# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Annie K. Powell'
_publ_contact_author_address     
;
Inst fuer Anorganische Chemie
Universitaet Karlsruhe
Engesserstrasse Geb. 30.45
Karlsruhe
D76128
GERMANY
;

_publ_contact_author_email       powell@chemie.uni-karlsruhe.de
_publ_contact_author_phone       '+44 721 608 2135'

_publ_section_title              
;
Encapsulation of [Fe(H2O)6]3+ by dinuclear
{Fe2(hpdta)} units leads to  a nonanuclear S = 13/2 Fe(III) oxo cluster
showing magnetic hysteresis
;

loop_
_publ_author_name
_publ_author_address

'Wolfgang Schmitt'
;
Institut fur Anorganische Chemie
Universitat Karlsruhe
Engesserstr. Geb. 30.45
D-76128 Karlsruhe
Germany
;
'Christopher E. Anson'
;
Institut fur Anorganische Chemie
Universitat Karlsruhe
Engesserstr. Geb. 30.45
D-76128 Karlsruhe
Germany
;
'Wolfgang Wernsdorfer'
;
Laboratoire Louis Neel
CNRS
B.P. 166
38042 Grenoble Cedex 9
France
;
'Annie K. Powell'
;
Institut fur Anorganische Chemie
Universitat Karlsruhe
Engesserstr. Geb. 30.45
D-76128 Karlsruhe
Germany
;

data_fe9ka
_database_code_depnum_ccdc_archive 'CCDC 255071'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H86 Fe9 K5 N8 O54'
_chemical_formula_weight         2349.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   12.9507(15)
_cell_length_b                   13.7625(17)
_cell_length_c                   13.7737(16)
_cell_angle_alpha                105.880(9)
_cell_angle_beta                 113.106(9)
_cell_angle_gamma                102.777(9)
_cell_volume                     2016.5(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    8385
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      25.76

_exptl_crystal_description       cuboid
_exptl_crystal_colour            orange-brown
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1197
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15893
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.20
_reflns_number_total             8248
_reflns_number_gt                6151
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.05 (Stoe & Cie GmbH, 2000)'
_computing_cell_refinement       'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_data_reduction        'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'

_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.
The Fe9 aggregate is mostly ordered (the exception being the carboxylate
group containing O(8) and O(9) and the hydrogen on the hydroxo ligand O(4))
but the K^+^ cations and solvent molecules are two-fold disordered, with
two superimposed assemblages (one containing three K^+^, the other two
K^+^) that were each assigned 50% occupancy in order to achieve overall
charge neutrality. Within each assemblage the geometries were unexceptional
and the slight disorder within the Fe9 aggregate was correlated to this
cation disorder. In particular, O(4) is coordinated to a K^+^ in each
assemblage, and the disorder of its hydroxo hydrogen reflects this.
All hydroxo hydrogens (including the disordered H(4)) could be located
from difference maps and their positions refined with restrained O-H bond
distances; all H atoms of the hpdta ligands were placed in calculated
positions. No attempt was made to position the H atoms of the disordered
MeOH and water molecules. Some of the disordered half solvent molecules
could be refined anisotropically; in some cases the thermal ellipsoids
indicated that further disorder was present, but attempts to further
divide and refine them (as quarter occupancy atoms) did not converge
well.
The K+ cations and solvent molecules are disordered, and were refined as
two superimposed assemblages (each with half occupancy) with appropriate
geometries, one conatining two, the other three K^+^. Very weak reflections
corresponding to a doubling of the unit cell along c could be observed,
giving a conventional cell with a =13.7809(12), b = 13.7959(16),
c = 22.545(2) Å, alpha = 89.598(9)º,  beta = 79.108(8)º,  gamma =
74.041(8)º. This superstructure appears to correspond an ordering of
the two cation assemblages between the Fe9 aggregates, but attempted
refinement indicated that this ordering was in any case not complete,
and correlation between what are now two “independent” Fe9 aggregates
became excessively high. We therefore prefer the refinement in the
smaller cell with fully disordered cations presented here, which
nonetheless gives quite respectable R-factors.
;

_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^)+(0.1105P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8248
_refine_ls_number_parameters     672
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1645
_refine_ls_wR_factor_gt          0.1509
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 0.5000 0.5000 0.5000 0.0216(2) Uani 1 2 d S . .
Fe2 Fe 0.53944(6) 0.35150(6) 0.61731(5) 0.02186(16) Uani 1 1 d . D .
Fe3 Fe 0.78961(5) 0.58384(5) 0.73245(5) 0.02202(16) Uani 1 1 d . . .
Fe4 Fe 0.72530(6) 0.76785(5) 0.59088(5) 0.02180(16) Uani 1 1 d . . .
Fe5 Fe 0.70177(6) 0.36918(6) 0.47372(6) 0.02822(18) Uani 1 1 d . . .
O1 O 0.6242(3) 0.5005(3) 0.6452(3) 0.0226(6) Uani 1 1 d . D .
O2 O 0.4114(3) 0.3562(3) 0.4851(3) 0.0284(7) Uani 1 1 d . . .
O3 O 0.8234(3) 0.5015(3) 0.6118(3) 0.0299(8) Uani 1 1 d D . .
H3 H 0.878(5) 0.534(5) 0.604(5) 0.036 Uiso 1 1 d D . .
O4 O 0.5829(3) 0.4310(3) 0.4127(3) 0.0290(7) Uani 1 1 d D . .
H4A H 0.535(10) 0.402(10) 0.339(4) 0.035 Uiso 0.50 1 d PD A 1
H4B H 0.601(11) 0.471(9) 0.375(10) 0.035 Uiso 0.50 1 d PD B 2
O5 O 0.6522(3) 0.3072(3) 0.5689(3) 0.0266(7) Uani 1 1 d . D .
C1 C 0.6940(5) 0.2250(4) 0.5948(5) 0.0345(11) Uani 1 1 d . . .
H1 H 0.6366 0.1527 0.5357 0.041 Uiso 1 1 calc R . .
C2 C 0.7084(5) 0.2342(5) 0.7140(5) 0.0373(12) Uani 1 1 d . . .
H2A H 0.7156 0.1686 0.7244 0.045 Uiso 1 1 calc R . .
H2B H 0.7815 0.2953 0.7740 0.045 Uiso 1 1 calc R . .
N1 N 0.6039(4) 0.2494(4) 0.7232(4) 0.0330(10) Uani 1 1 d . . .
C3 C 0.5039(6) 0.1458(6) 0.6795(6) 0.0519(18) Uani 1 1 d . . .
H3A H 0.4685 0.1523 0.7302 0.062 Uiso 1 1 calc R . .
H3B H 0.5365 0.0890 0.6823 0.062 Uiso 1 1 calc R . .
