# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1R

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Fe4-NO2(R)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C90 H72 Fe4 N12 O24'
_chemical_absolute_configuration ad
_chemical_formula_sum            'C90 H72 Fe4 N12 O24'
_chemical_formula_weight         1929.00

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'

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

_cell_length_a                   29.7005(17)
_cell_length_b                   29.7005(17)
_cell_length_c                   13.7937(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     10537.5(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5421
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      28.33

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Blessing, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  Triumph
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            41624
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         28.33
_reflns_number_total             5850
_reflns_number_gt                5421
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0657P)²+17.8434P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.084(17)
_refine_ls_number_reflns         5850
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1185
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.5000 0.01292(17) Uani 1 6 d S . .
Fe2 Fe 0.107939(15) 0.0000 0.5000 0.01417(11) Uani 1 2 d S . .
C1 C 0.20362(9) 0.06865(10) 0.38700(17) 0.0175(5) Uani 1 1 d . . .
C2 C 0.23747(11) 0.07244(12) 0.3092(2) 0.0293(6) Uani 1 1 d . . .
H2 H 0.2296 0.0420 0.2734 0.035 Uiso 1 1 calc R . .
C3 C 0.28016(11) 0.11785(11) 0.2853(2) 0.0273(6) Uani 1 1 d . . .
H3 H 0.3019 0.1190 0.2338 0.033 Uiso 1 1 calc R . .
C4 C 0.29225(11) 0.16344(11) 0.33707(18) 0.0242(5) Uani 1 1 d . . .
C5 C 0.26121(10) 0.16228(10) 0.41038(18) 0.0196(5) Uani 1 1 d . . .
H5 H 0.2692 0.1936 0.4428 0.023 Uiso 1 1 calc R . .
C6 C 0.21725(10) 0.11533(10) 0.43925(17) 0.0189(5) Uani 1 1 d . . .
C7 C 0.18784(9) 0.11729(10) 0.52046(18) 0.0180(5) Uani 1 1 d . . .
H7 H 0.1990 0.1502 0.5496 0.022 Uiso 1 1 calc R . .
C8 C 0.11976(9) 0.08575(10) 0.64109(17) 0.0164(5) Uani 1 1 d . . .
H8 H 0.1016 0.1042 0.6168 0.020 Uiso 1 1 calc R . .
C9 C 0.15378(9) 0.11604(9) 0.72386(17) 0.0180(5) Uani 1 1 d . . .
C10 C 0.15162(17) 0.15744(14) 0.7607(3) 0.0462(9) Uani 1 1 d . . .
H10 H 0.1291 0.1675 0.7313 0.055 Uiso 1 1 calc R . .
C11 C 0.1811(2) 0.18528(18) 0.8396(3) 0.0746(18) Uani 1 1 d . . .
H11 H 0.1800 0.2151 0.8608 0.090 Uiso 1 1 calc R . .
C12 C 0.21176(16) 0.17048(15) 0.8873(2) 0.0474(9) Uani 1 1 d . . .
H12 H 0.2301 0.1879 0.9443 0.057 Uiso 1 1 calc R . .
C13 C 0.21524(12) 0.12906(13) 0.84965(19) 0.0297(6) Uani 1 1 d . . .
H13 H 0.2382 0.1197 0.8797 0.036 Uiso 1 1 calc R . .
C14 C 0.18670(11) 0.10079(11) 0.77007(19) 0.0253(5) Uani 1 1 d . . .
H14 H 0.1891 0.0719 0.7470 0.030 Uiso 1 1 calc R . .
C15 C 0.07855(9) 0.03095(9) 0.67184(16) 0.0176(4) Uani 1 1 d . . .
H15A H 0.0949 0.0148 0.7103 0.021 Uiso 1 1 calc R . .
H15B H 0.0521 0.0326 0.7128 0.021 Uiso 1 1 calc R . .
N1 N 0.14729(8) 0.07753(8) 0.55668(14) 0.0160(4) Uani 1 1 d . . .
N2 N 0.33749(9) 0.21195(10) 0.30939(18) 0.0301(5) Uani 1 1 d . . .
O1 O 0.16281(7) 0.02427(7) 0.40367(13) 0.0221(4) Uani 1 1 d . . .
O2 O 0.05457(7) 0.00047(6) 0.58814(11) 0.0166(3) Uani 1 1 d . . .
O3 O 0.36983(10) 0.21091(11) 0.2546(2) 0.0537(8) Uani 1 1 d . . .
O4 O 0.34177(10) 0.25248(9) 0.3415(2) 0.0497(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 2.0206(18) . ?
Fe1 O2 2.0207(18) 2 ?
Fe1 O2 2.0207(18) 3 ?
Fe1 O2 2.0207(18) 6_556 ?
Fe1 O2 2.0207(18) 4_556 ?
Fe1 O2 2.0207(18) 5_556 ?
Fe2 O1 1.9408(17) . ?
Fe2 O1 1.9408(17) 5_556 ?
Fe2 O2 2.0031(18) 5_556 ?
Fe2 O2 2.0031(18) . ?
Fe2 N1 2.142(2) . ?
Fe2 N1 2.142(2) 5_556 ?
C1 O1 1.289(3) . ?
C1 C6 1.430(3) . ?
C1 C2 1.436(4) . ?
C2 C3 1.351(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.409(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.357(4) . ?
C4 N2 1.446(3) . ?
C5 C6 1.410(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.440(3) . ?
C7 N1 1.293(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.492(3) . ?
C8 N1 1.511(3) . ?
C8 C15 1.528(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.361(4) . ?
C9 C14 1.418(4) . ?
C10 C11 1.382(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(4) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O2 1.419(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N2 O4 1.228(4) . ?
N2 O3 1.235(3) . ?

