# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_address     
;
Dr Stephen Moggach
RSE Personal Research Fellow
The University of Edinburgh
Joseph Black Building
West Mains Road
Edinburgh
EH9 3JJ
;
_publ_contact_author_email       mark.murrie@glasgow.ac.uk

_publ_contact_author_phone       '+44(0)131 6504806'

#looking for refcif

_publ_contact_author_name        'Mark Murrie'
_publ_author_name                M.Murrie

data_ST1022
_database_code_depnum_ccdc_archive 'CCDC 826248'
#TrackingRef '- Fe12_MMcorrect.cif'

_audit_creation_date             11-05-11
_audit_creation_method           CRYSTALS_ver_14.21

_oxford_structure_analysis_title 'ST1022_0m in F-43c'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_publ_section_exptl_refinement   
;
601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 13005.00 A**3

The structure contains very large solvent containing voids. The electron
density in the voids was very diffuse and could not be modelled reliably (see
SQUEEZE output below)

F(000), M, mu, D and the formulae have been re-calculated to give a better
estimate of the cell contents.

220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.87 Ratio
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.53 Ratio
220_ALERT_2_G Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.63 Ratio
242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C44

These are all due to an acetyl ligand on the periphery
of the complex. The principle axes of its thermal elipsoids are reasonable.
Min Med Max Uarith Ugeom Uprime
C 4. 0.0230 0.0516 0.2015 0.0920 0.0621 0.4518
O 10. 0.0273 0.0464 0.0799 0.0512 0.0466 0.1354

420_ALERT_2_C D-H Without Acceptor O7 - H71 ... ?

This H-atom was located in a difference map, and is probably H-bonding to
disordered water/EtO in the pore.

034_ALERT_1_G No Flack Parameter Given. Z .GT. Si, NonCentro . ?

The SQUEEZE routine was used to model disordered solvent. Refinement of
the flack parameter is not advised if this is performed.

061_ALERT_4_G Tmax/Tmin Range Test RR' too Large ............. 0.90

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of equivalent data. It is possible that the larger than expected
range of transmission is accounted for by crystal decay or absorption by
the mounting fibre.

232_ALERT_2_G Hirshfeld Test Diff (M-X) Fe1 -- O4 .. 5.55 su

No action taken.

910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) ..... 1
912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 40

#===============================================================================
Resolution & Completeness Statistics (Cumulative)
#===============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#-------------------------------------------------------------------------------
20.82 0.500 0.999 1410 1409 1
23.01 0.550 0.999 1870 1869 1
25.24 0.600 1.000 2420 2419 1
#----------------------------------------------------------- ACTA Min. Res. ----
27.51 0.650 1.000 3059 3058 1
28.95 0.681 0.988 3506 3465 41

;

_publ_section_exptl_prep         
# Brief details or a reference. Include solvent if known
;
?
;

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
_platon_squeeze_void_content
1 0.000 0.000 0.000 664 273 ' '
2 0.500 0.000 0.000 664 273 ' '
3 0.237 -0.001 0.167 13723 3505 ' '
4 0.500 0.000 0.500 664 273 ' '
5 0.000 0.000 0.500 664 273 ' '
6 0.000 0.500 0.000 663 273 ' '
7 0.500 0.500 0.000 664 273 ' '
8 0.000 0.500 0.500 664 273 ' '
9 0.500 0.500 0.500 664 273 ' '
_platon_squeeze_details          
;
The total electron count in the pores equates to 5689 electrons per unit cell.
A massive amount. Most of this electron density is completely diffuse,
and there is no evidence (at least crystallographically) for the presence of
Cl- ions. Though clearly there could be disordered anions in the pore.
The presence of chloride is confirmed by a positive test using a solution of
silver nitrate.
;

#end of refcif
_cell_length_a                   39.2647(9)
_cell_length_b                   39.2647(9)
_cell_length_c                   39.2647(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     60535(2)

