# Supplementary Material (ESI) for Chemical Science
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               'Chemical Science'

_journal_coden_Cambridge         1475

_publ_contact_author_name        'Lindoy, Leonard'
_publ_contact_author_email       lindoy@gmail.com

_publ_section_title              
;
Encapsulation of a [FeIIICl4]- Anion in a Cationic
[FeII4L6]8+ Tetrahedral Cage Derived from 5,5$B!l!l!l
(B-Dimethyl-2,2$B!l(B:5$B!l(B,5$B!l!l
(B:2$B!l!l(B,2$B!l!l!l(B-quaterpyridine
;
loop_
_publ_author_name
C.Glasson
J.Clegg
J.McMurtrie
G.Meehan
L.Lindoy
C.Motti
;
B.Moubaraki
;
K.Murray
J.Cashion

# Attachment 'LJ282SADx.CIF'

data_lj282sad
_database_code_depnum_ccdc_archive 'CCDC 783500'
#TrackingRef 'LJ282SADx.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H49 Cl10.667 Fe4 N9 O4'
_chemical_formula_sum            'C47 H49 Cl10.667 Fe4 N9 O4'
_chemical_formula_weight         1405.49

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   F23
_symmetry_space_group_name_Hall  F223
_symmetry_intl_tables_number     196

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

_cell_length_a                   29.6690(3)
_cell_length_b                   29.6690(3)
_cell_length_c                   29.6690(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     26116.1(5)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9808
_cell_measurement_theta_min      2.255
_cell_measurement_theta_max      33.039

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8536
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'

_exptl_special_details           
;
The crystal was coated in Exxon Paratone N hydrocarbon
oil and mounted on a thin mohair fibre attached to a copper pin.
Upon mounting on the diffractometer,
the crystal was quenched to 150(K) under a cold nitrogen gas stream
supplied by an Oxford Cryosystems Cryostream and data were
collected at this temperature.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            107440
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         33.07
_reflns_number_total             8252
_reflns_number_gt                7472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX (Bruker-Nonius, 2003)'
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_reduction        
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
POV-Ray 3.5 (Cason, 2002)
WebLab ViewerPro 3.7 (Molecular Simulations, 2000)
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+21.0217P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.492(15)
_refine_ls_number_reflns         8252
_refine_ls_number_parameters     250
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1299
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.186
_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
C1 C 0.46340(9) 0.07262(15) 0.13815(12) 0.0634(11) Uani 1 1 d . . .
H1A H 0.4470 0.1013 0.1381 0.095 Uiso 1 1 calc R . .
H1B H 0.4452 0.0495 0.1532 0.095 Uiso 1 1 calc R . .
H1C H 0.4694 0.0634 0.1070 0.095 Uiso 1 1 calc R . .
C2 C 0.50731(7) 0.07827(9) 0.16292(8) 0.0367(5) Uani 1 1 d . . .
C3 C 0.54352(6) 0.10063(7) 0.14251(7) 0.0285(4) Uani 1 1 d . . .
H3 H 0.5392 0.1129 0.1133 0.034 Uiso 1 1 calc R . .
C4 C 0.58982(5) 0.08895(6) 0.20480(6) 0.0223(3) Uani 1 1 d . . .
C5 C 0.55510(7) 0.06719(9) 0.22756(8) 0.0350(4) Uani 1 1 d . . .
H5 H 0.5596 0.0563 0.2573 0.042 Uiso 1 1 calc R . .
C6 C 0.51356(7) 0.06147(10) 0.20625(9) 0.0401(5) Uani 1 1 d . . .
H6 H 0.4897 0.0462 0.2212 0.048 Uiso 1 1 calc R . .
C7 C 0.63582(6) 0.09424(6) 0.22235(6) 0.0221(3) Uani 1 1 d . . .
C8 C 0.70886(5) 0.11660(5) 0.20466(5) 0.0190(3) Uani 1 1 d . . .
H8 H 0.7294 0.1301 0.1841 0.023 Uiso 1 1 calc R . .
C9 C 0.72548(5) 0.10013(6) 0.24551(6) 0.0207(3) Uani 1 1 d . . .
C10 C 0.69478(6) 0.08310(8) 0.27692(6) 0.0283(3) Uani 1 1 d . . .
H10 H 0.7047 0.0739 0.3060 0.034 Uiso 1 1 calc R . .
C11 C 0.64952(6) 0.07976(8) 0.26510(7) 0.0293(4) Uani 1 1 d . . .
H11 H 0.6282 0.0678 0.2858 0.035 Uiso 1 1 calc R . .
N1 N 0.58400(5) 0.10557(5) 0.16217(5) 0.0195(2) Uani 1 1 d . . .
N2 N 0.66488(5) 0.11419(5) 0.19317(5) 0.0173(2) Uani 1 1 d . . .
Cl1 Cl 0.55371(4) 0.11250(3) 0.34790(3) 0.0621(2) Uani 1 1 d . . .
Cl2 Cl 0.54904(3) 0.04904(3) 0.45096(3) 0.0785(5) Uani 1 3 d S . .
Cl3 Cl 0.707074(16) 0.207074(16) 0.292926(16) 0.02873(15) Uani 1 3 d S . .
Cl4 Cl 0.54212(3) 0.04212(3) 0.04212(3) 0.0802(7) Uani 0.83 3 d SP A 1
Cl4A Cl 0.5606(8) 0.0241(8) 0.0367(8) 0.0802(7) Uani 0.057 1 d P A 2
Fe1 Fe 0.637050(7) 0.137050(7) 0.137050(7) 0.01586(8) Uani 1 3 d S . .
Fe2 Fe 0.591571(14) 0.091571(14) 0.408429(14) 0.04707(17) Uani 1 3 d S . .
Fe3 Fe 0.7500 0.2500 0.2500 0.02352(16) Uani 1 12 d S . .
Fe4 Fe 0.5000 0.0000 0.0000 0.02607(17) Uani 1 12 d S . .
Fe5 Fe 0.4309(4) 0.2120(4) 0.1762(5) 0.084(3) Uani 0.083 1 d PD . 1
Cl5 Cl 0.4893(7) 0.1819(9) 0.2104(9) 0.110(3) Uani 0.083 1 d PD . 1
Cl6 Cl 0.4605(8) 0.2432(8) 0.1160(7) 0.110(3) Uani 0.083 1 d PD . 1
Cl7 Cl 0.3921(7) 0.2498(9) 0.2269(8) 0.110(3) Uani 0.083 1 d PD . 1
Cl8 Cl 0.3807(7) 0.1616(8) 0.1548(9) 0.110(3) Uani 0.083 1 d PD . 1
Fe5A Fe 0.4409(6) 0.2036(6) 0.1802(8) 0.084(3) Uani 0.056 1 d PD . 2
Cl8A Cl 0.3986(9) 0.1466(9) 0.1554(12) 0.110(3) Uani 0.056 1 d PD . 2
Cl5A Cl 0.4883(10) 0.1894(12) 0.2371(10) 0.110(3) Uani 0.056 1 d PD . 2
Cl6A Cl 0.4708(10) 0.2144(11) 0.1123(9) 0.110(3) Uani 0.056 1 d PD . 2
Cl7A Cl 0.4062(10) 0.2610(9) 0.2137(13) 0.110(3) Uani 0.056 1 d PD . 2
O4W O 0.4752(13) 0.1710(14) 0.2530(14) 0.082(10) Uiso 0.125 1 d P B 4
O7W O 0.5121(7) 0.1783(7) 0.2301(8) 0.049(4) Uiso 0.125 1 d P C 6
C1A C 0.4830(9) 0.1640(9) 0.2412(9) 0.074(5) Uiso 0.25 1 d P D 5
N1A N 0.5018(7) 0.1851(7) 0.2163(7) 0.067(4) Uiso 0.25 1 d P D 5
C2A C 0.4525(13) 0.1438(13) 0.2741(13) 0.124(10) Uiso 0.25 1 d P D 5
H2A1 H 0.4457 0.1126 0.2658 0.186 Uiso 0.25 1 d PR D 5
H2A2 H 0.4246 0.1616 0.2737 0.186 Uiso 0.25 1 d PR D 5
H2A3 H 0.4656 0.1446 0.3044 0.186 Uiso 0.25 1 d PR D 5
Fe6 Fe 0.3082(3) 0.3082(3) 0.1918(3) 0.063(3) Uani 0.083 3 d SPD . 3
Cl9 Cl 0.3505(5) 0.3505(5) 0.1495(5) 0.104(5) Uani 0.083 3 d SPD . 3
Cl10 Cl 0.3518(7) 0.2601(8) 0.2262(7) 0.104(5) Uani 0.083 1 d PD . 3
O5W O 0.5000 0.0000 0.3278(7) 0.072(4) Uiso 0.25 2 d SP E 3
O6W O 0.4785(7) 0.0151(7) 0.3300(8) 0.053(4) Uiso 0.125 1 d P F -4
O1M O 0.4715(10) 0.0136(9) 0.3032(8) 0.063(5) Uiso 0.125 1 d PD G -5
H1M H 0.4523 0.0189 0.2831 0.095 Uiso 0.125 1 d PR G -5
C1M C 0.4559(11) 0.0268(11) 0.3418(8) 0.061(6) Uiso 0.125 1 d PD G -5
H1M1 H 0.4606 0.0029 0.3642 0.092 Uiso 0.125 1 d PR G -5
H1M2 H 0.4236 0.0332 0.3392 0.092 Uiso 0.125 1 d PR G -5
H1M3 H 0.4718 0.0541 0.3514 0.092 Uiso 0.125 1 d PR G -5
C2M C 0.4461(13) 0.0214(12) 0.3020(12) 0.064(7) Uiso 0.125 1 d P H -6
H2M1 H 0.4341 0.0219 0.3327 0.096 Uiso 0.125 1 d PR H -6
H2M2 H 0.4280 0.0010 0.2834 0.096 Uiso 0.125 1 d PR H -6
H2M3 H 0.4449 0.0518 0.2892 0.096 Uiso 0.125 1 d PR H -6
O2M O 0.4901(6) 0.0062(7) 0.3011(7) 0.048(4) Uiso 0.125 1 d P H -6
H2M H 0.5036 0.0154 0.2780 0.072 Uiso 0.125 1 d PR H -6
O1W O 0.4654(10) 0.2167(10) 0.1402(11) 0.077(7) Uiso 0.125 1 d P I 7
O2W O 0.3718(8) 0.0426(8) 0.2582(8) 0.058(5) Uiso 0.125 1 d P J 7