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 87.53(7) . 2 ?
O2 Fe1 O2 87.53(7) . 3 ?
O2 Fe1 O2 87.53(7) 2 3 ?
O2 Fe1 O2 133.57(9) . 6_556 ?
O2 Fe1 O2 132.28(9) 2 6_556 ?
O2 Fe1 O2 73.98(9) 3 6_556 ?
O2 Fe1 O2 132.28(9) . 4_556 ?
O2 Fe1 O2 73.98(9) 2 4_556 ?
O2 Fe1 O2 133.57(9) 3 4_556 ?
O2 Fe1 O2 87.53(7) 6_556 4_556 ?
O2 Fe1 O2 73.99(9) . 5_556 ?
O2 Fe1 O2 133.57(9) 2 5_556 ?
O2 Fe1 O2 132.28(9) 3 5_556 ?
O2 Fe1 O2 87.53(7) 6_556 5_556 ?
O2 Fe1 O2 87.53(7) 4_556 5_556 ?
O1 Fe2 O1 98.30(11) . 5_556 ?
O1 Fe2 O2 96.09(7) . 5_556 ?
O1 Fe2 O2 158.97(7) 5_556 5_556 ?
O1 Fe2 O2 158.97(7) . . ?
O1 Fe2 O2 96.10(7) 5_556 . ?
O2 Fe2 O2 74.74(10) 5_556 . ?
O1 Fe2 N1 86.85(8) . . ?
O1 Fe2 N1 92.54(8) 5_556 . ?
O2 Fe2 N1 103.51(7) 5_556 . ?
O2 Fe2 N1 77.25(7) . . ?
O1 Fe2 N1 92.54(8) . 5_556 ?
O1 Fe2 N1 86.85(8) 5_556 5_556 ?
O2 Fe2 N1 77.25(7) 5_556 5_556 ?
O2 Fe2 N1 103.51(7) . 5_556 ?
N1 Fe2 N1 179.07(11) . 5_556 ?
O1 C1 C6 124.6(2) . . ?
O1 C1 C2 118.5(2) . . ?
C6 C1 C2 116.9(2) . . ?
C3 C2 C1 122.1(3) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.6(2) . . ?
C5 C4 N2 120.2(2) . . ?
C3 C4 N2 119.2(2) . . ?
C4 C5 C6 121.1(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 C7 117.4(2) . . ?
C1 C6 C7 123.2(2) . . ?
N1 C7 C6 124.8(2) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C9 C8 N1 115.42(19) . . ?
C9 C8 C15 111.7(2) . . ?
N1 C8 C15 104.59(18) . . ?
C9 C8 H8 108.3 . . ?
N1 C8 H8 108.3 . . ?
C15 C8 H8 108.3 . . ?
C10 C9 C14 118.2(3) . . ?
C10 C9 C8 120.5(2) . . ?
C14 C9 C8 121.2(2) . . ?
C9 C10 C11 122.2(3) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 117.7(3) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 122.7(3) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
C13 C14 C9 118.3(3) . . ?
C13 C14 H14 120.9 . . ?
C9 C14 H14 120.9 . . ?
O2 C15 C8 109.44(18) . . ?
O2 C15 H15A 109.8 . . ?
C8 C15 H15A 109.8 . . ?
O2 C15 H15B 109.8 . . ?
C8 C15 H15B 109.8 . . ?
H15A C15 H15B 108.2 . . ?
C7 N1 C8 118.8(2) . . ?
C7 N1 Fe2 126.80(17) . . ?
C8 N1 Fe2 113.98(14) . . ?
O4 N2 O3 123.0(3) . . ?
O4 N2 C4 118.1(2) . . ?
O3 N2 C4 118.9(3) . . ?
C1 O1 Fe2 133.44(16) . . ?
C15 O2 Fe2 110.59(14) . . ?
C15 O2 Fe1 129.69(14) . . ?
Fe2 O2 Fe1 105.64(7) . . ?