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'F -4 3 c '
_symmetry_space_group_name_Hall  'F -4c 2 3'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,y+1/2,z+1/2
x+1/2,y,z+1/2
x+1/2,y+1/2,z
y,z,x
y,z+1/2,x+1/2
y+1/2,z,x+1/2
y+1/2,z+1/2,x
z,x,y
z,x+1/2,y+1/2
z+1/2,x,y+1/2
z+1/2,x+1/2,y
y+1/2,-x+1/2,-z+1/2
y+1/2,-x+1,-z+1
y+1,-x+1/2,-z+1
y+1,-x+1,-z+1/2
z+1/2,-y+1/2,-x+1/2
z+1/2,-y+1,-x+1
z+1,-y+1/2,-x+1
z+1,-y+1,-x+1/2
x+1/2,-z+1/2,-y+1/2
x+1/2,-z+1,-y+1
x+1,-z+1/2,-y+1
x+1,-z+1,-y+1/2
-x,-y,z
-x,-y+1/2,z+1/2
-x+1/2,-y,z+1/2
-x+1/2,-y+1/2,z
-z,x,-y
-z,x+1/2,-y+1/2
-z+1/2,x,-y+1/2
-z+1/2,x+1/2,-y
-x,y,-z
-x,y+1/2,-z+1/2
-x+1/2,y,-z+1/2
-x+1/2,y+1/2,-z
-y,-z,x
-y,-z+1/2,x+1/2
-y+1/2,-z,x+1/2
-y+1/2,-z+1/2,x
-z,-x,y
-z,-x+1/2,y+1/2
-z+1/2,-x,y+1/2
-z+1/2,-x+1/2,y
-y+1/2,x+1/2,-z+1/2
-y+1/2,x+1,-z+1
-y+1,x+1/2,-z+1
-y+1,x+1,-z+1/2
-z+1/2,y+1/2,-x+1/2
-z+1/2,y+1,-x+1
-z+1,y+1/2,-x+1
-z+1,y+1,-x+1/2
-x+1/2,z+1/2,-y+1/2
-x+1/2,z+1,-y+1
-x+1,z+1/2,-y+1
-x+1,z+1,-y+1/2
-y,z,-x
-y,z+1/2,-x+1/2
-y+1/2,z,-x+1/2
-y+1/2,z+1/2,-x
z+1/2,y+1/2,x+1/2
z+1/2,y+1,x+1
z+1,y+1/2,x+1
z+1,y+1,x+1/2
x+1/2,z+1/2,y+1/2
x+1/2,z+1,y+1
x+1,z+1/2,y+1
x+1,z+1,y+1/2
y+1/2,x+1/2,z+1/2
y+1/2,x+1,z+1
y+1,x+1/2,z+1
y+1,x+1,z+1/2
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+1/2,-x+1/2,z+1/2
-y+1/2,-x+1,z+1
-y+1,-x+1/2,z+1
-y+1,-x+1,z+1/2
-z+1/2,-y+1/2,x+1/2
-z+1/2,-y+1,x+1
-z+1,-y+1/2,x+1
-z+1,-y+1,x+1/2
-x+1/2,-z+1/2,y+1/2
-x+1/2,-z+1,y+1
-x+1,-z+1/2,y+1
-x+1,-z+1,y+1/2
x,-y,-z
x,-y+1/2,-z+1/2
x+1/2,-y,-z+1/2
x+1/2,-y+1/2,-z
z,-x,-y
z,-x+1/2,-y+1/2
z+1/2,-x,-y+1/2
z+1/2,-x+1/2,-y

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            24

# Given Formula = C74.67 H53.33 Cl0.42 Fe16 N10.67 O40
# Dc = 1.74 Fooo = 26736.00 Mu = 23.20 M = 662.07
# Found Formula = C56 H106 Fe12 N8 O38
# Dc = 1.43 FOOO = 26736.00 Mu = 17.44 M = 542.41

_chemical_formula_sum            'C56 H106 Fe12 N8 O38 Cl2'
_chemical_formula_moiety         '[Fe12O4(OH)2(L)4(OAc)8][Cl]2'
_chemical_compound_source        ?
_chemical_formula_weight         2240.51