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0302(11) 0.105(3) 0.0552(16) 0.0291(18) -0.0208(12) -0.0303(14)
C2 0.0209(8) 0.0517(12) 0.0374(10) 0.0122(9) -0.0094(7) -0.0125(8)
C3 0.0207(7) 0.0377(9) 0.0270(8) 0.0058(7) -0.0073(6) -0.0091(6)
C4 0.0166(6) 0.0272(7) 0.0232(7) 0.0041(6) -0.0029(5) -0.0033(5)
C5 0.0234(8) 0.0481(12) 0.0334(10) 0.0172(9) -0.0048(7) -0.0114(8)
C6 0.0234(8) 0.0554(14) 0.0414(11) 0.0175(10) -0.0060(8) -0.0148(8)
C7 0.0169(6) 0.0273(7) 0.0220(6) 0.0038(5) -0.0033(5) -0.0026(5)
C8 0.0160(6) 0.0219(6) 0.0192(6) -0.0011(5) -0.0028(5) -0.0022(5)
C9 0.0177(6) 0.0238(7) 0.0207(6) 0.0001(5) -0.0052(5) -0.0009(5)
C10 0.0211(7) 0.0398(9) 0.0240(7) 0.0087(7) -0.0061(6) -0.0033(7)
C11 0.0209(7) 0.0425(10) 0.0245(7) 0.0099(7) -0.0039(6) -0.0046(7)
N1 0.0165(5) 0.0212(5) 0.0208(5) -0.0003(4) -0.0035(4) -0.0030(4)
N2 0.0162(5) 0.0176(5) 0.0179(5) -0.0009(4) -0.0023(4) -0.0005(4)
Cl1 0.0685(5) 0.0515(4) 0.0663(5) 0.0100(3) -0.0141(4) -0.0075(3)
Cl2 0.0785(5) 0.0785(5) 0.0785(5) 0.0217(4) 0.0217(4) -0.0217(4)
Cl3 0.02873(15) 0.02873(15) 0.02873(15) 0.00185(14) 0.00185(14) -0.00185(14)
Cl4 0.0802(7) 0.0802(7) 0.0802(7) -0.0282(5) -0.0282(5) -0.0282(5)
Cl4A 0.0802(7) 0.0802(7) 0.0802(7) -0.0282(5) -0.0282(5) -0.0282(5)
Fe1 0.01586(8) 0.01586(8) 0.01586(8) -0.00187(7) -0.00187(7) -0.00187(7)
Fe2 0.04707(17) 0.04707(17) 0.04707(17) 0.00556(15) 0.00556(15) -0.00556(15)
Fe3 0.02352(16) 0.02352(16) 0.02352(16) 0.000 0.000 0.000
Fe4 0.02607(17) 0.02607(17) 0.02607(17) 0.000 0.000 0.000
Fe5 0.073(6) 0.084(6) 0.095(5) -0.015(4) 0.005(5) 0.009(5)
Cl5 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl6 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl7 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl8 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Fe5A 0.073(6) 0.084(6) 0.095(5) -0.015(4) 0.005(5) 0.009(5)
Cl8A 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl5A 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl6A 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Cl7A 0.092(6) 0.107(6) 0.131(7) -0.044(6) 0.016(5) -0.013(5)
Fe6 0.063(3) 0.063(3) 0.063(3) -0.009(3) -0.009(3) 0.009(3)
Cl9 0.104(5) 0.104(5) 0.104(5) -0.017(6) -0.017(6) 0.017(6)
Cl10 0.104(5) 0.104(5) 0.104(5) -0.017(6) -0.017(6) 0.017(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