C4 C 0.4055(5) 0.1118(4) 0.5579(5) 0.0314(11) Uani 1 1 d . . .
O6 O 0.4036(3) 0.1902(3) 0.5244(3) 0.0289(7) Uani 1 1 d . . .
O7 O 0.3333(4) 0.0181(4) 0.5024(4) 0.0546(13) Uani 1 1 d . . .
C5 C 0.6347(8) 0.3196(7) 0.8411(6) 0.061(2) Uani 1 1 d . D .
H51A H 0.6189 0.2730 0.8793 0.074 Uiso 0.50 1 calc PR C 1
H52A H 0.7208 0.3622 0.8832 0.074 Uiso 0.50 1 calc PR C 1
H51B H 0.7095 0.3816 0.8766 0.074 Uiso 0.50 1 d PR C 2
H52B H 0.6421 0.2791 0.8896 0.074 Uiso 0.50 1 d PR C 2
C6A C 0.5749(14) 0.3896(12) 0.8495(12) 0.038(3) Uani 0.50 1 d PU D 1
C6B C 0.5200(14) 0.3581(14) 0.8190(11) 0.039(3) Uani 0.50 1 d PU D 2
O8 O 0.4986(4) 0.3935(4) 0.7441(4) 0.0398(9) Uani 1 1 d . . .
O9A O 0.5745(11) 0.4354(11) 0.9395(8) 0.060(3) Uani 0.50 1 d PU D 1
O9B O 0.4777(11) 0.3729(13) 0.8857(9) 0.072(4) Uani 0.50 1 d PU . 2
C7 C 0.8169(5) 0.2465(5) 0.5996(6) 0.0427(14) Uani 1 1 d . . .
H7A H 0.8772 0.3104 0.6684 0.051 Uiso 1 1 calc R . .
H7B H 0.8409 0.1850 0.6028 0.051 Uiso 1 1 calc R . .
N2 N 0.8098(4) 0.2637(4) 0.4975(5) 0.0444(13) Uani 1 1 d . . .
C8 C 0.9258(6) 0.3288(5) 0.5102(7) 0.0544(19) Uani 1 1 d . . .
H8A H 0.9698 0.2825 0.4971 0.065 Uiso 1 1 calc R . .
H8B H 0.9755 0.3852 0.5876 0.065 Uiso 1 1 calc R . .
C9 C 0.8977(6) 0.3799(5) 0.4222(7) 0.055(2) Uani 1 1 d . . .
O10 O 0.8015(4) 0.4007(4) 0.3940(4) 0.0463(11) Uani 1 1 d . . .
O11 O 0.9675(5) 0.3984(5) 0.3821(5) 0.078(2) Uani 1 1 d . . .
C10 C 0.7478(7) 0.1594(5) 0.3933(7) 0.057(2) Uani 1 1 d . . .
H10A H 0.7352 0.0991 0.4165 0.068 Uiso 1 1 calc R . .
H10B H 0.7995 0.1532 0.3585 0.068 Uiso 1 1 calc R . .
C11 C 0.6270(7) 0.1511(5) 0.3046(6) 0.055(2) Uani 1 1 d . . .
O12 O 0.5893(4) 0.2270(4) 0.3275(4) 0.0472(11) Uani 1 1 d . . .
O13 O 0.5683(6) 0.0666(5) 0.2125(5) 0.082(2) Uani 1 1 d . . .
O14 O 0.8339(3) 0.7195(3) 0.6981(3) 0.0246(7) Uani 1 1 d . . .
C12 C 0.9415(4) 0.8098(4) 0.7878(4) 0.0284(10) Uani 1 1 d . . .
H12 H 0.9246 0.8511 0.8462 0.034 Uiso 1 1 calc R . .
C13 C 1.0372(4) 0.7666(4) 0.8419(5) 0.0315(11) Uani 1 1 d . . .
H13A H 1.0627 0.7351 0.7874 0.038 Uiso 1 1 calc R . .
H13B H 1.1071 0.8251 0.9095 0.038 Uiso 1 1 calc R . .
N3 N 0.9837(4) 0.6833(4) 0.8743(3) 0.0291(9) Uani 1 1 d . . .
C14 C 1.0419(5) 0.6042(5) 0.8817(5) 0.0377(13) Uani 1 1 d . . .
H14A H 1.1116 0.6320 0.9576 0.045 Uiso 1 1 calc R . .
H14B H 1.0696 0.5919 0.8250 0.045 Uiso 1 1 calc R . .
C15 C 0.9525(5) 0.4978(5) 0.8598(4) 0.0355(12) Uani 1 1 d . . .
O15 O 0.8416(3) 0.4891(3) 0.8201(3) 0.0355(9) Uani 1 1 d . . .
O16 O 0.9894(4) 0.4255(4) 0.8780(4) 0.0457(10) Uani 1 1 d . . .
C16 C 0.9772(5) 0.7315(5) 0.9807(4) 0.0350(12) Uani 1 1 d . . .
H16A H 1.0398 0.8037 1.0269 0.042 Uiso 1 1 calc R . .
H16B H 0.9934 0.6876 1.0250 0.042 Uiso 1 1 calc R . .
C17 C 0.8561(5) 0.7400(5) 0.9577(5) 0.0384(13) Uani 1 1 d . . .
O17 O 0.7656(3) 0.6770(3) 0.8595(3) 0.0344(8) Uani 1 1 d . . .
O18 O 0.8472(4) 0.8042(4) 1.0348(4) 0.0578(14) Uani 1 1 d . . .
C18 C 0.9868(4) 0.8825(5) 0.7367(5) 0.0335(11) Uani 1 1 d . . .
H18A H 1.0555 0.9466 0.7983 0.040 Uiso 1 1 calc R . .
H18B H 1.0136 0.8439 0.6870 0.040 Uiso 1 1 calc R . .
N4 N 0.8902(4) 0.9166(4) 0.6687(4) 0.0301(9) Uani 1 1 d . . .
C19 C 0.8769(5) 1.0070(4) 0.7414(5) 0.0397(13) Uani 1 1 d . . .
H19A H 0.8512 1.0510 0.6995 0.048 Uiso 1 1 calc R . .
H19B H 0.9545 1.0525 0.8094 0.048 Uiso 1 1 calc R . .
C20 C 0.7844(6) 0.9660(5) 0.7783(5) 0.0437(14) Uani 1 1 d . . .
O19 O 0.7125(3) 0.8656(3) 0.7210(3) 0.0340(8) Uani 1 1 d . . .
O20 O 0.7810(5) 1.0302(5) 0.8585(5) 0.0745(19) Uani 1 1 d . . .
C21 C 0.9090(5) 0.9350(5) 0.5756(5) 0.0398(13) Uani 1 1 d . . .