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
O1 C1 C2 C3 178.0(3) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
C1 C2 C3 C4 -0.5(5) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C2 C3 C4 N2 -178.8(3) . . . . ?
C3 C4 C5 C6 2.4(4) . . . . ?
N2 C4 C5 C6 -179.3(2) . . . . ?
C4 C5 C6 C1 -3.4(4) . . . . ?
C4 C5 C6 C7 177.3(2) . . . . ?
O1 C1 C6 C5 -176.1(2) . . . . ?
C2 C1 C6 C5 2.3(4) . . . . ?
O1 C1 C6 C7 3.3(4) . . . . ?
C2 C1 C6 C7 -178.4(2) . . . . ?
C5 C6 C7 N1 -178.6(2) . . . . ?
C1 C6 C7 N1 2.0(4) . . . . ?
N1 C8 C9 C10 129.0(3) . . . . ?
C15 C8 C9 C10 -111.7(3) . . . . ?
N1 C8 C9 C14 -55.0(3) . . . . ?
C15 C8 C9 C14 64.3(3) . . . . ?
C14 C9 C10 C11 1.4(6) . . . . ?
C8 C9 C10 C11 177.6(4) . . . . ?
C9 C10 C11 C12 -3.6(8) . . . . ?
C10 C11 C12 C13 4.6(8) . . . . ?
C11 C12 C13 C14 -3.9(6) . . . . ?
C12 C13 C14 C9 1.9(5) . . . . ?
C10 C9 C14 C13 -0.6(4) . . . . ?
C8 C9 C14 C13 -176.7(2) . . . . ?
C9 C8 C15 O2 -167.92(19) . . . . ?
N1 C8 C15 O2 -42.4(2) . . . . ?
C6 C7 N1 C8 -178.9(2) . . . . ?
C6 C7 N1 Fe2 -6.4(4) . . . . ?
C9 C8 N1 C7 -50.5(3) . . . . ?
C15 C8 N1 C7 -173.7(2) . . . . ?
C9 C8 N1 Fe2 136.07(18) . . . . ?
C15 C8 N1 Fe2 12.9(2) . . . . ?
O1 Fe2 N1 C7 5.0(2) . . . . ?
O1 Fe2 N1 C7 103.1(2) 5_556 . . . ?
O2 Fe2 N1 C7 -90.6(2) 5_556 . . . ?
O2 Fe2 N1 C7 -161.2(2) . . . . ?
N1 Fe2 N1 C7 54.0(2) 5_556 . . . ?
O1 Fe2 N1 C8 177.72(17) . . . . ?
O1 Fe2 N1 C8 -84.10(16) 5_556 . . . ?
O2 Fe2 N1 C8 82.20(16) 5_556 . . . ?
O2 Fe2 N1 C8 11.58(15) . . . . ?
N1 Fe2 N1 C8 -133.21(15) 5_556 . . . ?
C5 C4 N2 O4 -12.5(4) . . . . ?
C3 C4 N2 O4 165.8(3) . . . . ?
C5 C4 N2 O3 167.8(3) . . . . ?
C3 C4 N2 O3 -13.9(4) . . . . ?
C6 C1 O1 Fe2 -3.5(4) . . . . ?
C2 C1 O1 Fe2 178.10(19) . . . . ?
O1 Fe2 O1 C1 -92.2(2) 5_556 . . . ?
O2 Fe2 O1 C1 103.2(2) 5_556 . . . ?
O2 Fe2 O1 C1 40.6(4) . . . . ?
N1 Fe2 O1 C1 -0.1(2) . . . . ?
N1 Fe2 O1 C1 -179.3(2) 5_556 . . . ?
C8 C15 O2 Fe2 56.0(2) . . . . ?
C8 C15 O2 Fe1 -77.3(2) . . . . ?
O1 Fe2 O2 C15 -78.2(3) . . . . ?
O1 Fe2 O2 C15 54.84(15) 5_556 . . . ?
O2 Fe2 O2 C15 -144.45(17) 5_556 . . . ?
N1 Fe2 O2 C15 -36.40(14) . . . . ?
N1 Fe2 O2 C15 143.05(14) 5_556 . . . ?
O1 Fe2 O2 Fe1 66.2(2) . . . . ?
O1 Fe2 O2 Fe1 -160.71(8) 5_556 . . . ?
O2 Fe2 O2 Fe1 0.0 5_556 . . . ?
N1 Fe2 O2 Fe1 108.06(8) . . . . ?
N1 Fe2 O2 Fe1 -72.50(8) 5_556 . . . ?
O2 Fe1 O2 C15 -1.91(18) 2 . . . ?
O2 Fe1 O2 C15 -89.54(15) 3 . . . ?
O2 Fe1 O2 C15 -154.58(19) 6_556 . . . ?
O2 Fe1 O2 C15 63.74(17) 4_556 . . . ?
O2 Fe1 O2 C15 135.0(2) 5_556 . . . ?
O2 Fe1 O2 Fe2 -136.89(9) 2 . . . ?
O2 Fe1 O2 Fe2 135.47(10) 3 . . . ?
O2 Fe1 O2 Fe2 70.44(5) 6_556 . . . ?
O2 Fe1 O2 Fe2 -71.25(6) 4_556 . . . ?
O2 Fe1 O2 Fe2 0.0 5_556 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.068

