# Electronic Supplementary Material (ESI) for RSC Advances.
# 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.
#
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#  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
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#  data retrieval see:
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data_sos073

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H44 Cu F6 Fe N4 P'
_chemical_formula_weight         941.23

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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)/n

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

_cell_length_a                   12.6769(12)
_cell_length_b                   17.8460(16)
_cell_length_c                   18.8833(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.382(5)
_cell_angle_gamma                90.00
_cell_volume                     4226.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9249
_cell_measurement_theta_min      2.5295
_cell_measurement_theta_max      26.163

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6340
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            97906
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.42
_reflns_number_total             8666
_reflns_number_gt                7369
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of 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)+(0.0442P)²+5.8037P] 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         8666
_refine_ls_number_parameters     556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1142
_refine_ls_wR_factor_gt          0.1078
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Cu1 Cu 0.38190(3) 0.222119(18) 0.829192(16) 0.02078(10) Uani 1 1 d . . .
Fe1 Fe -0.13583(3) 0.11427(2) 0.83179(2) 0.02625(11) Uani 1 1 d . . .
P1 P -0.18198(6) 0.44912(4) 0.92789(4) 0.02409(16) Uani 1 1 d . . .
F1 F -0.06104(13) 0.42695(10) 0.95546(10) 0.0378(4) Uani 1 1 d . . .
F2 F -0.14926(14) 0.53549(10) 0.92259(10) 0.0387(4) Uani 1 1 d . . .
F3 F -0.16296(14) 0.43630(11) 0.84658(9) 0.0384(4) Uani 1 1 d . . .
F4 F -0.30405(12) 0.47131(10) 0.90017(9) 0.0335(4) Uani 1 1 d . . .
F5 F -0.20236(15) 0.46156(10) 1.00843(9) 0.0379(4) Uani 1 1 d . . .
F6 F -0.21647(14) 0.36269(9) 0.93183(10) 0.0362(4) Uani 1 1 d . . .
N4 N 0.43947(17) 0.11605(12) 0.82465(11) 0.0196(5) Uani 1 1 d . . .
N3 N 0.42143(17) 0.22151(12) 0.72853(11) 0.0205(5) Uani 1 1 d . . .
N1 N 0.23143(17) 0.24277(12) 0.84942(11) 0.0214(5) Uani 1 1 d . . .
N2 N 0.41711(17) 0.30384(12) 0.90292(11) 0.0203(5) Uani 1 1 d . . .
C35 C 0.4701(2) 0.09639(15) 0.76152(14) 0.0226(6) Uani 1 1 d . . .
C36 C 0.5169(2) 0.02705(16) 0.75220(15) 0.0260(6) Uani 1 1 d . . .
H36 H 0.5379 0.0142 0.7086 0.031 Uiso 1 1 calc R . .
C37 C 0.5312(2) -0.02227(16) 0.80951(16) 0.0284(6) Uani 1 1 d . . .
H37 H 0.5626 -0.0687 0.8048 0.034 Uiso 1 1 calc R . .
C38 C 0.4986(2) -0.00228(16) 0.87370(16) 0.0268(6) Uani 1 1 d . . .
H38 H 0.5074 -0.0353 0.9122 0.032 Uiso 1 1 calc R . .
C39 C 0.4528(2) 0.06739(15) 0.87994(14) 0.0227(6) Uani 1 1 d . . .
C40 C 0.4148(2) 0.09651(15) 0.94623(14) 0.0233(6) Uani 1 1 d . . .
C47 C 0.4781(2) 0.14755(15) 0.99043(14) 0.0247(6) Uani 1 1 d . . .
C46 C 0.4355(2) 0.18227(16) 1.04584(15) 0.0291(6) Uani 1 1 d . . .
H46 H 0.4770 0.2165 1.0748 0.035 Uiso 1 1 calc R . .
C44 C 0.3333(2) 0.16728(17) 1.05902(15) 0.0308(7) Uani 1 1 d . . .
C45 C 0.2872(3) 0.20764(19) 1.11814(18) 0.0432(8) Uani 1 1 d . . .
H45A H 0.2115 0.1997 1.1125 0.065 Uiso 1 1 calc R . .
H45B H 0.3015 0.2603 1.1157 0.065 Uiso 1 1 calc R . .
H45C H 0.3193 0.1885 1.1637 0.065 Uiso 1 1 calc R . .
C43 C 0.2739(2) 0.11444(16) 1.01713(15) 0.0295(6) Uani 1 1 d . . .
H43 H 0.2061 0.1026 1.0270 0.035 Uiso 1 1 calc R . .
C41 C 0.3121(2) 0.07804(16) 0.96026(15) 0.0269(6) Uani 1 1 d . . .
C42 C 0.2425(2) 0.02391(18) 0.91375(16) 0.0334(7) Uani 1 1 d . . .
H42A H 0.1839 0.0090 0.9375 0.050 Uiso 1 1 calc R . .
H42B H 0.2835 -0.0194 0.9049 0.050 Uiso 1 1 calc R . .
H42C H 0.2156 0.0476 0.8691 0.050 Uiso 1 1 calc R . .
C48 C 0.5911(2) 0.16295(17) 0.97917(15) 0.0295(6) Uani 1 1 d . . .
H48A H 0.6174 0.2060 1.0066 0.044 Uiso 1 1 calc R . .
H48B H 0.5932 0.1723 0.9293 0.044 Uiso 1 1 calc R . .
H48C H 0.6348 0.1203 0.9944 0.044 Uiso 1 1 calc R . .
C34 C 0.4524(2) 0.15479(15) 0.70514(14) 0.0230(6) Uani 1 1 d . . .
C30 C 0.4092(2) 0.28048(16) 0.68364(14) 0.0260(6) Uani 1 1 d . . .
C31 C 0.4247(3) 0.27352(18) 0.61259(16) 0.0365(7) Uani 1 1 d . . .
H31 H 0.4165 0.3147 0.5822 0.044 Uiso 1 1 calc R . .
C32 C 0.4526(3) 0.20442(19) 0.58775(16) 0.0385(8) Uani 1 1 d . . .
H32 H 0.4610 0.1985 0.5400 0.046 Uiso 1 1 calc R . .
C33 C 0.4678(2) 0.14432(18) 0.63421(15) 0.0315(7) Uani 1 1 d . . .
H33 H 0.4880 0.0978 0.6185 0.038 Uiso 1 1 calc R . .
C29 C 0.3840(2) 0.35231(15) 0.71773(14) 0.0242(6) Uani 1 1 d . . .
C22 C 0.2777(2) 0.37378(16) 0.71950(14) 0.0267(6) Uani 1 1 d . . .
C21 C 0.1858(2) 0.33009(18) 0.68041(17) 0.0354(7) Uani 1 1 d . . .
H21A H 0.1240 0.3373 0.7035 0.053 Uiso 1 1 calc R . .
H21B H 0.2038 0.2778 0.6810 0.053 Uiso 1 1 calc R . .
H21C H 0.1711 0.3472 0.6318 0.053 Uiso 1 1 calc R . .
C23 C 0.2589(2) 0.43751(16) 0.75861(15) 0.0272(6) Uani 1 1 d . . .
H23 H 0.1889 0.4518 0.7605 0.033 Uiso 1 1 calc R . .
C24 C 0.3409(2) 0.48034(16) 0.79476(14) 0.0258(6) Uani 1 1 d . . .
C26 C 0.4454(2) 0.45757(15) 0.79219(14) 0.0251(6) Uani 1 1 d . . .
H26 H 0.5013 0.4855 0.8164 0.030 Uiso 1 1 calc R . .
C27 C 0.4685(2) 0.39400(16) 0.75435(14) 0.0249(6) Uani 1 1 d . . .
C28 C 0.5820(2) 0.36889(17) 0.75542(16) 0.0315(6) Uani 1 1 d . . .
H28A H 0.6294 0.4056 0.7799 0.047 Uiso 1 1 calc R . .
H28B H 0.5965 0.3634 0.7072 0.047 Uiso 1 1 calc R . .
H28C H 0.5925 0.3217 0.7798 0.047 Uiso 1 1 calc R . .
C25 C 0.3165(2) 0.54827(16) 0.83643(15) 0.0309(6) Uani 1 1 d . . .
H25A H 0.2705 0.5812 0.8059 0.046 Uiso 1 1 calc R . .
H25B H 0.3817 0.5739 0.8540 0.046 Uiso 1 1 calc R . .
H25C H 0.2819 0.5331 0.8760 0.046 Uiso 1 1 calc R . .
C11 C 0.1393(2) 0.21282(15) 0.81781(14) 0.0236(6) Uani 1 1 d . . .
H11 H 0.1429 0.1735 0.7859 0.028 Uiso 1 1 calc R . .
C12 C 0.0389(2) 0.23662(15) 0.82948(14) 0.0236(6) Uani 1 1 d . . .
C13 C 0.0361(2) 0.29582(17) 0.87775(16) 0.0296(6) Uani 1 1 d . . .
H13 H -0.0290 0.3145 0.8869 0.035 Uiso 1 1 calc R . .
C14 C 0.1298(2) 0.32650(16) 0.91170(15) 0.0281(6) Uani 1 1 d . . .
H14 H 0.1280 0.3654 0.9442 0.034 Uiso 1 1 calc R . .
C15 C 0.2271(2) 0.29887(15) 0.89705(14) 0.0211(5) Uani 1 1 d . . .
C16 C 0.3310(2) 0.32991(14) 0.93000(13) 0.0192(5) Uani 1 1 d . . .
C20 C 0.5133(2) 0.33231(15) 0.92950(14) 0.0231(6) Uani 1 1 d . . .
H20 H 0.5725 0.3160 0.9100 0.028 Uiso 1 1 calc R . .
C19 C 0.5285(2) 0.38432(16) 0.98414(15) 0.0265(6) Uani 1 1 d . . .
H19 H 0.5963 0.4022 1.0012 0.032 Uiso 1 1 calc R . .
C18 C 0.4405(2) 0.40918(16) 1.01291(15) 0.0275(6) Uani 1 1 d . . .
H18 H 0.4483 0.4438 1.0501 0.033 Uiso 1 1 calc R . .
C17 C 0.3402(2) 0.38176(15) 0.98560(15) 0.0254(6) Uani 1 1 d . . .
H17 H 0.2801 0.3978 1.0042 0.030 Uiso 1 1 calc R . .
C10 C -0.0596(2) 0.20219(16) 0.79254(15) 0.0275(6) Uani 1 1 d . . .
C9 C -0.1667(2) 0.22257(17) 0.80105(16) 0.0310(7) Uani 1 1 d . . .
H9 H -0.1861 0.2611 0.8297 0.037 Uiso 1 1 calc R . .
C8 C -0.2374(2) 0.17388(18) 0.75831(17) 0.0345(7) Uani 1 1 d . . .
H8 H -0.3113 0.1749 0.7541 0.041 Uiso 1 1 calc R . .
C7 C -0.1765(2) 0.12309(18) 0.72281(16) 0.0329(7) Uani 1 1 d . . .
H7 H -0.2034 0.0855 0.6912 0.039 Uiso 1 1 calc R . .
C6 C -0.0673(2) 0.14013(17) 0.74438(15) 0.0293(6) Uani 1 1 d . . .
H6 H -0.0101 0.1150 0.7296 0.035 Uiso 1 1 calc R . .
C2 C -0.1700(3) 0.00770(18) 0.85965(17) 0.0360(7) Uani 1 1 d . . .
H2 H -0.1996 -0.0296 0.8286 0.043 Uiso 1 1 calc R . .
C1 C -0.0596(3) 0.02221(19) 0.87897(17) 0.0385(7) Uani 1 1 d . . .
H1 H -0.0042 -0.0038 0.8629 0.046 Uiso 1 1 calc R . .
C5 C -0.0488(3) 0.0835(2) 0.92721(16) 0.0389(8) Uani 1 1 d . . .
H5 H 0.0151 0.1045 0.9486 0.047 Uiso 1 1 calc R . .
C4 C -0.1523(3) 0.1072(2) 0.93715(17) 0.0392(8) Uani 1 1 d . . .
H4 H -0.1683 0.1469 0.9657 0.047 Uiso 1 1 calc R . .
C3 C -0.2274(3) 0.05965(19) 0.89567(17) 0.0376(7) Uani 1 1 d . . .
H3 H -0.3012 0.0623 0.8928 0.045 Uiso 1 1 calc R . .


_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
Cu1 N2 2.021(2) . ?
Cu1 N1 2.033(2) . ?
Cu1 N4 2.035(2) . ?
Cu1 N3 2.035(2) . ?
Fe1 C6 2.027(3) . ?
Fe1 C4 2.034(3) . ?
Fe1 C2 2.037(3) . ?
Fe1 C10 2.038(3) . ?
Fe1 C9 2.039(3) . ?
Fe1 C3 2.040(3) . ?
Fe1 C1 2.044(3) . ?
Fe1 C5 2.046(3) . ?
Fe1 C8 2.048(3) . ?
Fe1 C7 2.053(3) . ?
P1 F5 1.5950(18) . ?
P1 F1 1.5954(18) . ?
P1 F2 1.6032(18) . ?
P1 F3 1.6049(18) . ?
P1 F6 1.6078(18) . ?
P1 F4 1.6091(17) . ?
N4 C39 1.350(3) . ?
N4 C35 1.353(3) . ?
N3 C30 1.346(3) . ?
N3 C34 1.348(3) . ?
N1 C11 1.343(3) . ?
N1 C15 1.352(3) . ?
N2 C20 1.348(3) . ?
N2 C16 1.354(3) . ?
C35 C36 1.394(4) . ?
C35 C34 1.483(4) . ?
C36 C37 1.386(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.383(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.385(4) . ?
C38 H38 0.9300 . ?
C39 C40 1.498(4) . ?
C40 C41 1.405(4) . ?
C40 C47 1.406(4) . ?
C47 C46 1.391(4) . ?
C47 C48 1.503(4) . ?
C46 C44 1.382(4) . ?
C46 H46 0.9300 . ?
C44 C43 1.381(4) . ?
C44 C45 1.515(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C43 C41 1.401(4) . ?
C43 H43 0.9300 . ?
C41 C42 1.503(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C34 C33 1.394(4) . ?
C30 C31 1.390(4) . ?
C30 C29 1.490(4) . ?
C31 C32 1.383(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.381(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C29 C27 1.401(4) . ?
C29 C22 1.405(4) . ?
C22 C23 1.395(4) . ?
C22 C21 1.503(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C23 C24 1.387(4) . ?
C23 H23 0.9300 . ?
C24 C26 1.394(4) . ?
C24 C25 1.502(4) . ?
C26 C27 1.394(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.505(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.399(4) . ?
C12 C10 1.474(4) . ?
C13 C14 1.378(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.480(4) . ?
C16 C17 1.392(4) . ?
C20 C19 1.380(4) . ?
C20 H20 0.9300 . ?
C19 C18 1.383(4) . ?
C19 H19 0.9300 . ?
C18 C17 1.389(4) . ?
C18 H18 0.9300 . ?
C17 H17 0.9300 . ?
C10 C6 1.427(4) . ?
C10 C9 1.436(4) . ?
C9 C8 1.414(4) . ?
C9 H9 0.9300 . ?
C8 C7 1.420(4) . ?
C8 H8 0.9300 . ?
C7 C6 1.418(4) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C2 C3 1.413(5) . ?
C2 C1 1.418(5) . ?
C2 H2 0.9300 . ?
C1 C5 1.417(5) . ?
C1 H1 0.9300 . ?
C5 C4 1.418(5) . ?
C5 H5 0.9300 . ?
C4 C3 1.422(4) . ?
C4 H4 0.9300 . ?
C3 H3 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
N2 Cu1 N1 81.88(9) . . ?
N2 Cu1 N4 130.98(9) . . ?
N1 Cu1 N4 121.91(9) . . ?
N2 Cu1 N3 125.99(9) . . ?
N1 Cu1 N3 122.82(9) . . ?
N4 Cu1 N3 79.46(9) . . ?
C6 Fe1 C4 158.07(12) . . ?
C6 Fe1 C2 123.73(12) . . ?
C4 Fe1 C2 68.50(13) . . ?
C6 Fe1 C10 41.11(11) . . ?
C4 Fe1 C10 121.68(12) . . ?
C2 Fe1 C10 160.53(12) . . ?
C6 Fe1 C9 68.88(12) . . ?
C4 Fe1 C9 107.11(14) . . ?
C2 Fe1 C9 156.84(13) . . ?
C10 Fe1 C9 41.25(12) . . ?
C6 Fe1 C3 159.81(12) . . ?
C4 Fe1 C3 40.85(13) . . ?
C2 Fe1 C3 40.56(13) . . ?
C10 Fe1 C3 157.48(12) . . ?
C9 Fe1 C3 121.28(13) . . ?
C6 Fe1 C1 107.84(13) . . ?
C4 Fe1 C1 68.49(14) . . ?
C2 Fe1 C1 40.67(13) . . ?
C10 Fe1 C1 123.95(12) . . ?
C9 Fe1 C1 160.88(13) . . ?
C3 Fe1 C1 68.39(14) . . ?
C6 Fe1 C5 122.55(13) . . ?
C4 Fe1 C5 40.65(13) . . ?
C2 Fe1 C5 68.24(14) . . ?
C10 Fe1 C5 107.68(13) . . ?
C9 Fe1 C5 124.17(13) . . ?
C3 Fe1 C5 68.36(13) . . ?
C1 Fe1 C5 40.54(14) . . ?
C6 Fe1 C8 68.38(13) . . ?
C4 Fe1 C8 123.42(14) . . ?
C2 Fe1 C8 121.59(13) . . ?
C10 Fe1 C8 68.77(12) . . ?
C9 Fe1 C8 40.48(12) . . ?
C3 Fe1 C8 107.06(13) . . ?
C1 Fe1 C8 157.47(13) . . ?
C5 Fe1 C8 160.28(14) . . ?
C6 Fe1 C7 40.66(12) . . ?
C4 Fe1 C7 159.76(13) . . ?
C2 Fe1 C7 107.38(13) . . ?
C10 Fe1 C7 68.87(12) . . ?
C9 Fe1 C7 68.43(12) . . ?
C3 Fe1 C7 123.22(13) . . ?
C1 Fe1 C7 122.16(13) . . ?
C5 Fe1 C7 158.05(13) . . ?
C8 Fe1 C7 40.52(12) . . ?
F5 P1 F1 90.28(10) . . ?
F5 P1 F2 90.28(10) . . ?
F1 P1 F2 90.78(10) . . ?
F5 P1 F3 179.30(11) . . ?
F1 P1 F3 90.32(10) . . ?
F2 P1 F3 90.06(10) . . ?
F5 P1 F6 90.37(10) . . ?
F1 P1 F6 90.11(10) . . ?
F2 P1 F6 178.90(11) . . ?
F3 P1 F6 89.28(10) . . ?
F5 P1 F4 89.66(10) . . ?
F1 P1 F4 179.87(13) . . ?
F2 P1 F4 89.34(10) . . ?
F3 P1 F4 89.74(10) . . ?
F6 P1 F4 89.77(10) . . ?
C39 N4 C35 119.7(2) . . ?
C39 N4 Cu1 124.83(18) . . ?
C35 N4 Cu1 115.41(18) . . ?
C30 N3 C34 119.8(2) . . ?
C30 N3 Cu1 124.24(18) . . ?
C34 N3 Cu1 115.71(17) . . ?
C11 N1 C15 118.2(2) . . ?
C11 N1 Cu1 128.57(18) . . ?
C15 N1 Cu1 112.92(17) . . ?
C20 N2 C16 117.7(2) . . ?
C20 N2 Cu1 128.70(18) . . ?
C16 N2 Cu1 113.51(17) . . ?
N4 C35 C36 121.6(3) . . ?
N4 C35 C34 114.7(2) . . ?
C36 C35 C34 123.7(2) . . ?
C37 C36 C35 118.3(3) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C38 C37 C36 119.9(3) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C39 119.3(3) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N4 C39 C38 121.2(3) . . ?
N4 C39 C40 113.8(2) . . ?
C38 C39 C40 124.9(3) . . ?
C41 C40 C47 120.3(3) . . ?
C41 C40 C39 119.7(2) . . ?
C47 C40 C39 119.7(2) . . ?
C46 C47 C40 119.0(3) . . ?
C46 C47 C48 120.5(3) . . ?
C40 C47 C48 120.5(2) . . ?
C44 C46 C47 121.8(3) . . ?
C44 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C43 C44 C46 118.5(3) . . ?
C43 C44 C45 120.7(3) . . ?
C46 C44 C45 120.9(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C43 C41 122.3(3) . . ?
C44 C43 H43 118.8 . . ?
C41 C43 H43 118.8 . . ?
C43 C41 C40 118.0(3) . . ?
C43 C41 C42 120.5(3) . . ?
C40 C41 C42 121.5(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N3 C34 C33 121.4(3) . . ?
N3 C34 C35 114.0(2) . . ?
C33 C34 C35 124.6(3) . . ?
N3 C30 C31 121.3(3) . . ?
N3 C30 C29 114.4(2) . . ?
C31 C30 C29 124.3(3) . . ?
C32 C31 C30 119.1(3) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 118.7(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C27 C29 C22 120.6(3) . . ?
C27 C29 C30 118.2(2) . . ?
C22 C29 C30 120.8(2) . . ?
C23 C22 C29 118.2(3) . . ?
C23 C22 C21 120.2(3) . . ?
C29 C22 C21 121.6(3) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C23 C22 122.4(3) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C26 118.0(3) . . ?
C23 C24 C25 120.4(3) . . ?
C26 C24 C25 121.5(3) . . ?
C24 C26 C27 121.7(3) . . ?
C24 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C29 118.9(3) . . ?
C26 C27 C28 120.4(3) . . ?
C29 C27 C28 120.6(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C11 C12 124.4(2) . . ?
N1 C11 H11 117.8 . . ?
C12 C11 H11 117.8 . . ?
C11 C12 C13 116.4(2) . . ?
C11 C12 C10 122.0(2) . . ?
C13 C12 C10 121.5(2) . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N1 C15 C14 121.2(2) . . ?
N1 C15 C16 115.9(2) . . ?
C14 C15 C16 122.9(2) . . ?
N2 C16 C17 122.0(2) . . ?
N2 C16 C15 115.5(2) . . ?
C17 C16 C15 122.6(2) . . ?
N2 C20 C19 123.5(3) . . ?
N2 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
C19 C18 C17 119.2(3) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C6 C10 C9 106.9(3) . . ?
C6 C10 C12 126.8(3) . . ?
C9 C10 C12 126.2(3) . . ?
C6 C10 Fe1 69.05(16) . . ?
C9 C10 Fe1 69.43(17) . . ?
C12 C10 Fe1 124.3(2) . . ?
C8 C9 C10 108.1(3) . . ?
C8 C9 Fe1 70.08(18) . . ?
C10 C9 Fe1 69.32(17) . . ?
C8 C9 H9 125.9 . . ?
C10 C9 H9 125.9 . . ?
Fe1 C9 H9 126.2 . . ?
C9 C8 C7 108.6(3) . . ?
C9 C8 Fe1 69.45(17) . . ?
C7 C8 Fe1 69.96(18) . . ?
C9 C8 H8 125.7 . . ?
C7 C8 H8 125.7 . . ?
Fe1 C8 H8 126.5 . . ?
C6 C7 C8 107.6(3) . . ?
C6 C7 Fe1 68.69(16) . . ?
C8 C7 Fe1 69.52(17) . . ?
C6 C7 H7 126.2 . . ?
C8 C7 H7 126.2 . . ?
Fe1 C7 H7 127.1 . . ?
C7 C6 C10 108.8(3) . . ?
C7 C6 Fe1 70.65(17) . . ?
C10 C6 Fe1 69.84(17) . . ?
C7 C6 H6 125.6 . . ?
C10 C6 H6 125.6 . . ?
Fe1 C6 H6 125.5 . . ?
C3 C2 C1 108.3(3) . . ?
C3 C2 Fe1 69.85(18) . . ?
C1 C2 Fe1 69.93(18) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
Fe1 C2 H2 126.0 . . ?
C5 C1 C2 107.8(3) . . ?
C5 C1 Fe1 69.83(19) . . ?
C2 C1 Fe1 69.40(19) . . ?
C5 C1 H1 126.1 . . ?
C2 C1 H1 126.1 . . ?
Fe1 C1 H1 126.2 . . ?
C1 C5 C4 108.1(3) . . ?
C1 C5 Fe1 69.63(18) . . ?
C4 C5 Fe1 69.23(18) . . ?
C1 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
Fe1 C5 H5 126.8 . . ?
C5 C4 C3 107.9(3) . . ?
C5 C4 Fe1 70.12(18) . . ?
C3 C4 Fe1 69.78(18) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
Fe1 C4 H4 125.6 . . ?
C2 C3 C4 107.8(3) . . ?
C2 C3 Fe1 69.59(18) . . ?
C4 C3 Fe1 69.37(18) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 H3 126.1 . . ?
Fe1 C3 H3 126.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.42
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.079
_database_code_depnum_ccdc_archive 'CCDC 1000093'
#######################################################################
#
#                 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_sos072