H21A H 0.9947 0.9708 0.6035 0.048 Uiso 1 1 calc R . .
H21B H 0.8682 0.9819 0.5509 0.048 Uiso 1 1 calc R . .
C22 C 0.8598(5) 0.8273(5) 0.4749(5) 0.0390(13) Uani 1 1 d . . .
O21 O 0.7897(3) 0.7454(3) 0.4760(3) 0.0365(9) Uani 1 1 d . . .
O22 O 0.8873(6) 0.8229(5) 0.3982(5) 0.0703(16) Uani 1 1 d . . .
K1 K 0.6977(5) 0.5400(5) 0.2925(4) 0.0464(10) Uani 0.50 1 d P . 1
K2 K 0.7447(3) 0.7616(3) 0.1610(3) 0.0567(8) Uani 0.50 1 d P . 1
K3 K 0.6358(2) 0.8492(3) -0.1089(2) 0.0532(8) Uani 0.50 1 d P . 1
O31 O 0.7930(11) 0.5714(11) 0.1406(12) 0.073(3) Uani 0.50 1 d P . 1
C31 C 0.7781(13) 0.5522(15) 0.0276(14) 0.061(4) Uani 0.50 1 d P . 1
O32 O 0.6898(12) 0.9491(14) 0.1353(12) 0.091(5) Uani 0.50 1 d P . 1
O33 O 0.585(5) 0.319(3) 0.127(3) 0.26(3) Uani 0.50 1 d P . 1
O34 O 0.3546(16) -0.1265(18) 0.032(2) 0.175(12) Uani 0.50 1 d P E 1
C34 C 0.367(5) -0.195(4) -0.051(6) 0.24(3) Uani 0.50 1 d P E 1
K4 K 0.3778(4) 0.4851(6) 0.8835(4) 0.0968(17) Uani 0.50 1 d P . 2
K5 K 0.5924(3) 0.7428(3) 0.7911(3) 0.0532(7) Uani 0.50 1 d P . 2
O41 O 0.3279(16) 0.3379(16) 0.9469(15) 0.108(5) Uani 0.50 1 d P . 2
O42 O 0.2715(15) 0.4537(14) 0.6654(11) 0.042(3) Uani 0.50 1 d P F 2
O43 O 0.6376(11) 0.9628(13) 0.9322(10) 0.078(4) Uani 0.50 1 d P G 2
C44 C 0.309(5) 0.653(5) 0.858(4) 0.23(3) Uani 0.50 1 d P H 2
O45 O 0.531(3) 0.6350(15) 0.868(3) 0.195(17) Uani 0.50 1 d P I 2
C45 C 0.522(6) 0.688(9) 0.918(7) 0.37(7) Uani 0.50 1 d P I 2
O46 O 0.149(4) 0.371(6) 0.778(4) 0.40(4) Uani 0.50 1 d P J 2
O47 O 0.6289(19) 0.9004(17) 1.1020(17) 0.104(6) Uiso 0.50 1 d P K 2
C47 C 0.709(7) 0.807(7) 1.208(6) 0.29(3) Uiso 0.50 1 d P L 2

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 0.0178(4) 0.0190(5) 0.0268(4) 0.0117(4) 0.0095(3) 0.0042(3)
Fe2 0.0204(3) 0.0213(3) 0.0259(3) 0.0117(3) 0.0118(2) 0.0071(2)
Fe3 0.0193(3) 0.0193(3) 0.0238(3) 0.0084(2) 0.0085(2) 0.0048(2)
Fe4 0.0194(3) 0.0170(3) 0.0258(3) 0.0081(2) 0.0099(2) 0.0036(2)
Fe5 0.0266(3) 0.0222(4) 0.0367(4) 0.0069(3) 0.0214(3) 0.0051(3)
O1 0.0202(14) 0.0203(16) 0.0240(15) 0.0094(12) 0.0083(12) 0.0058(12)
O2 0.0198(15) 0.0250(18) 0.0344(17) 0.0169(14) 0.0078(13) 0.0020(13)
O3 0.0229(16) 0.0245(18) 0.0420(19) 0.0090(15) 0.0214(15) 0.0032(14)
O4 0.0285(17) 0.0293(19) 0.0282(16) 0.0116(14) 0.0149(14) 0.0066(14)
O5 0.0276(16) 0.0195(17) 0.0378(18) 0.0120(14) 0.0189(14) 0.0107(13)
C1 0.029(2) 0.022(3) 0.055(3) 0.013(2) 0.023(2) 0.013(2)
C2 0.033(3) 0.033(3) 0.048(3) 0.024(2) 0.015(2) 0.014(2)
N1 0.029(2) 0.034(3) 0.035(2) 0.0188(19) 0.0117(18) 0.0115(18)
C3 0.038(3) 0.054(4) 0.059(4) 0.040(3) 0.016(3) 0.003(3)
C4 0.033(2) 0.023(3) 0.041(3) 0.018(2) 0.017(2) 0.010(2)
O6 0.0293(17) 0.0195(17) 0.0323(17) 0.0125(14) 0.0092(14) 0.0071(14)
O7 0.056(3) 0.024(2) 0.063(3) 0.021(2) 0.012(2) 0.006(2)
C5 0.088(5) 0.075(5) 0.031(3) 0.030(3) 0.024(3) 0.044(5)
C6A 0.029(7) 0.045(8) 0.025(6) 0.010(5) 0.009(6) -0.002(6)
C6B 0.028(7) 0.057(10) 0.019(6) 0.008(6) 0.008(5) 0.010(6)
O8 0.052(2) 0.043(2) 0.047(2) 0.0260(19) 0.036(2) 0.0236(19)
O9A 0.064(7) 0.088(8) 0.032(4) 0.019(5) 0.027(5) 0.036(6)
O9B 0.071(7) 0.136(12) 0.047(6) 0.048(7) 0.044(6) 0.062(8)
C7 0.032(3) 0.035(3) 0.064(4) 0.016(3) 0.027(3) 0.015(2)
N2 0.036(2) 0.025(3) 0.073(4) 0.006(2) 0.037(3) 0.009(2)
C8 0.037(3) 0.031(3) 0.100(6) 0.013(3) 0.049(4) 0.008(3)
C9 0.050(4) 0.029(3) 0.076(4) -0.008(3) 0.053(4) -0.007(3)
O10 0.045(2) 0.041(2) 0.055(2) 0.0084(19) 0.041(2) 0.0023(19)
O11 0.065(3) 0.054(3) 0.104(4) -0.006(3) 0.072(3) -0.007(3)
C10 0.065(4) 0.020(3) 0.093(5) 0.001(3) 0.063(4) 0.010(3)