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.006 -0.003 -0.003 5159 1388 ' '
_platon_squeeze_details          
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 1338e per unit cell were accumulated which corresponds 
to 446e per formula(C90H72Fe4N12O24). The 446e might come from solvent DMA molecules (calculated number is about 9) and were not included in the formula.
;

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMA'
_chemical_compound_source        no
_exptl_crystal_preparation       'Magnetic properties'
_database_code_depnum_ccdc_archive 'CCDC 941225'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1S

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Fe4-NO2(S)
_chemical_name_common            Fe4L6-NO2-S
_chemical_melting_point          ?
_chemical_formula_moiety         C90H72Fe4N12O24
_chemical_formula_sum            'C90 H72 Fe4 N12 O24'
_chemical_formula_weight         1929.00
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'

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

_cell_length_a                   29.778(4)
_cell_length_b                   29.778(4)
_cell_length_c                   13.885(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     10663(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    12535
_cell_measurement_theta_min      1.3680
_cell_measurement_theta_max      27.4814

_exptl_crystal_description       block
_exptl_crystal_colour            'red brown'
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.251
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29068
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5438
_reflns_number_gt                5288
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1053P)²+8.1444P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_number_reflns         5438
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1743
_refine_ls_wR_factor_gt          0.1735
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 1.0000 1.0000 0.0247(2) Uani 1 6 d S . .
Fe2 Fe 0.0000 0.89232(2) 1.0000 0.02717(17) Uani 1 2 d S . .
C1 C 0.06883(14) 0.86561(13) 1.1122(2) 0.0317(6) Uani 1 1 d . . .
C2 C 0.07263(16) 0.83614(16) 1.1900(3) 0.0428(8) Uani 1 1 d . . .
H2 H 0.0423 0.8143 1.2261 0.051 Uiso 1 1 calc R . .
C3 C 0.11670(17) 0.83804(18) 1.2140(3) 0.0475(9) Uani 1 1 d . . .
H3 H 0.1174 0.8175 1.2656 0.057 Uiso 1 1 calc R . .
C4 C 0.16271(16) 0.87084(17) 1.1623(3) 0.0413(8) Uani 1 1 d . . .
