 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H22 Cl2 Fe Pd S4'
_chemical_formula_weight          623.77
 
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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3010   0.8450
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'  -1.1770   1.0070
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
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                    12.3174(18)
_cell_length_b                    12.9617(9)
_cell_length_c                    14.791(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  107.619(15)
_cell_angle_gamma                 90.00
_cell_volume                      2250.7(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.841
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1248
_exptl_absorpt_coefficient_mu     1.980
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             9468
_diffrn_reflns_av_R_equivalents   0.0620
_diffrn_reflns_av_sigmaI/netI     0.0526
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          2.13
_diffrn_reflns_theta_max          24.91
_reflns_number_total              3436
_reflns_number_gt                 3037
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_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 > 2σ(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)+(0.0463P)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     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3436
_refine_ls_number_parameters      275
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0379
_refine_ls_R_factor_gt            0.0330
_refine_ls_wR_factor_ref          0.0814
_refine_ls_wR_factor_gt           0.0805
_refine_ls_goodness_of_fit_ref    1.013
_refine_ls_restrained_S_all       1.013
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pd Pd 0.28942(2) 0.233142(19) 0.357448(19) 0.01576(12) Uani 1 1 d . . .
Fe Fe 0.21112(5) -0.28133(4) 0.37885(4) 0.01648(15) Uani 1 1 d . . .
Cl1 Cl 0.43469(8) 0.34270(7) 0.34793(7) 0.0298(2) Uani 1 1 d . . .
Cl2 Cl 0.17364(8) 0.37749(6) 0.34527(7) 0.0260(2) Uani 1 1 d . . .
S1 S 0.13283(8) 0.13817(6) 0.36460(6) 0.0174(2) Uani 1 1 d . . .
S2 S 0.27603(8) 0.01697(7) 0.53415(6) 0.0206(2) Uani 1 1 d . . .
S3 S 0.41547(8) 0.09738(6) 0.36859(6) 0.0185(2) Uani 1 1 d . . .
S4 S 0.23716(8) -0.00481(7) 0.20763(6) 0.0199(2) Uani 1 1 d . . .
C1 C 0.1686(3) 0.0166(3) 0.4243(2) 0.0157(8) Uani 1 1 d . . .
C2 C 0.2124(4) 0.1053(3) 0.6002(3) 0.0275(9) Uani 1 1 d . . .
H2A H 0.1462 0.0724 0.6103 0.040(13) Uiso 1 1 calc R . .
H2B H 0.2669 0.1180 0.6620 0.034(11) Uiso 1 1 calc R . .
C3 C 0.1765(4) 0.2081(3) 0.5504(3) 0.0280(10) Uani 1 1 d . . .
H3A H 0.1503 0.2529 0.5920 0.032(11) Uiso 1 1 calc R . .
H3B H 0.2426 0.2403 0.5398 0.034(12) Uiso 1 1 calc R . .
C4 C 0.0835(3) 0.2000(3) 0.4564(3) 0.0251(9) Uani 1 1 d . . .
H4A H 0.0558 0.2687 0.4354 0.058(15) Uiso 1 1 calc R . .
H4B H 0.0205 0.1607 0.4652 0.042(13) Uiso 1 1 calc R . .
C5 C 0.1081(3) -0.0650(2) 0.3804(2) 0.0147(8) Uani 1 1 d . . .
H5 H 0.0568 -0.0512 0.3212 0.022(10) Uiso 1 1 calc R . .
C6 C 0.1105(3) -0.1713(3) 0.4112(2) 0.0171(8) Uani 1 1 d . . .
C7 C 0.0418(3) -0.2487(3) 0.3509(3) 0.0215(8) Uani 1 1 d . . .
H7 H -0.0105 -0.2369 0.2916 0.039(12) Uiso 1 1 calc R . .
C8 C 0.0663(3) -0.3456(3) 0.3961(3) 0.0246(9) Uani 1 1 d . . .