C11 0.057(4) 0.033(3) 0.065(4) -0.005(3) 0.048(4) -0.003(3)
O12 0.045(2) 0.030(2) 0.050(2) -0.0061(18) 0.029(2) 0.0006(18)
O13 0.092(4) 0.049(3) 0.073(4) -0.017(3) 0.048(3) 0.006(3)
O14 0.0202(15) 0.0179(16) 0.0299(16) 0.0094(13) 0.0091(13) 0.0029(12)
C12 0.023(2) 0.021(2) 0.031(2) 0.0082(19) 0.0091(19) -0.0001(18)
C13 0.021(2) 0.028(3) 0.036(3) 0.014(2) 0.0081(19) 0.0032(19)
N3 0.0251(19) 0.025(2) 0.0271(19) 0.0101(16) 0.0070(16) 0.0037(16)
C14 0.024(2) 0.038(3) 0.043(3) 0.022(2) 0.006(2) 0.011(2)
C15 0.027(2) 0.037(3) 0.030(2) 0.016(2) 0.001(2) 0.011(2)
O15 0.0301(18) 0.031(2) 0.043(2) 0.0222(17) 0.0120(16) 0.0088(15)
O16 0.045(2) 0.037(2) 0.053(2) 0.025(2) 0.0134(19) 0.0205(19)
C16 0.035(3) 0.032(3) 0.023(2) 0.010(2) 0.006(2) 0.003(2)
C17 0.041(3) 0.034(3) 0.030(2) 0.005(2) 0.019(2) 0.002(2)
O17 0.0284(17) 0.035(2) 0.0259(17) 0.0046(15) 0.0112(14) 0.0022(15)
O18 0.051(3) 0.057(3) 0.038(2) -0.008(2) 0.023(2) 0.003(2)
C18 0.018(2) 0.031(3) 0.042(3) 0.017(2) 0.0080(19) 0.0012(19)
N4 0.028(2) 0.025(2) 0.031(2) 0.0113(17) 0.0104(17) 0.0052(17)
C19 0.044(3) 0.015(2) 0.040(3) 0.001(2) 0.012(2) 0.003(2)
C20 0.044(3) 0.030(3) 0.044(3) 0.000(2) 0.019(3) 0.013(3)
O19 0.0322(18) 0.027(2) 0.0344(18) 0.0043(15) 0.0146(15) 0.0086(15)
O20 0.067(3) 0.046(3) 0.074(4) -0.020(3) 0.040(3) 0.004(3)
C21 0.033(3) 0.037(3) 0.051(3) 0.028(3) 0.021(2) 0.000(2)
C22 0.038(3) 0.049(4) 0.049(3) 0.031(3) 0.031(3) 0.018(3)
O21 0.0329(18) 0.037(2) 0.0366(19) 0.0131(16) 0.0192(16) 0.0057(16)
O22 0.100(4) 0.074(4) 0.072(3) 0.037(3) 0.069(4) 0.030(3)
K1 0.051(3) 0.041(2) 0.056(3) 0.019(2) 0.031(2) 0.023(2)
K2 0.0598(18) 0.061(2) 0.0656(19) 0.0306(16) 0.0380(16) 0.0287(15)
K3 0.0322(12) 0.074(2) 0.0373(13) 0.0081(13) 0.0143(10) 0.0138(13)
O31 0.058(7) 0.063(8) 0.075(8) 0.019(6) 0.021(6) 0.015(6)
C31 0.045(7) 0.078(12) 0.065(9) 0.035(8) 0.023(7) 0.030(7)
O32 0.055(7) 0.098(11) 0.083(9) -0.013(8) 0.034(7) 0.025(8)
O33 0.32(5) 0.17(3) 0.18(3) 0.03(2) 0.16(4) -0.09(3)
O34 0.064(10) 0.086(14) 0.23(3) 0.025(15) -0.027(13) 0.002(9)
C34 0.26(6) 0.12(4) 0.46(9) 0.12(5) 0.27(7) 0.11(4)
K4 0.076(3) 0.159(5) 0.060(2) 0.030(3) 0.032(2) 0.068(3)
K5 0.0380(14) 0.0535(19) 0.0527(16) 0.0146(13) 0.0116(12) 0.0184(13)
O41 0.107(12) 0.118(14) 0.108(12) 0.041(10) 0.069(10) 0.032(10)
O42 0.048(8) 0.025(5) 0.043(8) 0.012(7) 0.020(6) 0.004(5)
O43 0.059(7) 0.115(12) 0.059(6) 0.031(7) 0.030(6) 0.034(7)
C44 0.24(5) 0.28(6) 0.21(4) 0.10(4) 0.18(4) 0.01(5)
O45 0.114(17) 0.036(9) 0.31(4) -0.004(14) 0.05(2) 0.010(10)
C45 0.18(5) 0.80(19) 0.33(8) 0.46(12) 0.16(6) 0.15(8)
O46 0.20(4) 0.47(9) 0.21(4) -0.08(5) -0.03(3) 0.09(5)

_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 O2 1.966(3) 2_666 ?
Fe1 O2 1.966(3) . ?
Fe1 O1 2.013(3) . ?
Fe1 O1 2.013(3) 2_666 ?
Fe1 O4 2.083(4) . ?
Fe1 O4 2.083(4) 2_666 ?
Fe1 Fe2 2.9444(7) . ?
Fe1 Fe2 2.9444(7) 2_666 ?
Fe2 O1 1.949(3) . ?
Fe2 O2 1.952(3) . ?
Fe2 O5 1.971(4) . ?
Fe2 O8 1.993(4) . ?
Fe2 O6 2.148(3) . ?
Fe2 N1 2.342(4) . ?
Fe3 O1 1.867(3) . ?
Fe3 O3 2.000(4) . ?
Fe3 O17 2.044(4) . ?
Fe3 O15 2.055(4) . ?
Fe3 O14 2.064(3) . ?
Fe3 N3 2.274(4) . ?
Fe3 K5 3.884(3) . ?
Fe4 O2 1.837(3) 2_666 ?
Fe4 O14 1.981(3) . ?
Fe4 O19 2.015(4) . ?
Fe4 O21 2.044(4) . ?
Fe4 O6 2.119(4) 2_666 ?
Fe4 N4 2.229(4) . ?
Fe5 O4 1.938(4) . ?
Fe5 O5 1.972(3) . ?
Fe5 O3 1.974(4) . ?
Fe5 O10 2.046(4) . ?
Fe5 O12 2.071(4) . ?
O2 Fe4 1.837(3) 2_666 ?
O3 H3 0.81(4) . ?
O4 K5 2.771(5) 2_666 ?
O4 K1 3.083(7) . ?
O4 H4A 0.87(4) . ?
O4 H4B 0.90(4) . ?