C5 C 0.16166(14) 0.90078(15) 1.0886(2) 0.0349(7) Uani 1 1 d . . .
H5 H 0.1930 0.9240 1.0564 0.042 Uiso 1 1 calc R . .
C6 C 0.11494(14) 0.89784(14) 1.0597(2) 0.0345(7) Uani 1 1 d . . .
C7 C 0.11750(13) 0.92942(14) 0.9794(2) 0.0320(6) Uani 1 1 d . . .
H7 H 0.1504 0.9509 0.9506 0.038 Uiso 1 1 calc R . .
C8 C 0.08598(13) 0.96592(12) 0.8615(2) 0.0273(6) Uani 1 1 d . . .
H8 H 0.1045 1.0023 0.8862 0.033 Uiso 1 1 calc R . .
C9 C 0.11654(13) 0.96253(13) 0.7782(2) 0.0313(6) Uani 1 1 d . . .
C10 C 0.15639(19) 1.0053(2) 0.7404(4) 0.0616(13) Uani 1 1 d . . .
H10 H 0.1664 1.0377 0.7700 0.074 Uiso 1 1 calc R . .
C11 C 0.1836(3) 1.0045(3) 0.6607(4) 0.091(3) Uani 1 1 d . . .
H11 H 0.2119 1.0360 0.6376 0.109 Uiso 1 1 calc R . .
C12 C 0.1704(2) 0.9593(2) 0.6148(3) 0.0638(14) Uani 1 1 d . . .
H12 H 0.1886 0.9583 0.5593 0.077 Uiso 1 1 calc R . .
C13 C 0.1292(2) 0.9148(2) 0.6528(3) 0.0521(10) Uani 1 1 d . . .
H13 H 0.1196 0.8826 0.6228 0.063 Uiso 1 1 calc R . .
C14 C 0.10126(17) 0.91478(17) 0.7322(3) 0.0427(8) Uani 1 1 d . . .
H14 H 0.0726 0.8835 0.7552 0.051 Uiso 1 1 calc R . .
C15 C 0.03186(13) 0.95316(12) 0.8293(2) 0.0297(6) Uani 1 1 d . . .
H15A H 0.0342 0.9817 0.7891 0.036 Uiso 1 1 calc R . .
H15B H 0.0158 0.9210 0.7902 0.036 Uiso 1 1 calc R . .
N1 N 0.07762(11) 0.93051(11) 0.94373(18) 0.0282(5) Uani 1 1 d . . .
N2 N 0.21054(15) 0.87360(18) 1.1897(3) 0.0521(9) Uani 1 1 d . . .
O1 O 0.02415(10) 0.86197(11) 1.09616(18) 0.0385(5) Uani 1 1 d . . .
O2 O 0.00085(8) 0.94633(10) 0.91214(14) 0.0289(4) Uani 1 1 d . . .
O3 O 0.20955(18) 0.8402(2) 1.2416(3) 0.0813(14) Uani 1 1 d . . .
O4 O 0.25168(13) 0.90907(18) 1.1557(3) 0.0721(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 2.021(2) 5_677 ?
Fe1 O2 2.021(2) 6_557 ?
Fe1 O2 2.021(2) . ?
Fe1 O2 2.021(2) 3_465 ?
Fe1 O2 2.021(2) 2_675 ?
Fe1 O2 2.021(2) 4_467 ?
Fe2 O1 1.941(3) 6_557 ?
Fe2 O1 1.941(3) . ?
Fe2 O2 2.009(2) . ?
Fe2 O2 2.009(2) 6_557 ?
Fe2 N1 2.149(3) . ?
Fe2 N1 2.149(3) 6_557 ?
C1 O1 1.299(4) . ?
C1 C6 1.421(5) . ?
C1 C2 1.432(5) . ?
C2 C3 1.327(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.417(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(5) . ?
C4 N2 1.437(5) . ?
C5 C6 1.408(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.436(5) . ?
C7 N1 1.302(4) . ?
C7 H7 0.9500 . ?
C8 N1 1.488(4) . ?
C8 C9 1.507(4) . ?
C8 C15 1.526(5) . ?
C8 H8 1.0000 . ?
C9 C10 1.339(6) . ?
C9 C14 1.410(5) . ?
C10 C11 1.378(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.358(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O2 1.424(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N2 O3 1.217(5) . ?