C1 C2 1.505(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C6 1.391(3) . ?
C2 C3 1.400(3) . ?
C3 N1 1.343(2) . ?
C3 H3 0.9500 . ?
C4 N1 1.368(2) . ?
C4 C5 1.391(2) . ?
C4 C7 1.469(2) . ?
C5 C6 1.395(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N2 1.358(2) . ?
C7 C11 1.399(2) . ?
C8 N2 1.350(2) . ?
C8 C9 1.397(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(3) . ?
C9 C9 1.479(3) 28_655 ?
C10 C11 1.391(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
N1 Fe1 1.9762(14) . ?
N2 Fe1 1.9784(14) . ?
Cl1 Fe2 2.2075(9) . ?
Cl2 Fe2 2.1854(17) . ?
Cl3 Fe3 2.2059(8) . ?
Cl4 Fe4 2.1646(17) . ?
Cl4A Fe4 2.219(17) . ?
Fe1 N1 1.9762(14) 41_545 ?
Fe1 N1 1.9762(14) 30_554 ?
Fe1 N2 1.9784(14) 41_545 ?
Fe1 N2 1.9784(14) 30_554 ?
Fe2 Cl1 2.2074(9) 48_556 ?
Fe2 Cl1 2.2074(9) 23_645 ?
Fe3 Cl3 2.2059(8) 38_655 ?
Fe3 Cl3 2.2059(8) 28_655 ?
Fe3 Cl3 2.2059(8) 15 ?
Fe4 Cl4 2.1646(17) 3 ?
Fe4 Cl4 2.1646(17) 4_655 ?
Fe4 Cl4 2.1646(17) 2_655 ?
Fe4 Cl4A 2.219(17) 41_545 ?
Fe4 Cl4A 2.219(17) 36 ?
Fe4 Cl4A 2.219(17) 30_554 ?
Fe4 Cl4A 2.219(17) 45 ?
Fe4 Cl4A 2.219(17) 34_554 ?
Fe4 Cl4A 2.219(17) 3 ?
Fe4 Cl4A 2.219(17) 43 ?
Fe5 Cl6 2.193(11) . ?
Fe5 Cl5 2.198(11) . ?
Fe5 Cl7 2.202(11) . ?
Fe5 Cl8 2.204(8) . ?
Fe5A Cl6A 2.224(9) . ?
Fe5A Cl7A 2.227(12) . ?
Fe5A Cl8A 2.231(12) . ?
Fe5A Cl5A 2.238(12) . ?
C1A N1A 1.12(4) . ?
C1A C2A 1.46(5) . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C2A H2A3 0.9800 . ?
Fe6 Cl9 2.18(2) . ?
Fe6 Cl10 2.18(2) 24 ?
Fe6 Cl10 2.18(2) . ?
Fe6 Cl10 2.18(2) 35 ?
O1M C1M 1.295(10) . ?
O1M H1M 0.8400 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
C1M H2M1 0.7158 . ?
C2M O2M 1.38(4) . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?
O2M H1M 1.2969 . ?
O2M H2M 0.8400 . ?

