# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_ig209bdssq
_database_code_depnum_ccdc_archive 'CCDC 869158'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe2 N12 Na O12'
_chemical_formula_sum            'C36 H30 Fe2 N12 Na O12'
_chemical_formula_weight         957.41

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'
Na Na 0.0362 0.0249 '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           cubic
_symmetry_space_group_name_H-M   'P n -3 n'
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'

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

_cell_length_a                   22.280(3)
_cell_length_b                   22.280(3)
_cell_length_c                   22.280(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11059(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    20556
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      26.73

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3912
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8777
_exptl_absorpt_correction_T_max  0.9488
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50908
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1639
_reflns_number_gt                1442
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2008)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond v.3.2e (Brandenburg, 2010)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+46.3734P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1639
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2208
_refine_ls_wR_factor_gt          0.2107
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_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 0.07881(3) 0.07881(3) 0.07881(3) 0.0270(5) Uani 1 3 d S . .
Na1 Na 0.0000 0.0000 0.0000 0.0248(10) Uani 1 6 d S . .
O1 O 0.05040(17) 0.11238(16) 0.15610(15) 0.0350(9) Uani 1 1 d . . .
O2 O 0.01150(15) 0.02061(15) 0.10193(14) 0.0281(8) Uani 1 1 d . . .
N1 N 0.0031(2) 0.08076(19) 0.18231(19) 0.0368(11) Uani 1 1 d . . .
H1 H -0.0132 0.0911 0.2168 0.044 Uiso 1 1 calc R . .
N2 N -0.1608(2) -0.0749(2) 0.2097(2) 0.0396(12) Uani 1 1 d . . .
C1 C -0.0146(2) 0.0354(2) 0.1516(2) 0.0284(11) Uani 1 1 d . . .
C2 C -0.0660(2) -0.0009(2) 0.1729(2) 0.0292(11) Uani 1 1 d . . .
C3 C -0.0886(2) -0.0462(2) 0.1362(2) 0.0337(12) Uani 1 1 d . . .
H3 H -0.0718 -0.0528 0.0975 0.040 Uiso 1 1 calc R . .
C4 C -0.1355(2) -0.0815(2) 0.1562(2) 0.0368(12) Uani 1 1 d . . .
H4 H -0.1504 -0.1119 0.1303 0.044 Uiso 1 1 calc R . .
C5 C -0.1398(2) -0.0305(3) 0.2448(3) 0.0394(13) Uani 1 1 d . . .
H5 H -0.1578 -0.0247 0.2830 0.047 Uiso 1 1 calc R . .
C6 C -0.0930(2) 0.0072(2) 0.2280(2) 0.0335(12) Uani 1 1 d . . .
H6 H -0.0797 0.0382 0.2542 0.040 Uiso 1 1 calc R . .

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 0.0270(5) 0.0270(5) 0.0270(5) -0.0031(3) -0.0031(3) -0.0031(3)
Na1 0.0248(10) 0.0248(10) 0.0248(10) -0.0013(10) -0.0013(10) -0.0013(10)
O1 0.046(2) 0.0323(19) 0.0265(18) -0.0067(15) 0.0020(16) -0.0064(17)
O2 0.0324(19) 0.0292(18) 0.0229(16) -0.0032(14) 0.0026(14) -0.0005(14)
N1 0.051(3) 0.038(2) 0.022(2) -0.0046(18) 0.004(2) -0.005(2)
N2 0.027(2) 0.043(3) 0.048(3) 0.011(2) 0.008(2) 0.004(2)
C1 0.036(3) 0.025(3) 0.024(2) 0.004(2) -0.002(2) 0.008(2)
C2 0.028(2) 0.032(3) 0.028(3) 0.006(2) -0.001(2) 0.008(2)
C3 0.037(3) 0.035(3) 0.029(3) 0.006(2) 0.001(2) 0.002(2)
C4 0.031(3) 0.041(3) 0.039(3) -0.001(2) -0.001(2) 0.001(2)
C5 0.036(3) 0.046(3) 0.036(3) 0.011(3) 0.011(2) 0.016(2)
C6 0.034(3) 0.034(3) 0.032(3) 0.006(2) 0.004(2) 0.011(2)