N2 O4 1.243(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O2 87.32(9) 5_677 6_557 ?
O2 Fe1 O2 131.85(13) 5_677 . ?
O2 Fe1 O2 74.29(13) 6_557 . ?
O2 Fe1 O2 134.19(12) 5_677 3_465 ?
O2 Fe1 O2 131.85(13) 6_557 3_465 ?
O2 Fe1 O2 87.32(9) . 3_465 ?
O2 Fe1 O2 74.29(13) 5_677 2_675 ?
O2 Fe1 O2 134.19(12) 6_557 2_675 ?
O2 Fe1 O2 87.32(9) . 2_675 ?
O2 Fe1 O2 87.32(9) 3_465 2_675 ?
O2 Fe1 O2 87.32(9) 5_677 4_467 ?
O2 Fe1 O2 87.32(9) 6_557 4_467 ?
O2 Fe1 O2 134.19(13) . 4_467 ?
O2 Fe1 O2 74.29(13) 3_465 4_467 ?
O2 Fe1 O2 131.85(13) 2_675 4_467 ?
O1 Fe2 O1 98.78(17) 6_557 . ?
O1 Fe2 O2 95.90(11) 6_557 . ?
O1 Fe2 O2 158.66(11) . . ?
O1 Fe2 O2 158.66(10) 6_557 6_557 ?
O1 Fe2 O2 95.90(11) . 6_557 ?
O2 Fe2 O2 74.81(13) . 6_557 ?
O1 Fe2 N1 92.47(11) 6_557 . ?
O1 Fe2 N1 86.88(11) . . ?
O2 Fe2 N1 77.05(10) . . ?
O2 Fe2 N1 103.76(10) 6_557 . ?
O1 Fe2 N1 86.88(11) 6_557 6_557 ?
O1 Fe2 N1 92.47(11) . 6_557 ?
O2 Fe2 N1 103.76(10) . 6_557 ?
O2 Fe2 N1 77.05(10) 6_557 6_557 ?
N1 Fe2 N1 179.00(16) . 6_557 ?
O1 C1 C6 124.9(3) . . ?
O1 C1 C2 118.0(3) . . ?
C6 C1 C2 117.0(3) . . ?
C3 C2 C1 122.8(4) . . ?
C3 C2 H2 118.6 . . ?
C1 C2 H2 118.6 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 N2 120.4(4) . . ?
C3 C4 N2 119.6(4) . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.2(3) . . ?
C5 C6 C7 117.0(3) . . ?
C1 C6 C7 123.9(3) . . ?
N1 C7 C6 124.2(3) . . ?
N1 C7 H7 117.9 . . ?
C6 C7 H7 117.9 . . ?
N1 C8 C9 115.7(3) . . ?
N1 C8 C15 105.5(2) . . ?
C9 C8 C15 110.9(3) . . ?
N1 C8 H8 108.2 . . ?
C9 C8 H8 108.2 . . ?
C15 C8 H8 108.2 . . ?
C10 C9 C14 117.9(4) . . ?
C10 C9 C8 121.0(3) . . ?
C14 C9 C8 120.9(3) . . ?
C9 C10 C11 123.2(5) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
C12 C11 C10 120.8(5) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 116.6(4) . . ?
C11 C12 H12 121.7 . . ?
C13 C12 H12 121.7 . . ?
C14 C13 C12 123.4(4) . . ?
C14 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C13 C14 C9 118.0(4) . . ?
C13 C14 H14 121.0 . . ?
C9 C14 H14 121.0 . . ?
O2 C15 C8 109.1(2) . . ?
O2 C15 H15A 109.9 . . ?
C8 C15 H15A 109.9 . . ?
O2 C15 H15B 109.9 . . ?
C8 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C7 N1 C8 118.6(3) . . ?
C7 N1 Fe2 127.0(2) . . ?
C8 N1 Fe2 114.1(2) . . ?
O3 N2 O4 122.1(4) . . ?
O3 N2 C4 119.5(4) . . ?
O4 N2 C4 118.4(4) . . ?
C1 O1 Fe2 133.0(2) . . ?
C15 O2 Fe2 110.63(18) . . ?
C15 O2 Fe1 129.7(2) . . ?
Fe2 O2 Fe1 105.45(9) . . ?