H8 H 0.0339 -0.4084 0.3718 0.011(9) Uiso 1 1 calc R . .
C9 C 0.1493(3) -0.3297(3) 0.4853(3) 0.0239(9) Uani 1 1 d . . .
H9 H 0.1798 -0.3807 0.5300 0.011(9) Uiso 1 1 calc R . .
C10 C 0.1783(3) -0.2236(3) 0.4951(3) 0.0194(8) Uani 1 1 d . . .
H10 H 0.2316 -0.1932 0.5467 0.020(10) Uiso 1 1 calc R . .
C11 C 0.3423(3) -0.0176(3) 0.3182(2) 0.0168(8) Uani 1 1 d . . .
C12 C 0.3264(3) 0.0418(3) 0.1370(3) 0.0247(9) Uani 1 1 d . . .
H12A H 0.3765 -0.0135 0.1304 0.046(13) Uiso 1 1 calc R . .
H12B H 0.2778 0.0595 0.0740 0.026(10) Uiso 1 1 calc R . .
C13 C 0.3982(3) 0.1350(3) 0.1793(3) 0.0273(9) Uani 1 1 d . . .
H13A H 0.4389 0.1571 0.1359 0.029(11) Uiso 1 1 calc R . .
H13B H 0.3475 0.1907 0.1840 0.031(11) Uiso 1 1 calc R . .
C14 C 0.4835(3) 0.1188(3) 0.2758(3) 0.0255(9) Uani 1 1 d . . .
H14A H 0.5326 0.1788 0.2922 0.024(10) Uiso 1 1 calc R . .
H14B H 0.5308 0.0597 0.2732 0.016(9) Uiso 1 1 calc R . .
C15 C 0.3764(3) -0.1058(3) 0.3667(3) 0.0173(8) Uani 1 1 d . . .
H15 H 0.4316 -0.0976 0.4251 0.007(8) Uiso 1 1 calc R . .
C16 C 0.3407(3) -0.2116(3) 0.3422(3) 0.0201(8) Uani 1 1 d . . .
C17 C 0.2588(4) -0.2561(3) 0.2601(3) 0.0260(9) Uani 1 1 d . . .
H17 H 0.2167 -0.2205 0.2063 0.023(11) Uiso 1 1 calc R . .
C18 C 0.2538(4) -0.3636(3) 0.2761(3) 0.0287(10) Uani 1 1 d . . .
H18 H 0.2080 -0.4107 0.2341 0.029(11) Uiso 1 1 calc R . .
C19 C 0.3305(4) -0.3876(3) 0.3669(3) 0.0295(10) Uani 1 1 d . . .
H19 H 0.3435 -0.4528 0.3943 0.023(10) Uiso 1 1 calc R . .
C20 C 0.3834(3) -0.2947(3) 0.4080(3) 0.0249(9) Uani 1 1 d . . .
H20 H 0.4368 -0.2884 0.4675 0.023(11) Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Pd S1 2.3175(9) . ?
Pd S3 2.3193(9) . ?
Pd Cl1 2.3217(10) . ?
Pd Cl2 2.3262(9) . ?
Fe C10 2.026(4) . ?
Fe C6 2.039(3) . ?
Fe C17 2.040(4) . ?
Fe C20 2.041(4) . ?
Fe C9 2.044(4) . ?
Fe C7 2.044(4) . ?
Fe C16 2.045(4) . ?
Fe C18 2.052(4) . ?
Fe C8 2.053(4) . ?
Fe C19 2.061(4) . ?
S1 C1 1.795(3) . ?
S1 C4 1.832(4) . ?
S2 C1 1.757(4) . ?
S2 C2 1.828(4) . ?
S3 C11 1.784(3) . ?
S3 C14 1.832(4) . ?
S4 C11 1.760(4) . ?
S4 C12 1.833(4) . ?
C1 C5 1.343(5) . ?
C2 C3 1.523(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.513(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.449(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.436(5) . ?