_cell_measurement_reflns_used    9860
_cell_measurement_theta_min      2
_cell_measurement_theta_max      28
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.240

_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             27936
_exptl_absorpt_coefficient_mu    1.800

# Sheldrick geometric approximatio 0.71 0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.71
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            169895
_reflns_number_total             6568
_diffrn_reflns_av_R_equivalents  0.070
# Number of reflections without Friedels Law is 6568
# Number of reflections with Friedels Law is 2733
# Theoretical number of reflections is about 3337

_diffrn_reflns_theta_min         1.467
_diffrn_reflns_theta_max         28.948
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        28.369
_diffrn_measured_fraction_theta_full 0.996

_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_limit_l_max       53
_reflns_limit_h_min              -30
_reflns_limit_h_max              30
_reflns_limit_k_min              0
_reflns_limit_k_max              36
_reflns_limit_l_min              2
_reflns_limit_l_max              53

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.62
_refine_diff_density_max         0.51

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6568
_refine_ls_number_restraints     4
_refine_ls_number_parameters     260
_oxford_refine_ls_R_factor_ref   0.0334
_refine_ls_wR_factor_ref         0.0741
_refine_ls_goodness_of_fit_ref   0.8240
_refine_ls_shift/su_max          0.0005169
_refine_ls_shift/su_mean         0.0000358

# The values computed from all data
_oxford_reflns_number_all        6568
_refine_ls_R_factor_all          0.0334
_refine_ls_wR_factor_all         0.0741

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                5795
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_gt          0.0614

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration unk

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.53 1.92 0.481
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.

Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.

Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.086116(9) 0.222171(9) 0.035549(9) 0.0195 1.0000 Uani . . . . . .
Fe2 Fe 0.083710(10) 0.225567(10) -0.048448(10) 0.0226 1.0000 Uani . . . . . .
Fe3 Fe 0.005195(9) 0.218123(8) 0.045267(9) 0.0181 1.0000 Uani . . . . . .
C2 C 0.14733(8) 0.25898(8) 0.06676(8) 0.0331 1.0000 Uani . . . . . .
C3 C 0.12201(8) 0.25135(9) 0.09519(8) 0.0327 1.0000 Uani . . . . . .
C4 C 0.15797(16) 0.17766(16) -0.09868(12) 0.0920 1.0000 Uani . . . . . .
C14 C 0.12538(6) 0.27733(7) -0.00685(7) 0.0238 1.0000 Uani . . . . . .
C15 C 0.15358(7) 0.25388(8) 0.00524(8) 0.0305 1.0000 Uani . . . . . .
C24 C 0.16386(7) 0.20395(8) 0.04021(9) 0.0325 1.0000 Uani . . . . . .
C25 C 0.14703(8) 0.17841(8) 0.06330(9) 0.0338 1.0000 Uani . . . . . .
C27 C 0.09098(7) 0.16080(8) 0.08209(7) 0.0297 1.0000 Uani . . . . . .
C28 C 0.05346(8) 0.16198(7) 0.07257(8) 0.0264 1.0000 Uani . . . . . .
C32 C 0.10987(8) 0.14962(7) 0.02288(8) 0.0286 1.0000 Uani . . . . . .
C33 C 0.08280(8) 0.16021(7) -0.00289(8) 0.0282 1.0000 Uani . . . . . .
C39 C -0.04584(8) 0.16625(7) 0.07645(7) 0.0280 1.0000 Uani . . . . . .
C42 C -0.04837(9) 0.13082(8) 0.09127(9) 0.0388 1.0000 Uani . . . . . .
C44 C 0.14942(8) 0.19000(9) -0.06365(9) 0.0373 1.0000 Uani . . . . . .
N1 N 0.14321(6) 0.23595(6) 0.03684(6) 0.0266 1.0000 Uani . . . . . .
N2 N 0.11141(6) 0.17299(6) 0.05299(6) 0.0253 1.0000 Uani . . . . . .
O1 O 0.08462(5) 0.19615(4) -0.00741(5) 0.0228 1.0000 Uani . . . . . .
O2 O 0.04804(5) 0.19312(4) 0.05518(5) 0.0221 1.0000 Uani . . . . . .
O3 O 0.08970(5) 0.24502(5) 0.08062(5) 0.0272 1.0000 Uani . . . . . .
O4 O 0.09383(5) 0.25879(5) -0.00733(5) 0.0226 1.0000 Uani . . . . . .
O5 O 0.04188(4) 0.25360(4) 0.03611(5) 0.0195 1.0000 Uani . . . . . .
O6 O -0.01763(5) 0.17526(5) 0.06485(5) 0.0286 1.0000 Uani . . . . . .
O7 O 0.000000(7) 0.19969(6) 0.000000(7) 0.0206 1.0000 Uani S T . . . .
O8 O 0.07207(5) 0.18445(5) -0.07683(5) 0.0298 1.0000 Uani . . . . . .
O9 O 0.13171(5) 0.21799(6) -0.06209(6) 0.0328 1.0000 Uani . . . . . .
O10 O 0.15953(7) 0.17373(7) -0.03913(7) 0.0512 1.0000 Uani . . . . . .
H41 H 0.1703 0.1560 -0.0970 0.1087 1.0000 Uiso R . . . . .
H42 H 0.1371 0.1755 -0.1123 0.1087 1.0000 Uiso R . . . . .
H43 H 0.1726 0.1947 -0.1096 0.1087 1.0000 Uiso R . . . . .
H421 H -0.0651 0.1170 0.0784 0.0482 1.0000 Uiso R . . . . .
H422 H -0.0266 0.1192 0.0891 0.0482 1.0000 Uiso R . . . . .
H423 H -0.0544 0.1326 0.1152 0.0482 1.0000 Uiso R . . . . .
H21 H 0.1707 0.2564 0.0759 0.0382 1.0000 Uiso R . . . . .
H22 H 0.1439 0.2828 0.0592 0.0382 1.0000 Uiso R . . . . .