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 . . ?
C6 C2 C3 117.83(18) . . ?
C6 C2 C1 121.8(2) . . ?
C3 C2 C1 120.4(2) . . ?
N1 C3 C2 123.36(18) . . ?
N1 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
N1 C4 C5 121.50(15) . . ?
N1 C4 C7 113.98(14) . . ?
C5 C4 C7 124.45(16) . . ?
C4 C5 C6 119.39(19) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C2 C6 C5 119.53(19) . . ?
C2 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N2 C7 C11 121.83(16) . . ?
N2 C7 C4 114.23(14) . . ?
C11 C7 C4 123.94(16) . . ?
N2 C8 C9 122.79(15) . . ?
N2 C8 H8 118.6 . . ?
C9 C8 H8 118.6 . . ?
C8 C9 C10 118.35(15) . . ?
C8 C9 C9 120.23(18) . 28_655 ?
C10 C9 C9 121.40(17) . 28_655 ?
C11 C10 C9 119.13(16) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C7 119.13(17) . . ?
C10 C11 H11 120.4 . . ?
C7 C11 H11 120.4 . . ?
C3 N1 C4 118.36(15) . . ?
C3 N1 Fe1 126.86(12) . . ?
C4 N1 Fe1 114.73(10) . . ?
C8 N2 C7 118.40(14) . . ?
C8 N2 Fe1 126.69(11) . . ?
C7 N2 Fe1 114.91(11) . . ?
Cl4A Cl4A Cl4A 60.000(4) 41_545 30_554 ?
Cl4A Cl4A Fe4 72.3(6) 41_545 . ?
Cl4A Cl4A Fe4 72.3(6) 30_554 . ?
N1 Fe1 N1 95.86(6) 41_545 . ?
N1 Fe1 N1 95.86(6) 41_545 30_554 ?
N1 Fe1 N1 95.86(6) . 30_554 ?
N1 Fe1 N2 81.55(6) 41_545 41_545 ?
N1 Fe1 N2 175.46(6) . 41_545 ?
N1 Fe1 N2 88.13(6) 30_554 41_545 ?
N1 Fe1 N2 88.13(6) 41_545 . ?
N1 Fe1 N2 81.55(6) . . ?
N1 Fe1 N2 175.46(6) 30_554 . ?
N2 Fe1 N2 94.61(5) 41_545 . ?
N1 Fe1 N2 175.46(6) 41_545 30_554 ?
N1 Fe1 N2 88.13(6) . 30_554 ?
N1 Fe1 N2 81.55(6) 30_554 30_554 ?
N2 Fe1 N2 94.61(5) 41_545 30_554 ?
N2 Fe1 N2 94.61(5) . 30_554 ?
Cl2 Fe2 Cl1 109.77(3) . 48_556 ?
Cl2 Fe2 Cl1 109.77(3) . 23_645 ?
Cl1 Fe2 Cl1 109.17(3) 48_556 23_645 ?
Cl2 Fe2 Cl1 109.77(3) . . ?
Cl1 Fe2 Cl1 109.17(3) 48_556 . ?
Cl1 Fe2 Cl1 109.17(3) 23_645 . ?
Cl3 Fe3 Cl3 109.5 38_655 . ?
Cl3 Fe3 Cl3 109.471(1) 38_655 28_655 ?
Cl3 Fe3 Cl3 109.5 . 28_655 ?
Cl3 Fe3 Cl3 109.5 38_655 15 ?
Cl3 Fe3 Cl3 109.471(1) . 15 ?
Cl3 Fe3 Cl3 109.5 28_655 15 ?
Cl4 Fe4 Cl4 109.5 3 . ?
Cl4 Fe4 Cl4 109.5 3 4_655 ?
Cl4 Fe4 Cl4 109.5 . 4_655 ?
Cl4 Fe4 Cl4 109.5 3 2_655 ?
Cl4 Fe4 Cl4 109.5 . 2_655 ?
Cl4 Fe4 Cl4 109.5 4_655 2_655 ?
Cl4 Fe4 Cl4A 111.7(7) 3 41_545 ?
Cl4 Fe4 Cl4A 20.5(7) . 41_545 ?
Cl4 Fe4 Cl4A 90.1(7) 4_655 41_545 ?
Cl4 Fe4 Cl4A 124.4(7) 2_655 41_545 ?
Cl4 Fe4 Cl4A 20.5(7) 3 36 ?
Cl4 Fe4 Cl4A 124.4(7) . 36 ?
Cl4 Fe4 Cl4A 90.1(7) 4_655 36 ?
Cl4 Fe4 Cl4A 111.7(7) 2_655 36 ?
Cl4A Fe4 Cl4A 120.000(3) 41_545 36 ?
Cl4 Fe4 Cl4A 124.4(7) 3 30_554 ?
Cl4 Fe4 Cl4A 20.5(7) . 30_554 ?
Cl4 Fe4 Cl4A 111.7(7) 4_655 30_554 ?
Cl4 Fe4 Cl4A 90.1(7) 2_655 30_554 ?
Cl4A Fe4 Cl4A 35.3(12) 41_545 30_554 ?
Cl4A Fe4 Cl4A 142.4(14) 36 30_554 ?
Cl4 Fe4 Cl4A 20.5(7) 3 45 ?
Cl4 Fe4 Cl4A 111.7(7) . 45 ?
Cl4 Fe4 Cl4A 124.4(7) 4_655 45 ?
Cl4 Fe4 Cl4A 90.1(7) 2_655 45 ?
Cl4A Fe4 Cl4A 121.3(14) 41_545 45 ?
Cl4A Fe4 Cl4A 35.3(12) 36 45 ?
Cl4A Fe4 Cl4A 120.000(3) 30_554 45 ?
Cl4 Fe4 Cl4A 111.7(7) 3 34_554 ?
Cl4 Fe4 Cl4A 90.1(7) . 34_554 ?
Cl4 Fe4 Cl4A 124.4(7) 4_655 34_554 ?
Cl4 Fe4 Cl4A 20.5(7) 2_655 34_554 ?
Cl4A Fe4 Cl4A 107.1(7) 41_545 34_554 ?
Cl4A Fe4 Cl4A 121.3(14) 36 34_554 ?
Cl4A Fe4 Cl4A 71.8(13) 30_554 34_554 ?
Cl4A Fe4 Cl4A 91.2(10) 45 34_554 ?
Cl4 Fe4 Cl4A 20.5(7) 3 3 ?
Cl4 Fe4 Cl4A 90.1(7) . 3 ?
Cl4 Fe4 Cl4A 111.7(7) 4_655 3 ?
Cl4 Fe4 Cl4A 124.4(7) 2_655 3 ?
Cl4A Fe4 Cl4A 91.2(10) 41_545 3 ?
Cl4A Fe4 Cl4A 35.3(12) 36 3 ?
Cl4A Fe4 Cl4A 107.1(7) 30_554 3 ?
Cl4A Fe4 Cl4A 35.3(12) 45 3 ?
Cl4A Fe4 Cl4A 120.000(3) 34_554 3 ?
Cl4 Fe4 Cl4A 90.1(7) 3 . ?
Cl4 Fe4 Cl4A 20.5(7) . . ?
Cl4 Fe4 Cl4A 124.4(7) 4_655 . ?
Cl4 Fe4 Cl4A 111.7(7) 2_655 . ?
Cl4A Fe4 Cl4A 35.3(12) 41_545 . ?
Cl4A Fe4 Cl4A 107.1(7) 36 . ?
Cl4A Fe4 Cl4A 35.3(12) 30_554 . ?
Cl4A Fe4 Cl4A 91.2(10) 45 . ?
Cl4A Fe4 Cl4A 91.2(10) 34_554 . ?
Cl4A Fe4 Cl4A 71.8(13) 3 . ?
Cl4 Fe4 Cl4A 90.1(7) 3 43 ?
Cl4 Fe4 Cl4A 124.4(7) . 43 ?
Cl4 Fe4 Cl4A 111.7(7) 4_655 43 ?
Cl4 Fe4 Cl4A 20.5(7) 2_655 43 ?
Cl4A Fe4 Cl4A 142.4(14) 41_545 43 ?
Cl4A Fe4 Cl4A 91.2(10) 36 43 ?
Cl4A Fe4 Cl4A 107.1(7) 30_554 43 ?
Cl4A Fe4 Cl4A 71.8(13) 45 43 ?
Cl4A Fe4 Cl4A 35.3(12) 34_554 43 ?
Cl4A Fe4 Cl4A 107.1(7) 3 43 ?
Cl4A Fe4 Cl4A 120.000(3) . 43 ?
Cl6 Fe5 Cl5 103.5(11) . . ?
Cl6 Fe5 Cl7 123.5(12) . . ?
Cl5 Fe5 Cl7 107.6(12) . . ?
Cl6 Fe5 Cl8 108.7(11) . . ?
Cl5 Fe5 Cl8 112.9(12) . . ?
Cl7 Fe5 Cl8 100.9(9) . . ?
Cl7 Cl7 Fe5 133(2) 15 . ?
Cl8 Cl8 Cl8 60.000(3) 32 43 ?
Cl8 Cl8 Fe5 141(3) 32 . ?
Cl8 Cl8 Fe5 156(2) 43 . ?
Cl6A Fe5A Cl7A 118.6(7) . . ?
Cl6A Fe5A Cl8A 92.0(15) . . ?
Cl7A Fe5A Cl8A 117.8(7) . . ?
Cl6A Fe5A Cl5A 117.4(7) . . ?
Cl7A Fe5A Cl5A 95.5(17) . . ?
Cl8A Fe5A Cl5A 117.4(7) . . ?
Cl8A Cl8A Cl8A 60.000(2) 43 32 ?
Cl8A Cl8A Fe5A 162.2(10) 43 . ?
Cl8A Cl8A Fe5A 121(2) 32 . ?
Fe5A Cl7A Cl7A 101.9(18) . 15 ?
N1A C1A C2A 169(3) . . ?
C1A C2A H2A1 110.3 . . ?
C1A C2A H2A2 107.1 . . ?
H2A1 C2A H2A2 109.5 . . ?
C1A C2A H2A3 110.9 . . ?
H2A1 C2A H2A3 109.5 . . ?
H2A2 C2A H2A3 109.5 . . ?
Cl9 Fe6 Cl10 107.8(7) . 24 ?
Cl9 Fe6 Cl10 107.8(7) . . ?
Cl10 Fe6 Cl10 111.1(7) 24 . ?
Cl9 Fe6 Cl10 107.8(7) . 35 ?
Cl10 Fe6 Cl10 111.1(7) 24 35 ?
Cl10 Fe6 Cl10 111.1(7) . 35 ?
Cl10 Cl10 Fe6 133.3(13) 15 . ?
H1M1 O6W H1M3 78.1 . . ?
H1M1 O6W H2M1 63.8 . . ?
H1M3 O6W H2M1 72.1 . . ?
C1M O1M H1M 109.1 . . ?
C1M O1M H2M 144.4 . . ?
O1M C1M H1M1 109.2 . . ?
O1M C1M H1M2 109.8 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.4 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
O1M C1M H2M1 86.0 . . ?
H1M1 C1M H2M1 103.9 . . ?
H1M3 C1M H2M1 135.2 . . ?
O2M C2M H1M2 125.0 . . ?
H1M C2M H1M2 165.1 . . ?
O2M C2M H2M1 111.6 . . ?
H1M C2M H2M1 172.8 . . ?
O2M C2M H2M2 107.7 . . ?
H1M2 C2M H2M2 110.6 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.1 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?
C2M O2M H2M 111.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag

C6 C2 C3 N1 1.7(4) . . . . ?
C1 C2 C3 N1 -177.8(3) . . . . ?
N1 C4 C5 C6 1.1(4) . . . . ?
C7 C4 C5 C6 -175.6(2) . . . . ?
C3 C2 C6 C5 -0.2(4) . . . . ?
C1 C2 C6 C5 179.3(3) . . . . ?
C4 C5 C6 C2 -1.1(4) . . . . ?
N1 C4 C7 N2 -0.8(2) . . . . ?
C5 C4 C7 N2 176.1(2) . . . . ?
N1 C4 C7 C11 179.99(19) . . . . ?
C5 C4 C7 C11 -3.1(3) . . . . ?
N2 C8 C9 C10 -4.2(3) . . . . ?
N2 C8 C9 C9 174.64(12) . . . 28_655 ?
C8 C9 C10 C11 5.1(3) . . . . ?
C9 C9 C10 C11 -173.70(17) 28_655 . . . ?
C9 C10 C11 C7 -1.0(3) . . . . ?
N2 C7 C11 C10 -4.4(3) . . . . ?
C4 C7 C11 C10 174.8(2) . . . . ?
C2 C3 N1 C4 -1.8(3) . . . . ?
C2 C3 N1 Fe1 -179.08(19) . . . . ?
C5 C4 N1 C3 0.3(3) . . . . ?
C7 C4 N1 C3 177.32(17) . . . . ?
C5 C4 N1 Fe1 177.96(18) . . . . ?
C7 C4 N1 Fe1 -5.0(2) . . . . ?
C9 C8 N2 C7 -1.1(2) . . . . ?
C9 C8 N2 Fe1 178.92(12) . . . . ?
C11 C7 N2 C8 5.5(3) . . . . ?
C4 C7 N2 C8 -173.79(15) . . . . ?
C11 C7 N2 Fe1 -174.52(16) . . . . ?
C4 C7 N2 Fe1 6.20(19) . . . . ?
C3 N1 Fe1 N1 -88.83(14) . . . 41_545 ?
C4 N1 Fe1 N1 93.77(15) . . . 41_545 ?
C3 N1 Fe1 N1 7.71(17) . . . 30_554 ?
C4 N1 Fe1 N1 -169.69(13) . . . 30_554 ?
C3 N1 Fe1 N2 -176.05(17) . . . . ?
C4 N1 Fe1 N2 6.55(13) . . . . ?
C3 N1 Fe1 N2 89.01(17) . . . 30_554 ?
C4 N1 Fe1 N2 -88.39(13) . . . 30_554 ?
C8 N2 Fe1 N1 76.77(14) . . . 41_545 ?
C7 N2 Fe1 N1 -103.22(12) . . . 41_545 ?
C8 N2 Fe1 N1 172.98(14) . . . . ?
C7 N2 Fe1 N1 -7.00(12) . . . . ?
C8 N2 Fe1 N2 -4.59(14) . . . 41_545 ?
C7 N2 Fe1 N2 175.42(12) . . . 41_545 ?
C8 N2 Fe1 N2 -99.60(10) . . . 30_554 ?
C7 N2 Fe1 N2 80.41(15) . . . 30_554 ?
Cl4A Cl4A Fe4 Cl4 129.7(19) 41_545 . . 3 ?
Cl4A Cl4A Fe4 Cl4 -167.0(19) 30_554 . . 3 ?
Cl4A Cl4A Fe4 Cl4 -31.65(11) 41_545 . . . ?
Cl4A Cl4A Fe4 Cl4 31.65(12) 30_554 . . . ?
Cl4A Cl4A Fe4 Cl4 16(2) 41_545 . . 4_655 ?
Cl4A Cl4A Fe4 Cl4 79(2) 30_554 . . 4_655 ?
Cl4A Cl4A Fe4 Cl4 -119.2(19) 41_545 . . 2_655 ?
Cl4A Cl4A Fe4 Cl4 -55.9(19) 30_554 . . 2_655 ?
Cl4A Cl4A Fe4 Cl4A 63.3(2) 30_554 . . 41_545 ?
Cl4A Cl4A Fe4 Cl4A 118.1(12) 41_545 . . 36 ?
Cl4A Cl4A Fe4 Cl4A -178.6(11) 30_554 . . 36 ?
Cl4A Cl4A Fe4 Cl4A -63.3(2) 41_545 . . 30_554 ?
Cl4A Cl4A Fe4 Cl4A 150.2(19) 41_545 . . 45 ?
Cl4A Cl4A Fe4 Cl4A -146.5(19) 30_554 . . 45 ?
Cl4A Cl4A Fe4 Cl4A -119(3) 41_545 . . 34_554 ?
Cl4A Cl4A Fe4 Cl4A -55(3) 30_554 . . 34_554 ?
Cl4A Cl4A Fe4 Cl4A 120(3) 41_545 . . 3 ?
Cl4A Cl4A Fe4 Cl4A -177(3) 30_554 . . 3 ?
Cl4A Cl4A Fe4 Cl4A -140(2) 41_545 . . 43 ?
Cl4A Cl4A Fe4 Cl4A -76.9(18) 30_554 . . 43 ?
Cl6 Fe5 Cl7 Cl7 -135(3) . . . 15 ?
Cl5 Fe5 Cl7 Cl7 -15(3) . . . 15 ?
Cl8 Fe5 Cl7 Cl7 103(3) . . . 15 ?
Cl6 Fe5 Cl8 Cl8 -45.6(16) . . . 32 ?
Cl5 Fe5 Cl8 Cl8 -159.8(13) . . . 32 ?
Cl7 Fe5 Cl8 Cl8 85.6(17) . . . 32 ?
Cl6 Fe5 Cl8 Cl8 169(3) . . . 43 ?
Cl5 Fe5 Cl8 Cl8 55(3) . . . 43 ?
Cl7 Fe5 Cl8 Cl8 -60(3) . . . 43 ?
Cl6A Fe5A Cl8A Cl8A -144(9) . . . 43 ?
Cl7A Fe5A Cl8A Cl8A -20(9) . . . 43 ?
Cl5A Fe5A Cl8A Cl8A 93(8) . . . 43 ?
Cl6A Fe5A Cl8A Cl8A -56.6(14) . . . 32 ?
Cl7A Fe5A Cl8A Cl8A 68(2) . . . 32 ?
Cl5A Fe5A Cl8A Cl8A -179.1(13) . . . 32 ?
Cl6A Fe5A Cl7A Cl7A -160.5(13) . . . 15 ?
Cl8A Fe5A Cl7A Cl7A 89.9(13) . . . 15 ?
Cl5A Fe5A Cl7A Cl7A -35.1(9) . . . 15 ?
Cl9 Fe6 Cl10 Cl10 142(2) . . . 15 ?
Cl10 Fe6 Cl10 Cl10 -100(2) 24 . . 15 ?
Cl10 Fe6 Cl10 Cl10 24(3) 35 . . 15 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        33.07
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.112