O5 C1 1.428(7) . ?
C1 C7 1.524(7) . ?
C1 C2 1.542(8) . ?
C1 H1 0.9800 . ?
C2 N1 1.462(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N1 C3 1.474(7) . ?
N1 C5 1.480(8) . ?
C3 C4 1.510(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O7 1.219(7) . ?
C4 O6 1.286(6) . ?
O6 Fe4 2.119(4) 2_666 ?
C5 C6A 1.371(18) . ?
C5 C6B 1.631(16) . ?
C5 H51A 0.9700 . ?
C5 H52A 0.9700 . ?
C5 H51B 0.9700 . ?
C5 H52B 0.9700 . ?
C6A O9A 1.230(17) . ?
C6A O8 1.423(15) . ?
C6B O8 1.220(15) . ?
C6B O9B 1.235(16) . ?
O8 K1 2.799(7) 2_666 ?
O8 K4 3.104(6) . ?
O9B K4 2.782(13) 2_667 ?
C7 N2 1.460(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N2 C8 1.484(7) . ?
N2 C10 1.491(8) . ?
C8 C9 1.527(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O11 1.247(7) . ?
C9 O10 1.275(9) . ?
O10 K1 2.927(8) . ?
C10 C11 1.516(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O13 1.259(8) . ?
C11 O12 1.263(9) . ?
O12 K5 2.483(6) 2_666 ?
O12 K3 2.948(5) 2_665 ?
O13 K3 3.108(9) 2_665 ?
O14 C12 1.434(5) . ?
C12 C13 1.511(7) . ?
C12 C18 1.513(7) . ?
C12 H12 0.9800 . ?
C13 N3 1.473(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N3 C14 1.459(8) . ?
N3 C16 1.476(7) . ?
C14 C15 1.520(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O16 1.239(7) . ?
C15 O15 1.284(6) . ?
C16 C17 1.512(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 O18 1.245(7) . ?
C17 O17 1.273(7) . ?
O17 K5 2.539(5) . ?
O17 K3 3.226(6) 1_556 ?
O18 K2 2.673(6) 1_556 ?
O18 K3 2.995(7) 1_556 ?
C18 N4 1.498(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N4 C19 1.459(8) . ?
N4 C21 1.471(7) . ?
C19 C20 1.532(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 O20 1.234(8) . ?
C20 O19 1.288(7) . ?
O19 K5 2.668(5) . ?
O19 K3 2.923(5) 1_556 ?
O20 K3 3.023(7) 1_556 ?
C21 C22 1.513(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O22 1.232(7) . ?
C22 O21 1.289(7) . ?
O21 K1 2.834(7) . ?
O22 K2 2.805(7) . ?
K1 O8 2.799(7) 2_666 ?
K1 O33 2.87(3) . ?
K1 O31 2.894(15) . ?
K1 K2 4.003(7) . ?
K2 O18 2.673(6) 1_554 ?
K2 O31 2.789(15) . ?
K2 O32 2.900(19) . ?
K2 K3 4.044(5) . ?
K3 O19 2.923(5) 1_554 ?
K3 O12 2.948(5) 2_665 ?
K3 O32 2.982(14) . ?
K3 O18 2.995(7) 1_554 ?
K3 O20 3.023(7) 1_554 ?
K3 O13 3.108(9) 2_665 ?
K3 O33 3.13(3) 2_665 ?
K3 O17 3.226(6) 1_554 ?
O31 C31 1.43(2) . ?
O33 K3 3.13(3) 2_665 ?
O34 C34 1.36(5) . ?
K4 O41 2.47(2) . ?
K4 O46 2.58(5) . ?
K4 O42 2.625(13) . ?
K4 O45 2.64(3) . ?
K4 O9B 2.782(14) 2_667 ?
K4 O41 3.422(19) 2_667 ?
K5 O45 2.23(4) . ?
K5 O12 2.483(6) 2_666 ?
K5 O4 2.771(5) 2_666 ?
K5 O43 2.896(16) . ?
O41 K4 3.422(18) 2_667 ?
O45 C45 0.92(12) . ?

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
O2 Fe1 O2 180.0 2_666 . ?
O2 Fe1 O1 98.01(13) 2_666 . ?
O2 Fe1 O1 81.99(13) . . ?
O2 Fe1 O1 81.99(13) 2_666 2_666 ?
O2 Fe1 O1 98.01(13) . 2_666 ?
O1 Fe1 O1 180.000(1) . 2_666 ?
O2 Fe1 O4 89.49(15) 2_666 . ?
O2 Fe1 O4 90.51(15) . . ?
O1 Fe1 O4 88.78(14) . . ?
O1 Fe1 O4 91.22(14) 2_666 . ?
O2 Fe1 O4 90.51(15) 2_666 2_666 ?
O2 Fe1 O4 89.49(15) . 2_666 ?
O1 Fe1 O4 91.22(14) . 2_666 ?
O1 Fe1 O4 88.78(14) 2_666 2_666 ?
O4 Fe1 O4 180.00(17) . 2_666 ?
O2 Fe1 Fe2 138.90(10) 2_666 . ?
O2 Fe1 Fe2 41.10(10) . . ?
O1 Fe1 Fe2 41.16(9) . . ?
O1 Fe1 Fe2 138.84(9) 2_666 . ?
O4 Fe1 Fe2 85.83(10) . . ?
O4 Fe1 Fe2 94.17(10) 2_666 . ?
O2 Fe1 Fe2 41.10(10) 2_666 2_666 ?
O2 Fe1 Fe2 138.90(10) . 2_666 ?
O1 Fe1 Fe2 138.84(9) . 2_666 ?
O1 Fe1 Fe2 41.16(9) 2_666 2_666 ?
O4 Fe1 Fe2 94.17(10) . 2_666 ?
O4 Fe1 Fe2 85.83(10) 2_666 2_666 ?
Fe2 Fe1 Fe2 180.0 . 2_666 ?
O1 Fe2 O2 84.01(14) . . ?
O1 Fe2 O5 88.71(14) . . ?
O2 Fe2 O5 107.77(15) . . ?
O1 Fe2 O8 94.99(16) . . ?
O2 Fe2 O8 105.38(17) . . ?
O5 Fe2 O8 146.85(17) . . ?
O1 Fe2 O6 157.61(13) . . ?
O2 Fe2 O6 74.18(14) . . ?
O5 Fe2 O6 93.07(15) . . ?
O8 Fe2 O6 95.62(16) . . ?
O1 Fe2 N1 128.89(15) . . ?
O2 Fe2 N1 147.09(15) . . ?
O5 Fe2 N1 76.97(16) . . ?
O8 Fe2 N1 75.16(18) . . ?
O6 Fe2 N1 73.04(15) . . ?