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H46 Cu F6 Fe N4 P'
_chemical_formula_weight         955.26

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'

_cell_length_a                   39.118(3)
_cell_length_b                   39.118(3)
_cell_length_c                   12.8349(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     19640(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9837
_cell_measurement_theta_min      2.3285
_cell_measurement_theta_max      24.354

_exptl_crystal_description       irregular
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.43
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7872
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5258
_exptl_absorpt_correction_T_max  0.7195
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            136258
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.04
_diffrn_reflns_theta_max         26.46
_reflns_number_total             10065
_reflns_number_gt                8201
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of 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)+(0.0413P)²+71.7227P] 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         10065
_refine_ls_number_parameters     566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1278
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_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
Cu1 Cu 0.851721(10) 0.201944(10) 0.00281(3) 0.02533(11) Uani 1 1 d . . .
Fe1 Fe 0.863063(12) 0.231078(13) 0.53001(4) 0.02951(13) Uani 1 1 d . . .
P1 P 0.86427(3) 0.08065(3) 0.56139(8) 0.0390(2) Uani 1 1 d . . .
F1 F 0.89692(6) 0.10528(7) 0.55104(19) 0.0597(7) Uani 1 1 d . . .
F2 F 0.88752(8) 0.04792(7) 0.5436(2) 0.0747(9) Uani 1 1 d . . .
F3 F 0.85951(8) 0.08293(7) 0.43725(19) 0.0635(8) Uani 1 1 d . . .
F4 F 0.86966(8) 0.07842(7) 0.68313(18) 0.0634(8) Uani 1 1 d . . .
F5 F 0.84141(7) 0.11369(7) 0.5756(2) 0.0643(8) Uani 1 1 d . . .
F6 F 0.83131(8) 0.05686(7) 0.5698(2) 0.0762(9) Uani 1 1 d . . .
N4 N 0.88994(6) 0.22666(7) -0.0726(2) 0.0226(6) Uani 1 1 d . . .
N3 N 0.82704(6) 0.24506(7) -0.0372(2) 0.0240(6) Uani 1 1 d . . .
N1 N 0.86088(7) 0.18535(7) 0.1497(2) 0.0235(6) Uani 1 1 d . . .
N2 N 0.83436(7) 0.15402(7) -0.0152(2) 0.0277(6) Uani 1 1 d . . .
C31 C 0.92178(8) 0.21411(8) -0.0875(2) 0.0233(7) Uani 1 1 d . . .
C32 C 0.94724(8) 0.23396(8) -0.1322(3) 0.0274(7) Uani 1 1 d . . .
H32 H 0.9690 0.2250 -0.1422 0.033 Uiso 1 1 calc R . .
C33 C 0.93984(9) 0.26733(9) -0.1619(3) 0.0330(8) Uani 1 1 d . . .
H33 H 0.9567 0.2811 -0.1912 0.040 Uiso 1 1 calc R . .
C34 C 0.90714(9) 0.27975(9) -0.1472(3) 0.0302(8) Uani 1 1 d . . .
H34 H 0.9017 0.3019 -0.1674 0.036 Uiso 1 1 calc R . .
C35 C 0.88259(8) 0.25904(8) -0.1022(2) 0.0228(7) Uani 1 1 d . . .
C36 C 0.84645(8) 0.26926(8) -0.0839(3) 0.0242(7) Uani 1 1 d . . .
C40 C 0.79335(8) 0.25090(9) -0.0226(3) 0.0276(7) Uani 1 1 d . . .
C41 C 0.77411(8) 0.22132(9) 0.0220(3) 0.0282(7) Uani 1 1 d . . .
C48 C 0.75755(8) 0.19901(10) -0.0464(3) 0.0319(8) Uani 1 1 d . . .
C49 C 0.75585(10) 0.20614(11) -0.1622(3) 0.0434(10) Uani 1 1 d . . .
H49A H 0.7462 0.1867 -0.1973 0.065 Uiso 1 1 calc R . .
H49B H 0.7785 0.2103 -0.1883 0.065 Uiso 1 1 calc R . .
H49C H 0.7418 0.2259 -0.1744 0.065 Uiso 1 1 calc R . .
C47 C 0.74324(9) 0.16909(10) -0.0069(3) 0.0362(8) Uani 1 1 d . . .
H47 H 0.7321 0.1542 -0.0522 0.043 Uiso 1 1 calc R . .
C45 C 0.74506(9) 0.16083(10) 0.0983(3) 0.0357(9) Uani 1 1 d . . .
C44 C 0.76065(9) 0.18386(10) 0.1652(3) 0.0336(8) Uani 1 1 d . . .
H44 H 0.7614 0.1790 0.2360 0.040 Uiso 1 1 calc R . .
C42 C 0.77525(8) 0.21427(9) 0.1289(3) 0.0304(8) Uani 1 1 d . . .
C43 C 0.79174(10) 0.23867(10) 0.2036(3) 0.0401(9) Uani 1 1 d . . .
H43A H 0.7786 0.2593 0.2069 0.060 Uiso 1 1 calc R . .
H43B H 0.8145 0.2439 0.1802 0.060 Uiso 1 1 calc R . .
H43C H 0.7928 0.2284 0.2715 0.060 Uiso 1 1 calc R . .
C46 C 0.73089(11) 0.12683(10) 0.1364(4) 0.0471(10) Uani 1 1 d . . .
H46A H 0.7465 0.1088 0.1184 0.071 Uiso 1 1 calc R . .
H46B H 0.7092 0.1226 0.1041 0.071 Uiso 1 1 calc R . .
H46C H 0.7281 0.1276 0.2106 0.071 Uiso 1 1 calc R . .
C39 C 0.77839(9) 0.28160(10) -0.0528(3) 0.0371(9) Uani 1 1 d . . .
H39 H 0.7552 0.2854 -0.0417 0.045 Uiso 1 1 calc R . .
C38 C 0.79846(9) 0.30631(10) -0.0995(3) 0.0372(9) Uani 1 1 d . . .
H38 H 0.7888 0.3270 -0.1200 0.045 Uiso 1 1 calc R . .
C37 C 0.83288(9) 0.30026(9) -0.1156(3) 0.0311(8) Uani 1 1 d . . .
H37 H 0.8466 0.3167 -0.1471 0.037 Uiso 1 1 calc R . .
C30 C 0.92655(8) 0.17822(8) -0.0528(2) 0.0224(7) Uani 1 1 d . . .
C23 C 0.94145(8) 0.17134(9) 0.0451(3) 0.0258(7) Uani 1 1 d . . .
C24 C 0.94197(9) 0.13808(9) 0.0816(3) 0.0294(7) Uani 1 1 d . . .
H24 H 0.9518 0.1335 0.1461 0.035 Uiso 1 1 calc R . .
C25 C 0.92818(9) 0.11132(9) 0.0243(3) 0.0332(8) Uani 1 1 d . . .
C27 C 0.91491(9) 0.11815(9) -0.0735(3) 0.0315(8) Uani 1 1 d . . .
H27 H 0.9067 0.1002 -0.1137 0.038 Uiso 1 1 calc R . .
C28 C 0.91354(8) 0.15119(8) -0.1130(3) 0.0270(7) Uani 1 1 d . . .
C29 C 0.89819(10) 0.15769(10) -0.2199(3) 0.0382(9) Uani 1 1 d . . .
H29A H 0.8891 0.1367 -0.2473 0.057 Uiso 1 1 calc R . .
H29B H 0.9156 0.1662 -0.2659 0.057 Uiso 1 1 calc R . .
H29C H 0.8802 0.1742 -0.2141 0.057 Uiso 1 1 calc R . .
C26 C 0.92635(12) 0.07555(10) 0.0693(4) 0.0472(10) Uani 1 1 d . . .
H26A H 0.9423 0.0735 0.1258 0.071 Uiso 1 1 calc R . .
H26B H 0.9319 0.0592 0.0162 0.071 Uiso 1 1 calc R . .
H26C H 0.9036 0.0713 0.0945 0.071 Uiso 1 1 calc R . .
C22 C 0.95515(9) 0.20036(10) 0.1111(3) 0.0370(9) Uani 1 1 d . . .
H22A H 0.9626 0.1916 0.1771 0.055 Uiso 1 1 calc R . .
H22B H 0.9374 0.2170 0.1220 0.055 Uiso 1 1 calc R . .
H22C H 0.9741 0.2109 0.0759 0.055 Uiso 1 1 calc R . .
C11 C 0.87369(8) 0.20281(8) 0.2306(3) 0.0246(7) Uani 1 1 d . . .
H11 H 0.8793 0.2257 0.2202 0.029 Uiso 1 1 calc R . .
C12 C 0.87920(8) 0.18903(9) 0.3290(3) 0.0271(7) Uani 1 1 d . . .
C10 C 0.89233(8) 0.20944(9) 0.4157(3) 0.0278(7) Uani 1 1 d . . .
C9 C 0.89688(9) 0.24555(10) 0.4176(3) 0.0341(8) Uani 1 1 d . . .
H9 H 0.8925 0.2604 0.3626 0.041 Uiso 1 1 calc R . .
C8 C 0.90935(10) 0.25520(10) 0.5178(3) 0.0390(9) Uani 1 1 d . . .
H8 H 0.9146 0.2773 0.5393 0.047 Uiso 1 1 calc R . .
C7 C 0.91226(9) 0.22518(10) 0.5784(3) 0.0348(8) Uani 1 1 d . . .
H7 H 0.9198 0.2241 0.6471 0.042 Uiso 1 1 calc R . .
C6 C 0.90185(9) 0.19702(10) 0.5169(3) 0.0315(8) Uani 1 1 d . . .
H6 H 0.9013 0.1743 0.5384 0.038 Uiso 1 1 calc R . .
C1 C 0.82348(10) 0.20498(12) 0.5959(3) 0.0446(10) Uani 1 1 d . . .
H1 H 0.8236 0.1821 0.6150 0.054 Uiso 1 1 calc R . .
C2 C 0.83288(10) 0.23300(13) 0.6600(3) 0.0516(11) Uani 1 1 d . . .
H2 H 0.8403 0.2317 0.7288 0.062 Uiso 1 1 calc R . .
C3 C 0.82895(11) 0.26302(13) 0.6008(4) 0.0552(12) Uani 1 1 d . . .
H3 H 0.8334 0.2851 0.6237 0.066 Uiso 1 1 calc R . .
C4 C 0.81698(10) 0.25384(12) 0.5001(4) 0.0528(11) Uani 1 1 d . . .
H4 H 0.8121 0.2688 0.4457 0.063 Uiso 1 1 calc R . .
C5 C 0.81392(9) 0.21820(12) 0.4977(3) 0.0440(10) Uani 1 1 d . . .
H5 H 0.8068 0.2053 0.4408 0.053 Uiso 1 1 calc R . .
C13 C 0.87163(10) 0.15435(9) 0.3404(3) 0.0367(9) Uani 1 1 d . . .
H13 H 0.8753 0.1436 0.4041 0.044 Uiso 1 1 calc R . .
C14 C 0.85884(10) 0.13603(9) 0.2577(3) 0.0365(9) Uani 1 1 d . . .
H14 H 0.8541 0.1129 0.2653 0.044 Uiso 1 1 calc R . .
C15 C 0.85302(8) 0.15206(8) 0.1626(3) 0.0270(7) Uani 1 1 d . . .
C16 C 0.83785(8) 0.13470(9) 0.0721(3) 0.0280(7) Uani 1 1 d . . .
C21 C 0.81959(9) 0.14021(9) -0.0986(3) 0.0306(8) Uani 1 1 d . . .
H21 H 0.8171 0.1538 -0.1576 0.037 Uiso 1 1 calc R . .
C19 C 0.80756(9) 0.10663(10) -0.1035(3) 0.0370(9) Uani 1 1 d . . .
C20 C 0.79022(12) 0.09338(12) -0.2002(3) 0.0518(11) Uani 1 1 d . . .
H20A H 0.7995 0.0714 -0.2180 0.078 Uiso 1 1 calc R . .
H20B H 0.7940 0.1091 -0.2566 0.078 Uiso 1 1 calc R . .
H20C H 0.7661 0.0912 -0.1876 0.078 Uiso 1 1 calc R . .
C18 C 0.81219(11) 0.08707(10) -0.0145(3) 0.0423(9) Uani 1 1 d . . .
H18 H 0.8052 0.0644 -0.0138 0.051 Uiso 1 1 calc R . .
C17 C 0.82704(10) 0.10094(9) 0.0726(3) 0.0363(8) Uani 1 1 d . . .
H17 H 0.8299 0.0877 0.1321 0.044 Uiso 1 1 calc R . .