# Attachment 'lflj63_X.cif'

data_ncent
_database_code_depnum_ccdc_archive 'CCDC 783501'
#TrackingRef 'lflj63_X.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;C132 H108 Fe4 N24, Fe Cl4, 6(P F6), 12(H2 O)
;
_chemical_formula_sum            'C132 H132 Cl4 F36 Fe5 N24 O12 P6'
_chemical_formula_weight         3537.49

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P-43n
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_international_tables_no 218

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

_cell_length_a                   21.7946(6)
_cell_length_b                   21.7946(6)
_cell_length_c                   21.7946(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10352.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13879
_cell_measurement_theta_min      2.289
_cell_measurement_theta_max      23.292

_exptl_crystal_description       multi-faced
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3600
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.825404
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'

_exptl_special_details           
;
The crystal was coated in Exxon Paratone N hydrocarbon
oil and mounted on a thin mohair fibre attached to a copper pin.
Upon mounting on the diffractometer,
the crystal was quenched to 150(K) under a cold nitrogen gas stream
supplied by an Oxford Cryosystems Cryostream and data were
collected at this temperature.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         279
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.11
_diffrn_reflns_number            95183
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         28.31
_reflns_number_total             4262
_reflns_number_gt                2740
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1995)'
_computing_cell_refinement       'SAINT (Bruker, 1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.0 (CCDC, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_number_reflns         4262
_refine_ls_number_parameters     171
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1783
_refine_ls_wR_factor_gt          0.1636
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.990
_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
Fe1 Fe 0.84706(2) 0.15294(2) 0.15294(2) 0.0192(2) Uani 1 3 d S . .
N1 N 0.80496(15) 0.22485(14) 0.11871(14) 0.0222(7) Uani 1 1 d . . .
N2 N 0.81617(14) 0.11532(14) 0.07657(14) 0.0206(6) Uani 1 1 d . . .
C1 C 0.7685(3) 0.3916(2) 0.1490(3) 0.0525(13) Uani 1 1 d . . .
H1A H 0.7705 0.3853 0.1935 0.079 Uiso 1 1 calc R . .
H1B H 0.7291 0.4104 0.1384 0.079 Uiso 1 1 calc R . .
H1C H 0.8020 0.4187 0.1362 0.079 Uiso 1 1 calc R . .
C2 C 0.7746(2) 0.3304(2) 0.1166(2) 0.0373(10) Uani 1 1 d . . .
C3 C 0.7524(3) 0.3226(2) 0.0568(2) 0.0476(13) Uani 1 1 d . . .
H3 H 0.7346 0.3561 0.0353 0.057 Uiso 1 1 calc R . .
C4 C 0.7567(3) 0.2659(2) 0.0297(2) 0.0433(12) Uani 1 1 d . . .
H4 H 0.7416 0.2599 -0.0107 0.052 Uiso 1 1 calc R . .
C5 C 0.78334(19) 0.21730(17) 0.06136(18) 0.0274(8) Uani 1 1 d . . .
C6 C 0.80012(18) 0.28078(17) 0.14503(18) 0.0291(9) Uani 1 1 d . . .
H6 H 0.8154 0.2858 0.1856 0.035 Uiso 1 1 calc R . .
C7 C 0.78865(18) 0.15557(18) 0.03762(17) 0.0266(8) Uani 1 1 d . . .
C8 C 0.7671(2) 0.1357(2) -0.01924(19) 0.0359(10) Uani 1 1 d . . .
H8 H 0.7492 0.1643 -0.0469 0.043 Uiso 1 1 calc R . .
C9 C 0.7716(2) 0.0753(2) -0.03537(18) 0.0361(10) Uani 1 1 d . . .
H9 H 0.7586 0.0620 -0.0748 0.043 Uiso 1 1 calc R . .
C10 C 0.79533(16) 0.03323(17) 0.00645(18) 0.0244(8) Uani 1 1 d . . .
C11 C 0.81785(16) 0.05546(17) 0.06116(17) 0.0225(7) Uani 1 1 d . . .
H11 H 0.8354 0.0272 0.0894 0.027 Uiso 1 1 calc R . .
P1 P 0.80717(6) 0.19283(6) -0.19283(6) 0.0479(6) Uani 1 3 d S . .
F1 F 0.8240(2) 0.26021(16) -0.21394(19) 0.0880(12) Uani 1 1 d . . .
F2 F 0.78923(19) 0.12562(15) -0.17145(19) 0.0784(11) Uani 1 1 d . . .
Fe2 Fe 1.0000 0.0000 0.0000 0.0271(4) Uani 1 12 d S . .
Cl1 Cl 1.05826(4) 0.05826(4) 0.05826(4) 0.0336(4) Uani 1 3 d S . .
P2 P 0.8465(3) 0.5000 0.0000 0.0527(14) Uani 0.3334 2 d SPD . .
F3 F 0.9201(5) 0.5000 0.0000 0.152(3) Uiso 0.334 2 d SPD . .
F4 F 0.8470(7) 0.4281(4) -0.0035(9) 0.152(3) Uiso 0.333 1 d PD . .
F5 F 0.8471(7) 0.5002(9) 0.0721(4) 0.152(3) Uiso 0.333 1 d PD . .
F6 F 0.7752(5) 0.5000 0.0000 0.152(3) Uiso 0.334 2 d SPD . .
O1 O 0.9465(4) 0.6277(4) 0.2200(4) 0.0681(18) Uiso 0.45 1 d P A 1
O2 O 0.9320(7) 0.3853(6) 0.1876(7) 0.0681(18) Uiso 0.30 1 d P B 2
O3 O 0.9062(8) 0.6152(8) 0.1628(7) 0.0681(18) Uiso 0.25 1 d P C 3