H31 H 0.1296 0.2309 0.1079 0.0395 1.0000 Uiso R . . . . .
H32 H 0.1204 0.2709 0.1110 0.0395 1.0000 Uiso R . . . . .
H141 H 0.1234 0.2970 0.0088 0.0281 1.0000 Uiso R . . . . .
H142 H 0.1308 0.2856 -0.0301 0.0281 1.0000 Uiso R . . . . .
H151 H 0.1585 0.2369 -0.0127 0.0378 1.0000 Uiso R . . . . .
H152 H 0.1743 0.2675 0.0098 0.0378 1.0000 Uiso R . . . . .
H241 H 0.1864 0.2097 0.0499 0.0395 1.0000 Uiso R . . . . .
H242 H 0.1669 0.1937 0.0174 0.0395 1.0000 Uiso R . . . . .
H251 H 0.1475 0.1870 0.0870 0.0403 1.0000 Uiso R . . . . .
H252 H 0.1594 0.1565 0.0621 0.0403 1.0000 Uiso R . . . . .
H271 H 0.0975 0.1371 0.0877 0.0371 1.0000 Uiso R . . . . .
H272 H 0.0952 0.1756 0.1020 0.0371 1.0000 Uiso R . . . . .
H281 H 0.0392 0.1611 0.0934 0.0311 1.0000 Uiso R . . . . .
H282 H 0.0476 0.1425 0.0576 0.0311 1.0000 Uiso R . . . . .
H321 H 0.1045 0.1264 0.0311 0.0350 1.0000 Uiso R . . . . .
H322 H 0.1324 0.1495 0.0115 0.0350 1.0000 Uiso R . . . . .
H331 H 0.0599 0.1538 0.0056 0.0357 1.0000 Uiso R . . . . .
H332 H 0.0871 0.1487 -0.0249 0.0357 1.0000 Uiso R . . . . .
H71 H 0.0000 0.1783 0.0000 0.0240 1.0000 Uiso RS . . . . .
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 0.01978(16) 0.01784(16) 0.02083(16) 0.00034(13) -0.00097(13) 0.00244(13)
Fe2 0.02275(17) 0.02224(18) 0.02266(17) 0.00030(14) 0.00123(14) 0.00252(14)
Fe3 0.01972(16) 0.01475(15) 0.01988(16) 0.00133(12) 0.00048(13) 0.00074(12)
C2 0.0234(13) 0.0353(16) 0.0405(17) -0.0052(12) -0.0070(12) -0.0006(11)
C3 0.0325(15) 0.0368(16) 0.0289(14) -0.0037(12) -0.0099(11) 0.0026(12)
C4 0.108(5) 0.119(5) 0.049(3) -0.034(3) -0.013(3) 0.081(4)
C14 0.0186(11) 0.0220(12) 0.0308(13) 0.0005(10) -0.0013(10) -0.0034(9)
C15 0.0222(12) 0.0315(14) 0.0377(17) 0.0035(12) 0.0010(11) -0.0024(11)
C24 0.0220(12) 0.0355(15) 0.0400(17) 0.0030(13) -0.0037(11) 0.0075(11)
C25 0.0275(14) 0.0333(15) 0.0407(17) 0.0029(13) -0.0077(12) 0.0060(11)
C27 0.0314(15) 0.0293(14) 0.0283(14) 0.0087(11) -0.0010(11) 0.0070(11)
C28 0.0299(14) 0.0186(12) 0.0307(13) 0.0088(10) 0.0006(10) 0.0047(10)
C32 0.0318(14) 0.0209(13) 0.0330(15) -0.0020(10) -0.0002(11) 0.0052(11)
C33 0.0344(14) 0.0194(12) 0.0308(14) 0.0019(10) 0.0014(11) 0.0028(10)
C39 0.0350(15) 0.0238(13) 0.0251(13) 0.0040(10) -0.0058(11) -0.0061(11)
C42 0.0365(16) 0.0311(15) 0.0487(19) 0.0189(13) -0.0060(14) -0.0060(13)
C44 0.0262(14) 0.0432(18) 0.0424(17) -0.0094(14) 0.0011(13) 0.0072(13)
N1 0.0227(11) 0.0267(11) 0.0303(12) 0.0012(9) -0.0029(9) 0.0042(9)
N2 0.0239(11) 0.0232(11) 0.0289(12) 0.0047(9) -0.0014(9) 0.0069(8)
O1 0.0289(9) 0.0172(8) 0.0224(9) 0.0013(7) 0.0003(7) 0.0034(7)