_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
Cu1 N2 2.007(3) . ?
Cu1 N3 2.010(3) . ?
Cu1 N1 2.026(3) . ?
Cu1 N4 2.026(3) . ?
Fe1 C6 2.026(3) . ?
Fe1 C5 2.030(4) . ?
Fe1 C7 2.036(4) . ?
Fe1 C9 2.038(4) . ?
Fe1 C1 2.038(4) . ?
Fe1 C3 2.041(4) . ?
Fe1 C10 2.044(3) . ?
Fe1 C2 2.046(4) . ?
Fe1 C4 2.047(4) . ?
Fe1 C8 2.048(4) . ?
P1 F4 1.579(3) . ?
P1 F5 1.582(3) . ?
P1 F2 1.587(3) . ?
P1 F6 1.594(3) . ?
P1 F1 1.605(3) . ?
P1 F3 1.607(3) . ?
N4 C31 1.352(4) . ?
N4 C35 1.353(4) . ?
N3 C40 1.351(4) . ?
N3 C36 1.353(4) . ?
N1 C11 1.340(4) . ?
N1 C15 1.348(4) . ?
N2 C21 1.331(4) . ?
N2 C16 1.358(4) . ?
C31 C32 1.387(4) . ?
C31 C30 1.485(4) . ?
C32 C33 1.390(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.381(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.488(4) . ?
C36 C37 1.385(5) . ?
C40 C39 1.391(5) . ?
C40 C41 1.494(5) . ?
C41 C48 1.397(5) . ?
C41 C42 1.400(5) . ?
C48 C47 1.393(5) . ?
C48 C49 1.513(5) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C47 C45 1.389(5) . ?
C47 H47 0.9300 . ?
C45 C44 1.386(5) . ?
C45 C46 1.522(5) . ?
C44 C42 1.399(5) . ?
C44 H44 0.9300 . ?
C42 C43 1.499(5) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C39 C38 1.382(5) . ?
C39 H39 0.9300 . ?
C38 C37 1.383(5) . ?
C38 H38 0.9300 . ?
C37 H37 0.9300 . ?
C30 C28 1.405(4) . ?
C30 C23 1.410(4) . ?
C23 C24 1.383(5) . ?
C23 C22 1.514(5) . ?
C24 C25 1.388(5) . ?
C24 H24 0.9300 . ?
C25 C27 1.384(5) . ?
C25 C26 1.516(5) . ?
C27 C28 1.389(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.520(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C11 C12 1.391(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(5) . ?
C12 C10 1.463(5) . ?
C10 C9 1.424(5) . ?
C10 C6 1.436(5) . ?
C9 C8 1.426(5) . ?
C9 H9 0.9300 . ?
C8 C7 1.414(5) . ?
C8 H8 0.9300 . ?
C7 C6 1.415(5) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C1 C5 1.413(6) . ?
C1 C2 1.419(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.408(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.421(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C13 C14 1.375(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.391(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.470(5) . ?
C16 C17 1.387(5) . ?
C21 C19 1.397(5) . ?
C21 H21 0.9300 . ?
C19 C18 1.387(6) . ?
C19 C20 1.507(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 C17 1.371(5) . ?
C18 H18 0.9300 . ?
C17 H17 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
N2 Cu1 N3 126.29(11) . . ?
N2 Cu1 N1 82.39(11) . . ?
N3 Cu1 N1 126.27(11) . . ?
N2 Cu1 N4 129.81(11) . . ?
N3 Cu1 N4 80.33(10) . . ?
N1 Cu1 N4 117.82(10) . . ?
C6 Fe1 C5 121.93(17) . . ?
C6 Fe1 C7 40.78(14) . . ?
C5 Fe1 C7 158.37(17) . . ?
C6 Fe1 C9 68.77(15) . . ?
C5 Fe1 C9 122.61(16) . . ?
C7 Fe1 C9 68.53(15) . . ?
C6 Fe1 C1 105.90(16) . . ?
C5 Fe1 C1 40.64(16) . . ?
C7 Fe1 C1 122.33(16) . . ?
C9 Fe1 C1 157.82(16) . . ?
C6 Fe1 C3 158.26(18) . . ?
C5 Fe1 C3 67.90(18) . . ?
C7 Fe1 C3 123.47(17) . . ?
C9 Fe1 C3 124.71(19) . . ?
C1 Fe1 C3 68.00(19) . . ?
C6 Fe1 C10 41.32(13) . . ?
C5 Fe1 C10 106.31(15) . . ?
C7 Fe1 C10 69.07(14) . . ?
C9 Fe1 C10 40.83(14) . . ?
C1 Fe1 C10 121.05(15) . . ?
C3 Fe1 C10 159.85(18) . . ?
C6 Fe1 C2 121.60(17) . . ?
C5 Fe1 C2 68.24(17) . . ?
C7 Fe1 C2 107.50(16) . . ?
C9 Fe1 C2 160.41(17) . . ?
C1 Fe1 C2 40.67(17) . . ?
C3 Fe1 C2 40.29(19) . . ?
C10 Fe1 C2 157.50(18) . . ?
C6 Fe1 C4 158.43(17) . . ?
C5 Fe1 C4 40.16(18) . . ?
C7 Fe1 C4 159.92(18) . . ?
C9 Fe1 C4 108.54(17) . . ?
C1 Fe1 C4 68.08(19) . . ?
C3 Fe1 C4 40.67(18) . . ?
C10 Fe1 C4 122.59(17) . . ?
C2 Fe1 C4 68.21(19) . . ?
C6 Fe1 C8 68.56(16) . . ?
C5 Fe1 C8 159.38(17) . . ?
C7 Fe1 C8 40.51(15) . . ?
C9 Fe1 C8 40.86(14) . . ?
C1 Fe1 C8 159.12(16) . . ?
C3 Fe1 C8 109.28(18) . . ?
C10 Fe1 C8 68.93(15) . . ?
C2 Fe1 C8 123.78(17) . . ?
C4 Fe1 C8 124.32(18) . . ?
F4 P1 F5 90.38(15) . . ?
F4 P1 F2 91.21(14) . . ?
F5 P1 F2 178.21(16) . . ?
F4 P1 F6 90.50(17) . . ?
F5 P1 F6 90.69(16) . . ?
F2 P1 F6 90.13(18) . . ?
F4 P1 F1 90.51(16) . . ?
F5 P1 F1 88.22(15) . . ?
F2 P1 F1 90.94(17) . . ?
F6 P1 F1 178.52(18) . . ?
F4 P1 F3 178.99(18) . . ?
F5 P1 F3 90.19(16) . . ?
F2 P1 F3 88.21(15) . . ?
F6 P1 F3 90.33(16) . . ?
F1 P1 F3 88.67(14) . . ?
C31 N4 C35 119.7(3) . . ?
C31 N4 Cu1 125.0(2) . . ?
C35 N4 Cu1 115.1(2) . . ?
C40 N3 C36 119.4(3) . . ?
C40 N3 Cu1 125.1(2) . . ?
C36 N3 Cu1 115.5(2) . . ?
C11 N1 C15 118.9(3) . . ?
C11 N1 Cu1 128.6(2) . . ?
C15 N1 Cu1 112.5(2) . . ?
C21 N2 C16 118.8(3) . . ?
C21 N2 Cu1 128.2(2) . . ?
C16 N2 Cu1 113.0(2) . . ?
N4 C31 C32 121.1(3) . . ?
N4 C31 C30 114.6(3) . . ?
C32 C31 C30 124.3(3) . . ?
C31 C32 C33 119.3(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 119.6(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
N4 C35 C34 121.2(3) . . ?
N4 C35 C36 114.2(3) . . ?
C34 C35 C36 124.6(3) . . ?
N3 C36 C37 121.9(3) . . ?
N3 C36 C35 114.5(3) . . ?
C37 C36 C35 123.6(3) . . ?
N3 C40 C39 121.2(3) . . ?
N3 C40 C41 114.4(3) . . ?
C39 C40 C41 124.3(3) . . ?
C48 C41 C42 120.5(3) . . ?
C48 C41 C40 118.4(3) . . ?
C42 C41 C40 120.8(3) . . ?
C47 C48 C41 118.8(3) . . ?
C47 C48 C49 119.7(3) . . ?
C41 C48 C49 121.5(3) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C45 C47 C48 121.9(4) . . ?
C45 C47 H47 119.0 . . ?
C48 C47 H47 119.0 . . ?
C44 C45 C47 118.2(3) . . ?
C44 C45 C46 122.0(4) . . ?
C47 C45 C46 119.8(4) . . ?
C45 C44 C42 121.8(3) . . ?
C45 C44 H44 119.1 . . ?
C42 C44 H44 119.1 . . ?
C44 C42 C41 118.7(3) . . ?
C44 C42 C43 120.3(3) . . ?
C41 C42 C43 121.0(3) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C38 C39 C40 119.1(3) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
C39 C38 C37 119.9(3) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
C38 C37 C36 118.6(3) . . ?
C38 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C28 C30 C23 119.7(3) . . ?
C28 C30 C31 120.1(3) . . ?
C23 C30 C31 120.0(3) . . ?
C24 C23 C30 119.2(3) . . ?
C24 C23 C22 120.7(3) . . ?
C30 C23 C22 120.1(3) . . ?
C23 C24 C25 121.6(3) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C27 C25 C24 118.7(3) . . ?
C27 C25 C26 120.4(3) . . ?
C24 C25 C26 120.8(3) . . ?
C25 C27 C28 121.7(3) . . ?
C25 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C30 119.0(3) . . ?
C27 C28 C29 120.1(3) . . ?
C30 C28 C29 120.9(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C11 C12 124.3(3) . . ?
N1 C11 H11 117.8 . . ?
C12 C11 H11 117.8 . . ?
C11 C12 C13 116.0(3) . . ?
C11 C12 C10 122.3(3) . . ?
C13 C12 C10 121.7(3) . . ?
C9 C10 C6 106.7(3) . . ?
C9 C10 C12 126.8(3) . . ?
C6 C10 C12 126.5(3) . . ?
C9 C10 Fe1 69.3(2) . . ?
C6 C10 Fe1 68.65(19) . . ?
C12 C10 Fe1 125.1(2) . . ?
C10 C9 C8 108.7(3) . . ?
C10 C9 Fe1 69.83(19) . . ?
C8 C9 Fe1 69.9(2) . . ?
C10 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
Fe1 C9 H9 126.2 . . ?
C7 C8 C9 107.7(3) . . ?
C7 C8 Fe1 69.3(2) . . ?
C9 C8 Fe1 69.2(2) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 H8 126.1 . . ?
Fe1 C8 H8 126.9 . . ?
C8 C7 C6 108.4(3) . . ?
C8 C7 Fe1 70.2(2) . . ?
C6 C7 Fe1 69.2(2) . . ?
C8 C7 H7 125.8 . . ?
C6 C7 H7 125.8 . . ?
Fe1 C7 H7 126.3 . . ?
C7 C6 C10 108.4(3) . . ?
C7 C6 Fe1 70.0(2) . . ?
C10 C6 Fe1 70.03(19) . . ?
C7 C6 H6 125.8 . . ?
C10 C6 H6 125.8 . . ?
Fe1 C6 H6 125.8 . . ?
C5 C1 C2 107.7(4) . . ?
C5 C1 Fe1 69.4(2) . . ?
C2 C1 Fe1 69.9(2) . . ?
C5 C1 H1 126.2 . . ?
C2 C1 H1 126.2 . . ?
Fe1 C1 H1 126.1 . . ?
C3 C2 C1 107.6(4) . . ?
C3 C2 Fe1 69.7(3) . . ?
C1 C2 Fe1 69.4(2) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
Fe1 C2 H2 126.3 . . ?
C2 C3 C4 108.5(4) . . ?
C2 C3 Fe1 70.0(2) . . ?
C4 C3 Fe1 69.9(2) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
Fe1 C3 H3 125.9 . . ?
C5 C4 C3 107.5(4) . . ?
C5 C4 Fe1 69.3(2) . . ?
C3 C4 Fe1 69.5(2) . . ?
C5 C4 H4 126.3 . . ?
C3 C4 H4 126.3 . . ?
Fe1 C4 H4 126.6 . . ?
C4 C5 C1 108.8(4) . . ?
C4 C5 Fe1 70.6(2) . . ?
C1 C5 Fe1 70.0(2) . . ?
C4 C5 H5 125.6 . . ?
C1 C5 H5 125.6 . . ?
Fe1 C5 H5 125.4 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N1 C15 C14 120.4(3) . . ?
N1 C15 C16 116.2(3) . . ?
C14 C15 C16 123.4(3) . . ?
N2 C16 C17 120.2(3) . . ?
N2 C16 C15 115.8(3) . . ?
C17 C16 C15 124.0(3) . . ?
N2 C21 C19 124.3(3) . . ?
N2 C21 H21 117.8 . . ?
C19 C21 H21 117.8 . . ?
C18 C19 C21 116.0(3) . . ?
C18 C19 C20 123.2(4) . . ?
C21 C19 C20 120.8(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.46
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.075

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.250 0.625 36.8 -3.8
2 0.000 0.750 0.375 36.8 -4.0
3 0.250 0.000 0.800 771.4 220.3
4 0.250 0.500 0.191 771.4 220.1
5 0.500 0.250 0.875 36.7 -4.0
6 0.500 0.750 0.125 36.7 -3.8
7 0.750 0.000 0.690 771.3 220.1
8 0.750 0.500 0.303 771.4 220.3
_platon_squeeze_details          
;
The packing of the crystal shows sizeable solvent channels containing significant 
amounts of diffuse electron density, accounted for by disordered 
solvent which could not be modelled as discrete molecules. As such, PLATON SQUEEZE 
was employed to calculate the contribution to the diffraction from the solvent 
channels and thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated four 'voids' containing 220 electrons each. This can be attributed to a 
number of different solvent combinations including water, acetone and various
hydrocarbons originating from petroleum ether.
;

_database_code_depnum_ccdc_archive 'CCDC 1000094'
#######################################################################
#
#                 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_jdc535

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H16 Fe N2'
_chemical_formula_sum            'C20 H16 Fe N2'
_chemical_formula_weight         340.20

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.186(2)
_cell_length_b                   12.531(3)
_cell_length_c                   11.828(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.469(7)
_cell_angle_gamma                90.00
_cell_volume                     1508.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3234
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      22.72

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11348
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         22.89
_reflns_number_total             2057
_reflns_number_gt                1761
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1209P)²+4.0154P] 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         2057
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1929
_refine_ls_wR_factor_gt          0.1847
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_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
C1 C 0.7368(6) 1.0215(5) 0.2777(5) 0.0331(15) Uani 1 1 d . . .
H1 H 0.7461 1.0526 0.2053 0.040 Uiso 1 1 calc R . .
C2 C 0.8246(5) 0.9483(5) 0.3318(5) 0.0313(15) Uani 1 1 d . . .
H2 H 0.9029 0.9213 0.3017 0.038 Uiso 1 1 calc R . .
C3 C 0.7765(6) 0.9225(5) 0.4370(5) 0.0326(15) Uani 1 1 d . . .
H3 H 0.8167 0.8752 0.4908 0.039 Uiso 1 1 calc R . .
C4 C 0.6580(5) 0.9787(5) 0.4498(5) 0.0283(14) Uani 1 1 d . . .
H4 H 0.6048 0.9756 0.5138 0.034 Uiso 1 1 calc R . .
C5 C 0.6320(6) 1.0403(5) 0.3512(5) 0.0317(15) Uani 1 1 d . . .
H5 H 0.5585 1.0858 0.3367 0.038 Uiso 1 1 calc R . .
C6 C 0.6005(6) 0.7237(4) 0.3289(5) 0.0255(13) Uani 1 1 d . . .
H6 H 0.6324 0.6785 0.3884 0.031 Uiso 1 1 calc R . .
C7 C 0.4831(5) 0.7839(4) 0.3269(5) 0.0248(13) Uani 1 1 d . . .
H7 H 0.4225 0.7868 0.3857 0.030 Uiso 1 1 calc R . .
C8 C 0.4705(5) 0.8399(4) 0.2218(4) 0.0188(12) Uani 1 1 d . . .
C9 C 0.3615(5) 0.9106(5) 0.1848(4) 0.0188(13) Uani 1 1 d . . .
C10 C 0.3440(5) 0.9412(4) 0.0719(4) 0.0203(12) Uani 1 1 d . . .
H10 H 0.4039 0.9136 0.0198 0.024 Uiso 1 1 calc R . .
C11 C 0.1628(5) 1.0434(4) 0.1044(4) 0.0184(12) Uani 1 1 d . . .
C12 C 0.0652(5) 1.1215(4) 0.0604(5) 0.0192(13) Uani 1 1 d . . .
C13 C -0.1065(6) 1.2329(5) 0.0963(5) 0.0286(14) Uani 1 1 d . . .
H13 H -0.1682 1.2589 0.1476 0.034 Uiso 1 1 calc R . .
C14 C -0.1126(5) 1.2721(4) -0.0128(5) 0.0274(14) Uani 1 1 d . . .
H14 H -0.1750 1.3252 -0.0354 0.033 Uiso 1 1 calc R . .
C15 C -0.0250(5) 1.2318(4) -0.0885(5) 0.0269(14) Uani 1 1 d . . .
H15 H -0.0269 1.2564 -0.1646 0.032 Uiso 1 1 calc R . .
C16 C 0.0652(5) 1.1554(4) -0.0521(5) 0.0222(13) Uani 1 1 d . . .
H16 H 0.1260 1.1265 -0.1025 0.027 Uiso 1 1 calc R . .
C17 C 0.1689(5) 1.0134(4) 0.2171(4) 0.0184(12) Uani 1 1 d . . .
H17 H 0.1039 1.0376 0.2663 0.022 Uiso 1 1 calc R . .
C18 C 0.2687(5) 0.9487(4) 0.2579(4) 0.0197(12) Uani 1 1 d . . .
H18 H 0.2744 0.9299 0.3358 0.024 Uiso 1 1 calc R . .
C19 C 0.5833(5) 0.8150(4) 0.1598(5) 0.0224(12) Uani 1 1 d . . .
H19 H 0.6022 0.8419 0.0871 0.027 Uiso 1 1 calc R . .
C20 C 0.6622(5) 0.7435(4) 0.2251(5) 0.0232(13) Uani 1 1 d . . .
H20 H 0.7430 0.7135 0.2034 0.028 Uiso 1 1 calc R . .
N1 N 0.2497(4) 1.0063(4) 0.0314(4) 0.0213(11) Uani 1 1 d . . .
N2 N -0.0184(4) 1.1599(4) 0.1343(4) 0.0252(11) Uani 1 1 d . . .
Fe1 Fe 0.64079(7) 0.88231(6) 0.31124(6) 0.0186(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.415(9) . ?
C1 C5 1.425(9) . ?
C1 Fe1 2.047(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.394(9) . ?
C2 Fe1 2.052(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.411(8) . ?
C3 Fe1 2.050(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.415(9) . ?
C4 Fe1 2.038(5) . ?
C4 H4 0.9500 . ?
C5 Fe1 2.039(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.414(8) . ?
C6 C20 1.425(8) . ?
C6 Fe1 2.041(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.428(8) . ?
C7 Fe1 2.039(5) . ?
C7 H7 0.9500 . ?
C8 C19 1.424(8) . ?
C8 C9 1.472(8) . ?
C8 Fe1 2.062(5) . ?
C9 C18 1.393(7) . ?
C9 C10 1.394(7) . ?
C10 N1 1.333(7) . ?
C10 H10 0.9500 . ?
C11 N1 1.346(7) . ?
C11 C17 1.385(7) . ?
C11 C12 1.473(8) . ?
C12 N2 1.335(7) . ?
C12 C16 1.397(8) . ?
C13 N2 1.345(7) . ?
C13 C14 1.381(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.371(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.411(8) . ?
C19 Fe1 2.043(5) . ?
C19 H19 0.9500 . ?
C20 Fe1 2.032(5) . ?
C20 H20 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 C1 C5 107.9(5) . . ?
C2 C1 Fe1 70.0(3) . . ?
C5 C1 Fe1 69.3(3) . . ?
C2 C1 H1 126.1 . . ?
C5 C1 H1 126.1 . . ?
Fe1 C1 H1 126.2 . . ?
C3 C2 C1 108.3(5) . . ?
C3 C2 Fe1 70.0(3) . . ?
C1 C2 Fe1 69.6(3) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
Fe1 C2 H2 126.1 . . ?
C2 C3 C4 108.4(6) . . ?
C2 C3 Fe1 70.2(3) . . ?
C4 C3 Fe1 69.3(3) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
Fe1 C3 H3 126.2 . . ?
C3 C4 C5 108.3(5) . . ?
C3 C4 Fe1 70.3(3) . . ?
C5 C4 Fe1 69.7(3) . . ?
C3 C4 H4 125.8 . . ?
C5 C4 H4 125.8 . . ?
Fe1 C4 H4 125.7 . . ?
C4 C5 C1 107.1(5) . . ?
C4 C5 Fe1 69.7(3) . . ?
C1 C5 Fe1 69.9(3) . . ?
C4 C5 H5 126.5 . . ?
C1 C5 H5 126.5 . . ?
Fe1 C5 H5 125.6 . . ?
C7 C6 C20 107.2(5) . . ?
C7 C6 Fe1 69.7(3) . . ?
C20 C6 Fe1 69.2(3) . . ?
C7 C6 H6 126.4 . . ?
C20 C6 H6 126.4 . . ?
Fe1 C6 H6 126.3 . . ?
C6 C7 C8 108.7(5) . . ?
C6 C7 Fe1 69.8(3) . . ?
C8 C7 Fe1 70.5(3) . . ?
C6 C7 H7 125.6 . . ?
C8 C7 H7 125.6 . . ?
Fe1 C7 H7 125.6 . . ?
C19 C8 C7 107.3(5) . . ?
C19 C8 C9 126.4(5) . . ?
C7 C8 C9 126.3(5) . . ?
C19 C8 Fe1 69.0(3) . . ?
C7 C8 Fe1 68.8(3) . . ?
C9 C8 Fe1 127.2(4) . . ?
C18 C9 C10 116.0(5) . . ?
C18 C9 C8 123.0(5) . . ?
C10 C9 C8 120.9(5) . . ?
N1 C10 C9 125.0(5) . . ?
N1 C10 H10 117.5 . . ?
C9 C10 H10 117.5 . . ?
N1 C11 C17 121.3(5) . . ?
N1 C11 C12 117.1(5) . . ?
C17 C11 C12 121.5(5) . . ?
N2 C12 C16 122.7(5) . . ?
N2 C12 C11 116.6(5) . . ?
C16 C12 C11 120.7(5) . . ?
N2 C13 C14 123.8(5) . . ?
N2 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C13 C14 C15 118.0(5) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C16 C15 C14 119.2(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C12 118.7(5) . . ?
C15 C16 H16 120.6 . . ?
C12 C16 H16 120.6 . . ?
C18 C17 C11 120.1(5) . . ?
C18 C17 H17 119.9 . . ?
C11 C17 H17 119.9 . . ?
C17 C18 C9 119.8(5) . . ?
C17 C18 H18 120.1 . . ?
C9 C18 H18 120.1 . . ?
C20 C19 C8 108.0(5) . . ?
C20 C19 Fe1 69.3(3) . . ?
C8 C19 Fe1 70.4(3) . . ?
C20 C19 H19 126.0 . . ?
C8 C19 H19 126.0 . . ?
Fe1 C19 H19 125.8 . . ?
C19 C20 C6 108.7(5) . . ?
C19 C20 Fe1 70.1(3) . . ?
C6 C20 Fe1 69.9(3) . . ?
C19 C20 H20 125.6 . . ?
C6 C20 H20 125.6 . . ?
Fe1 C20 H20 125.9 . . ?
C10 N1 C11 117.7(5) . . ?
C12 N2 C13 117.5(5) . . ?
C20 Fe1 C4 154.6(2) . . ?
C20 Fe1 C5 162.6(2) . . ?
C4 Fe1 C5 40.6(3) . . ?
C20 Fe1 C7 68.3(2) . . ?
C4 Fe1 C7 109.0(2) . . ?
C5 Fe1 C7 121.6(2) . . ?
C20 Fe1 C6 40.9(2) . . ?
C4 Fe1 C6 120.3(2) . . ?
C5 Fe1 C6 155.6(3) . . ?
C7 Fe1 C6 40.5(2) . . ?
C20 Fe1 C19 40.5(2) . . ?
C4 Fe1 C19 164.1(2) . . ?
C5 Fe1 C19 126.2(2) . . ?
C7 Fe1 C19 68.5(2) . . ?
C6 Fe1 C19 68.7(2) . . ?
C20 Fe1 C1 124.7(2) . . ?
C4 Fe1 C1 68.0(2) . . ?
C5 Fe1 C1 40.8(2) . . ?
C7 Fe1 C1 156.5(2) . . ?
C6 Fe1 C1 161.6(3) . . ?
C19 Fe1 C1 107.6(2) . . ?
C20 Fe1 C3 119.4(2) . . ?
C4 Fe1 C3 40.4(2) . . ?
C5 Fe1 C3 68.1(3) . . ?
C7 Fe1 C3 126.3(2) . . ?
C6 Fe1 C3 107.3(3) . . ?
C19 Fe1 C3 153.7(2) . . ?
C1 Fe1 C3 67.5(3) . . ?
C20 Fe1 C2 106.7(2) . . ?
C4 Fe1 C2 67.6(2) . . ?
C5 Fe1 C2 68.3(2) . . ?
C7 Fe1 C2 162.0(2) . . ?
C6 Fe1 C2 124.5(2) . . ?
C19 Fe1 C2 119.7(2) . . ?
C1 Fe1 C2 40.4(3) . . ?
C3 Fe1 C2 39.7(2) . . ?
C20 Fe1 C8 68.1(2) . . ?
C4 Fe1 C8 127.4(2) . . ?
C5 Fe1 C8 109.0(2) . . ?
C7 Fe1 C8 40.7(2) . . ?
C6 Fe1 C8 68.5(2) . . ?
C19 Fe1 C8 40.6(2) . . ?
C1 Fe1 C8 121.3(2) . . ?
C3 Fe1 C8 164.1(2) . . ?
C2 Fe1 C8 155.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        22.89
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.161
_database_code_depnum_ccdc_archive 'CCDC 1000095'
#######################################################################
#
#                 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_JCSK3