C6 C10 1.439(5) . ?
C7 C8 1.412(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.418(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.417(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C15 1.347(5) . ?
C12 C13 1.516(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.509(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.453(5) . ?
C15 H15 0.9300 . ?
C16 C20 1.441(5) . ?
C16 C17 1.443(5) . ?
C17 C18 1.418(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.423(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.416(5) . ?
C19 H19 0.9300 . ?
C20 H20 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
S1 Pd S3 98.18(3) . . ?
S1 Pd Cl1 174.29(3) . . ?
S3 Pd Cl1 87.52(3) . . ?
S1 Pd Cl2 86.08(3) . . ?
S3 Pd Cl2 175.74(3) . . ?
Cl1 Pd Cl2 88.23(4) . . ?
C10 Fe C6 41.46(14) . . ?
C10 Fe C17 148.80(14) . . ?
C6 Fe C17 116.34(15) . . ?
C10 Fe C20 108.31(16) . . ?
C6 Fe C20 132.61(15) . . ?
C17 Fe C20 69.13(17) . . ?
C10 Fe C9 40.76(14) . . ?
C6 Fe C9 68.85(14) . . ?
C17 Fe C9 169.70(15) . . ?
C20 Fe C9 114.64(16) . . ?
C10 Fe C7 69.00(15) . . ?
C6 Fe C7 41.17(14) . . ?
C17 Fe C7 109.54(16) . . ?
C20 Fe C7 172.94(14) . . ?
C9 Fe C7 67.93(15) . . ?
C10 Fe C16 115.76(15) . . ?
C6 Fe C16 109.40(14) . . ?
C17 Fe C16 41.37(15) . . ?
C20 Fe C16 41.29(14) . . ?
C9 Fe C16 147.41(16) . . ?
C7 Fe C16 133.27(15) . . ?
C10 Fe C18 169.44(15) . . ?
C6 Fe C18 147.98(16) . . ?
C17 Fe C18 40.56(15) . . ?
C20 Fe C18 68.22(17) . . ?
C9 Fe C18 130.54(15) . . ?
C7 Fe C18 115.61(17) . . ?
C16 Fe C18 68.74(15) . . ?
C10 Fe C8 68.89(15) . . ?
C6 Fe C8 69.00(14) . . ?
C17 Fe C8 131.25(16) . . ?
C20 Fe C8 145.69(15) . . ?
C9 Fe C8 40.50(15) . . ?
C7 Fe C8 40.31(14) . . ?
C16 Fe C8 171.60(15) . . ?
C18 Fe C8 107.96(15) . . ?
C10 Fe C19 130.60(15) . . ?
C6 Fe C19 170.98(16) . . ?
C17 Fe C19 68.57(16) . . ?
C20 Fe C19 40.38(15) . . ?
C9 Fe C19 107.61(15) . . ?
C7 Fe C19 146.26(15) . . ?
C16 Fe C19 68.79(14) . . ?
C18 Fe C19 40.48(16) . . ?
C8 Fe C19 114.12(15) . . ?
C1 S1 C4 96.11(16) . . ?
C1 S1 Pd 113.89(12) . . ?
C4 S1 Pd 105.57(13) . . ?
C1 S2 C2 99.87(17) . . ?
C11 S3 C14 95.84(17) . . ?
C11 S3 Pd 111.18(12) . . ?
C14 S3 Pd 106.25(13) . . ?
C11 S4 C12 99.29(17) . . ?
C5 C1 S2 127.0(3) . . ?
C5 C1 S1 115.8(3) . . ?
S2 C1 S1 117.16(19) . . ?
C3 C2 S2 113.4(3) . . ?
C3 C2 H2A 108.9 . . ?
S2 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
S2 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 114.4(3) . . ?
C4 C3 H3A 108.7 . . ?
C2 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 S1 112.5(3) . . ?
C3 C4 H4A 109.1 . . ?