O2 0.0245(9) 0.0156(8) 0.0261(9) 0.0071(6) -0.0004(7) 0.0038(7)
O3 0.0260(10) 0.0292(10) 0.0263(10) -0.0062(8) -0.0062(8) 0.0053(8)
O4 0.0187(8) 0.0205(8) 0.0285(10) 0.0004(7) -0.0018(7) -0.0007(7)
O5 0.0201(8) 0.0158(7) 0.0227(8) 0.0018(6) -0.0013(6) 0.0001(6)
O6 0.0305(10) 0.0233(9) 0.0321(11) 0.0061(8) 0.0010(8) -0.0035(8)
O7 0.0245(12) 0.0148(10) 0.0224(12) 0.0000 -0.0001(9) 0.0000
O8 0.0289(10) 0.0318(11) 0.0287(11) -0.0056(8) 0.0022(8) 0.0006(8)
O9 0.0255(10) 0.0358(11) 0.0370(11) -0.0016(9) 0.0037(8) 0.0038(8)
O10 0.0556(16) 0.0469(15) 0.0510(16) 0.0047(12) 0.0124(13) 0.0226(12)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.006(0)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N1 . 2.306(2) yes
Fe1 . N2 . 2.277(2) yes
Fe1 . O1 . 1.9731(19) yes
Fe1 . O2 . 2.0322(19) yes
Fe1 . O3 . 1.989(2) yes
Fe1 . O4 . 2.2347(19) yes
Fe1 . O5 . 2.1310(18) yes
Fe2 . O5 19_454 2.0564(18) yes
Fe2 . O3 19_454 1.993(2) yes
Fe2 . O1 . 1.9828(18) yes
Fe2 . O4 . 2.113(2) yes
Fe2 . O8 . 2.014(2) yes
Fe2 . O9 . 1.982(2) yes
Fe3 . O4 83_454 2.1131(18) yes
Fe3 . O5 83_454 1.9699(18) yes
Fe3 . O2 . 1.9862(18) yes
Fe3 . O5 . 2.0359(17) yes
Fe3 . O6 . 2.056(2) yes
Fe3 . O7 . 1.9300(10) yes
C2 . C3 . 1.525(5) yes
C2 . N1 . 1.491(4) yes
C2 . H21 . 0.990 no
C2 . H22 . 0.990 no
C3 . O3 . 1.414(3) yes
C3 . H31 . 0.990 no
C3 . H32 . 0.990 no
C4 . C44 . 1.496(5) yes
C4 . H41 . 0.981 no
C4 . H42 . 0.980 no
C4 . H43 . 0.980 no
C14 . C15 . 1.516(4) yes
C14 . O4 . 1.437(3) yes
C14 . H141 . 0.990 no
C14 . H142 . 0.990 no
C15 . N1 . 1.484(4) yes
C15 . H151 . 0.990 no
C15 . H152 . 0.990 no
C24 . C25 . 1.505(5) yes
C24 . N1 . 1.501(4) yes
C24 . H241 . 0.990 no
C24 . H242 . 0.990 no
C25 . N2 . 1.471(4) yes
C25 . H251 . 0.990 no
C25 . H252 . 0.990 no
C27 . C28 . 1.521(4) yes
C27 . N2 . 1.476(4) yes
C27 . H271 . 0.990 no
C27 . H272 . 0.990 no
C28 . O2 . 1.417(3) yes
C28 . H281 . 0.990 no
C28 . H282 . 0.990 no
C32 . C33 . 1.525(4) yes
C32 . N2 . 1.498(4) yes
C32 . H321 . 0.990 no
C32 . H322 . 0.990 no
C33 . O1 . 1.424(3) yes
C33 . H331 . 0.990 no
C33 . H332 . 0.990 no
C39 . O8 33_555 1.254(4) yes
C39 . C42 . 1.511(4) yes
C39 . O6 . 1.249(4) yes
C42 . H421 . 0.992 no
C42 . H422 . 0.972 no
C42 . H423 . 0.972 no
C44 . O9 . 1.302(4) yes
C44 . O10 . 1.222(4) yes
O7 . H71 . 0.840 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Fe1 . N2 . 76.61(9) yes
N1 . Fe1 . O1 . 99.73(9) yes
N2 . Fe1 . O1 . 80.27(8) yes
N1 . Fe1 . O2 . 146.96(8) yes
N2 . Fe1 . O2 . 74.39(8) yes
O1 . Fe1 . O2 . 90.67(8) yes
N1 . Fe1 . O3 . 78.81(9) yes
N2 . Fe1 . O3 . 94.82(9) yes
O1 . Fe1 . O3 . 175.09(8) yes
O2 . Fe1 . O3 . 88.15(8) yes