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
O1 C1 C2 C3 -178.3(4) . . . . ?
C6 C1 C2 C3 0.1(6) . . . . ?
C1 C2 C3 C4 0.8(7) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
C2 C3 C4 N2 178.7(4) . . . . ?
C3 C4 C5 C6 -3.2(6) . . . . ?
N2 C4 C5 C6 178.9(4) . . . . ?
C4 C5 C6 C1 4.0(6) . . . . ?
C4 C5 C6 C7 -177.8(3) . . . . ?
O1 C1 C6 C5 175.8(3) . . . . ?
C2 C1 C6 C5 -2.4(5) . . . . ?
O1 C1 C6 C7 -2.3(6) . . . . ?
C2 C1 C6 C7 179.5(3) . . . . ?
C5 C6 C7 N1 179.2(3) . . . . ?
C1 C6 C7 N1 -2.7(6) . . . . ?
N1 C8 C9 C10 -130.9(4) . . . . ?
C15 C8 C9 C10 109.1(4) . . . . ?
N1 C8 C9 C14 54.7(4) . . . . ?
C15 C8 C9 C14 -65.3(4) . . . . ?
C14 C9 C10 C11 -1.5(9) . . . . ?
C8 C9 C10 C11 -176.1(6) . . . . ?
C9 C10 C11 C12 1.0(12) . . . . ?
C10 C11 C12 C13 -0.7(11) . . . . ?
C11 C12 C13 C14 1.1(9) . . . . ?
C12 C13 C14 C9 -1.7(7) . . . . ?
C10 C9 C14 C13 1.8(6) . . . . ?
C8 C9 C14 C13 176.3(4) . . . . ?
N1 C8 C15 O2 42.2(3) . . . . ?
C9 C8 C15 O2 168.2(3) . . . . ?
C6 C7 N1 C8 178.7(3) . . . . ?
C6 C7 N1 Fe2 6.0(5) . . . . ?
C9 C8 N1 C7 50.3(4) . . . . ?
C15 C8 N1 C7 173.2(3) . . . . ?
C9 C8 N1 Fe2 -136.1(2) . . . . ?
C15 C8 N1 Fe2 -13.2(3) . . . . ?
O1 Fe2 N1 C7 -102.8(3) 6_557 . . . ?
O1 Fe2 N1 C7 -4.1(3) . . . . ?
O2 Fe2 N1 C7 161.7(3) . . . . ?
O2 Fe2 N1 C7 91.2(3) 6_557 . . . ?
N1 Fe2 N1 C7 -53.5(3) 6_557 . . . ?
O1 Fe2 N1 C8 84.2(2) 6_557 . . . ?
O1 Fe2 N1 C8 -177.1(2) . . . . ?
O2 Fe2 N1 C8 -11.3(2) . . . . ?
O2 Fe2 N1 C8 -81.8(2) 6_557 . . . ?
N1 Fe2 N1 C8 133.5(2) 6_557 . . . ?
C5 C4 N2 O3 -165.8(5) . . . . ?
C3 C4 N2 O3 16.2(7) . . . . ?
C5 C4 N2 O4 10.9(7) . . . . ?
C3 C4 N2 O4 -167.1(5) . . . . ?