S1 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
S1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C1 C5 C6 129.9(3) . . ?
C1 C5 H5 115.0 . . ?
C6 C5 H5 115.0 . . ?
C7 C6 C10 106.6(3) . . ?
C7 C6 C5 121.1(3) . . ?
C10 C6 C5 132.1(3) . . ?
C7 C6 Fe 69.6(2) . . ?
C10 C6 Fe 68.8(2) . . ?
C5 C6 Fe 123.2(2) . . ?
C8 C7 C6 109.0(3) . . ?
C8 C7 Fe 70.2(2) . . ?
C6 C7 Fe 69.2(2) . . ?
C8 C7 H7 125.5 . . ?
C6 C7 H7 125.5 . . ?
Fe C7 H7 126.7 . . ?
C7 C8 C9 107.6(3) . . ?
C7 C8 Fe 69.5(2) . . ?
C9 C8 Fe 69.4(2) . . ?
C7 C8 H8 126.2 . . ?
C9 C8 H8 126.2 . . ?
Fe C8 H8 126.5 . . ?
C10 C9 C8 108.9(3) . . ?
C10 C9 Fe 68.9(2) . . ?
C8 C9 Fe 70.1(2) . . ?
C10 C9 H9 125.5 . . ?
C8 C9 H9 125.5 . . ?
Fe C9 H9 127.0 . . ?
C9 C10 C6 107.8(3) . . ?
C9 C10 Fe 70.3(2) . . ?
C6 C10 Fe 69.8(2) . . ?
C9 C10 H10 126.1 . . ?
C6 C10 H10 126.1 . . ?
Fe C10 H10 125.4 . . ?
C15 C11 S4 126.7(3) . . ?
C15 C11 S3 116.7(3) . . ?
S4 C11 S3 116.50(19) . . ?
C13 C12 S4 113.7(3) . . ?
C13 C12 H12A 108.8 . . ?
S4 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
S4 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 C12 115.6(3) . . ?
C14 C13 H13A 108.4 . . ?
C12 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.4 . . ?
C13 C14 S3 112.6(3) . . ?
C13 C14 H14A 109.1 . . ?
S3 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
S3 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C11 C15 C16 130.3(4) . . ?
C11 C15 H15 114.9 . . ?
C16 C15 H15 114.9 . . ?
C20 C16 C17 106.8(3) . . ?
C20 C16 C15 121.1(3) . . ?
C17 C16 C15 132.0(3) . . ?
C20 C16 Fe 69.2(2) . . ?
C17 C16 Fe 69.1(2) . . ?
C15 C16 Fe 123.5(3) . . ?
C18 C17 C16 107.9(4) . . ?
C18 C17 Fe 70.2(2) . . ?
C16 C17 Fe 69.5(2) . . ?
C18 C17 H17 126.1 . . ?
C16 C17 H17 126.1 . . ?
Fe C17 H17 125.8 . . ?
C17 C18 C19 108.8(4) . . ?
C17 C18 Fe 69.3(2) . . ?
C19 C18 Fe 70.1(2) . . ?
C17 C18 H18 125.6 . . ?
C19 C18 H18 125.6 . . ?
Fe C18 H18 126.6 . . ?
C20 C19 C18 107.9(3) . . ?
C20 C19 Fe 69.0(2) . . ?
C18 C19 Fe 69.4(2) . . ?
C20 C19 H19 126.0 . . ?
C18 C19 H19 126.0 . . ?
Fe C19 H19 127.1 . . ?
C19 C20 C16 108.6(4) . . ?
C19 C20 Fe 70.6(2) . . ?
C16 C20 Fe 69.5(2) . . ?
C19 C20 H20 125.7 . . ?
C16 C20 H20 125.7 . . ?
Fe C20 H20 125.8 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
S3 Pd S1 C1 25.33(13) . . . . ?
Cl2 Pd S1 C1 -154.80(13) . . . . ?