N1 . Fe1 . O4 . 74.57(8) yes
N2 . Fe1 . O4 . 135.49(8) yes
O1 . Fe1 . O4 . 72.13(7) yes
O2 . Fe1 . O4 . 138.30(7) yes
O3 . Fe1 . O4 . 111.74(8) yes
N1 . Fe1 . O5 . 131.01(8) yes
N2 . Fe1 . O5 . 147.53(8) yes
O1 . Fe1 . O5 . 106.53(8) yes
O2 . Fe1 . O5 . 73.83(7) yes
O3 . Fe1 . O5 . 77.72(7) yes
O4 . Fe1 . O5 . 75.26(7) yes
O5 19_454 Fe2 . O3 19_454 79.41(7) yes
O5 19_454 Fe2 . O1 . 98.40(7) yes
O3 19_454 Fe2 . O1 . 177.54(8) yes
O5 19_454 Fe2 . O4 . 80.19(7) yes
O3 19_454 Fe2 . O4 . 105.94(8) yes
O1 . Fe2 . O4 . 74.66(7) yes
O5 19_454 Fe2 . O8 . 100.48(8) yes
O3 19_454 Fe2 . O8 . 90.06(9) yes
O1 . Fe2 . O8 . 89.24(8) yes
O4 . Fe2 . O8 . 163.75(8) yes
O5 19_454 Fe2 . O9 . 163.33(8) yes
O3 19_454 Fe2 . O9 . 85.71(9) yes
O1 . Fe2 . O9 . 96.60(9) yes
O4 . Fe2 . O9 . 96.91(8) yes
O8 . Fe2 . O9 . 86.90(9) yes
O4 83_454 Fe3 . O5 83_454 81.48(7) yes
O4 83_454 Fe3 . O2 . 90.09(8) yes
O5 83_454 Fe3 . O2 . 171.52(8) yes
O4 83_454 Fe3 . O5 . 80.67(7) yes
O5 83_454 Fe3 . O5 . 100.65(6) yes
O2 . Fe3 . O5 . 76.91(7) yes
O4 83_454 Fe3 . O6 . 91.77(8) yes
O5 83_454 Fe3 . O6 . 97.34(8) yes
O2 . Fe3 . O6 . 83.76(8) yes
O5 . Fe3 . O6 . 159.17(8) yes
O4 83_454 Fe3 . O7 . 175.00(7) yes
O5 83_454 Fe3 . O7 . 93.56(7) yes
O2 . Fe3 . O7 . 94.85(7) yes
O5 . Fe3 . O7 . 99.72(7) yes
O6 . Fe3 . O7 . 89.51(9) yes
C3 . C2 . N1 . 112.8(2) yes
C3 . C2 . H21 . 108.6 no
N1 . C2 . H21 . 108.9 no
C3 . C2 . H22 . 108.4 no
N1 . C2 . H22 . 108.7 no
H21 . C2 . H22 . 109.5 no
C2 . C3 . O3 . 108.9(2) yes
C2 . C3 . H31 . 109.3 no
O3 . C3 . H31 . 109.4 no
C2 . C3 . H32 . 110.4 no
O3 . C3 . H32 . 109.4 no
H31 . C3 . H32 . 109.5 no
C44 . C4 . H41 . 109.2 no
C44 . C4 . H42 . 109.9 no
H41 . C4 . H42 . 112.0 no
C44 . C4 . H43 . 108.2 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 108.0 no
C15 . C14 . O4 . 109.0(2) yes
C15 . C14 . H141 . 109.7 no
O4 . C14 . H141 . 109.6 no
C15 . C14 . H142 . 109.3 no
O4 . C14 . H142 . 109.8 no
H141 . C14 . H142 . 109.5 no
C14 . C15 . N1 . 110.5(2) yes
C14 . C15 . H151 . 109.2 no
N1 . C15 . H151 . 109.2 no
C14 . C15 . H152 . 109.2 no
N1 . C15 . H152 . 109.4 no
H151 . C15 . H152 . 109.5 no
C25 . C24 . N1 . 111.9(2) yes
C25 . C24 . H241 . 108.3 no
N1 . C24 . H241 . 109.1 no
C25 . C24 . H242 . 109.0 no
N1 . C24 . H242 . 109.0 no
H241 . C24 . H242 . 109.5 no
C24 . C25 . N2 . 110.4(2) yes
C24 . C25 . H251 . 109.3 no
N2 . C25 . H251 . 109.0 no
C24 . C25 . H252 . 109.6 no
N2 . C25 . H252 . 109.2 no
H251 . C25 . H252 . 109.5 no
C28 . C27 . N2 . 109.0(2) yes
C28 . C27 . H271 . 109.6 no
N2 . C27 . H271 . 109.7 no
C28 . C27 . H272 . 109.7 no
N2 . C27 . H272 . 109.4 no