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0192(2) 0.0192(2) 0.0192(2) -0.00207(19) 0.00207(19) 0.00207(19)
N1 0.0241(16) 0.0186(15) 0.0239(16) -0.0028(12) 0.0044(13) 0.0006(12)
N2 0.0216(15) 0.0211(16) 0.0190(16) -0.0027(12) 0.0014(12) 0.0042(12)
C1 0.080(4) 0.029(2) 0.048(3) -0.007(2) -0.011(3) 0.014(2)
C2 0.057(3) 0.024(2) 0.031(2) -0.0014(17) 0.004(2) 0.0095(19)
C3 0.082(4) 0.030(2) 0.030(2) -0.0001(19) -0.004(3) 0.016(2)
C4 0.073(3) 0.031(2) 0.026(2) 0.0016(18) -0.010(2) 0.013(2)
C5 0.036(2) 0.0234(19) 0.0229(18) 0.0019(15) -0.0005(17) 0.0034(16)
C6 0.035(2) 0.026(2) 0.026(2) -0.0049(16) 0.0039(17) 0.0062(17)
C7 0.032(2) 0.0247(19) 0.0232(18) 0.0018(16) -0.0017(15) 0.0059(17)
C8 0.056(3) 0.030(2) 0.021(2) -0.0035(16) -0.0075(18) 0.0097(19)
C9 0.049(3) 0.036(2) 0.023(2) -0.0082(18) -0.0065(19) 0.005(2)
C10 0.0221(18) 0.0252(19) 0.0259(19) -0.0049(15) 0.0033(15) 0.0007(15)
C11 0.0203(16) 0.027(2) 0.0207(19) -0.0010(15) 0.0009(14) 0.0035(14)
P1 0.0479(6) 0.0479(6) 0.0479(6) 0.0085(5) -0.0085(5) 0.0085(5)
F1 0.131(4) 0.051(2) 0.082(3) 0.0122(19) 0.017(2) -0.001(2)
F2 0.097(3) 0.0453(19) 0.093(3) 0.0126(19) 0.007(2) -0.0013(19)
Fe2 0.0271(4) 0.0271(4) 0.0271(4) 0.000 0.000 0.000
Cl1 0.0336(4) 0.0336(4) 0.0336(4) -0.0013(4) -0.0013(4) -0.0013(4)
P2 0.064(4) 0.060(4) 0.034(3) 0.006(3) 0.000 0.000