S3 Pd S1 C4 129.48(13) . . . . ?
Cl2 Pd S1 C4 -50.66(13) . . . . ?
S1 Pd S3 C11 30.09(13) . . . . ?
Cl1 Pd S3 C11 -149.50(13) . . . . ?
S1 Pd S3 C14 133.19(13) . . . . ?
Cl1 Pd S3 C14 -46.40(14) . . . . ?
C2 S2 C1 C5 -119.2(3) . . . . ?
C2 S2 C1 S1 59.4(2) . . . . ?
C4 S1 C1 C5 116.3(3) . . . . ?
Pd S1 C1 C5 -133.6(2) . . . . ?
C4 S1 C1 S2 -62.4(2) . . . . ?
Pd S1 C1 S2 47.6(2) . . . . ?
C1 S2 C2 C3 -53.3(3) . . . . ?
S2 C2 C3 C4 63.7(4) . . . . ?
C2 C3 C4 S1 -69.5(4) . . . . ?
C1 S1 C4 C3 61.6(3) . . . . ?
Pd S1 C4 C3 -55.3(3) . . . . ?
S2 C1 C5 C6 2.6(6) . . . . ?
S1 C1 C5 C6 -176.0(3) . . . . ?
C1 C5 C6 C7 -177.0(4) . . . . ?
C1 C5 C6 C10 -1.8(7) . . . . ?
C1 C5 C6 Fe -92.3(4) . . . . ?
C10 Fe C6 C7 -118.2(3) . . . . ?
C17 Fe C6 C7 90.0(2) . . . . ?
C20 Fe C6 C7 175.2(2) . . . . ?
C9 Fe C6 C7 -80.2(2) . . . . ?
C16 Fe C6 C7 134.5(2) . . . . ?
C18 Fe C6 C7 53.8(4) . . . . ?
C8 Fe C6 C7 -36.7(2) . . . . ?
C17 Fe C6 C10 -151.8(2) . . . . ?
C20 Fe C6 C10 -66.6(3) . . . . ?
C9 Fe C6 C10 37.9(2) . . . . ?
C7 Fe C6 C10 118.2(3) . . . . ?
C16 Fe C6 C10 -107.3(2) . . . . ?
C18 Fe C6 C10 172.0(3) . . . . ?
C8 Fe C6 C10 81.5(2) . . . . ?
C10 Fe C6 C5 127.2(4) . . . . ?
C17 Fe C6 C5 -24.5(4) . . . . ?
C20 Fe C6 C5 60.6(4) . . . . ?
C9 Fe C6 C5 165.2(3) . . . . ?
C7 Fe C6 C5 -114.6(4) . . . . ?
C16 Fe C6 C5 19.9(3) . . . . ?
C18 Fe C6 C5 -60.7(4) . . . . ?
C8 Fe C6 C5 -151.3(3) . . . . ?
C10 C6 C7 C8 0.0(4) . . . . ?
C5 C6 C7 C8 176.3(3) . . . . ?
Fe C6 C7 C8 59.1(3) . . . . ?
C10 C6 C7 Fe -59.1(2) . . . . ?
C5 C6 C7 Fe 117.2(3) . . . . ?
C10 Fe C7 C8 -81.7(2) . . . . ?
C6 Fe C7 C8 -120.4(3) . . . . ?
C17 Fe C7 C8 131.5(2) . . . . ?
C9 Fe C7 C8 -37.8(2) . . . . ?
C16 Fe C7 C8 172.1(2) . . . . ?
C18 Fe C7 C8 87.9(2) . . . . ?
C19 Fe C7 C8 51.1(4) . . . . ?
C10 Fe C7 C6 38.7(2) . . . . ?
C17 Fe C7 C6 -108.0(2) . . . . ?
C9 Fe C7 C6 82.7(2) . . . . ?
C16 Fe C7 C6 -67.5(3) . . . . ?
C18 Fe C7 C6 -151.7(2) . . . . ?