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         'C20 H16 Fe N2'
_chemical_formula_sum            'C20 H16 Fe N2'
_chemical_formula_weight         340.20
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0963(23)
_cell_length_b                   20.1531(35)
_cell_length_c                   11.7129(24)
_cell_measurement_reflns_used    4220
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.208
_cell_measurement_theta_min      2.543
_cell_volume                     3091.4(9)
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 SADABS-2004/1 (Bruker,2004) was used for absorption correction.
 R(int) was 0.0850 before and 0.0566 after correction.
 The Ratio of minimum to maximum transmission is 0.703204.
 The λ/2 correction factor is 0.0015
;
_exptl_crystal_F_000             1408
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhomb
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_exptl_special_details           ?
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12480
_diffrn_reflns_theta_full        22.25
_diffrn_reflns_theta_max         22.25
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                1742
_reflns_number_total             1959
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    
;
Olex2, Durham University (compiled Apr 2 2009 15:09:25)
;
_computing_publication_material  
;
Olex2, Durham University (compiled Apr 2 2009 15:09:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.092
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0320
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0885
_refine_ls_weighting_details     
;
calc w=1/[σ²(Fo²)+(0.0420P)²+2.4531P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.5089(2) 0.44173(15) 0.3000(2) 0.0292(8) Uani 1 1 d . . .
H2 H 0.5399 0.4034 0.3275 0.035 Uiso 1 1 calc R . .
C8 C 0.2821(2) 0.62239(13) 0.2243(2) 0.0220(7) Uani 1 1 d . . .
H8 H 0.3017 0.6160 0.1487 0.026 Uiso 1 1 calc R . .
C4 C 0.4054(2) 0.53444(14) 0.2863(2) 0.0231(7) Uani 1 1 d . . .
C6 C 0.3273(2) 0.58476(13) 0.3104(2) 0.0207(6) Uani 1 1 d . . .
C23 C 0.2291(2) 0.44632(15) 0.1546(3) 0.0354(8) Uani 1 1 d . . .
H23 H 0.1836 0.4814 0.1634 0.043 Uiso 1 1 calc R . .
C3 C 0.4342(2) 0.47963(14) 0.3573(2) 0.0260(7) Uani 1 1 d . . .
H3 H 0.4079 0.4705 0.4294 0.031 Uiso 1 1 calc R . .
N1 N 0.22125(17) 0.64201(11) 0.44846(18) 0.0245(6) Uani 1 1 d . . .
C1 C 0.5286(2) 0.47216(15) 0.1932(2) 0.0316(7) Uani 1 1 d . . .
H1 H 0.5750 0.4575 0.1387 0.038 Uiso 1 1 calc R . .
C24 C 0.2924(2) 0.43518(16) 0.0602(3) 0.0362(8) Uani 1 1 d . . .
H24 H 0.2964 0.4617 -0.0047 0.043 Uiso 1 1 calc R . .
C5 C 0.4648(2) 0.52926(15) 0.1838(2) 0.0281(7) Uani 1 1 d . . .
H5 H 0.4622 0.5581 0.1220 0.034 Uiso 1 1 calc R . .
C22 C 0.2465(3) 0.39510(17) 0.2338(3) 0.0436(9) Uani 1 1 d . . .
H22 H 0.2147 0.3904 0.3043 0.052 Uiso 1 1 calc R . .
C21 C 0.3206(3) 0.35214(16) 0.1877(3) 0.0483(10) Uani 1 1 d . . .
H21 H 0.3461 0.3140 0.2222 0.058 Uiso 1 1 calc R . .
C11 C 0.0964(2) 0.72474(13) 0.3959(2) 0.0211(6) Uani 1 1 d . . .
C10 C 0.1783(2) 0.67702(13) 0.3632(2) 0.0205(6) Uani 1 1 d . . .
C12 C 0.0703(2) 0.73544(13) 0.5091(2) 0.0253(7) Uani 1 1 d . . .
H12 H 0.1041 0.7130 0.5672 0.030 Uiso 1 1 calc R . .
C7 C 0.2942(2) 0.59838(14) 0.4212(2) 0.0255(7) Uani 1 1 d . . .
H7 H 0.3252 0.5753 0.4806 0.031 Uiso 1 1 calc R . .
N2 N 0.04976(17) 0.75641(12) 0.30909(18) 0.0271(6) Uani 1 1 d . . .
C15 C -0.0554(2) 0.81277(14) 0.4461(2) 0.0312(7) Uani 1 1 d . . .
H15 H -0.1079 0.8427 0.4605 0.037 Uiso 1 1 calc R . .
C13 C -0.0237(2) 0.79987(15) 0.3363(3) 0.0333(8) Uani 1 1 d . . .
H13 H -0.0553 0.8228 0.2771 0.040 Uiso 1 1 calc R . .
C14 C -0.0069(2) 0.77989(14) 0.5343(2) 0.0301(7) Uani 1 1 d . . .
H14 H -0.0259 0.7876 0.6097 0.036 Uiso 1 1 calc R . .
C25 C 0.3490(2) 0.37705(17) 0.0804(3) 0.0454(9) Uani 1 1 d . . .
H25 H 0.3969 0.3584 0.0314 0.054 Uiso 1 1 calc R . .
C9 C 0.2088(2) 0.66893(13) 0.2504(2) 0.0210(6) Uani 1 1 d . . .
H9 H 0.1799 0.6947 0.1931 0.025 Uiso 1 1 calc R . .
Fe1 Fe 0.37833(3) 0.446056(19) 0.20433(3) 0.02394(19) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix. The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry. An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 C3 1.411(4) . ?
C2 C1 1.416(4) . ?
C2 Fe1 2.047(3) . ?
C2 H2 0.9300 . ?
C8 C9 1.377(4) . ?
C8 C6 1.394(4) . ?
C8 H8 0.9300 . ?
C4 C3 1.433(4) . ?
C4 C5 1.435(4) . ?
C4 C6 1.467(4) . ?
C4 Fe1 2.054(3) . ?
C6 C7 1.395(4) . ?
C23 C24 1.401(4) . ?
C23 C22 1.406(5) . ?
C23 Fe1 2.039(3) . ?
C23 H23 0.9300 . ?
C3 Fe1 2.050(3) . ?
C3 H3 0.9300 . ?
N1 C7 1.337(3) . ?
N1 C10 1.346(3) . ?
C1 C5 1.426(4) . ?
C1 Fe1 2.041(3) . ?
C1 H1 0.9300 . ?
C24 C25 1.406(5) . ?
C24 Fe1 2.040(3) . ?
C24 H24 0.9300 . ?
C5 Fe1 2.038(3) . ?
C5 H5 0.9300 . ?
C22 C21 1.408(5) . ?
C22 Fe1 2.038(3) . ?
C22 H22 0.9300 . ?
C21 C25 1.403(5) . ?
C21 Fe1 2.048(3) . ?
C21 H21 0.9300 . ?
C11 N2 1.347(3) . ?
C11 C12 1.386(4) . ?
C11 C10 1.491(4) . ?
C10 C9 1.389(4) . ?
C12 C14 1.382(4) . ?
C12 H12 0.9300 . ?
C7 H7 0.9300 . ?
N2 C13 1.339(4) . ?
C15 C13 1.377(4) . ?
C15 C14 1.382(4) . ?
C15 H15 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C25 Fe1 2.046(3) . ?
C25 H25 0.9300 . ?
C9 H9 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 C2 C1 108.2(3) . . ?
C3 C2 Fe1 69.99(16) . . ?
C1 C2 Fe1 69.51(16) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Fe1 C2 H2 126.2 . . ?
C9 C8 C6 120.4(2) . . ?
C9 C8 H8 119.8 . . ?
C6 C8 H8 119.8 . . ?
C3 C4 C5 106.6(2) . . ?
C3 C4 C6 127.2(2) . . ?
C5 C4 C6 126.1(2) . . ?
C3 C4 Fe1 69.41(16) . . ?
C5 C4 Fe1 68.85(16) . . ?
C6 C4 Fe1 124.67(19) . . ?
C8 C6 C7 115.7(3) . . ?
C8 C6 C4 122.2(2) . . ?
C7 C6 C4 122.1(2) . . ?
C24 C23 C22 107.9(3) . . ?
C24 C23 Fe1 69.96(17) . . ?
C22 C23 Fe1 69.78(18) . . ?
C24 C23 H23 126.1 . . ?
C22 C23 H23 126.1 . . ?
Fe1 C23 H23 125.8 . . ?
C2 C3 C4 108.9(3) . . ?
C2 C3 Fe1 69.71(16) . . ?
C4 C3 Fe1 69.72(15) . . ?
C2 C3 H3 125.5 . . ?
C4 C3 H3 125.5 . . ?
Fe1 C3 H3 126.6 . . ?
C7 N1 C10 117.8(2) . . ?
C2 C1 C5 108.1(3) . . ?
C2 C1 Fe1 69.94(17) . . ?
C5 C1 Fe1 69.42(16) . . ?
C2 C1 H1 125.9 . . ?
C5 C1 H1 125.9 . . ?
Fe1 C1 H1 126.3 . . ?
C23 C24 C25 108.2(3) . . ?
C23 C24 Fe1 69.88(17) . . ?
C25 C24 Fe1 70.10(18) . . ?
C23 C24 H24 125.9 . . ?
C25 C24 H24 125.9 . . ?
Fe1 C24 H24 125.7 . . ?
C1 C5 C4 108.2(2) . . ?
C1 C5 Fe1 69.65(16) . . ?
C4 C5 Fe1 70.10(16) . . ?
C1 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
Fe1 C5 H5 125.9 . . ?
C23 C22 C21 108.1(3) . . ?
C23 C22 Fe1 69.88(18) . . ?
C21 C22 Fe1 70.21(19) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
Fe1 C22 H22 125.5 . . ?
C25 C21 C22 107.8(3) . . ?
C25 C21 Fe1 69.90(19) . . ?
C22 C21 Fe1 69.48(18) . . ?
C25 C21 H21 126.1 . . ?
C22 C21 H21 126.1 . . ?
Fe1 C21 H21 126.1 . . ?
N2 C11 C12 122.4(2) . . ?
N2 C11 C10 115.9(2) . . ?
C12 C11 C10 121.6(2) . . ?
N1 C10 C9 121.6(2) . . ?
N1 C10 C11 116.6(2) . . ?
C9 C10 C11 121.8(2) . . ?
C14 C12 C11 119.1(3) . . ?
C14 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
N1 C7 C6 125.0(2) . . ?
N1 C7 H7 117.5 . . ?
C6 C7 H7 117.5 . . ?
C13 N2 C11 117.1(2) . . ?
C13 C15 C14 118.0(3) . . ?
C13 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
N2 C13 C15 124.2(3) . . ?
N2 C13 H13 117.9 . . ?
C15 C13 H13 117.9 . . ?
C15 C14 C12 119.2(3) . . ?
C15 C14 H14 120.4 . . ?
C12 C14 H14 120.4 . . ?
C21 C25 C24 108.0(3) . . ?
C21 C25 Fe1 70.01(18) . . ?
C24 C25 Fe1 69.65(17) . . ?
C21 C25 H25 126.0 . . ?
C24 C25 H25 126.0 . . ?
Fe1 C25 H25 125.9 . . ?
C8 C9 C10 119.5(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C5 Fe1 C22 154.88(13) . . ?
C5 Fe1 C23 119.80(12) . . ?
C22 Fe1 C23 40.35(13) . . ?
C5 Fe1 C24 107.30(12) . . ?
C22 Fe1 C24 67.60(13) . . ?
C23 Fe1 C24 40.15(12) . . ?
C5 Fe1 C1 40.93(12) . . ?
C22 Fe1 C1 163.19(14) . . ?
C23 Fe1 C1 154.84(13) . . ?
C24 Fe1 C1 120.43(12) . . ?
C5 Fe1 C25 125.44(13) . . ?
C22 Fe1 C25 67.59(14) . . ?
C23 Fe1 C25 67.63(12) . . ?
C24 Fe1 C25 40.25(13) . . ?
C1 Fe1 C25 108.11(13) . . ?
C5 Fe1 C2 68.60(12) . . ?
C22 Fe1 C2 126.42(13) . . ?
C23 Fe1 C2 163.21(13) . . ?
C24 Fe1 C2 155.39(12) . . ?
C1 Fe1 C2 40.55(11) . . ?
C25 Fe1 C2 121.07(12) . . ?
C5 Fe1 C21 162.71(14) . . ?
C22 Fe1 C21 40.30(14) . . ?
C23 Fe1 C21 67.73(13) . . ?
C24 Fe1 C21 67.56(13) . . ?
C1 Fe1 C21 126.05(14) . . ?
C25 Fe1 C21 40.10(14) . . ?
C2 Fe1 C21 108.76(13) . . ?
C5 Fe1 C3 68.48(11) . . ?
C22 Fe1 C3 108.70(12) . . ?
C23 Fe1 C3 126.20(12) . . ?
C24 Fe1 C3 162.79(12) . . ?
C1 Fe1 C3 68.08(11) . . ?
C25 Fe1 C3 155.65(13) . . ?
C2 Fe1 C3 40.30(11) . . ?
C21 Fe1 C3 121.34(13) . . ?
C5 Fe1 C4 41.05(11) . . ?
C22 Fe1 C4 120.24(13) . . ?
C23 Fe1 C4 107.24(12) . . ?
C24 Fe1 C4 125.10(12) . . ?
C1 Fe1 C4 68.92(12) . . ?
C25 Fe1 C4 162.39(13) . . ?
C2 Fe1 C4 68.71(11) . . ?
C21 Fe1 C4 155.44(14) . . ?
C3 Fe1 C4 40.87(11) . . ?
_database_code_depnum_ccdc_archive 'CCDC 1000096'
#######################################################################
#
#                 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_dt78

_audit_creation_date             2010-04-22T13:25:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H36 Fe N6 Pd, 2(F6 Sb), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H42 F12 Fe N8 Pd Sb2'
_chemical_formula_weight         1244.55

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.635(2)
_cell_length_b                   13.391(2)
_cell_length_c                   15.929(2)
_cell_angle_alpha                67.083(7)
_cell_angle_beta                 84.398(7)
_cell_angle_gamma                82.022(7)
_cell_volume                     2261.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    89(2)
_cell_measurement_reflns_used    8727
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      30.98

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.781
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_type   multi-scan

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      89(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_number            32184
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             8362
_reflns_number_gt                7595
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)'
_computing_publication_material  
'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0199P)²+3.3239P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8362
_refine_ls_number_parameters     609
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0589
_refine_ls_wR_factor_gt          0.056
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.079

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 1.1638(3) 0.1048(3) 0.1950(2) 0.0299(7) Uani 1 1 d . . .
H1 H 1.1743 0.16 0.2143 0.036 Uiso 1 1 calc R . .
C2 C 1.0644(3) 0.0470(3) 0.2153(2) 0.0329(8) Uani 1 1 d . . .
H2 H 0.9985 0.0575 0.2503 0.04 Uiso 1 1 calc R . .
C3 C 1.0839(3) -0.0298(2) 0.1726(2) 0.0313(7) Uani 1 1 d . . .
H3 H 1.0328 -0.0783 0.1745 0.038 Uiso 1 1 calc R . .
C4 C 1.1945(3) -0.0195(2) 0.1268(2) 0.0290(7) Uani 1 1 d . . .
H4 H 1.2291 -0.0602 0.0934 0.035 Uiso 1 1 calc R . .
C5 C 1.2438(3) 0.0638(3) 0.1404(2) 0.0287(7) Uani 1 1 d . . .
H5 H 1.3162 0.0873 0.1175 0.034 Uiso 1 1 calc R . .
C6 C 0.9404(2) 0.2246(2) 0.03419(19) 0.0206(6) Uani 1 1 d . . .
H6 H 0.8733 0.2302 0.0697 0.025 Uiso 1 1 calc R . .
C7 C 0.9644(2) 0.1540(2) -0.0136(2) 0.0218(6) Uani 1 1 d U . .
H7 H 0.9162 0.1044 -0.0142 0.026 Uiso 1 1 calc R . .
C8 C 1.0744(3) 0.1714(2) -0.06034(19) 0.0218(6) Uani 1 1 d . . .
H8 H 1.1103 0.1356 -0.0972 0.026 Uiso 1 1 calc R . .
C9 C 1.1205(2) 0.2528(2) -0.04145(19) 0.0193(6) Uani 1 1 d . . .
H9 H 1.1916 0.2798 -0.0637 0.023 Uiso 1 1 calc R . .
C10 C 1.0374(2) 0.2860(2) 0.01830(19) 0.0171(6) Uani 1 1 d . . .
C11 C 0.9697(2) 0.3785(2) 0.12494(18) 0.0159(5) Uani 1 1 d . . .
H11 H 0.9026 0.3438 0.1363 0.019 Uiso 1 1 calc R . .
C12 C 1.0547(2) 0.3601(2) 0.06291(18) 0.0165(6) Uani 1 1 d U . .
C13 C 1.1550(2) 0.4127(2) 0.0483(2) 0.0199(6) Uani 1 1 d . . .
H13 H 1.2147 0.402 0.0083 0.024 Uiso 1 1 calc R . .
C14 C 1.1655(2) 0.4808(2) 0.09350(19) 0.0190(6) Uani 1 1 d . . .
H14 H 1.2322 0.5156 0.0838 0.023 Uiso 1 1 calc R . .
C15 C 1.0767(2) 0.4969(2) 0.15308(18) 0.0162(6) Uani 1 1 d . . .
C16 C 1.0755(2) 0.5689(2) 0.20310(18) 0.0161(5) Uani 1 1 d . . .
C17 C 1.1659(2) 0.6294(2) 0.19715(19) 0.0195(6) Uani 1 1 d . . .
H17 H 1.2317 0.6261 0.1598 0.023 Uiso 1 1 calc R . .
C18 C 1.1574(3) 0.6950(2) 0.2474(2) 0.0221(6) Uani 1 1 d . . .
H18 H 1.2175 0.7355 0.2444 0.027 Uiso 1 1 calc R . .
C19 C 1.0583(3) 0.6991(2) 0.3019(2) 0.0228(6) Uani 1 1 d . . .
H19 H 1.0508 0.7427 0.3359 0.027 Uiso 1 1 calc R . .
C20 C 0.9704(3) 0.6375(2) 0.30517(19) 0.0211(6) Uani 1 1 d . . .
H20 H 0.9037 0.6406 0.3417 0.025 Uiso 1 1 calc R . .
C21 C 0.7842(3) 0.4507(2) 0.4486(2) 0.0237(6) Uani 1 1 d U . .
H21 H 0.8453 0.3952 0.4642 0.028 Uiso 1 1 calc R . .
C22 C 0.7241(3) 0.4769(2) 0.5163(2) 0.0230(6) Uani 1 1 d . . .
H22 H 0.7441 0.4386 0.5766 0.028 Uiso 1 1 calc R . .
C23 C 0.6316(2) 0.5620(2) 0.49576(19) 0.0193(6) Uani 1 1 d . . .
C24 C 0.6055(2) 0.6139(2) 0.40254(19) 0.0197(6) Uani 1 1 d . . .
H24 H 0.5449 0.6698 0.3848 0.024 Uiso 1 1 calc R . .
C25 C 0.6691(2) 0.5820(2) 0.3385(2) 0.0201(6) Uani 1 1 d U . .
H25 H 0.6496 0.6169 0.2779 0.024 Uiso 1 1 calc R . .
C26 C 0.6022(3) 0.5339(3) 0.6571(2) 0.0275(7) Uani 1 1 d . . .
C27 C 0.4855(3) 0.6847(3) 0.5394(2) 0.0301(7) Uani 1 1 d . . .
C28 C 0.7986(2) 0.2480(2) 0.3230(2) 0.0207(6) Uani 1 1 d . . .
H28 H 0.8667 0.2316 0.3542 0.025 Uiso 1 1 calc R . .
C29 C 0.7360(2) 0.1644(2) 0.3335(2) 0.0214(6) Uani 1 1 d . . .
H29 H 0.7618 0.0934 0.3711 0.026 Uiso 1 1 calc R . .
C30 C 0.6318(2) 0.1857(2) 0.28707(19) 0.0212(6) Uani 1 1 d . . .
C31 C 0.6024(2) 0.2954(2) 0.22808(19) 0.0211(6) Uani 1 1 d . . .
H31 H 0.5372 0.3141 0.1934 0.025 Uiso 1 1 calc R . .
C32 C 0.6700(2) 0.3739(2) 0.22226(19) 0.0199(6) Uani 1 1 d . . .
H32 H 0.6483 0.4455 0.1836 0.024 Uiso 1 1 calc R . .
C33 C 0.5938(4) -0.0040(3) 0.3660(3) 0.0399(9) Uani 1 1 d . . .
C34 C 0.4557(3) 0.1306(4) 0.2539(3) 0.0391(9) Uani 1 1 d . . .
C100 C 0.7050(4) 0.1355(3) 0.6345(2) 0.0393(9) Uani 1 1 d . . .
C101 C 0.7806(4) 0.0779(3) 0.5857(3) 0.0540(11) Uani 1 1 d . . .
H10A H 0.7544 0.0997 0.5252 0.081 Uiso 1 1 calc R . .
H10B H 0.7786 0.0007 0.6175 0.081 Uiso 1 1 calc R . .
H10C H 0.8587 0.0953 0.5823 0.081 Uiso 1 1 calc R . .
C102 C 0.3158(5) 0.0333(4) 0.8447(4) 0.0687(13) Uani 1 1 d U . .
C103 C 0.4075(4) 0.0802(4) 0.8665(4) 0.0793(16) Uani 1 1 d . . .
H10D H 0.3743 0.1346 0.8897 0.119 Uiso 1 1 calc R . .
H10E H 0.4551 0.1132 0.8124 0.119 Uiso 1 1 calc R . .
H10F H 0.4542 0.0241 0.9117 0.119 Uiso 1 1 calc R . .
N1 N 0.97868(19) 0.57340(18) 0.25732(16) 0.0172(5) Uani 1 1 d . . .
N2 N 0.98034(19) 0.44362(18) 0.16873(15) 0.0159(5) Uani 1 1 d . . .
N3 N 0.76682(18) 0.35320(18) 0.26971(15) 0.0166(5) Uani 1 1 d . . .
N4 N 0.75894(19) 0.50190(19) 0.35936(16) 0.0189(5) Uani 1 1 d . . .
N5 N 0.5644(2) 0.1062(2) 0.29987(17) 0.0264(6) Uani 1 1 d . . .
N6 N 0.5731(2) 0.5911(2) 0.56174(16) 0.0225(5) Uani 1 1 d . . .
N100 N 0.6447(3) 0.1804(3) 0.6710(3) 0.0575(10) Uani 1 1 d . . .
N101 N 0.2431(4) -0.0038(5) 0.8278(4) 0.111(2) Uani 1 1 d . . .
F1 F 0.29405(18) 0.2073(2) 0.42090(18) 0.0653(7) Uani 1 1 d . . .
F2 F 0.1299(2) 0.37640(18) 0.39083(18) 0.0638(7) Uani 1 1 d . . .
F3 F 0.1831(2) 0.24777(19) 0.55926(16) 0.0548(6) Uani 1 1 d . . .
F4 F 0.14296(19) 0.07700(16) 0.52733(17) 0.0538(6) Uani 1 1 d . . .
F5 F 0.0905(2) 0.2054(2) 0.35869(16) 0.0629(7) Uani 1 1 d . . .
F6 F -0.01840(16) 0.24345(17) 0.49709(15) 0.0442(5) Uani 1 1 d . . .
F7 F 0.44343(16) 0.54366(15) 0.12366(13) 0.0334(4) Uani 1 1 d . . .
F8 F 0.56276(16) 0.63462(18) -0.03561(13) 0.0418(5) Uani 1 1 d . . .
F9 F 0.62086(15) 0.65270(16) 0.11257(12) 0.0350(4) Uani 1 1 d . . .
F10 F 0.40682(19) 0.73505(19) 0.13751(16) 0.0530(6) Uani 1 1 d . . .
F11 F 0.34372(17) 0.7100(2) -0.00919(15) 0.0524(6) Uani 1 1 d . . .
F12 F 0.52089(19) 0.82491(17) -0.01994(16) 0.0526(6) Uani 1 1 d . . .
Fe1 Fe 1.08958(3) 0.12519(3) 0.07768(3) 0.01747(9) Uani 1 1 d . . .
Pd1 Pd 0.865238(17) 0.469368(17) 0.263157(14) 0.01544(6) Uani 1 1 d . . .
Sb1 Sb 0.138786(17) 0.226394(17) 0.458565(14) 0.02586(6) Uani 1 1 d . . .
Sb2 Sb 0.482033(16) 0.683940(17) 0.050508(13) 0.02384(6) Uani 1 1 d . . .
H26A H 0.678(4) 0.546(3) 0.671(3) 0.049(11) Uiso 1 1 d . . .
H26B H 0.598(3) 0.458(3) 0.678(2) 0.028(9) Uiso 1 1 d . . .
H26C H 0.543(3) 0.555(3) 0.695(3) 0.051(11) Uiso 1 1 d . . .
H27A H 0.453(4) 0.693(4) 0.595(3) 0.070(14) Uiso 1 1 d . . .
H27B H 0.425(4) 0.677(4) 0.514(3) 0.067(14) Uiso 1 1 d . . .
H27C H 0.515(4) 0.748(4) 0.501(3) 0.066(14) Uiso 1 1 d . . .
H33A H 0.540(4) -0.049(3) 0.364(3) 0.053(12) Uiso 1 1 d . . .
H33B H 0.671(4) -0.033(3) 0.352(3) 0.060(13) Uiso 1 1 d . . .
H33C H 0.589(3) -0.001(3) 0.424(3) 0.053(12) Uiso 1 1 d . . .
H34A H 0.468(3) 0.164(3) 0.194(3) 0.044(11) Uiso 1 1 d . . .
H34B H 0.400(4) 0.174(3) 0.276(3) 0.058(13) Uiso 1 1 d . . .
H34C H 0.429(3) 0.058(3) 0.267(3) 0.046(11) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 C5 1.412(5) . ?
C1 C2 1.422(5) . ?
C1 Fe1 2.041(3) . ?
C1 H1 0.93 . ?
C2 C3 1.422(5) . ?
C2 Fe1 2.040(3) . ?
C2 H2 0.93 . ?
C3 C4 1.413(5) . ?
C3 Fe1 2.043(3) . ?
C3 H3 0.93 . ?
C4 C5 1.418(4) . ?
C4 Fe1 2.051(3) . ?
C4 H4 0.93 . ?
C5 Fe1 2.049(3) . ?
C5 H5 0.93 . ?
C6 C7 1.412(4) . ?
C6 C10 1.434(4) . ?
C6 Fe1 2.035(3) . ?
C6 H6 0.93 . ?
C7 C8 1.417(4) . ?
C7 Fe1 2.050(3) . ?
C7 H7 0.93 . ?
C8 C9 1.420(4) . ?
C8 Fe1 2.058(3) . ?
C8 H8 0.93 . ?
C9 C10 1.439(4) . ?
C9 Fe1 2.040(3) . ?
C9 H9 0.93 . ?
C10 C12 1.470(4) . ?
C10 Fe1 2.016(3) . ?
C11 N2 1.335(3) . ?
C11 C12 1.395(4) . ?
C11 H11 0.93 . ?
C12 C13 1.400(4) . ?
C13 C14 1.386(4) . ?
C13 H13 0.93 . ?
C14 C15 1.386(4) . ?
C14 H14 0.93 . ?
C15 N2 1.362(3) . ?
C15 C16 1.469(4) . ?
C16 N1 1.360(3) . ?
C16 C17 1.390(4) . ?
C17 C18 1.388(4) . ?
C17 H17 0.93 . ?
C18 C19 1.382(4) . ?
C18 H18 0.93 . ?
C19 C20 1.386(4) . ?
C19 H19 0.93 . ?
C20 N1 1.341(4) . ?
C20 H20 0.93 . ?
C21 N4 1.358(4) . ?
C21 C22 1.362(4) . ?
C21 H21 0.93 . ?
C22 C23 1.415(4) . ?
C22 H22 0.93 . ?
C23 N6 1.351(3) . ?
C23 C24 1.416(4) . ?
C24 C25 1.369(4) . ?
C24 H24 0.93 . ?
C25 N4 1.354(4) . ?
C25 H25 0.93 . ?
C26 N6 1.460(4) . ?
C26 H26A 0.98(4) . ?
C26 H26B 0.95(3) . ?
C26 H26C 0.96(4) . ?
C27 N6 1.451(4) . ?
C27 H27A 0.97(5) . ?
C27 H27B 0.88(5) . ?
C27 H27C 0.92(5) . ?
C28 N3 1.352(4) . ?
C28 C29 1.367(4) . ?
C28 H28 0.93 . ?
C29 C30 1.418(4) . ?
C29 H29 0.93 . ?
C30 N5 1.349(4) . ?
C30 C31 1.417(4) . ?
C31 C32 1.368(4) . ?
C31 H31 0.93 . ?
C32 N3 1.354(4) . ?
C32 H32 0.93 . ?
C33 N5 1.458(4) . ?
C33 H33A 0.94(4) . ?
C33 H33B 0.98(4) . ?
C33 H33C 0.94(4) . ?
C34 N5 1.457(4) . ?
C34 H34A 0.88(4) . ?
C34 H34B 0.94(4) . ?
C34 H34C 1.00(4) . ?
C100 N100 1.125(5) . ?
C100 C101 1.456(6) . ?
C101 H10A 0.96 . ?
C101 H10B 0.96 . ?
C101 H10C 0.96 . ?
C102 N101 1.141(7) . ?
C102 C103 1.442(7) . ?
C103 H10D 0.96 . ?
C103 H10E 0.96 . ?
C103 H10F 0.96 . ?
N1 Pd1 2.019(2) . ?
N2 Pd1 2.014(2) . ?
N3 Pd1 2.022(2) . ?
N4 Pd1 2.017(2) . ?
F1 Sb1 1.862(2) . ?
F2 Sb1 1.867(2) . ?
F3 Sb1 1.866(2) . ?
F4 Sb1 1.866(2) . ?
F5 Sb1 1.869(2) . ?
F6 Sb1 1.883(2) . ?
F7 Sb2 1.8750(19) . ?
F8 Sb2 1.8661(18) . ?
F9 Sb2 1.8878(19) . ?
F10 Sb2 1.8683(19) . ?
F11 Sb2 1.871(2) . ?
F12 Sb2 1.875(2) . ?