O1 Fe2 Fe1 42.84(9) . . ?
O2 Fe2 Fe1 41.46(10) . . ?
O5 Fe2 Fe1 97.42(10) . . ?
O8 Fe2 Fe1 107.60(13) . . ?
O6 Fe2 Fe1 114.91(9) . . ?
N1 Fe2 Fe1 170.79(11) . . ?
O1 Fe3 O3 92.32(14) . . ?
O1 Fe3 O17 91.26(15) . . ?
O3 Fe3 O17 176.02(14) . . ?
O1 Fe3 O15 98.39(14) . . ?
O3 Fe3 O15 88.99(17) . . ?
O17 Fe3 O15 92.23(17) . . ?
O1 Fe3 O14 111.86(13) . . ?
O3 Fe3 O14 89.42(14) . . ?
O17 Fe3 O14 87.63(15) . . ?
O15 Fe3 O14 149.75(14) . . ?
O1 Fe3 N3 166.28(15) . . ?
O3 Fe3 N3 98.48(16) . . ?
O17 Fe3 N3 78.24(16) . . ?
O15 Fe3 N3 73.51(15) . . ?
O14 Fe3 N3 76.86(14) . . ?
O2 Fe4 O14 98.32(14) 2_666 . ?
O2 Fe4 O19 105.92(16) 2_666 . ?
O14 Fe4 O19 90.50(16) . . ?
O2 Fe4 O21 100.49(16) 2_666 . ?
O14 Fe4 O21 97.28(16) . . ?
O19 Fe4 O21 151.05(16) . . ?
O2 Fe4 O6 77.20(14) 2_666 2_666 ?
O14 Fe4 O6 175.02(13) . 2_666 ?
O19 Fe4 O6 88.67(16) . 2_666 ?
O21 Fe4 O6 85.76(16) . 2_666 ?
O2 Fe4 N4 175.17(16) 2_666 . ?
O14 Fe4 N4 84.27(15) . . ?
O19 Fe4 N4 78.05(16) . . ?
O21 Fe4 N4 75.08(16) . . ?
O6 Fe4 N4 100.35(15) 2_666 . ?
O4 Fe5 O5 104.11(14) . . ?
O4 Fe5 O3 97.59(16) . . ?
O5 Fe5 O3 90.83(15) . . ?
O4 Fe5 O10 99.77(18) . . ?
O5 Fe5 O10 155.98(19) . . ?
O3 Fe5 O10 88.55(16) . . ?
O4 Fe5 O12 87.16(19) . . ?
O5 Fe5 O12 91.61(17) . . ?
O3 Fe5 O12 173.96(17) . . ?
O10 Fe5 O12 86.97(17) . . ?
O4 Fe5 N2 164.95(18) . . ?
O5 Fe5 N2 79.67(17) . . ?
O3 Fe5 N2 96.90(18) . . ?
O10 Fe5 N2 76.6(2) . . ?
O12 Fe5 N2 78.1(2) . . ?
Fe3 O1 Fe2 128.81(18) . . ?
Fe3 O1 Fe1 129.17(17) . . ?
Fe2 O1 Fe1 96.00(13) . . ?
Fe4 O2 Fe2 112.17(17) 2_666 . ?
Fe4 O2 Fe1 150.39(19) 2_666 . ?
Fe2 O2 Fe1 97.43(14) . . ?
Fe5 O3 Fe3 123.83(16) . . ?
Fe5 O3 H3 114(5) . . ?
Fe3 O3 H3 118(5) . . ?
Fe5 O4 Fe1 124.50(17) . . ?
Fe5 O4 K5 101.71(17) . 2_666 ?
Fe1 O4 K5 109.18(15) . 2_666 ?
Fe5 O4 K1 97.98(16) . . ?
Fe1 O4 K1 123.89(19) . . ?
K5 O4 K1 93.65(16) 2_666 . ?
Fe5 O4 H4A 117(9) . . ?
Fe1 O4 H4A 111(9) . . ?
Fe5 O4 H4B 113(8) . . ?
Fe1 O4 H4B 110(9) . . ?
K5 O4 H4B 93(8) 2_666 . ?
C1 O5 Fe2 121.5(3) . . ?
C1 O5 Fe5 118.1(3) . . ?
Fe2 O5 Fe5 120.22(18) . . ?
O5 C1 C7 107.8(4) . . ?
O5 C1 C2 108.4(4) . . ?
C7 C1 C2 109.4(5) . . ?
O5 C1 H1 110.4 . . ?
C7 C1 H1 110.4 . . ?
C2 C1 H1 110.4 . . ?
N1 C2 C1 110.2(4) . . ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C2 N1 C3 112.9(5) . . ?
C2 N1 C5 113.3(5) . . ?
C3 N1 C5 110.3(6) . . ?
C2 N1 Fe2 106.9(3) . . ?
C3 N1 Fe2 110.0(3) . . ?
C5 N1 Fe2 102.8(4) . . ?
N1 C3 C4 114.1(4) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
O7 C4 O6 125.6(5) . . ?
O7 C4 C3 120.3(5) . . ?
O6 C4 C3 114.0(5) . . ?
C4 O6 Fe4 137.9(3) . 2_666 ?
C4 O6 Fe2 125.1(3) . . ?
Fe4 O6 Fe2 94.98(14) 2_666 . ?
C6A C5 N1 116.5(7) . . ?
C6A C5 C6B 22.2(6) . . ?
N1 C5 C6B 102.8(6) . . ?
C6A C5 H51A 108.2 . . ?
N1 C5 H51A 108.2 . . ?
C6B C5 H51A 98.4 . . ?
C6A C5 H52A 108.2 . . ?
N1 C5 H52A 108.2 . . ?
C6B C5 H52A 130.4 . . ?
H51A C5 H52A 107.3 . . ?
C6A C5 H51B 89.2 . . ?
N1 C5 H51B 111.2 . . ?
C6B C5 H51B 111.0 . . ?
H51A C5 H51B 122.8 . . ?
H52A C5 H51B 20.7 . . ?
C6A C5 H52B 117.3 . . ?
N1 C5 H52B 111.1 . . ?
C6B C5 H52B 111.4 . . ?
H51A C5 H52B 15.3 . . ?
H52A C5 H52B 92.4 . . ?
H51B C5 H52B 109.1 . . ?
O9A C6A C5 122.0(13) . . ?
O9A C6A O8 121.4(14) . . ?
C5 C6A O8 115.9(10) . . ?
O8 C6B O9B 122.5(14) . . ?
O8 C6B C5 111.6(10) . . ?
O9B C6B C5 124.0(11) . . ?
C6B O8 Fe2 124.4(7) . . ?
C6A O8 Fe2 116.6(7) . . ?