C8 Fe C7 C6 120.4(3) . . . . ?
C19 Fe C7 C6 171.6(2) . . . . ?
C6 C7 C8 C9 0.7(4) . . . . ?
Fe C7 C8 C9 59.1(3) . . . . ?
C6 C7 C8 Fe -58.5(3) . . . . ?
C10 Fe C8 C7 82.0(2) . . . . ?
C6 Fe C8 C7 37.4(2) . . . . ?
C17 Fe C8 C7 -69.7(3) . . . . ?
C20 Fe C8 C7 173.8(3) . . . . ?
C9 Fe C8 C7 119.1(3) . . . . ?
C18 Fe C8 C7 -108.7(2) . . . . ?
C19 Fe C8 C7 -151.7(2) . . . . ?
C10 Fe C8 C9 -37.0(2) . . . . ?
C6 Fe C8 C9 -81.6(2) . . . . ?
C17 Fe C8 C9 171.2(2) . . . . ?
C20 Fe C8 C9 54.8(3) . . . . ?
C7 Fe C8 C9 -119.1(3) . . . . ?
C18 Fe C8 C9 132.3(2) . . . . ?
C19 Fe C8 C9 89.2(2) . . . . ?
C7 C8 C9 C10 -1.1(4) . . . . ?
Fe C8 C9 C10 58.1(3) . . . . ?
C7 C8 C9 Fe -59.2(3) . . . . ?
C6 Fe C9 C10 -38.6(2) . . . . ?
C17 Fe C9 C10 -160.7(8) . . . . ?
C20 Fe C9 C10 89.8(2) . . . . ?
C7 Fe C9 C10 -83.0(2) . . . . ?
C16 Fe C9 C10 54.6(4) . . . . ?
C18 Fe C9 C10 171.5(2) . . . . ?
C8 Fe C9 C10 -120.6(3) . . . . ?
C19 Fe C9 C10 132.6(2) . . . . ?
C10 Fe C9 C8 120.6(3) . . . . ?
C6 Fe C9 C8 82.0(2) . . . . ?
C17 Fe C9 C8 -40.1(10) . . . . ?
C20 Fe C9 C8 -149.6(2) . . . . ?
C7 Fe C9 C8 37.6(2) . . . . ?
C16 Fe C9 C8 175.2(3) . . . . ?
C18 Fe C9 C8 -67.9(3) . . . . ?
C19 Fe C9 C8 -106.8(2) . . . . ?
C8 C9 C10 C6 1.1(4) . . . . ?
Fe C9 C10 C6 59.9(2) . . . . ?
C8 C9 C10 Fe -58.8(3) . . . . ?
C7 C6 C10 C9 -0.7(4) . . . . ?
C5 C6 C10 C9 -176.4(4) . . . . ?
Fe C6 C10 C9 -60.3(2) . . . . ?
C7 C6 C10 Fe 59.6(2) . . . . ?
C5 C6 C10 Fe -116.1(4) . . . . ?
C6 Fe C10 C9 118.6(3) . . . . ?
C17 Fe C10 C9 173.5(3) . . . . ?
C20 Fe C10 C9 -106.8(2) . . . . ?
C7 Fe C10 C9 80.1(2) . . . . ?
C16 Fe C10 C9 -150.8(2) . . . . ?
C18 Fe C10 C9 -37.7(10) . . . . ?
C8 Fe C10 C9 36.8(2) . . . . ?
C19 Fe C10 C9 -67.4(3) . . . . ?
C17 Fe C10 C6 54.9(4) . . . . ?
C20 Fe C10 C6 134.6(2) . . . . ?
C9 Fe C10 C6 -118.6(3) . . . . ?
C7 Fe C10 C6 -38.4(2) . . . . ?
C16 Fe C10 C6 90.6(2) . . . . ?
C18 Fe C10 C6 -156.3(8) . . . . ?
C8 Fe C10 C6 -81.8(2) . . . . ?