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
C5 C1 C2 108.2(3) . . ?
C5 C1 Fe1 70.10(17) . . ?
C2 C1 Fe1 69.59(18) . . ?
C5 C1 H1 125.9 . . ?
C2 C1 H1 125.9 . . ?
Fe1 C1 H1 126 . . ?
C3 C2 C1 107.6(3) . . ?
C3 C2 Fe1 69.71(18) . . ?
C1 C2 Fe1 69.63(18) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
Fe1 C2 H2 126 . . ?
C4 C3 C2 108.0(3) . . ?
C4 C3 Fe1 70.11(18) . . ?
C2 C3 Fe1 69.51(18) . . ?
C4 C3 H3 126 . . ?
C2 C3 H3 126 . . ?
Fe1 C3 H3 126 . . ?
C3 C4 C5 108.2(3) . . ?
C3 C4 Fe1 69.51(18) . . ?
C5 C4 Fe1 69.69(17) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Fe1 C4 H4 126.5 . . ?
C1 C5 C4 108.0(3) . . ?
C1 C5 Fe1 69.49(17) . . ?
C4 C5 Fe1 69.84(17) . . ?
C1 C5 H5 126 . . ?
C4 C5 H5 126 . . ?
Fe1 C5 H5 126.2 . . ?
C7 C6 C10 108.0(2) . . ?
C7 C6 Fe1 70.34(16) . . ?
C10 C6 Fe1 68.58(15) . . ?
C7 C6 H6 126 . . ?
C10 C6 H6 126 . . ?
Fe1 C6 H6 126.7 . . ?
C6 C7 C8 108.5(2) . . ?
C6 C7 Fe1 69.20(16) . . ?
C8 C7 Fe1 70.11(16) . . ?
C6 C7 H7 125.7 . . ?
C8 C7 H7 125.7 . . ?
Fe1 C7 H7 126.5 . . ?
C7 C8 C9 108.5(2) . . ?
C7 C8 Fe1 69.53(16) . . ?
C9 C8 Fe1 69.08(16) . . ?
C7 C8 H8 125.8 . . ?
C9 C8 H8 125.8 . . ?
Fe1 C8 H8 127.2 . . ?
C8 C9 C10 107.6(2) . . ?
C8 C9 Fe1 70.38(16) . . ?
C10 C9 Fe1 68.33(16) . . ?
C8 C9 H9 126.2 . . ?
C10 C9 H9 126.2 . . ?
Fe1 C9 H9 126.6 . . ?
C6 C10 C9 107.4(2) . . ?
C6 C10 C12 126.2(2) . . ?
C9 C10 C12 126.0(2) . . ?
C6 C10 Fe1 69.98(16) . . ?
C9 C10 Fe1 70.14(15) . . ?
C12 C10 Fe1 120.15(19) . . ?
N2 C11 C12 123.0(2) . . ?
N2 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C11 C12 C13 116.9(2) . . ?
C11 C12 C10 119.8(2) . . ?
C13 C12 C10 123.3(2) . . ?
C14 C13 C12 120.0(2) . . ?
C14 C13 H13 120 . . ?
C12 C13 H13 120 . . ?
C13 C14 C15 120.0(2) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
N2 C15 C14 119.8(2) . . ?
N2 C15 C16 114.7(2) . . ?
C14 C15 C16 125.5(2) . . ?
N1 C16 C17 120.8(2) . . ?
N1 C16 C15 115.7(2) . . ?
C17 C16 C15 123.6(2) . . ?
C18 C17 C16 119.5(3) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C19 C18 C17 119.1(3) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 119.1(3) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
N1 C20 C19 122.0(3) . . ?
N1 C20 H20 119 . . ?
C19 C20 H20 119 . . ?
N4 C21 C22 123.1(3) . . ?
N4 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
N6 C23 C24 122.9(3) . . ?
N6 C23 C22 121.3(3) . . ?
C24 C23 C22 115.8(2) . . ?
C25 C24 C23 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
N4 C25 C24 123.1(3) . . ?
N4 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N6 C26 H26A 114(2) . . ?
N6 C26 H26B 113(2) . . ?
H26A C26 H26B 109(3) . . ?
N6 C26 H26C 109(2) . . ?
H26A C26 H26C 109(3) . . ?
H26B C26 H26C 102(3) . . ?
N6 C27 H27A 109(3) . . ?
N6 C27 H27B 113(3) . . ?
H27A C27 H27B 104(4) . . ?
N6 C27 H27C 112(3) . . ?
H27A C27 H27C 110(4) . . ?
H27B C27 H27C 108(4) . . ?
N3 C28 C29 123.4(3) . . ?
N3 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
N5 C30 C31 122.4(3) . . ?
N5 C30 C29 121.7(3) . . ?
C31 C30 C29 115.9(3) . . ?
C32 C31 C30 119.9(3) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
N3 C32 C31 123.6(3) . . ?
N3 C32 H32 118.2 . . ?
C31 C32 H32 118.2 . . ?
N5 C33 H33A 109(3) . . ?
N5 C33 H33B 111(3) . . ?
H33A C33 H33B 108(3) . . ?
N5 C33 H33C 108(3) . . ?
H33A C33 H33C 110(3) . . ?
H33B C33 H33C 111(4) . . ?
N5 C34 H34A 110(3) . . ?
N5 C34 H34B 111(3) . . ?
H34A C34 H34B 110(4) . . ?
N5 C34 H34C 105(2) . . ?
H34A C34 H34C 109(3) . . ?
H34B C34 H34C 111(3) . . ?
N100 C100 C101 178.5(4) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
N101 C102 C103 179.7(6) . . ?
C102 C103 H10D 109.5 . . ?
C102 C103 H10E 109.5 . . ?
H10D C103 H10E 109.5 . . ?
C102 C103 H10F 109.5 . . ?
H10D C103 H10F 109.5 . . ?
H10E C103 H10F 109.5 . . ?
C20 N1 C16 119.5(2) . . ?
C20 N1 Pd1 126.68(19) . . ?
C16 N1 Pd1 113.65(17) . . ?
C11 N2 C15 120.3(2) . . ?
C11 N2 Pd1 125.44(18) . . ?
C15 N2 Pd1 114.27(17) . . ?
C28 N3 C32 116.9(2) . . ?
C28 N3 Pd1 119.32(18) . . ?
C32 N3 Pd1 123.74(19) . . ?
C25 N4 C21 117.3(2) . . ?
C25 N4 Pd1 122.63(19) . . ?
C21 N4 Pd1 119.69(19) . . ?
C30 N5 C34 120.8(3) . . ?
C30 N5 C33 120.6(3) . . ?
C34 N5 C33 118.4(3) . . ?
C23 N6 C27 121.1(3) . . ?
C23 N6 C26 120.8(2) . . ?
C27 N6 C26 118.0(2) . . ?
C10 Fe1 C6 41.45(11) . . ?
C10 Fe1 C2 119.56(13) . . ?
C6 Fe1 C2 105.93(13) . . ?
C10 Fe1 C1 105.83(12) . . ?
C6 Fe1 C1 123.07(12) . . ?
C2 Fe1 C1 40.78(13) . . ?
C10 Fe1 C9 41.54(11) . . ?
C6 Fe1 C9 69.23(11) . . ?
C2 Fe1 C9 156.37(12) . . ?
C1 Fe1 C9 121.25(12) . . ?
C10 Fe1 C3 155.79(12) . . ?
C6 Fe1 C3 120.60(13) . . ?
C2 Fe1 C3 40.77(13) . . ?
C1 Fe1 C3 68.41(13) . . ?
C9 Fe1 C3 161.57(12) . . ?
C10 Fe1 C5 123.56(12) . . ?
C6 Fe1 C5 160.26(12) . . ?
C2 Fe1 C5 68.30(14) . . ?
C1 Fe1 C5 40.40(13) . . ?
C9 Fe1 C5 108.05(12) . . ?
C3 Fe1 C5 68.18(13) . . ?
C10 Fe1 C7 68.99(11) . . ?
C6 Fe1 C7 40.46(11) . . ?
C2 Fe1 C7 123.64(13) . . ?
C1 Fe1 C7 159.98(13) . . ?
C9 Fe1 C7 68.49(12) . . ?
C3 Fe1 C7 107.94(12) . . ?
C5 Fe1 C7 158.32(12) . . ?
C10 Fe1 C4 161.23(12) . . ?
C6 Fe1 C4 156.79(12) . . ?
C2 Fe1 C4 68.21(13) . . ?
C1 Fe1 C4 68.06(13) . . ?
C9 Fe1 C4 125.15(12) . . ?
C3 Fe1 C4 40.39(13) . . ?
C5 Fe1 C4 40.47(12) . . ?
C7 Fe1 C4 122.78(12) . . ?
C10 Fe1 C8 68.94(11) . . ?
C6 Fe1 C8 68.26(11) . . ?
C2 Fe1 C8 160.91(13) . . ?
C1 Fe1 C8 157.61(13) . . ?
C9 Fe1 C8 40.54(11) . . ?
C3 Fe1 C8 125.20(12) . . ?
C5 Fe1 C8 123.18(13) . . ?
C7 Fe1 C8 40.36(11) . . ?
C4 Fe1 C8 109.53(12) . . ?
N2 Pd1 N4 175.53(9) . . ?
N2 Pd1 N1 81.33(9) . . ?
N4 Pd1 N1 94.27(9) . . ?
N2 Pd1 N3 94.36(9) . . ?
N4 Pd1 N3 89.98(9) . . ?
N1 Pd1 N3 173.77(9) . . ?
F1 Sb1 F3 90.41(11) . . ?
F1 Sb1 F4 90.19(11) . . ?
F3 Sb1 F4 89.94(11) . . ?
F1 Sb1 F2 91.53(12) . . ?
F3 Sb1 F2 90.09(11) . . ?
F4 Sb1 F2 178.27(11) . . ?
F1 Sb1 F5 91.03(11) . . ?
F3 Sb1 F5 178.56(10) . . ?
F4 Sb1 F5 90.04(12) . . ?
F2 Sb1 F5 89.88(12) . . ?
F1 Sb1 F6 179.11(11) . . ?
F3 Sb1 F6 89.90(10) . . ?
F4 Sb1 F6 88.98(10) . . ?
F2 Sb1 F6 89.29(10) . . ?
F5 Sb1 F6 88.65(10) . . ?
F8 Sb2 F10 177.67(9) . . ?
F8 Sb2 F11 90.95(10) . . ?
F10 Sb2 F11 91.11(11) . . ?
F8 Sb2 F12 89.37(10) . . ?
F10 Sb2 F12 89.48(10) . . ?
F11 Sb2 F12 91.94(10) . . ?
F8 Sb2 F7 91.84(9) . . ?
F10 Sb2 F7 89.28(9) . . ?
F11 Sb2 F7 88.86(9) . . ?
F12 Sb2 F7 178.54(10) . . ?
F8 Sb2 F9 88.73(9) . . ?
F10 Sb2 F9 89.25(10) . . ?
F11 Sb2 F9 178.10(9) . . ?
F12 Sb2 F9 89.93(9) . . ?
F7 Sb2 F9 89.28(8) . . ?