C6B O8 K1 111.4(7) . 2_666 ?
C6A O8 K1 124.4(7) . 2_666 ?
Fe2 O8 K1 119.0(2) . 2_666 ?
C6B O8 K4 74.5(7) . . ?
Fe2 O8 K4 160.3(2) . . ?
C6B O9B K4 118.7(11) . . ?
C6B O9B K4 121.3(11) . 2_667 ?
K4 O9B K4 83.2(4) . 2_667 ?
N2 C7 C1 109.6(5) . . ?
N2 C7 H7A 109.8 . . ?
C1 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C1 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C7 N2 C8 115.6(6) . . ?
C7 N2 C10 111.9(5) . . ?
C8 N2 C10 110.9(5) . . ?
C7 N2 Fe5 104.7(3) . . ?
C8 N2 Fe5 103.3(4) . . ?
C10 N2 Fe5 109.8(5) . . ?
N2 C8 C9 108.3(6) . . ?
N2 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N2 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O11 C9 O10 124.0(8) . . ?
O11 C9 C8 119.7(8) . . ?
O10 C9 C8 116.3(5) . . ?
C9 O10 Fe5 118.1(5) . . ?
C9 O10 K1 138.7(4) . . ?
Fe5 O10 K1 100.4(2) . . ?
N2 C10 C11 112.6(6) . . ?
N2 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
O13 C11 O12 123.6(8) . . ?
O13 C11 C10 117.4(7) . . ?
O12 C11 C10 118.9(6) . . ?
C11 O12 Fe5 119.9(5) . . ?
C11 O12 K5 131.2(5) . 2_666 ?
Fe5 O12 K5 107.9(2) . 2_666 ?
C11 O12 K3 100.4(4) . 2_665 ?
Fe5 O12 K3 138.1(2) . 2_665 ?
C11 O13 K3 92.8(6) . 2_665 ?
C12 O14 Fe4 110.8(3) . . ?
C12 O14 Fe3 116.3(3) . . ?
Fe4 O14 Fe3 128.45(16) . . ?
O14 C12 C13 108.6(4) . . ?
O14 C12 C18 109.5(4) . . ?
C13 C12 C18 108.8(4) . . ?
O14 C12 H12 110.0 . . ?
C13 C12 H12 110.0 . . ?
C18 C12 H12 110.0 . . ?
N3 C13 C12 107.5(4) . . ?
N3 C13 H13A 110.2 . . ?
C12 C13 H13A 110.2 . . ?
N3 C13 H13B 110.2 . . ?
C12 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
C14 N3 C13 113.5(4) . . ?
C14 N3 C16 111.2(4) . . ?
C13 N3 C16 112.2(4) . . ?
C14 N3 Fe3 104.8(3) . . ?
C13 N3 Fe3 108.3(3) . . ?
C16 N3 Fe3 106.2(3) . . ?
N3 C14 C15 109.5(4) . . ?
N3 C14 H14A 109.8 . . ?
C15 C14 H14A 109.8 . . ?
N3 C14 H14B 109.8 . . ?
C15 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
O16 C15 O15 124.7(5) . . ?
O16 C15 C14 119.1(5) . . ?
O15 C15 C14 116.2(5) . . ?
C15 O15 Fe3 117.0(3) . . ?
N3 C16 C17 113.2(4) . . ?
N3 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
N3 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
O18 C17 O17 122.6(6) . . ?
O18 C17 C16 120.0(5) . . ?
O17 C17 C16 117.4(5) . . ?
O18 C17 K5 82.7(4) . . ?
O17 C17 K5 43.8(3) . . ?
C16 C17 K5 152.6(3) . . ?
C17 O17 Fe3 120.3(4) . . ?
C17 O17 K5 115.9(4) . . ?
Fe3 O17 K5 115.47(17) . . ?
C17 O17 K3 88.7(4) . 1_556 ?
Fe3 O17 K3 137.78(17) . 1_556 ?
C17 O18 K2 129.3(4) . 1_556 ?
C17 O18 K3 100.2(4) . 1_556 ?
K2 O18 K3 90.86(18) 1_556 1_556 ?
C17 O18 K5 75.9(4) . . ?
N4 C18 C12 111.4(4) . . ?
N4 C18 H18A 109.3 . . ?
C12 C18 H18A 109.3 . . ?
N4 C18 H18B 109.3 . . ?
C12 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C19 N4 C21 114.3(5) . . ?
C19 N4 C18 112.6(4) . . ?
C21 N4 C18 109.9(4) . . ?
C19 N4 Fe4 108.9(3) . . ?
C21 N4 Fe4 108.7(3) . . ?
C18 N4 Fe4 101.6(3) . . ?
N4 C19 C20 111.2(4) . . ?
N4 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
N4 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
O20 C20 O19 123.9(6) . . ?
O20 C20 C19 119.1(6) . . ?
O19 C20 C19 117.0(5) . . ?
C20 O19 Fe4 120.7(4) . . ?
C20 O19 K5 127.0(4) . . ?
Fe4 O19 K5 108.96(18) . . ?
C20 O19 K3 96.4(4) . 1_556 ?
Fe4 O19 K3 139.0(2) . 1_556 ?
C20 O20 K3 92.9(5) . 1_556 ?
N4 C21 C22 109.7(4) . . ?
N4 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
N4 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O22 C22 O21 124.4(7) . . ?
O22 C22 C21 119.4(6) . . ?
O21 C22 C21 116.2(5) . . ?
C22 O21 Fe4 120.6(4) . . ?
C22 O21 K1 117.8(4) . . ?
Fe4 O21 K1 120.8(2) . . ?
C22 O22 K2 131.3(5) . . ?
O8 K1 O21 74.30(19) 2_666 . ?
O8 K1 O33 102.7(13) 2_666 . ?
O21 K1 O33 170.3(6) . . ?
O8 K1 O31 111.4(3) 2_666 . ?
O21 K1 O31 107.1(4) . . ?
O33 K1 O31 82.6(6) . . ?
O8 K1 O10 139.0(3) 2_666 . ?
O21 K1 O10 106.55(19) . . ?
O33 K1 O10 69.4(11) . . ?
O31 K1 O10 107.4(3) . . ?
O8 K1 O4 78.20(18) 2_666 . ?
O21 K1 O4 90.31(18) . . ?
O33 K1 O4 80.0(6) . . ?
O31 K1 O4 161.7(4) . . ?
O10 K1 O4 60.87(15) . . ?
O8 K1 Fe5 107.93(19) 2_666 . ?
O21 K1 Fe5 96.37(15) . . ?
O33 K1 Fe5 75.6(7) . . ?
O31 K1 Fe5 138.3(3) . . ?
O10 K1 Fe5 31.39(9) . . ?