H271 . C27 . H272 . 109.5 no
C27 . C28 . O2 . 106.9(2) yes
C27 . C28 . H281 . 110.1 no
O2 . C28 . H281 . 110.0 no
C27 . C28 . H282 . 110.2 no
O2 . C28 . H282 . 110.2 no
H281 . C28 . H282 . 109.5 no
C33 . C32 . N2 . 112.6(2) yes
C33 . C32 . H321 . 108.5 no
N2 . C32 . H321 . 108.5 no
C33 . C32 . H322 . 108.9 no
N2 . C32 . H322 . 108.8 no
H321 . C32 . H322 . 109.5 no
C32 . C33 . O1 . 108.5(2) yes
C32 . C33 . H331 . 109.8 no
O1 . C33 . H331 . 109.9 no
C32 . C33 . H332 . 109.6 no
O1 . C33 . H332 . 109.5 no
H331 . C33 . H332 . 109.5 no
O8 33_555 C39 . C42 . 117.8(3) yes
O8 33_555 C39 . O6 . 124.9(3) yes
C42 . C39 . O6 . 117.3(3) yes
C39 . C42 . H421 . 110.5 no
C39 . C42 . H422 . 110.0 no
H421 . C42 . H422 . 106.2 no
C39 . C42 . H423 . 108.7 no
H421 . C42 . H423 . 112.0 no
H422 . C42 . H423 . 109.4 no
C4 . C44 . O9 . 115.9(3) yes
C4 . C44 . O10 . 118.8(3) yes
O9 . C44 . O10 . 125.3(3) yes
C24 . N1 . C2 . 112.3(2) yes
C24 . N1 . C15 . 108.8(2) yes
C2 . N1 . C15 . 109.9(2) yes
C24 . N1 . Fe1 . 109.31(18) yes
C2 . N1 . Fe1 . 105.37(17) yes
C15 . N1 . Fe1 . 111.09(17) yes
C32 . N2 . C27 . 113.0(2) yes
C32 . N2 . C25 . 110.1(2) yes
C27 . N2 . C25 . 110.5(2) yes
C32 . N2 . Fe1 . 105.35(16) yes
C27 . N2 . Fe1 . 105.72(16) yes
C25 . N2 . Fe1 . 112.01(18) yes
C33 . O1 . Fe2 . 132.66(17) yes
C33 . O1 . Fe1 . 114.08(16) yes
Fe2 . O1 . Fe1 . 113.18(9) yes
C28 . O2 . Fe1 . 123.83(16) yes
C28 . O2 . Fe3 . 130.42(17) yes
Fe1 . O2 . Fe3 . 105.75(8) yes
C3 . O3 . Fe2 83_454 127.06(18) yes
C3 . O3 . Fe1 . 120.20(18) yes
Fe2 83_454 O3 . Fe1 . 104.95(9) yes
Fe1 . O4 . Fe2 . 98.79(7) yes
Fe1 . O4 . Fe3 19_454 97.11(7) yes
Fe2 . O4 . Fe3 19_454 97.20(8) yes
Fe1 . O4 . C14 . 115.66(15) yes
Fe2 . O4 . C14 . 118.99(16) yes
Fe3 19_454 O4 . C14 . 124.07(15) yes
Fe1 . O5 . Fe2 83_454 97.90(7) yes
Fe1 . O5 . Fe3 . 100.49(7) yes
Fe2 83_454 O5 . Fe3 . 101.56(8) yes
Fe1 . O5 . Fe3 19_454 105.24(8) yes
Fe2 83_454 O5 . Fe3 19_454 121.04(8) yes
Fe3 . O5 . Fe3 19_454 125.37(9) yes
Fe3 . O6 . C39 . 139.0(2) yes
Fe3 33_555 O7 . Fe3 . 135.95(13) yes
Fe3 33_555 O7 . H71 . 112.0 no
Fe3 . O7 . H71 . 112.0 no
Fe2 . O8 . C39 33_555 129.56(18) yes
Fe2 . O9 . C44 . 130.3(2) yes

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 11/05/11 at 10:40:11
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S)
RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S)
RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE O ( 7,X'S) H ( 71,X'S)
END
;

_iucr_refine_instruction_details_restraints 
;
#
# Punched on 11/05/11 at 10:40:11
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;