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 1000097'
#######################################################################
#
#                 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_kjs117

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H26 F12 Fe N4 Pd Sb2'
_chemical_formula_weight         1076.30

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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   31.201(4)
_cell_length_b                   11.3669(11)
_cell_length_c                   19.088(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.873(4)
_cell_angle_gamma                90.00
_cell_volume                     6734.2(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    89(2)
_cell_measurement_reflns_used    8105
_cell_measurement_theta_min      2.627
_cell_measurement_theta_max      24.40

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4128
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_process_details   'TWINABS(Bruker, 2004)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      89(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            13014
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.51
_reflns_number_total             13014
_reflns_number_gt                9368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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)+(0.1005P)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         13014
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1565
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.351657(17) 0.72193(4) 0.42490(3) 0.02383(14) Uani 1 1 d . . .
Sb1 Sb 0.278721(16) 0.26165(4) 0.31255(3) 0.02869(14) Uani 1 1 d . . .
F1 F 0.23897(19) 0.2889(4) 0.3762(4) 0.088(2) Uani 1 1 d . . .
F2 F 0.29219(17) 0.1195(4) 0.3563(2) 0.0633(15) Uani 1 1 d . . .
F3 F 0.23670(17) 0.1870(4) 0.2514(3) 0.0680(16) Uani 1 1 d . . .
F4 F 0.31867(18) 0.2364(4) 0.2476(2) 0.0550(14) Uani 1 1 d . . .
F5 F 0.26355(15) 0.4043(3) 0.2660(3) 0.0583(13) Uani 1 1 d . . .
F6 F 0.31978(16) 0.3425(5) 0.3702(2) 0.0716(16) Uani 1 1 d . . .
Sb2 Sb 0.542471(17) 0.22318(4) 0.39640(3) 0.03499(15) Uani 1 1 d . . .
F11 F 0.5448(2) 0.3537(5) 0.4552(3) 0.092(2) Uani 1 1 d . . .
F12 F 0.5213(2) 0.3144(4) 0.3211(3) 0.085(2) Uani 1 1 d . . .
F13 F 0.4865(2) 0.1969(7) 0.4155(3) 0.121(3) Uani 1 1 d . . .
F14 F 0.5401(2) 0.0940(4) 0.3369(3) 0.099(2) Uani 1 1 d . . .
F15 F 0.5645(3) 0.1393(6) 0.4733(3) 0.144(4) Uani 1 1 d . . .
F16 F 0.5970(2) 0.2459(8) 0.3758(4) 0.184(5) Uani 1 1 d . . .
C1 C 0.4706(2) 0.1937(7) 0.6594(4) 0.044(2) Uani 1 1 d . . .
H1 H 0.4751 0.1205 0.6830 0.053 Uiso 1 1 calc R . .
C2 C 0.4500(3) 0.2936(6) 0.6855(4) 0.0409(19) Uani 1 1 d . . .
H2 H 0.4379 0.2982 0.7291 0.049 Uiso 1 1 calc R . .
C3 C 0.4505(2) 0.3853(6) 0.6352(4) 0.0417(19) Uani 1 1 d . . .
H3 H 0.4393 0.4623 0.6399 0.050 Uiso 1 1 calc R . .
C4 C 0.4704(2) 0.3435(6) 0.5770(4) 0.0417(19) Uani 1 1 d . . .
H4 H 0.4746 0.3865 0.5355 0.050 Uiso 1 1 calc R . .
C5 C 0.4833(3) 0.2221(7) 0.5922(5) 0.050(2) Uani 1 1 d . . .
H5 H 0.4976 0.1713 0.5625 0.060 Uiso 1 1 calc R . .
Fe1 Fe 0.41911(3) 0.24172(8) 0.59135(5) 0.0278(2) Uani 1 1 d . . .
C6 C 0.3573(2) 0.2017(6) 0.6049(4) 0.0390(19) Uani 1 1 d . . .
H6 H 0.3439 0.2122 0.6469 0.047 Uiso 1 1 calc R . .
C7 C 0.3792(2) 0.0987(6) 0.5864(4) 0.0401(19) Uani 1 1 d . . .
H7 H 0.3829 0.0285 0.6134 0.048 Uiso 1 1 calc R . .
C8 C 0.3945(3) 0.1202(6) 0.5197(4) 0.0396(19) Uani 1 1 d . . .
H8 H 0.4102 0.0658 0.4945 0.047 Uiso 1 1 calc R . .
C9 C 0.3826(3) 0.2349(6) 0.4967(4) 0.0384(19) Uani 1 1 d . . .
H9 H 0.3890 0.2715 0.4543 0.046 Uiso 1 1 calc R . .
C10 C 0.3587(2) 0.2862(5) 0.5509(4) 0.0315(17) Uani 1 1 d . . .
C11 C 0.3513(2) 0.4866(5) 0.4981(3) 0.0277(15) Uani 1 1 d . . .
H11 H 0.3672 0.4589 0.4615 0.033 Uiso 1 1 calc R . .
C12 C 0.3424(2) 0.4077(6) 0.5510(3) 0.0290(16) Uani 1 1 d . . .
C13 C 0.3177(2) 0.4515(6) 0.6031(3) 0.0330(17) Uani 1 1 d . . .
H13 H 0.3099 0.4007 0.6393 0.040 Uiso 1 1 calc R . .
C14 C 0.3044(2) 0.5688(6) 0.6020(3) 0.0306(16) Uani 1 1 d . . .
H14 H 0.2882 0.5977 0.6377 0.037 Uiso 1 1 calc R . .
C15 C 0.3151(2) 0.6439(5) 0.5483(3) 0.0246(15) Uani 1 1 d . . .
C16 C 0.3033(2) 0.7673(5) 0.5411(3) 0.0238(15) Uani 1 1 d . . .
C17 C 0.2791(2) 0.8260(6) 0.5876(3) 0.0311(16) Uani 1 1 d . . .
H17 H 0.2695 0.7858 0.6267 0.037 Uiso 1 1 calc R . .
C18 C 0.2693(2) 0.9417(6) 0.5762(4) 0.0331(17) Uani 1 1 d . . .
H18 H 0.2525 0.9822 0.6073 0.040 Uiso 1 1 calc R . .
C19 C 0.2837(2) 1.0001(6) 0.5202(4) 0.0344(17) Uani 1 1 d . . .
H19 H 0.2770 1.0807 0.5118 0.041 Uiso 1 1 calc R . .
C20 C 0.3084(2) 0.9379(6) 0.4761(4) 0.0317(16) Uani 1 1 d . . .
H20 H 0.3188 0.9776 0.4374 0.038 Uiso 1 1 calc R . .
N1 N 0.33833(18) 0.6010(4) 0.4964(3) 0.0276(13) Uani 1 1 d . . .
N2 N 0.31802(17) 0.8245(4) 0.4863(3) 0.0256(12) Uani 1 1 d . . .
N21 N 0.38287(18) 0.6079(4) 0.3658(3) 0.0273(13) Uani 1 1 d . . .
C21 C 0.3631(2) 0.5578(6) 0.3072(3) 0.0323(17) Uani 1 1 d . . .
H21 H 0.3347 0.5819 0.2907 0.039 Uiso 1 1 calc R . .
C22 C 0.3825(2) 0.4745(6) 0.2712(4) 0.0366(18) Uani 1 1 d . . .
H22 H 0.3677 0.4407 0.2301 0.044 Uiso 1 1 calc R . .
C23 C 0.4233(2) 0.4385(6) 0.2938(4) 0.0355(18) Uani 1 1 d . . .
H23 H 0.4368 0.3778 0.2698 0.043 Uiso 1 1 calc R . .
C24 C 0.4441(2) 0.4914(6) 0.3509(4) 0.0388(18) Uani 1 1 d . . .
H24 H 0.4729 0.4700 0.3667 0.047 Uiso 1 1 calc R . .
C25 C 0.4230(2) 0.5780(6) 0.3869(4) 0.0335(17) Uani 1 1 d . . .
H25 H 0.4377 0.6155 0.4268 0.040 Uiso 1 1 calc R . .
N31 N 0.36634(18) 0.8524(4) 0.3580(3) 0.0289(13) Uani 1 1 d . . .
C31 C 0.3385(2) 0.8855(6) 0.3043(3) 0.0330(17) Uani 1 1 d . . .
H31 H 0.3112 0.8478 0.2967 0.040 Uiso 1 1 calc R . .
C32 C 0.3487(3) 0.9738(6) 0.2597(4) 0.0413(19) Uani 1 1 d . . .
H32 H 0.3283 0.9973 0.2220 0.050 Uiso 1 1 calc R . .
C33 C 0.3878(3) 1.0280(6) 0.2688(4) 0.043(2) Uani 1 1 d . . .
H33 H 0.3948 1.0894 0.2382 0.052 Uiso 1 1 calc R . .
C34 C 0.4164(3) 0.9921(6) 0.3224(4) 0.044(2) Uani 1 1 d . . .
H34 H 0.4440 1.0278 0.3300 0.053 Uiso 1 1 calc R . .
C35 C 0.4051(2) 0.9033(6) 0.3662(4) 0.0384(18) Uani 1 1 d . . .
H35 H 0.4255 0.8775 0.4033 0.046 Uiso 1 1 calc R . .


_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 2.010(5) . ?
Pd1 N2 2.021(5) . ?
Pd1 N21 2.031(5) . ?
Pd1 N31 2.040(5) . ?
Sb1 F6 1.846(5) . ?
Sb1 F2 1.848(4) . ?
Sb1 F1 1.849(5) . ?
Sb1 F3 1.868(5) . ?
Sb1 F4 1.868(4) . ?
Sb1 F5 1.887(4) . ?
Sb2 F16 1.804(7) . ?
Sb2 F15 1.824(5) . ?
Sb2 F12 1.839(5) . ?
Sb2 F13 1.844(6) . ?
Sb2 F14 1.853(5) . ?
Sb2 F11 1.858(5) . ?
C1 C5 1.419(11) . ?
C1 C2 1.420(10) . ?
C1 Fe1 2.035(7) . ?
C2 C3 1.419(10) . ?
C2 Fe1 2.038(7) . ?
C3 C4 1.409(10) . ?
C3 Fe1 2.039(7) . ?
C4 C5 1.459(10) . ?
C4 Fe1 2.016(7) . ?
C5 Fe1 2.014(8) . ?
Fe1 C6 2.023(7) . ?
Fe1 C10 2.026(7) . ?
Fe1 C9 2.035(7) . ?
Fe1 C8 2.039(7) . ?
Fe1 C7 2.045(7) . ?
C6 C10 1.413(10) . ?
C6 C7 1.418(10) . ?
C7 C8 1.426(10) . ?
C8 C9 1.412(9) . ?
C9 C10 1.457(11) . ?
C10 C12 1.472(9) . ?
C11 N1 1.362(7) . ?
C11 C12 1.399(9) . ?
C12 C13 1.412(9) . ?
C13 C14 1.395(9) . ?
C14 C15 1.400(9) . ?
C15 N1 1.375(8) . ?
C15 C16 1.453(8) . ?
C16 N2 1.352(8) . ?
C16 C17 1.393(9) . ?
C17 C18 1.363(9) . ?
C18 C19 1.372(9) . ?
C19 C20 1.391(9) . ?
C20 N2 1.333(8) . ?
N21 C25 1.319(8) . ?
N21 C21 1.348(8) . ?
C21 C22 1.348(9) . ?
C22 C23 1.365(9) . ?
C23 C24 1.351(9) . ?
C24 C25 1.402(9) . ?
N31 C31 1.328(8) . ?
N31 C35 1.335(9) . ?
C31 C32 1.375(9) . ?
C32 C33 1.362(10) . ?
C33 C34 1.350(10) . ?
C34 C35 1.378(9) . ?

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 N2 81.1(2) . . ?
N1 Pd1 N21 94.9(2) . . ?
N2 Pd1 N21 175.5(2) . . ?
N1 Pd1 N31 176.0(2) . . ?
N2 Pd1 N31 96.1(2) . . ?
N21 Pd1 N31 88.0(2) . . ?
F6 Sb1 F2 93.1(2) . . ?
F6 Sb1 F1 89.8(3) . . ?
F2 Sb1 F1 89.2(2) . . ?
F6 Sb1 F3 177.0(2) . . ?
F2 Sb1 F3 89.8(2) . . ?
F1 Sb1 F3 90.7(3) . . ?
F6 Sb1 F4 90.2(2) . . ?
F2 Sb1 F4 91.69(19) . . ?
F1 Sb1 F4 179.1(2) . . ?
F3 Sb1 F4 89.4(2) . . ?
F6 Sb1 F5 88.8(2) . . ?
F2 Sb1 F5 178.1(2) . . ?
F1 Sb1 F5 90.7(2) . . ?
F3 Sb1 F5 88.3(2) . . ?
F4 Sb1 F5 88.4(2) . . ?
F16 Sb2 F15 87.9(4) . . ?
F16 Sb2 F12 91.2(4) . . ?
F15 Sb2 F12 177.2(3) . . ?
F16 Sb2 F13 178.4(3) . . ?
F15 Sb2 F13 92.5(4) . . ?
F12 Sb2 F13 88.5(3) . . ?
F16 Sb2 F14 87.6(3) . . ?
F15 Sb2 F14 93.8(3) . . ?
F12 Sb2 F14 88.8(2) . . ?
F13 Sb2 F14 90.8(3) . . ?
F16 Sb2 F11 92.1(3) . . ?
F15 Sb2 F11 86.7(3) . . ?
F12 Sb2 F11 90.6(2) . . ?
F13 Sb2 F11 89.4(3) . . ?
F14 Sb2 F11 179.4(2) . . ?
C5 C1 C2 108.3(7) . . ?
C5 C1 Fe1 68.7(5) . . ?
C2 C1 Fe1 69.7(4) . . ?
C3 C2 C1 108.3(7) . . ?
C3 C2 Fe1 69.7(4) . . ?
C1 C2 Fe1 69.5(4) . . ?
C4 C3 C2 108.8(6) . . ?
C4 C3 Fe1 68.8(4) . . ?
C2 C3 Fe1 69.6(4) . . ?
C3 C4 C5 107.3(7) . . ?
C3 C4 Fe1 70.5(4) . . ?
C5 C4 Fe1 68.7(4) . . ?
C1 C5 C4 107.3(7) . . ?
C1 C5 Fe1 70.3(5) . . ?
C4 C5 Fe1 68.8(4) . . ?
C5 Fe1 C4 42.5(3) . . ?
C5 Fe1 C6 159.1(3) . . ?
C4 Fe1 C6 157.9(3) . . ?
C5 Fe1 C10 156.4(3) . . ?
C4 Fe1 C10 121.7(3) . . ?
C6 Fe1 C10 40.9(3) . . ?
C5 Fe1 C1 41.0(3) . . ?
C4 Fe1 C1 69.8(3) . . ?
C6 Fe1 C1 123.9(3) . . ?
C10 Fe1 C1 162.4(3) . . ?
C5 Fe1 C9 117.9(4) . . ?
C4 Fe1 C9 106.3(3) . . ?
C6 Fe1 C9 69.6(3) . . ?
C10 Fe1 C9 42.1(3) . . ?
C1 Fe1 C9 152.9(3) . . ?
C5 Fe1 C2 69.2(3) . . ?
C4 Fe1 C2 69.1(3) . . ?
C6 Fe1 C2 108.8(3) . . ?
C10 Fe1 C2 126.9(3) . . ?
C1 Fe1 C2 40.8(3) . . ?
C9 Fe1 C2 164.7(3) . . ?
C5 Fe1 C8 103.7(3) . . ?
C4 Fe1 C8 123.2(3) . . ?
C6 Fe1 C8 68.6(3) . . ?
C10 Fe1 C8 69.0(3) . . ?
C1 Fe1 C8 117.8(3) . . ?
C9 Fe1 C8 40.6(3) . . ?
C2 Fe1 C8 154.2(3) . . ?
C5 Fe1 C3 69.5(3) . . ?
C4 Fe1 C3 40.7(3) . . ?
C6 Fe1 C3 123.5(3) . . ?
C10 Fe1 C3 110.2(3) . . ?
C1 Fe1 C3 68.8(3) . . ?
C9 Fe1 C3 126.6(3) . . ?
C2 Fe1 C3 40.7(3) . . ?
C8 Fe1 C3 161.9(3) . . ?
C5 Fe1 C7 120.9(3) . . ?
C4 Fe1 C7 159.8(3) . . ?
C6 Fe1 C7 40.8(3) . . ?
C10 Fe1 C7 69.0(3) . . ?
C1 Fe1 C7 104.7(3) . . ?
C9 Fe1 C7 69.2(3) . . ?
C2 Fe1 C7 120.1(3) . . ?
C8 Fe1 C7 40.9(3) . . ?
C3 Fe1 C7 157.0(3) . . ?
C10 C6 C7 109.1(7) . . ?
C10 C6 Fe1 69.7(4) . . ?
C7 C6 Fe1 70.4(4) . . ?
C6 C7 C8 107.1(6) . . ?
C6 C7 Fe1 68.8(4) . . ?
C8 C7 Fe1 69.3(4) . . ?
C9 C8 C7 109.5(7) . . ?
C9 C8 Fe1 69.6(4) . . ?
C7 C8 Fe1 69.8(4) . . ?
C8 C9 C10 106.6(7) . . ?
C8 C9 Fe1 69.8(4) . . ?
C10 C9 Fe1 68.6(4) . . ?
C6 C10 C9 107.6(6) . . ?
C6 C10 C12 126.9(7) . . ?
C9 C10 C12 125.3(6) . . ?
C6 C10 Fe1 69.5(4) . . ?
C9 C10 Fe1 69.3(4) . . ?
C12 C10 Fe1 122.8(5) . . ?
N1 C11 C12 123.2(6) . . ?
C11 C12 C13 116.5(6) . . ?
C11 C12 C10 120.4(6) . . ?
C13 C12 C10 123.1(6) . . ?
C14 C13 C12 120.5(6) . . ?
C13 C14 C15 120.1(6) . . ?
N1 C15 C14 119.6(6) . . ?
N1 C15 C16 114.9(6) . . ?
C14 C15 C16 125.5(6) . . ?
N2 C16 C17 120.8(6) . . ?
N2 C16 C15 115.8(6) . . ?
C17 C16 C15 123.5(6) . . ?
C18 C17 C16 119.3(6) . . ?
C17 C18 C19 120.3(6) . . ?
C18 C19 C20 118.2(6) . . ?
N2 C20 C19 122.2(7) . . ?
C11 N1 C15 120.0(6) . . ?
C11 N1 Pd1 125.9(5) . . ?
C15 N1 Pd1 114.1(4) . . ?
C20 N2 C16 119.3(6) . . ?
C20 N2 Pd1 126.5(5) . . ?
C16 N2 Pd1 114.1(4) . . ?
C25 N21 C21 118.9(6) . . ?
C25 N21 Pd1 119.3(5) . . ?
C21 N21 Pd1 121.8(5) . . ?
N21 C21 C22 121.9(7) . . ?
C21 C22 C23 120.2(7) . . ?
C24 C23 C22 118.4(7) . . ?
C23 C24 C25 119.9(7) . . ?
N21 C25 C24 120.6(7) . . ?
C31 N31 C35 118.7(6) . . ?
C31 N31 Pd1 121.2(5) . . ?
C35 N31 Pd1 120.0(5) . . ?
N31 C31 C32 120.6(7) . . ?
C33 C32 C31 120.9(7) . . ?
C34 C33 C32 118.2(7) . . ?
C33 C34 C35 119.4(7) . . ?
N31 C35 C34 122.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.51
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.188
_database_code_depnum_ccdc_archive 'CCDC 1000098'
#######################################################################
#
#                 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_al4

_audit_creation_date             2010-04-22T16:07:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C35 H38 Fe N6 Pd, 2(F6 Sb), C2 H3 N'
_chemical_formula_sum            'C37 H41 F12 Fe N7 Pd Sb2'
_chemical_formula_weight         1217.52

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.353(7)
_cell_length_b                   14.768(9)
_cell_length_c                   15.121(10)
_cell_angle_alpha                73.09(3)
_cell_angle_beta                 73.84(3)
_cell_angle_gamma                74.59(3)
_cell_volume                     2081(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6241
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      19.19

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       PLATE
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_crystal_density_meas      ?
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_T_max  0.7446
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_type   multi-scan

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_number            17648
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         21.92
_diffrn_reflns_theta_full        21.92
_diffrn_measured_fraction_theta_full 0.94
_diffrn_measured_fraction_theta_max 0.94
_reflns_number_total             4754
_reflns_number_gt                3602
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)'
_computing_publication_material  
'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0514P)²+10.2911P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4754
_refine_ls_number_parameters     547
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1282
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.129