C6 C1 O1 Fe2 3.4(6) . . . . ?
C2 C1 O1 Fe2 -178.4(3) . . . . ?
O1 Fe2 O1 C1 91.5(3) 6_557 . . . ?
O2 Fe2 O1 C1 -41.4(5) . . . . ?
O2 Fe2 O1 C1 -104.0(3) 6_557 . . . ?
N1 Fe2 O1 C1 -0.5(3) . . . . ?
N1 Fe2 O1 C1 178.7(3) 6_557 . . . ?
C8 C15 O2 Fe2 -55.2(3) . . . . ?
C8 C15 O2 Fe1 77.8(3) . . . . ?
O1 Fe2 O2 C15 -55.3(2) 6_557 . . . ?
O1 Fe2 O2 C15 78.0(3) . . . . ?
O2 Fe2 O2 C15 144.2(2) 6_557 . . . ?
N1 Fe2 O2 C15 35.86(19) . . . . ?
N1 Fe2 O2 C15 -143.55(19) 6_557 . . . ?
O1 Fe2 O2 Fe1 160.43(11) 6_557 . . . ?
O1 Fe2 O2 Fe1 -66.3(3) . . . . ?
O2 Fe2 O2 Fe1 0.0 6_557 . . . ?
N1 Fe2 O2 Fe1 -108.38(12) . . . . ?
N1 Fe2 O2 Fe1 72.21(12) 6_557 . . . ?
O2 Fe1 O2 C15 -63.2(2) 5_677 . . . ?
O2 Fe1 O2 C15 -134.7(3) 6_557 . . . ?
O2 Fe1 O2 C15 90.3(2) 3_465 . . . ?
O2 Fe1 O2 C15 2.8(2) 2_675 . . . ?
O2 Fe1 O2 C15 155.2(3) 4_467 . . . ?
O2 Fe1 O2 Fe2 71.51(8) 5_677 . . . ?
O2 Fe1 O2 Fe2 0.0 6_557 . . . ?
O2 Fe1 O2 Fe2 -134.99(14) 3_465 . . . ?
O2 Fe1 O2 Fe2 137.57(13) 2_675 . . . ?
O2 Fe1 O2 Fe2 -70.05(8) 4_467 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.079

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.007 -0.004 0.454 5519.3 941.0 ' '
_platon_squeeze_details          
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 941e per unit cell were accumulated which corresponds 
to 314e per formula(C90H72Fe4N12O24). The 314e might come from solvent DMA molecules (calculated number is about 7) and were not included in the formula.
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMA'
_chemical_compound_source        no
_exptl_crystal_preparation       'Magnetic properties'
_database_code_depnum_ccdc_archive 'CCDC 941226'