C19 Fe C10 C6 174.0(2) . . . . ?
C12 S4 C11 C15 -115.6(3) . . . . ?
C12 S4 C11 S3 61.3(2) . . . . ?
C14 S3 C11 C15 112.6(3) . . . . ?
Pd S3 C11 C15 -137.5(3) . . . . ?
C14 S3 C11 S4 -64.6(2) . . . . ?
Pd S3 C11 S4 45.3(2) . . . . ?
C11 S4 C12 C13 -52.7(3) . . . . ?
S4 C12 C13 C14 61.6(4) . . . . ?
C12 C13 C14 S3 -67.5(4) . . . . ?
C11 S3 C14 C13 61.6(3) . . . . ?
Pd S3 C14 C13 -52.5(3) . . . . ?
S4 C11 C15 C16 1.8(6) . . . . ?
S3 C11 C15 C16 -175.1(3) . . . . ?
C11 C15 C16 C20 -175.8(4) . . . . ?
C11 C15 C16 C17 -0.2(7) . . . . ?
C11 C15 C16 Fe -91.4(5) . . . . ?
C10 Fe C16 C20 88.8(2) . . . . ?
C6 Fe C16 C20 133.4(2) . . . . ?
C17 Fe C16 C20 -118.4(3) . . . . ?
C9 Fe C16 C20 52.5(4) . . . . ?
C7 Fe C16 C20 173.5(2) . . . . ?
C18 Fe C16 C20 -80.8(2) . . . . ?
C19 Fe C16 C20 -37.2(2) . . . . ?
C10 Fe C16 C17 -152.8(2) . . . . ?
C6 Fe C16 C17 -108.2(2) . . . . ?
C20 Fe C16 C17 118.4(3) . . . . ?
C9 Fe C16 C17 171.0(3) . . . . ?
C7 Fe C16 C17 -68.0(3) . . . . ?
C18 Fe C16 C17 37.7(2) . . . . ?
C19 Fe C16 C17 81.2(2) . . . . ?
C10 Fe C16 C15 -25.5(4) . . . . ?
C6 Fe C16 C15 19.1(4) . . . . ?
C17 Fe C16 C15 127.3(4) . . . . ?
C20 Fe C16 C15 -114.3(4) . . . . ?
C9 Fe C16 C15 -61.7(4) . . . . ?
C7 Fe C16 C15 59.3(4) . . . . ?
C18 Fe C16 C15 165.0(4) . . . . ?
C19 Fe C16 C15 -151.5(4) . . . . ?
C20 C16 C17 C18 -0.8(4) . . . . ?
C15 C16 C17 C18 -176.8(4) . . . . ?
Fe C16 C17 C18 -59.9(3) . . . . ?
C20 C16 C17 Fe 59.2(3) . . . . ?
C15 C16 C17 Fe -116.9(4) . . . . ?
C10 Fe C17 C18 171.6(3) . . . . ?
C6 Fe C17 C18 -151.2(2) . . . . ?
C20 Fe C17 C18 80.5(3) . . . . ?
C9 Fe C17 C18 -33.0(10) . . . . ?
C7 Fe C17 C18 -106.9(3) . . . . ?
C16 Fe C17 C18 118.9(4) . . . . ?
C8 Fe C17 C18 -66.8(3) . . . . ?
C19 Fe C17 C18 37.1(3) . . . . ?
C10 Fe C17 C16 52.7(4) . . . . ?
C6 Fe C17 C16 89.9(2) . . . . ?
C20 Fe C17 C16 -38.4(2) . . . . ?
C9 Fe C17 C16 -151.9(8) . . . . ?
C7 Fe C17 C16 134.2(2) . . . . ?
C18 Fe C17 C16 -118.9(4) . . . . ?
C8 Fe C17 C16 174.3(2) . . . . ?
C19 Fe C17 C16 -81.8(2) . . . . ?