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

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
C1 C 0.8810(12) 0.5191(7) 0.8811(8) 0.049(3) Uani 1 1 d . . .
H1A H 0.7833 0.5312 0.9043 0.074 Uiso 1 1 calc R . .
H1B H 0.9017 0.5405 0.8133 0.074 Uiso 1 1 calc R . .
H1C H 0.9214 0.5537 0.9076 0.074 Uiso 1 1 calc R . .
C2 C 0.9377(10) 0.4139(8) 0.9089(8) 0.034(3) Uani 1 1 d . . .
C3 C 1.0173(10) 0.3632(7) 0.8424(7) 0.032(3) Uani 1 1 d . . .
H3 H 1.0355 0.3964 0.7792 0.039 Uiso 1 1 calc R . .
C4 C 0.9133(11) 0.3633(8) 1.0003(8) 0.040(3) Uani 1 1 d . . .
H4 H 0.8609 0.3951 1.0473 0.048 Uiso 1 1 calc R . .
C5 C 0.9638(11) 0.2668(8) 1.0245(7) 0.038(3) Uani 1 1 d . . .
H5 H 0.9454 0.2329 1.0874 0.045 Uiso 1 1 calc R . .
C6 C 1.0424(9) 0.2198(7) 0.9552(7) 0.026(2) Uani 1 1 d . . .
C7 C 1.1010(9) 0.1180(7) 0.9731(7) 0.027(2) Uani 1 1 d . . .
C8 C 1.0876(10) 0.0539(8) 1.0610(7) 0.034(3) Uani 1 1 d . . .
H8 H 1.0365 0.0757 1.1147 0.041 Uiso 1 1 calc R . .
C9 C 1.1493(11) -0.0412(8) 1.0688(8) 0.037(3) Uani 1 1 d . . .
H9 H 1.1409 -0.084 1.128 0.044 Uiso 1 1 calc R . .
C10 C 1.2244(10) -0.0744(7) 0.9888(8) 0.031(3) Uani 1 1 d . . .
C11 C 1.2316(9) -0.0096(7) 0.9046(7) 0.025(2) Uani 1 1 d . . .
H11 H 1.2791 -0.0312 0.8502 0.03 Uiso 1 1 calc R . .
C12 C 1.2924(11) -0.1754(8) 0.9951(8) 0.038(3) Uani 1 1 d . . .
C13 C 1.2935(11) -0.2503(8) 1.0790(8) 0.042(3) Uani 1 1 d . . .
H13 H 1.2478 -0.2443 1.14 0.051 Uiso 1 1 calc R . .
C14 C 1.3745(12) -0.3334(8) 1.0537(9) 0.043(3) Uani 1 1 d . . .
H14 H 1.3912 -0.3936 1.0949 0.052 Uiso 1 1 calc R . .
C15 C 1.4274(12) -0.3125(8) 0.9561(10) 0.050(3) Uani 1 1 d . . .
H15 H 1.4864 -0.356 0.9217 0.06 Uiso 1 1 calc R . .
C16 C 1.3773(11) -0.2162(8) 0.9192(8) 0.040(3) Uani 1 1 d . . .
H16 H 1.396 -0.1838 0.8558 0.048 Uiso 1 1 calc R . .
C17 C 1.6234(12) -0.1410(8) 0.9636(10) 0.049(3) Uani 1 1 d . . .
H17 H 1.6279 -0.0919 0.9085 0.058 Uiso 1 1 calc R . .
C18 C 1.5477(12) -0.1307(8) 1.0543(9) 0.047(3) Uani 1 1 d . . .
H18 H 1.492 -0.0742 1.0696 0.057 Uiso 1 1 calc R . .
C19 C 1.5712(13) -0.2206(9) 1.1173(9) 0.052(3) Uani 1 1 d . . .
H19 H 1.5356 -0.2347 1.1823 0.062 Uiso 1 1 calc R . .
C20 C 1.6588(13) -0.2859(9) 1.0641(11) 0.057(4) Uani 1 1 d . . .
H20 H 1.6906 -0.3513 1.0879 0.068 Uiso 1 1 calc R . .
C21 C 1.6898(12) -0.2363(9) 0.9701(11) 0.054(3) Uani 1 1 d . . .
H21 H 1.7457 -0.2626 0.9201 0.065 Uiso 1 1 calc R . .
C22 C 1.4404(11) 0.0577(7) 0.7093(7) 0.035(3) Uani 1 1 d . . .
H22 H 1.4788 0.0856 0.741 0.042 Uiso 1 1 calc R . .
C23 C 1.5177(11) -0.0205(7) 0.6782(7) 0.032(3) Uani 1 1 d . . .
H23 H 1.6045 -0.0457 0.6914 0.038 Uiso 1 1 calc R . .
C24 C 1.4709(11) -0.0645(7) 0.6272(7) 0.031(3) Uani 1 1 d . . .
C25 C 1.3372(11) -0.0195(7) 0.6111(7) 0.035(3) Uani 1 1 d . . .
H25 H 1.2996 -0.043 0.5753 0.043 Uiso 1 1 calc R . .
C26 C 1.2640(11) 0.0574(7) 0.6474(7) 0.031(3) Uani 1 1 d . . .
H26 H 1.1758 0.0834 0.637 0.037 Uiso 1 1 calc R . .
C27 C 1.6720(12) -0.1905(8) 0.6231(9) 0.052(3) Uani 1 1 d . . .
H27A H 1.7384 -0.1507 0.5902 0.079 Uiso 1 1 calc R . .
H27B H 1.7023 -0.2515 0.6056 0.079 Uiso 1 1 calc R . .
H27C H 1.662 -0.201 0.6902 0.079 Uiso 1 1 calc R . .
C28 C 1.4891(12) -0.1874(7) 0.5449(8) 0.047(3) Uani 1 1 d . . .
H28A H 1.4231 -0.224 0.5873 0.07 Uiso 1 1 calc R . .
H28B H 1.5638 -0.2296 0.5135 0.07 Uiso 1 1 calc R . .
H28C H 1.4462 -0.1381 0.4986 0.07 Uiso 1 1 calc R . .
C29 C 1.2703(11) 0.3644(8) 0.6516(7) 0.035(3) Uani 1 1 d . . .
H29 H 1.3139 0.3586 0.6997 0.042 Uiso 1 1 calc R . .
C30 C 1.2806(11) 0.4411(8) 0.5770(7) 0.039(3) Uani 1 1 d . . .
H30 H 1.3283 0.4868 0.5758 0.047 Uiso 1 1 calc R . .
C31 C 1.2201(11) 0.4524(7) 0.5014(7) 0.036(3) Uani 1 1 d . . .
C32 C 1.1507(10) 0.3799(7) 0.5107(7) 0.032(3) Uani 1 1 d . . .
H32 H 1.1091 0.3823 0.4627 0.039 Uiso 1 1 calc R . .
C33 C 1.1435(10) 0.3077(8) 0.5870(7) 0.032(3) Uani 1 1 d . . .
H33 H 1.0953 0.2615 0.5903 0.039 Uiso 1 1 calc R . .
C34 C 1.2918(14) 0.6045(8) 0.4254(8) 0.062(4) Uani 1 1 d . . .
H34A H 1.2436 0.6335 0.4777 0.093 Uiso 1 1 calc R . .
H34B H 1.2879 0.6523 0.3671 0.093 Uiso 1 1 calc R . .
H34C H 1.3859 0.579 0.4299 0.093 Uiso 1 1 calc R . .
C35 C 1.1768(12) 0.5332(9) 0.3479(8) 0.060(4) Uani 1 1 d . . .
H35A H 1.228 0.481 0.3186 0.09 Uiso 1 1 calc R . .
H35B H 1.1855 0.5937 0.3032 0.09 Uiso 1 1 calc R . .
H35C H 1.0818 0.5285 0.3683 0.09 Uiso 1 1 calc R . .
C100 C -0.0248(18) 0.2802(14) 0.3559(11) 0.088(5) Uani 1 1 d . . .
C101 C -0.0840(18) 0.1992(11) 0.3593(11) 0.092(5) Uani 1 1 d . . .
H10A H -0.0524 0.1439 0.4059 0.138 Uiso 1 1 calc R . .
H10B H -0.0561 0.1839 0.2984 0.138 Uiso 1 1 calc R . .
H10C H -0.1823 0.2167 0.3759 0.138 Uiso 1 1 calc R . .
N1 N 1.0690(8) 0.2691(5) 0.8644(6) 0.0259(19) Uani 1 1 d . . .
N2 N 1.1731(8) 0.0854(6) 0.8953(6) 0.029(2) Uani 1 1 d . . .
N3 N 1.3119(8) 0.0984(6) 0.6978(5) 0.030(2) Uani 1 1 d . . .
N4 N 1.2017(8) 0.2964(6) 0.6607(5) 0.031(2) Uani 1 1 d . . .
N5 N 1.5410(9) -0.1428(6) 0.5980(6) 0.036(2) Uani 1 1 d . . .
N6 N 1.2290(10) 0.5277(7) 0.4279(6) 0.046(2) Uani 1 1 d . . .
N100 N 0.0129(19) 0.3479(14) 0.3529(11) 0.130(7) Uani 1 1 d . . .
F1 F 1.1628(7) -0.0013(5) 1.4032(5) 0.070(2) Uani 1 1 d . . .
F2 F 1.2855(8) -0.1787(5) 1.4000(5) 0.072(2) Uani 1 1 d . . .
F3 F 1.0207(7) -0.0040(5) 1.2854(5) 0.066(2) Uani 1 1 d . . .
F4 F 1.2862(6) -0.0509(4) 1.2408(4) 0.0533(17) Uani 1 1 d . . .
F5 F 1.0158(8) -0.1366(6) 1.4457(5) 0.077(2) Uani 1 1 d . . .
F6 F 1.1384(8) -0.1841(5) 1.2875(5) 0.064(2) Uani 1 1 d . . .
F7 F 0.3771(9) 0.6105(5) 0.6326(4) 0.075(2) Uani 1 1 d . . .
F8 F 0.2853(8) 0.6883(4) 0.7785(5) 0.066(2) Uani 1 1 d . . .
F9 F 0.2152(7) 0.5270(5) 0.7847(5) 0.067(2) Uani 1 1 d . . .
F10 F 0.4708(7) 0.4459(4) 0.7414(5) 0.063(2) Uani 1 1 d . . .
F11 F 0.5412(7) 0.6061(6) 0.7387(6) 0.084(2) Uani 1 1 d . . .
F12 F 0.3775(7) 0.5223(4) 0.8868(4) 0.0520(18) Uani 1 1 d . . .
Pd3 Pd 1.18923(8) 0.18835(5) 0.77505(5) 0.0283(2) Uani 1 1 d . . .
Sb1 Sb 1.15246(8) -0.09299(6) 1.34572(6) 0.0456(3) Uani 1 1 d . . .
Sb2 Sb 0.37953(8) 0.56719(5) 0.75911(5) 0.0391(3) Uani 1 1 d . . .
Fe1 Fe 1.48480(16) -0.22854(10) 1.01644(12) 0.0388(4) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 C2 1.486(14) . ?
C1 H1A 0.96 . ?
C1 H1B 0.96 . ?
C1 H1C 0.96 . ?
C2 C4 1.356(14) . ?
C2 C3 1.379(13) . ?
C3 N1 1.328(12) . ?
C3 H3 0.93 . ?
C4 C5 1.357(14) . ?
C4 H4 0.93 . ?
C5 C6 1.374(13) . ?
C5 H5 0.93 . ?
C6 N1 1.344(12) . ?
C6 C7 1.440(13) . ?
C7 N2 1.350(12) . ?
C7 C8 1.384(13) . ?
C8 C9 1.365(14) . ?
C8 H8 0.93 . ?
C9 C10 1.388(14) . ?
C9 H9 0.93 . ?
C10 C11 1.349(13) . ?
C10 C12 1.459(14) . ?
C11 N2 1.355(12) . ?
C11 H11 0.93 . ?
C12 C16 1.418(15) . ?
C12 C13 1.420(15) . ?
C12 Fe1 2.017(10) . ?
C13 C14 1.381(15) . ?
C13 Fe1 2.010(11) . ?
C13 H13 0.93 . ?
C14 C15 1.396(16) . ?
C14 Fe1 2.024(10) . ?
C14 H14 0.93 . ?
C15 C16 1.383(15) . ?
C15 Fe1 2.019(10) . ?
C15 H15 0.93 . ?
C16 Fe1 2.020(10) . ?
C16 H16 0.93 . ?
C17 C21 1.380(15) . ?
C17 C18 1.407(16) . ?
C17 Fe1 2.029(11) . ?
C17 H17 0.93 . ?
C18 C19 1.396(15) . ?
C18 Fe1 2.007(10) . ?
C18 H18 0.93 . ?
C19 C20 1.407(17) . ?
C19 Fe1 2.014(11) . ?
C19 H19 0.93 . ?
C20 C21 1.387(17) . ?
C20 Fe1 2.009(11) . ?
C20 H20 0.93 . ?
C21 Fe1 2.025(12) . ?
C21 H21 0.93 . ?
C22 N3 1.343(12) . ?
C22 C23 1.345(13) . ?
C22 H22 0.93 . ?
C23 C24 1.385(13) . ?
C23 H23 0.93 . ?
C24 N5 1.316(12) . ?
C24 C25 1.421(14) . ?
C25 C26 1.355(14) . ?
C25 H25 0.93 . ?
C26 N3 1.354(12) . ?
C26 H26 0.93 . ?
C27 N5 1.451(13) . ?
C27 H27A 0.96 . ?
C27 H27B 0.96 . ?
C27 H27C 0.96 . ?
C28 N5 1.450(13) . ?
C28 H28A 0.96 . ?
C28 H28B 0.96 . ?
C28 H28C 0.96 . ?
C29 N4 1.333(12) . ?
C29 C30 1.348(14) . ?
C29 H29 0.93 . ?
C30 C31 1.400(14) . ?
C30 H30 0.93 . ?
C31 N6 1.326(13) . ?
C31 C32 1.395(14) . ?
C32 C33 1.323(13) . ?
C32 H32 0.93 . ?
C33 N4 1.358(12) . ?
C33 H33 0.93 . ?
C34 N6 1.437(14) . ?
C34 H34A 0.96 . ?
C34 H34B 0.96 . ?
C34 H34C 0.96 . ?
C35 N6 1.430(14) . ?
C35 H35A 0.96 . ?
C35 H35B 0.96 . ?
C35 H35C 0.96 . ?
C100 N100 1.15(2) . ?
C100 C101 1.46(2) . ?
C101 H10A 0.96 . ?
C101 H10B 0.96 . ?
C101 H10C 0.96 . ?
N1 Pd3 2.002(8) . ?
N2 Pd3 2.000(8) . ?
N3 Pd3 1.980(8) . ?
N4 Pd3 1.984(8) . ?
F1 Sb1 1.848(6) . ?
F2 Sb1 1.808(7) . ?
F3 Sb1 1.860(6) . ?
F4 Sb1 1.866(6) . ?
F5 Sb1 1.852(7) . ?
F6 Sb1 1.863(6) . ?
F7 Sb2 1.837(6) . ?
F8 Sb2 1.859(6) . ?
F9 Sb2 1.853(6) . ?
F10 Sb2 1.848(6) . ?
F11 Sb2 1.829(7) . ?
F12 Sb2 1.846(6) . ?

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 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 C3 116.9(10) . . ?
C4 C2 C1 121.9(10) . . ?
C3 C2 C1 121.2(10) . . ?
N1 C3 C2 123.0(10) . . ?
N1 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C2 C4 C5 121.2(10) . . ?
C2 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 119.5(10) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
N1 C6 C5 120.2(9) . . ?
N1 C6 C7 115.9(8) . . ?
C5 C6 C7 124.0(9) . . ?
N2 C7 C8 119.6(9) . . ?
N2 C7 C6 114.8(9) . . ?
C8 C7 C6 125.6(9) . . ?
C9 C8 C7 120.0(10) . . ?
C9 C8 H8 120 . . ?
C7 C8 H8 120 . . ?
C8 C9 C10 120.4(10) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 117.3(9) . . ?
C11 C10 C12 121.1(10) . . ?
C9 C10 C12 121.6(10) . . ?
C10 C11 N2 123.3(9) . . ?
C10 C11 H11 118.3 . . ?
N2 C11 H11 118.3 . . ?
C16 C12 C13 107.0(10) . . ?
C16 C12 C10 126.3(10) . . ?
C13 C12 C10 126.5(11) . . ?
C16 C12 Fe1 69.6(6) . . ?
C13 C12 Fe1 69.1(6) . . ?
C10 C12 Fe1 123.4(7) . . ?
C14 C13 C12 107.7(10) . . ?
C14 C13 Fe1 70.5(7) . . ?
C12 C13 Fe1 69.6(6) . . ?
C14 C13 H13 126.2 . . ?
C12 C13 H13 126.2 . . ?
Fe1 C13 H13 125.3 . . ?
C13 C14 C15 108.9(10) . . ?
C13 C14 Fe1 69.5(6) . . ?
C15 C14 Fe1 69.6(6) . . ?
C13 C14 H14 125.5 . . ?
C15 C14 H14 125.5 . . ?
Fe1 C14 H14 127 . . ?
C16 C15 C14 108.4(11) . . ?
C16 C15 Fe1 70.0(6) . . ?
C14 C15 Fe1 70.0(6) . . ?
C16 C15 H15 125.8 . . ?
C14 C15 H15 125.8 . . ?
Fe1 C15 H15 125.8 . . ?
C15 C16 C12 108.0(11) . . ?
C15 C16 Fe1 69.9(6) . . ?
C12 C16 Fe1 69.3(6) . . ?
C15 C16 H16 126 . . ?
C12 C16 H16 126 . . ?
Fe1 C16 H16 126.3 . . ?
C21 C17 C18 108.4(11) . . ?
C21 C17 Fe1 69.9(6) . . ?
C18 C17 Fe1 68.8(6) . . ?
C21 C17 H17 125.8 . . ?
C18 C17 H17 125.8 . . ?
Fe1 C17 H17 127.1 . . ?
C19 C18 C17 107.7(11) . . ?
C19 C18 Fe1 70.0(6) . . ?
C17 C18 Fe1 70.4(6) . . ?
C19 C18 H18 126.1 . . ?
C17 C18 H18 126.1 . . ?
Fe1 C18 H18 125.1 . . ?
C18 C19 C20 107.2(12) . . ?
C18 C19 Fe1 69.4(6) . . ?
C20 C19 Fe1 69.3(7) . . ?
C18 C19 H19 126.4 . . ?
C20 C19 H19 126.4 . . ?
Fe1 C19 H19 126.4 . . ?
C21 C20 C19 108.5(11) . . ?
C21 C20 Fe1 70.5(7) . . ?
C19 C20 Fe1 69.7(7) . . ?
C21 C20 H20 125.8 . . ?
C19 C20 H20 125.8 . . ?
Fe1 C20 H20 125.6 . . ?
C17 C21 C20 108.2(12) . . ?
C17 C21 Fe1 70.3(7) . . ?
C20 C21 Fe1 69.3(7) . . ?
C17 C21 H21 125.9 . . ?
C20 C21 H21 125.9 . . ?
Fe1 C21 H21 126.1 . . ?
N3 C22 C23 124.8(9) . . ?
N3 C22 H22 117.6 . . ?
C23 C22 H22 117.6 . . ?
C22 C23 C24 121.6(10) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
N5 C24 C23 123.7(10) . . ?
N5 C24 C25 122.2(9) . . ?
C23 C24 C25 114.1(9) . . ?
C26 C25 C24 120.8(9) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
N3 C26 C25 123.8(10) . . ?
N3 C26 H26 118.1 . . ?
C25 C26 H26 118.1 . . ?
N5 C27 H27A 109.5 . . ?
N5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N5 C28 H28A 109.5 . . ?
N5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 C30 124.1(10) . . ?
N4 C29 H29 117.9 . . ?
C30 C29 H29 117.9 . . ?
C29 C30 C31 120.6(10) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
N6 C31 C32 124.0(10) . . ?
N6 C31 C30 121.1(10) . . ?
C32 C31 C30 114.9(9) . . ?
C33 C32 C31 120.8(10) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 N4 124.6(9) . . ?
C32 C33 H33 117.7 . . ?
N4 C33 H33 117.7 . . ?
N6 C34 H34A 109.5 . . ?
N6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C35 H35A 109.5 . . ?
N6 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N6 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N100 C100 C101 175(2) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C3 N1 C6 119.2(8) . . ?
C3 N1 Pd3 126.7(7) . . ?
C6 N1 Pd3 114.1(6) . . ?
C7 N2 C11 119.3(8) . . ?
C7 N2 Pd3 114.4(6) . . ?
C11 N2 Pd3 126.2(7) . . ?
C22 N3 C26 114.9(8) . . ?
C22 N3 Pd3 121.3(7) . . ?
C26 N3 Pd3 122.2(7) . . ?
C29 N4 C33 115.0(8) . . ?
C29 N4 Pd3 120.8(7) . . ?
C33 N4 Pd3 124.2(7) . . ?
C24 N5 C28 122.4(9) . . ?
C24 N5 C27 119.9(9) . . ?
C28 N5 C27 117.6(8) . . ?
C31 N6 C35 119.9(10) . . ?
C31 N6 C34 121.7(9) . . ?
C35 N6 C34 118.4(9) . . ?
N3 Pd3 N4 89.6(3) . . ?
N3 Pd3 N2 93.8(3) . . ?
N4 Pd3 N2 176.4(3) . . ?
N3 Pd3 N1 174.3(3) . . ?
N4 Pd3 N1 95.9(3) . . ?
N2 Pd3 N1 80.7(3) . . ?
F2 Sb1 F1 90.6(3) . . ?
F2 Sb1 F5 91.8(3) . . ?
F1 Sb1 F5 91.7(3) . . ?
F2 Sb1 F3 177.7(3) . . ?
F1 Sb1 F3 89.9(3) . . ?
F5 Sb1 F3 90.4(3) . . ?
F2 Sb1 F6 90.5(3) . . ?
F1 Sb1 F6 178.8(3) . . ?
F5 Sb1 F6 87.8(3) . . ?
F3 Sb1 F6 89.0(3) . . ?
F2 Sb1 F4 89.6(3) . . ?
F1 Sb1 F4 90.9(3) . . ?
F5 Sb1 F4 177.0(3) . . ?
F3 Sb1 F4 88.2(3) . . ?
F6 Sb1 F4 89.6(3) . . ?
F11 Sb2 F7 91.2(4) . . ?
F11 Sb2 F12 90.4(3) . . ?
F7 Sb2 F12 178.3(3) . . ?
F11 Sb2 F10 91.8(3) . . ?
F7 Sb2 F10 90.6(3) . . ?
F12 Sb2 F10 89.2(3) . . ?
F11 Sb2 F9 177.8(3) . . ?
F7 Sb2 F9 91.0(3) . . ?
F12 Sb2 F9 87.4(3) . . ?
F10 Sb2 F9 88.5(3) . . ?
F11 Sb2 F8 89.0(3) . . ?
F7 Sb2 F8 89.9(3) . . ?
F12 Sb2 F8 90.2(3) . . ?
F10 Sb2 F8 179.0(3) . . ?
F9 Sb2 F8 90.6(3) . . ?
C18 Fe1 C20 68.4(5) . . ?
C18 Fe1 C13 116.9(5) . . ?
C20 Fe1 C13 129.1(5) . . ?
C18 Fe1 C19 40.6(4) . . ?
C20 Fe1 C19 40.9(5) . . ?
C13 Fe1 C19 107.5(5) . . ?
C18 Fe1 C12 109.6(4) . . ?
C20 Fe1 C12 169.0(6) . . ?
C13 Fe1 C12 41.3(4) . . ?
C19 Fe1 C12 130.7(5) . . ?
C18 Fe1 C15 170.3(5) . . ?
C20 Fe1 C15 115.5(5) . . ?
C13 Fe1 C15 68.2(5) . . ?
C19 Fe1 C15 147.8(5) . . ?
C12 Fe1 C15 68.3(4) . . ?
C18 Fe1 C16 132.3(5) . . ?
C20 Fe1 C16 147.9(5) . . ?
C13 Fe1 C16 69.0(5) . . ?
C19 Fe1 C16 170.6(5) . . ?
C12 Fe1 C16 41.1(4) . . ?
C15 Fe1 C16 40.0(4) . . ?
C18 Fe1 C14 148.6(5) . . ?
C20 Fe1 C14 107.7(5) . . ?
C13 Fe1 C14 40.0(4) . . ?
C19 Fe1 C14 115.6(5) . . ?
C12 Fe1 C14 68.1(4) . . ?
C15 Fe1 C14 40.4(4) . . ?
C16 Fe1 C14 67.7(4) . . ?
C18 Fe1 C21 68.2(5) . . ?
C20 Fe1 C21 40.2(5) . . ?
C13 Fe1 C21 167.5(5) . . ?
C19 Fe1 C21 68.3(5) . . ?
C12 Fe1 C21 150.1(5) . . ?
C15 Fe1 C21 108.6(5) . . ?
C16 Fe1 C21 117.0(5) . . ?
C14 Fe1 C21 129.9(5) . . ?
C18 Fe1 C17 40.8(4) . . ?
C20 Fe1 C17 67.4(5) . . ?
C13 Fe1 C17 151.0(5) . . ?
C19 Fe1 C17 68.1(5) . . ?
C12 Fe1 C17 118.6(4) . . ?
C15 Fe1 C17 131.1(6) . . ?
C16 Fe1 C17 110.5(5) . . ?
C14 Fe1 C17 168.5(5) . . ?
C21 Fe1 C17 39.8(4) . . ?