O4 K1 Fe5 29.79(9) . . ?
O8 K1 K2 74.80(16) 2_666 . ?
O21 K1 K2 74.04(17) . . ?
O33 K1 K2 114.4(7) . . ?
O31 K1 K2 44.2(3) . . ?
O10 K1 K2 145.9(2) . . ?
O4 K1 K2 151.6(2) . . ?
Fe5 K1 K2 169.16(17) . . ?
O8 K1 H4A 72(3) 2_666 . ?
O21 K1 H4A 103.0(19) . . ?
O33 K1 H4A 67(2) . . ?
O31 K1 H4A 149.6(16) . . ?
O10 K1 H4A 67(2) . . ?
O4 K1 H4A 16.4(8) . . ?
Fe5 K1 H4A 40(2) . . ?
K2 K1 H4A 147(2) . . ?
O8 K1 H4B 72(3) 2_666 . ?
O21 K1 H4B 88(3) . . ?
O33 K1 H4B 82(4) . . ?
O31 K1 H4B 165(3) . . ?
O10 K1 H4B 67(3) . . ?
O4 K1 H4B 6(3) . . ?
Fe5 K1 H4B 36(3) . . ?
K2 K1 H4B 146(3) . . ?
H4A K1 H4B 16(4) . . ?
O18 K2 O31 91.2(3) 1_554 . ?
O18 K2 O22 120.3(2) 1_554 . ?
O31 K2 O22 84.2(3) . . ?
O18 K2 O32 78.8(3) 1_554 . ?
O31 K2 O32 168.2(4) . . ?
O22 K2 O32 106.2(3) . . ?
O19 K3 O12 74.51(13) 1_554 2_665 ?
O19 K3 O32 145.8(4) 1_554 . ?
O12 K3 O32 131.2(3) 2_665 . ?
O19 K3 O18 95.46(14) 1_554 1_554 ?
O12 K3 O18 148.14(18) 2_665 1_554 ?
O32 K3 O18 72.7(3) . 1_554 ?
O19 K3 O20 43.91(13) 1_554 1_554 ?
O12 K3 O20 96.91(19) 2_665 1_554 ?
O32 K3 O20 104.2(4) . 1_554 ?
O18 K3 O20 95.94(19) 1_554 1_554 ?
O19 K3 O13 91.20(17) 1_554 2_665 ?
O12 K3 O13 42.94(13) 2_665 2_665 ?
O32 K3 O13 96.7(3) . 2_665 ?
O18 K3 O13 168.63(17) 1_554 2_665 ?
O20 K3 O13 82.5(2) 1_554 2_665 ?
O19 K3 O33 132.1(6) 1_554 2_665 ?
O12 K3 O33 66.2(8) 2_665 2_665 ?
O32 K3 O33 82.1(7) . 2_665 ?
O18 K3 O33 103.5(11) 1_554 2_665 ?
O20 K3 O33 160.5(11) 1_554 2_665 ?
O13 K3 O33 78.5(12) 2_665 2_665 ?
O19 K3 O17 72.62(12) 1_554 1_554 ?
O12 K3 O17 107.33(14) 2_665 1_554 ?
O32 K3 O17 111.0(3) . 1_554 ?
O18 K3 O17 41.38(11) 1_554 1_554 ?
O20 K3 O17 101.00(16) 1_554 1_554 ?
O13 K3 O17 149.99(15) 2_665 1_554 ?
O33 K3 O17 93.6(11) 2_665 1_554 ?
C31 O31 K2 92.3(10) . . ?
C31 O31 K1 151.1(10) . . ?
K2 O31 K1 89.5(4) . . ?
O31 C31 K2 61.0(9) . . ?
K2 O32 K3 86.9(4) . . ?
K1 O33 K3 121.9(14) . 2_665 ?
O9B K4 O41 61.5(5) . . ?
O9B K4 O46 108.9(16) . . ?
O41 K4 O46 67.2(17) . . ?
O9B K4 O42 102.6(5) . . ?
O41 K4 O42 121.5(6) . . ?
O46 K4 O42 67.1(15) . . ?
O9B K4 O45 95.5(8) . . ?
O41 K4 O45 152.6(9) . . ?
O46 K4 O45 138.8(19) . . ?
O42 K4 O45 75.6(9) . . ?
O9B K4 O9B 96.8(4) . 2_667 ?
O41 K4 O9B 88.5(5) . 2_667 ?
O46 K4 O9B 127.8(12) . 2_667 ?
O42 K4 O9B 149.5(6) . 2_667 ?
O45 K4 O9B 79.3(8) . 2_667 ?
O9B K4 O8 43.9(3) . . ?
O41 K4 O8 100.5(5) . . ?
O46 K4 O8 110.5(12) . . ?
O42 K4 O8 64.8(4) . . ?
O45 K4 O8 65.7(7) . . ?
O9B K4 O8 119.2(3) 2_667 . ?
O9B K4 O41 78.0(5) . 2_667 ?
O41 K4 O41 113.0(4) . 2_667 ?
O46 K4 O41 171.1(12) . 2_667 ?
O42 K4 O41 117.7(5) . 2_667 ?
O45 K4 O41 43.1(9) . 2_667 ?
O9B K4 O41 44.2(4) 2_667 2_667 ?
O8 K4 O41 78.3(3) . 2_667 ?
O45 K5 O12 105.6(8) . 2_666 ?
O45 K5 O17 78.4(8) . . ?
O12 K5 O17 164.50(19) 2_666 . ?
O45 K5 O19 167.2(8) . . ?
O12 K5 O19 87.17(17) 2_666 . ?
O17 K5 O19 88.94(15) . . ?
O45 K5 O4 82.2(8) . 2_666 ?
O12 K5 O4 63.23(14) 2_666 2_666 ?
O17 K5 O4 103.20(17) . 2_666 ?
O19 K5 O4 103.05(15) . 2_666 ?
O45 K5 O43 107.1(8) . . ?
O12 K5 O43 77.7(3) 2_666 . ?
O17 K5 O43 115.9(3) . . ?
O19 K5 O43 76.3(3) . . ?
O4 K5 O43 140.9(3) 2_666 . ?
O45 K5 O18 76.9(8) . . ?
O12 K5 O18 154.27(18) 2_666 . ?
O17 K5 O18 40.87(13) . . ?
O19 K5 O18 92.12(15) . . ?
O4 K5 O18 141.24(18) 2_666 . ?
O43 K5 O18 77.1(3) . . ?
K4 O41 K4 67.0(4) . 2_667 ?
C45 O45 K5 94(4) . . ?
C45 O45 K4 90(5) . . ?
K5 O45 K4 157.1(16) . . ?

_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.939
_refine_diff_density_max         0.751
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.152