C16 C17 C18 C19 0.4(4) . . . . ?
Fe C17 C18 C19 -59.1(3) . . . . ?
C16 C17 C18 Fe 59.5(3) . . . . ?
C10 Fe C18 C17 -155.6(8) . . . . ?
C6 Fe C18 C17 54.5(4) . . . . ?
C20 Fe C18 C17 -82.9(3) . . . . ?
C9 Fe C18 C17 172.6(2) . . . . ?
C7 Fe C18 C17 90.6(3) . . . . ?
C16 Fe C18 C17 -38.4(3) . . . . ?
C8 Fe C18 C17 133.4(3) . . . . ?
C19 Fe C18 C17 -120.2(4) . . . . ?
C10 Fe C18 C19 -35.4(10) . . . . ?
C6 Fe C18 C19 174.7(2) . . . . ?
C17 Fe C18 C19 120.2(4) . . . . ?
C20 Fe C18 C19 37.3(2) . . . . ?
C9 Fe C18 C19 -67.1(3) . . . . ?
C7 Fe C18 C19 -149.2(2) . . . . ?
C16 Fe C18 C19 81.8(2) . . . . ?
C8 Fe C18 C19 -106.4(2) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
Fe C18 C19 C20 -58.5(3) . . . . ?
C17 C18 C19 Fe 58.6(3) . . . . ?
C10 Fe C19 C20 -68.3(3) . . . . ?
C17 Fe C19 C20 82.6(3) . . . . ?
C9 Fe C19 C20 -107.6(2) . . . . ?
C7 Fe C19 C20 176.0(3) . . . . ?
C16 Fe C19 C20 38.0(2) . . . . ?
C18 Fe C19 C20 119.7(3) . . . . ?
C8 Fe C19 C20 -150.5(2) . . . . ?
C10 Fe C19 C18 172.0(2) . . . . ?
C17 Fe C19 C18 -37.1(2) . . . . ?
C20 Fe C19 C18 -119.7(3) . . . . ?
C9 Fe C19 C18 132.7(2) . . . . ?
C7 Fe C19 C18 56.3(4) . . . . ?
C16 Fe C19 C18 -81.7(2) . . . . ?
C8 Fe C19 C18 89.8(2) . . . . ?
C18 C19 C20 C16 -0.6(4) . . . . ?
Fe C19 C20 C16 -59.3(3) . . . . ?
C18 C19 C20 Fe 58.7(3) . . . . ?
C17 C16 C20 C19 0.9(4) . . . . ?
C15 C16 C20 C19 177.4(3) . . . . ?
Fe C16 C20 C19 60.0(3) . . . . ?
C17 C16 C20 Fe -59.1(3) . . . . ?
C15 C16 C20 Fe 117.5(3) . . . . ?
C10 Fe C20 C19 132.0(2) . . . . ?
C6 Fe C20 C19 171.8(2) . . . . ?
C17 Fe C20 C19 -81.1(3) . . . . ?
C9 Fe C20 C19 88.5(3) . . . . ?
C16 Fe C20 C19 -119.5(3) . . . . ?
C18 Fe C20 C19 -37.4(2) . . . . ?
C8 Fe C20 C19 52.8(4) . . . . ?
C10 Fe C20 C16 -108.5(2) . . . . ?
C6 Fe C20 C16 -68.7(3) . . . . ?
C17 Fe C20 C16 38.5(2) . . . . ?
C9 Fe C20 C16 -151.9(2) . . . . ?
C18 Fe C20 C16 82.1(2) . . . . ?
C8 Fe C20 C16 172.4(3) . . . . ?
C19 Fe C20 C16 119.5(3) . . . . ?
 
_diffrn_measured_fraction_theta_max    0.876
_diffrn_reflns_theta_full              24.91
_diffrn_measured_fraction_theta_full   0.876
_refine_diff_density_max    1.234
_refine_diff_density_min   -0.544
_refine_diff_density_rms    0.127