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 1000099'
#######################################################################
#
#                 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_sos086

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H18 Cl2 Fe N2 Pd'
_chemical_formula_weight         531.55

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'
Cl Cl 0.1484 0.1585 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   16.5082(5)
_cell_length_b                   7.4003(2)
_cell_length_c                   16.7660(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5980(10)
_cell_angle_gamma                90.00
_cell_volume                     1876.95(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    89(2)
_cell_measurement_reflns_used    5937
_cell_measurement_theta_min      2.446
_cell_measurement_theta_max      26.427

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_T_max  0.6876
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      89(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13161
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         26.46
_reflns_number_total             3844
_reflns_number_gt                3418
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0418P)²+0.8569P] 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         3844
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_restrained_S_all      1.218
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.494444(16) 0.68658(3) 0.439844(15) 0.01396(10) Uani 1 1 d . . .
Fe1 Fe 0.87021(3) 0.82427(6) 0.81845(3) 0.01612(13) Uani 1 1 d . . .
Cl1 Cl 0.40850(5) 0.55258(10) 0.30997(5) 0.02046(18) Uani 1 1 d . . .
Cl2 Cl 0.61648(5) 0.66678(10) 0.40752(5) 0.02034(19) Uani 1 1 d . . .
N1 N 0.39237(18) 0.7211(3) 0.47614(17) 0.0154(5) Uani 1 1 d . . .
N2 N 0.55950(18) 0.8093(3) 0.55623(18) 0.0153(6) Uani 1 1 d . . .
C1 C 0.3084(2) 0.6714(4) 0.4305(2) 0.0171(7) Uani 1 1 d . . .
H1 H 0.2942 0.6096 0.3769 0.021 Uiso 1 1 calc R . .
C2 C 0.2418(2) 0.7062(4) 0.4580(2) 0.0187(7) Uani 1 1 d . . .
C3 C 0.1478(2) 0.6493(5) 0.4029(2) 0.0221(7) Uani 1 1 d . . .
H3A H 0.1188 0.7430 0.3595 0.033 Uiso 1 1 calc R . .
H3B H 0.1154 0.6326 0.4402 0.033 Uiso 1 1 calc R . .
H3C H 0.1484 0.5354 0.3733 0.033 Uiso 1 1 calc R . .
C4 C 0.2632(2) 0.7978(4) 0.5360(2) 0.0212(7) Uani 1 1 d . . .
H4 H 0.2184 0.8263 0.5560 0.025 Uiso 1 1 calc R . .
C5 C 0.3499(2) 0.8477(4) 0.5846(2) 0.0204(7) Uani 1 1 d . . .
H5 H 0.3653 0.9092 0.6385 0.024 Uiso 1 1 calc R . .
C6 C 0.4141(2) 0.8066(4) 0.5535(2) 0.0155(7) Uani 1 1 d . . .
C7 C 0.5083(2) 0.8536(4) 0.5992(2) 0.0161(6) Uani 1 1 d . . .
C8 C 0.6467(2) 0.8457(4) 0.5931(2) 0.0156(6) Uani 1 1 d . . .
H8 H 0.6821 0.8154 0.5623 0.019 Uiso 1 1 calc R . .
C9 C 0.6866(2) 0.9258(4) 0.6743(2) 0.0168(6) Uani 1 1 d . . .
C10 C 0.6328(2) 0.9713(4) 0.7177(2) 0.0170(6) Uani 1 1 d . . .
H10 H 0.6577 1.0273 0.7733 0.020 Uiso 1 1 calc R . .
C11 C 0.5433(2) 0.9351(4) 0.6799(2) 0.0172(7) Uani 1 1 d . . .
H11 H 0.5064 0.9659 0.7090 0.021 Uiso 1 1 calc R . .
C12 C 0.7827(2) 0.9593(4) 0.7129(2) 0.0164(6) Uani 1 1 d . . .
C13 C 0.9202(2) 1.0686(4) 0.8023(2) 0.0221(7) Uani 1 1 d . . .
H13 H 0.9657 1.1354 0.8458 0.027 Uiso 1 1 calc R . .
C14 C 0.9322(2) 0.9380(4) 0.7461(2) 0.0227(7) Uani 1 1 d . . .
H14 H 0.9872 0.9019 0.7455 0.027 Uiso 1 1 calc R . .
C15 C 0.8476(2) 0.8702(4) 0.6906(2) 0.0195(7) Uani 1 1 d . . .
H15 H 0.8362 0.7814 0.6465 0.023 Uiso 1 1 calc R . .
C16 C 0.8278(2) 1.0821(4) 0.7821(2) 0.0197(7) Uani 1 1 d . . .
H16 H 0.8010 1.1593 0.8098 0.024 Uiso 1 1 calc R . .
C17 C 0.9433(3) 0.6113(5) 0.8899(2) 0.0299(8) Uani 1 1 d . . .
H17 H 0.9979 0.5686 0.8906 0.036 Uiso 1 1 calc R . .
C18 C 0.9328(2) 0.7448(5) 0.9459(2) 0.0284(8) Uani 1 1 d . . .
H18 H 0.9790 0.8081 0.9903 0.034 Uiso 1 1 calc R . .
C19 C 0.8414(2) 0.7667(5) 0.9238(2) 0.0262(8) Uani 1 1 d . . .
H19 H 0.8155 0.8470 0.9511 0.031 Uiso 1 1 calc R . .
C20 C 0.7951(2) 0.6491(5) 0.8541(2) 0.0278(8) Uani 1 1 d . . .
H20 H 0.7327 0.6362 0.8263 0.033 Uiso 1 1 calc R . .
C21 C 0.8584(3) 0.5536(4) 0.8332(2) 0.0281(8) Uani 1 1 d . . .
H21 H 0.8457 0.4656 0.7885 0.034 Uiso 1 1 calc R . .


_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 2.024(3) . ?
Pd1 N2 2.027(3) . ?
Pd1 Cl2 2.2909(8) . ?
Pd1 Cl1 2.2943(8) . ?
Fe1 C21 2.037(3) . ?
Fe1 C16 2.039(3) . ?
Fe1 C12 2.042(3) . ?
Fe1 C20 2.042(3) . ?
Fe1 C19 2.049(3) . ?
Fe1 C13 2.050(3) . ?
Fe1 C15 2.051(3) . ?
Fe1 C18 2.052(3) . ?
Fe1 C17 2.054(3) . ?
Fe1 C14 2.055(3) . ?
N1 C1 1.339(4) . ?
N1 C6 1.356(4) . ?
N2 C8 1.346(4) . ?
N2 C7 1.352(4) . ?
C1 C2 1.377(5) . ?
C1 H1 0.9500 . ?
C2 C4 1.387(5) . ?
C2 C3 1.513(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.385(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.474(5) . ?
C7 C11 1.379(4) . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(4) . ?
C9 C12 1.476(4) . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C16 1.426(4) . ?
C12 C15 1.428(4) . ?
C13 C14 1.419(5) . ?
C13 C16 1.428(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.424(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C21 1.409(5) . ?
C17 C18 1.421(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.411(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.411(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.417(5) . ?
C20 H20 0.9500 . ?
C21 H21 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
N1 Pd1 N2 80.68(11) . . ?
N1 Pd1 Cl2 174.95(8) . . ?
N2 Pd1 Cl2 94.54(8) . . ?
N1 Pd1 Cl1 93.84(8) . . ?
N2 Pd1 Cl1 174.49(8) . . ?
Cl2 Pd1 Cl1 90.92(3) . . ?
C21 Fe1 C16 156.63(15) . . ?
C21 Fe1 C12 121.16(14) . . ?
C16 Fe1 C12 40.91(13) . . ?
C21 Fe1 C20 40.66(15) . . ?
C16 Fe1 C20 120.36(14) . . ?
C12 Fe1 C20 105.24(14) . . ?
C21 Fe1 C19 67.95(15) . . ?
C16 Fe1 C19 106.37(14) . . ?
C12 Fe1 C19 121.41(14) . . ?
C20 Fe1 C19 40.35(15) . . ?
C21 Fe1 C13 161.15(14) . . ?
C16 Fe1 C13 40.86(13) . . ?
C12 Fe1 C13 68.69(13) . . ?
C20 Fe1 C13 157.28(15) . . ?
C19 Fe1 C13 122.80(15) . . ?
C21 Fe1 C15 107.66(14) . . ?
C16 Fe1 C15 68.62(13) . . ?
C12 Fe1 C15 40.84(12) . . ?
C20 Fe1 C15 122.23(14) . . ?
C19 Fe1 C15 157.96(14) . . ?
C13 Fe1 C15 68.32(13) . . ?
C21 Fe1 C18 67.96(15) . . ?
C16 Fe1 C18 123.29(15) . . ?
C12 Fe1 C18 158.32(14) . . ?
C20 Fe1 C18 67.96(15) . . ?
C19 Fe1 C18 40.26(14) . . ?
C13 Fe1 C18 109.19(14) . . ?
C15 Fe1 C18 160.16(15) . . ?
C21 Fe1 C17 40.29(15) . . ?
C16 Fe1 C17 160.63(15) . . ?
C12 Fe1 C17 158.06(14) . . ?
C20 Fe1 C17 68.04(15) . . ?
C19 Fe1 C17 67.84(15) . . ?
C13 Fe1 C17 125.45(15) . . ?
C15 Fe1 C17 123.73(14) . . ?
C18 Fe1 C17 40.49(15) . . ?
C21 Fe1 C14 124.66(14) . . ?
C16 Fe1 C14 68.47(13) . . ?
C12 Fe1 C14 68.56(13) . . ?
C20 Fe1 C14 159.62(15) . . ?
C19 Fe1 C14 159.45(15) . . ?
C13 Fe1 C14 40.44(14) . . ?
C15 Fe1 C14 40.59(13) . . ?
C18 Fe1 C14 124.75(14) . . ?
C17 Fe1 C14 110.06(14) . . ?
C1 N1 C6 119.4(3) . . ?
C1 N1 Pd1 126.1(2) . . ?
C6 N1 Pd1 114.4(2) . . ?
C8 N2 C7 119.2(3) . . ?
C8 N2 Pd1 126.1(2) . . ?
C7 N2 Pd1 114.7(2) . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C4 118.1(3) . . ?
C1 C2 C3 120.3(3) . . ?
C4 C2 C3 121.6(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C2 119.9(3) . . ?
C5 C4 H4 120.0 . . ?
C2 C4 H4 120.0 . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
N1 C6 C5 120.8(3) . . ?
N1 C6 C7 115.2(3) . . ?
C5 C6 C7 123.9(3) . . ?
N2 C7 C11 121.5(3) . . ?
N2 C7 C6 114.9(3) . . ?
C11 C7 C6 123.6(3) . . ?
N2 C8 C9 122.5(3) . . ?
N2 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C10 117.6(3) . . ?
C8 C9 C12 120.5(3) . . ?
C10 C9 C12 121.9(3) . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C7 C11 C10 119.2(3) . . ?
C7 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C16 C12 C15 107.8(3) . . ?
C16 C12 C9 125.6(3) . . ?
C15 C12 C9 126.5(3) . . ?
C16 C12 Fe1 69.46(18) . . ?
C15 C12 Fe1 69.93(18) . . ?
C9 C12 Fe1 124.1(2) . . ?
C14 C13 C16 108.1(3) . . ?
C14 C13 Fe1 69.97(18) . . ?
C16 C13 Fe1 69.18(17) . . ?
C14 C13 H13 126.0 . . ?
C16 C13 H13 126.0 . . ?
Fe1 C13 H13 126.5 . . ?
C13 C14 C15 108.2(3) . . ?
C13 C14 Fe1 69.59(19) . . ?
C15 C14 Fe1 69.56(18) . . ?
C13 C14 H14 125.9 . . ?
C15 C14 H14 125.9 . . ?
Fe1 C14 H14 126.5 . . ?
C14 C15 C12 108.0(3) . . ?
C14 C15 Fe1 69.85(18) . . ?
C12 C15 Fe1 69.23(18) . . ?
C14 C15 H15 126.0 . . ?
C12 C15 H15 126.0 . . ?
Fe1 C15 H15 126.5 . . ?
C12 C16 C13 108.0(3) . . ?
C12 C16 Fe1 69.63(17) . . ?
C13 C16 Fe1 69.96(18) . . ?
C12 C16 H16 126.0 . . ?
C13 C16 H16 126.0 . . ?
Fe1 C16 H16 126.0 . . ?
C21 C17 C18 107.7(3) . . ?
C21 C17 Fe1 69.2(2) . . ?
C18 C17 Fe1 69.7(2) . . ?
C21 C17 H17 126.1 . . ?
C18 C17 H17 126.1 . . ?
Fe1 C17 H17 126.5 . . ?
C19 C18 C17 107.9(3) . . ?
C19 C18 Fe1 69.8(2) . . ?
C17 C18 Fe1 69.8(2) . . ?
C19 C18 H18 126.1 . . ?
C17 C18 H18 126.1 . . ?
Fe1 C18 H18 125.9 . . ?
C20 C19 C18 108.4(3) . . ?
C20 C19 Fe1 69.6(2) . . ?
C18 C19 Fe1 70.0(2) . . ?
C20 C19 H19 125.8 . . ?
C18 C19 H19 125.8 . . ?
Fe1 C19 H19 126.2 . . ?
C19 C20 C21 107.7(3) . . ?
C19 C20 Fe1 70.07(19) . . ?
C21 C20 Fe1 69.5(2) . . ?
C19 C20 H20 126.2 . . ?
C21 C20 H20 126.2 . . ?
Fe1 C20 H20 125.9 . . ?
C17 C21 C20 108.4(3) . . ?
C17 C21 Fe1 70.48(19) . . ?
C20 C21 Fe1 69.85(19) . . ?
C17 C21 H21 125.8 . . ?
C20 C21 H21 125.8 . . ?
Fe1 C21 H21 125.4 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.46
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.181
_database_code_depnum_ccdc_archive 'CCDC 1000100'
#######################################################################
#
#                 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_kjs122_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H32 F12 N4 O2 Pd Sb2'
_chemical_formula_weight         1010.46

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.745(5)
_cell_length_b                   19.021(5)
_cell_length_c                   10.628(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.519(5)
_cell_angle_gamma                90.00
_cell_volume                     1748.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9425
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      30.64

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5749
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42952
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3257
_reflns_number_gt                3031
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0397P)²+10.7111P] 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         3257
_refine_ls_number_parameters     216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.182
_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
C1 C 0.2333(6) 0.4065(3) 0.1379(5) 0.0195(10) Uani 1 1 d . . .
H1 H 0.2404 0.3913 0.0558 0.023 Uiso 1 1 calc R . .
C2 C 0.3299(6) 0.3773(3) 0.2395(5) 0.0238(11) Uani 1 1 d . . .
H2 H 0.4009 0.3428 0.2255 0.029 Uiso 1 1 calc R . .
C3 C 0.3200(7) 0.3996(3) 0.3620(5) 0.0275(12) Uani 1 1 d . . .
H3 H 0.3856 0.3815 0.4313 0.033 Uiso 1 1 calc R . .
C4 C 0.2095(6) 0.4498(3) 0.3788(5) 0.0244(11) Uani 1 1 d . . .
H4 H 0.1980 0.4649 0.4601 0.029 Uiso 1 1 calc R . .
C5 C 0.1168(6) 0.4772(3) 0.2737(5) 0.0225(11) Uani 1 1 d . . .
H5 H 0.0435 0.5110 0.2856 0.027 Uiso 1 1 calc R . .
C6 C -0.2173(6) 0.3913(3) 0.0612(5) 0.0217(11) Uani 1 1 d . . .
H6 H -0.2261 0.4212 0.1290 0.026 Uiso 1 1 calc R . .
C7 C -0.3013(7) 0.3298(3) 0.0490(5) 0.0276(12) Uani 1 1 d . . .
H7 H -0.3650 0.3181 0.1086 0.033 Uiso 1 1 calc R . .
C8 C -0.2901(6) 0.2852(3) -0.0529(5) 0.0264(12) Uani 1 1 d . . .
H8 H -0.3476 0.2439 -0.0636 0.032 Uiso 1 1 calc R . .
C9 C -0.1921(6) 0.3035(3) -0.1377(5) 0.0246(11) Uani 1 1 d . . .
H9 H -0.1822 0.2745 -0.2065 0.029 Uiso 1 1 calc R . .
C10 C -0.1085(6) 0.3652(3) -0.1198(5) 0.0219(11) Uani 1 1 d . . .
H10 H -0.0407 0.3767 -0.1762 0.026 Uiso 1 1 calc R . .
C100 C 0.6718(6) 0.5857(3) 0.2193(5) 0.0228(11) Uani 1 1 d . . .
C101 C 0.5208(7) 0.5481(4) 0.2144(7) 0.0419(16) Uani 1 1 d . . .
H10A H 0.5176 0.5092 0.1565 0.063 Uiso 1 1 calc R . .
H10B H 0.4376 0.5799 0.1857 0.063 Uiso 1 1 calc R . .
H10C H 0.5102 0.5311 0.2977 0.063 Uiso 1 1 calc R . .
C102 C 0.6872(7) 0.6557(3) 0.2831(6) 0.0344(14) Uani 1 1 d . . .
H10D H 0.7937 0.6700 0.2952 0.052 Uiso 1 1 calc R . .
H10E H 0.6518 0.6526 0.3642 0.052 Uiso 1 1 calc R . .
H10F H 0.6261 0.6897 0.2310 0.052 Uiso 1 1 calc R . .
N1 N 0.1291(5) 0.4566(2) 0.1555(4) 0.0184(9) Uani 1 1 d . . .
N2 N -0.1225(4) 0.4092(2) -0.0230(4) 0.0171(8) Uani 1 1 d . . .
F1 F 0.9268(4) 0.32358(18) 0.3407(3) 0.0290(7) Uani 1 1 d . . .
F2 F 0.9502(4) 0.3889(2) 0.5639(3) 0.0435(9) Uani 1 1 d . . .
F3 F 0.7287(5) 0.42468(19) 0.3738(3) 0.0412(9) Uani 1 1 d . . .
F4 F 0.6558(4) 0.3580(2) 0.5752(3) 0.0442(10) Uani 1 1 d . . .
F5 F 0.6349(4) 0.2918(2) 0.3539(3) 0.0364(8) Uani 1 1 d . . .
F6 F 0.8556(4) 0.2561(2) 0.5420(3) 0.0405(9) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.5000 0.0000 0.01505(14) Uani 1 2 d S . .
Sb1 Sb 0.79165(4) 0.34044(2) 0.45888(3) 0.02325(13) Uani 1 1 d . . .
O1 O 0.7789(5) 0.5602(2) 0.1730(4) 0.0320(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.350(7) . ?
C1 C2 1.384(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.385(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.335(7) . ?
C5 H5 0.9300 . ?
C6 N2 1.351(6) . ?
C6 C7 1.377(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.391(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(8) . ?
C9 H9 0.9300 . ?
C10 N2 1.345(7) . ?
C10 H10 0.9300 . ?
C100 O1 1.222(7) . ?
C100 C102 1.491(8) . ?
C100 C101 1.496(8) . ?
C101 H10A 0.9600 . ?
C101 H10B 0.9600 . ?
C101 H10C 0.9600 . ?
C102 H10D 0.9600 . ?
C102 H10E 0.9600 . ?
C102 H10F 0.9600 . ?
N1 Pd1 2.034(4) . ?
N2 Pd1 2.028(4) . ?
F1 Sb1 1.876(3) . ?
F2 Sb1 1.886(4) . ?
F3 Sb1 1.881(3) . ?
F4 Sb1 1.867(3) . ?
F5 Sb1 1.878(3) . ?
F6 Sb1 1.876(3) . ?
Pd1 N2 2.028(4) 3_565 ?
Pd1 N1 2.034(4) 3_565 ?

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 C1 C2 121.4(5) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 118.3(5) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
N2 C6 C7 121.5(5) . . ?
N2 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 119.6(5) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 118.5(5) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C10 119.5(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.9(5) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
O1 C100 C102 121.0(5) . . ?
O1 C100 C101 121.4(5) . . ?
C102 C100 C101 117.6(5) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C5 N1 C1 119.2(4) . . ?
C5 N1 Pd1 122.2(4) . . ?
C1 N1 Pd1 118.6(3) . . ?
C10 N2 C6 118.9(4) . . ?
C10 N2 Pd1 121.1(3) . . ?
C6 N2 Pd1 120.0(3) . . ?
N2 Pd1 N2 180.0 . 3_565 ?
N2 Pd1 N1 88.40(16) . . ?
N2 Pd1 N1 91.60(16) 3_565 . ?
N2 Pd1 N1 91.60(16) . 3_565 ?
N2 Pd1 N1 88.40(16) 3_565 3_565 ?
N1 Pd1 N1 180.0(2) . 3_565 ?
F4 Sb1 F6 90.89(17) . . ?
F4 Sb1 F1 179.33(16) . . ?
F6 Sb1 F1 89.74(15) . . ?
F4 Sb1 F5 90.08(17) . . ?
F6 Sb1 F5 89.97(17) . . ?
F1 Sb1 F5 89.71(15) . . ?
F4 Sb1 F3 89.79(17) . . ?
F6 Sb1 F3 179.30(16) . . ?
F1 Sb1 F3 89.57(15) . . ?
F5 Sb1 F3 89.87(17) . . ?
F4 Sb1 F2 90.25(18) . . ?
F6 Sb1 F2 89.84(18) . . ?
F1 Sb1 F2 89.96(16) . . ?
F5 Sb1 F2 179.62(16) . . ?
F3 Sb1 F2 90.32(18) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.385
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.138
_database_code_depnum_ccdc_archive 'CCDC 1000101'