_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
Fe1 N1 1.963(3) 7_665 ?
Fe1 N1 1.963(3) . ?
Fe1 N1 1.963(3) 10_656 ?
Fe1 N2 1.974(3) 7_665 ?
Fe1 N2 1.974(3) . ?
Fe1 N2 1.974(3) 10_656 ?
N1 C5 1.346(5) . ?
N1 C6 1.351(5) . ?
N2 C11 1.348(5) . ?
N2 C7 1.360(5) . ?
C1 C2 1.515(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C6 1.365(6) . ?
C2 C3 1.400(7) . ?
C3 C4 1.373(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(6) . ?
C4 H4 0.9500 . ?
C5 C7 1.446(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.394(5) . ?
C8 C9 1.368(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(5) . ?
C10 C10 1.476(8) 4 ?
C11 H11 0.9500 . ?
P1 F1 1.582(4) 6_665 ?
P1 F1 1.582(4) 12_654 ?
P1 F1 1.582(4) . ?
P1 F2 1.586(4) 12_654 ?
P1 F2 1.586(4) . ?
P1 F2 1.586(4) 6_665 ?
Fe2 Cl1 2.1994(17) . ?
Fe2 Cl1 2.1994(17) 4 ?
Fe2 Cl1 2.1994(17) 2_755 ?
Fe2 Cl1 2.1994(17) 3_755 ?
P2 F6 1.553(9) . ?
P2 F4 1.570(8) . ?
P2 F4 1.570(8) 4_565 ?
P2 F5 1.572(8) 4_565 ?
P2 F5 1.572(8) . ?
P2 F3 1.604(9) . ?
F6 F6 1.10(2) 18_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 96.19(12) 7_665 . ?
N1 Fe1 N1 96.19(12) 7_665 10_656 ?
N1 Fe1 N1 96.19(12) . 10_656 ?
N1 Fe1 N2 81.48(13) 7_665 7_665 ?
N1 Fe1 N2 87.93(13) . 7_665 ?
N1 Fe1 N2 175.47(14) 10_656 7_665 ?
N1 Fe1 N2 175.48(14) 7_665 . ?
N1 Fe1 N2 81.48(13) . . ?
N1 Fe1 N2 87.93(13) 10_656 . ?
N2 Fe1 N2 94.53(12) 7_665 . ?
N1 Fe1 N2 87.93(13) 7_665 10_656 ?
N1 Fe1 N2 175.47(14) . 10_656 ?
N1 Fe1 N2 81.48(13) 10_656 10_656 ?
N2 Fe1 N2 94.53(12) 7_665 10_656 ?
N2 Fe1 N2 94.53(12) . 10_656 ?
C5 N1 C6 118.5(3) . . ?
C5 N1 Fe1 114.8(2) . . ?
C6 N1 Fe1 126.5(3) . . ?
C11 N2 C7 118.7(3) . . ?
C11 N2 Fe1 127.1(3) . . ?
C7 N2 Fe1 114.1(2) . . ?
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 . . ?
C6 C2 C3 117.8(4) . . ?
C6 C2 C1 121.4(4) . . ?
C3 C2 C1 120.8(4) . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C7 114.7(3) . . ?
C4 C5 C7 124.4(4) . . ?
N1 C6 C2 123.7(4) . . ?
N1 C6 H6 118.2 . . ?
C2 C6 H6 118.2 . . ?
N2 C7 C8 120.2(4) . . ?
N2 C7 C5 114.3(3) . . ?
C8 C7 C5 125.4(4) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.5(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 117.9(4) . . ?
C11 C10 C10 120.7(4) . 4 ?
C9 C10 C10 121.4(4) . 4 ?
N2 C11 C10 123.1(3) . . ?
N2 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
F1 P1 F1 90.7(3) 6_665 12_654 ?
F1 P1 F1 90.7(3) 6_665 . ?
F1 P1 F1 90.7(3) 12_654 . ?
F1 P1 F2 88.4(2) 6_665 12_654 ?
F1 P1 F2 179.1(3) 12_654 12_654 ?
F1 P1 F2 89.3(2) . 12_654 ?
F1 P1 F2 89.3(2) 6_665 . ?
F1 P1 F2 88.4(2) 12_654 . ?
F1 P1 F2 179.1(3) . . ?
F2 P1 F2 91.6(2) 12_654 . ?
F1 P1 F2 179.1(3) 6_665 6_665 ?
F1 P1 F2 89.3(2) 12_654 6_665 ?
F1 P1 F2 88.4(2) . 6_665 ?
F2 P1 F2 91.6(2) 12_654 6_665 ?
F2 P1 F2 91.6(2) . 6_665 ?
Cl1 Fe2 Cl1 109.5 . 4 ?
Cl1 Fe2 Cl1 109.5 . 2_755 ?
Cl1 Fe2 Cl1 109.5 4 2_755 ?
Cl1 Fe2 Cl1 109.5 . 3_755 ?
Cl1 Fe2 Cl1 109.5 4 3_755 ?
Cl1 Fe2 Cl1 109.5 2_755 3_755 ?
F6 P2 F4 90.4(6) . . ?
F6 P2 F4 90.4(6) . 4_565 ?
F4 P2 F4 179.2(11) . 4_565 ?
F6 P2 F5 90.5(6) . 4_565 ?
F4 P2 F5 87.0(8) . 4_565 ?
F4 P2 F5 92.9(8) 4_565 4_565 ?
F6 P2 F5 90.5(6) . . ?
F4 P2 F5 92.9(8) . . ?
F4 P2 F5 87.0(8) 4_565 . ?
F5 P2 F5 179.1(11) 4_565 . ?
F6 P2 F3 180.0 . . ?
F4 P2 F3 89.6(6) . . ?
F4 P2 F3 89.6(6) 4_565 . ?
F5 P2 F3 89.5(6) 4_565 . ?
F5 P2 F3 89.5(6) . . ?
F6 F6 P2 180.0 18_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Fe1 N1 C5 169.1(3) 7_665 . . . ?
N1 Fe1 N1 C5 -94.0(3) 10_656 . . . ?
N2 Fe1 N1 C5 87.9(3) 7_665 . . . ?
N2 Fe1 N1 C5 -7.0(3) . . . . ?
N1 Fe1 N1 C6 -5.7(3) 7_665 . . . ?
N1 Fe1 N1 C6 91.3(3) 10_656 . . . ?
N2 Fe1 N1 C6 -86.9(3) 7_665 . . . ?
N2 Fe1 N1 C6 178.3(3) . . . . ?
N1 Fe1 N2 C11 -171.5(3) . . . . ?
N1 Fe1 N2 C11 -74.9(3) 10_656 . . . ?
N2 Fe1 N2 C11 101.3(2) 7_665 . . . ?
N2 Fe1 N2 C11 6.4(3) 10_656 . . . ?
N1 Fe1 N2 C7 6.1(3) . . . . ?
N1 Fe1 N2 C7 102.6(3) 10_656 . . . ?
N2 Fe1 N2 C7 -81.2(3) 7_665 . . . ?
N2 Fe1 N2 C7 -176.1(3) 10_656 . . . ?
C6 C2 C3 C4 0.5(8) . . . . ?
C1 C2 C3 C4 -177.7(5) . . . . ?
C2 C3 C4 C5 -0.5(8) . . . . ?
C6 N1 C5 C4 0.2(6) . . . . ?
Fe1 N1 C5 C4 -175.0(4) . . . . ?
C6 N1 C5 C7 -178.1(3) . . . . ?
Fe1 N1 C5 C7 6.7(4) . . . . ?
C3 C4 C5 N1 0.2(7) . . . . ?
C3 C4 C5 C7 178.3(5) . . . . ?
C5 N1 C6 C2 -0.2(6) . . . . ?
Fe1 N1 C6 C2 174.4(3) . . . . ?
C3 C2 C6 N1 -0.2(7) . . . . ?
C1 C2 C6 N1 178.0(5) . . . . ?
C11 N2 C7 C8 -5.0(6) . . . . ?
Fe1 N2 C7 C8 177.2(3) . . . . ?
C11 N2 C7 C5 173.6(3) . . . . ?
Fe1 N2 C7 C5 -4.2(4) . . . . ?
N1 C5 C7 N2 -1.6(5) . . . . ?
C4 C5 C7 N2 -179.9(4) . . . . ?
N1 C5 C7 C8 176.9(4) . . . . ?
C4 C5 C7 C8 -1.4(7) . . . . ?
N2 C7 C8 C9 2.2(7) . . . . ?
C5 C7 C8 C9 -176.2(4) . . . . ?
C7 C8 C9 C10 2.9(7) . . . . ?
C8 C9 C10 C11 -4.9(6) . . . . ?
C8 C9 C10 C10 173.8(4) . . . 4 ?
C7 N2 C11 C10 2.9(5) . . . . ?
Fe1 N2 C11 C10 -179.7(3) . . . . ?
C9 C10 C11 N2 2.1(5) . . . . ?
C10 C10 C11 N2 -176.6(3) 4 . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.119