C6A N7 C6B 39.3(13) . . ?
N8 N7 C6B 124.2(15) . . ?
C6B N6 N5 105.1(15) . . ?
C6B N6 C6A 40.6(14) . . ?
N5 N6 C6A 103.1(13) . . ?
C1 N1 Fe1 168.3(9) . 1_455 ?
C15 C16 C17 116.0(12) . . ?
C15 C16 H16 122.0 . . ?
C17 C16 H16 122.0 . . ?
C16 C15 C14 129.1(12) . . ?
C16 C15 S2A 105.7(10) . . ?
C14 C15 S2A 121.8(10) . . ?
C16 C15 S2B 106.1(10) . . ?
C14 C15 S2B 121.1(9) . . ?
S2A C15 S2B 41.1(5) . . ?
C18A C17 C16 109.9(14) . . ?
C18A C17 C18B 42.0(14) . . ?
C16 C17 C18B 109.9(15) . . ?
C18A C17 H17 110.5 . . ?
C16 C17 H17 125.0 . . ?
C18B C17 H17 125.0 . . ?
N8 C7 C8 126.8(12) . . ?
N8 C7 H7 116.6 . . ?
C8 C7 H7 116.6 . . ?
C17 C18A S2B 95.9(17) . . ?
C17 C18A H18A 132.1 . . ?
S2B C18A H18A 132.1 . . ?
C7 N8 N7 121.7(11) . . ?
C9 C8 C7 128.1(13) . . ?
C9 C8 S1B 104.6(12) . . ?
C7 C8 S1B 123.7(10) . . ?
C9 C8 S1A 106.5(12) . . ?
C7 C8 S1A 124.0(10) . . ?
S1B C8 S1A 33.1(4) . . ?
C8 C9 C10 117.2(17) . . ?
C8 C9 H9 121.4 . . ?
C10 C9 H9 121.4 . . ?
N6 C6B N7 104(2) . . ?
N6 C6B H6B 128.0 . . ?
N7 C6B H6B 128.0 . . ?
C10 C11 S1B 109.5(13) . . ?
C10 C11 S1A 110.3(13) . . ?
S1B C11 S1A 32.8(4) . . ?
C10 C11 H11 124.8 . . ?
S1B C11 H11 116.3 . . ?
S1A C11 H11 124.8 . . ?
C11 C10 C9 112.8(17) . . ?
C11 C10 H10 123.6 . . ?
C9 C10 H10 123.6 . . ?
C15 S2B C18A 81.6(9) . . ?
C15 S2A C18B 81.7(9) . . ?
C17 C18B S2A 95.2(15) . . ?
C17 C18B H18B 132.4 . . ?
S2A C18B H18B 132.4 . . ?
C8 S1B C11 87.9(7) . . ?
C8 S1A C11 87.9(8) . . ?
N7 C6A N6 102.4(18) . . ?
N7 C6A H6A 128.8 . . ?
N6 C6A H6A 128.8 . . ?

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        27.03
_diffrn_measured_fraction_theta_full 0.929
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.266

# start Validation Reply Form
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: all authors contributed
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.929       
RESPONSE: weakly diffracting and twinned crystal
;
_vrf_PLAT113_I                   
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group.       I2/m       
RESPONSE: space group tested, results in significant disorder
 not present in P-1. PXRD data confirms assigned SG.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 963506'