_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 O1 1.981(3) 12 ?
Fe1 O1 1.981(3) 11 ?
Fe1 O1 1.981(3) . yes
Fe1 O2 2.048(3) . yes
Fe1 O2 2.048(3) 11 ?
Fe1 O2 2.048(3) 12 ?
Fe1 Na1 3.0414(12) . yes
Na1 O2 2.331(3) 11 ?
Na1 O2 2.331(3) 12 ?
Na1 O2 2.331(3) . yes
Na1 O2 2.331(3) 36 ?
Na1 O2 2.331(3) 35 ?
Na1 O2 2.331(3) 25 ?
Na1 Fe1 3.0414(12) 25 ?
O1 N1 1.396(6) . yes
O2 C1 1.294(6) . yes
N1 C1 1.283(6) . yes
N1 H1 0.8800 . ?
N2 C4 1.328(7) . ?
N2 C5 1.344(8) . ?
C1 C2 1.477(7) . ?
C2 C6 1.380(7) . ?
C2 C3 1.394(7) . ?
C3 C4 1.382(8) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.391(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 94.03(14) 12 11 ?
O1 Fe1 O1 94.02(14) 12 . ?
O1 Fe1 O1 94.02(14) 11 . ?
O1 Fe1 O2 155.08(14) 12 . ?
O1 Fe1 O2 109.83(14) 11 . ?
O1 Fe1 O2 77.68(13) . . ?
O1 Fe1 O2 109.83(14) 12 11 ?
O1 Fe1 O2 77.68(13) 11 11 ?
O1 Fe1 O2 155.08(14) . 11 ?
O2 Fe1 O2 83.09(14) . 11 ?
O1 Fe1 O2 77.68(13) 12 12 ?
O1 Fe1 O2 155.08(14) 11 12 ?
O1 Fe1 O2 109.83(14) . 12 ?
O2 Fe1 O2 83.09(14) . 12 ?
O2 Fe1 O2 83.09(14) 11 12 ?
O1 Fe1 Na1 122.36(11) 12 . ?
O1 Fe1 Na1 122.36(11) 11 . ?
O1 Fe1 Na1 122.36(11) . . ?
O2 Fe1 Na1 49.98(9) . . ?
O2 Fe1 Na1 49.98(9) 11 . ?
O2 Fe1 Na1 49.98(9) 12 . ?
O2 Na1 O2 71.30(12) 11 12 ?
O2 Na1 O2 71.30(12) 11 . ?
O2 Na1 O2 71.30(12) 12 . ?
O2 Na1 O2 108.70(12) 11 36 ?
O2 Na1 O2 180.0 12 36 ?
O2 Na1 O2 108.70(12) . 36 ?
O2 Na1 O2 180.00(3) 11 35 ?
O2 Na1 O2 108.70(12) 12 35 ?
O2 Na1 O2 108.70(12) . 35 ?
O2 Na1 O2 71.29(12) 36 35 ?
O2 Na1 O2 108.70(12) 11 25 ?
O2 Na1 O2 108.70(12) 12 25 ?
O2 Na1 O2 180.0 . 25 ?
O2 Na1 O2 71.30(12) 36 25 ?
O2 Na1 O2 71.30(12) 35 25 ?
O2 Na1 Fe1 42.30(8) 11 . ?
O2 Na1 Fe1 42.30(8) 12 . ?
O2 Na1 Fe1 42.30(8) . . ?
O2 Na1 Fe1 137.70(8) 36 . ?
O2 Na1 Fe1 137.70(8) 35 . ?
O2 Na1 Fe1 137.70(8) 25 . ?
O2 Na1 Fe1 137.70(8) 11 25 ?
O2 Na1 Fe1 137.70(8) 12 25 ?
O2 Na1 Fe1 137.70(8) . 25 ?
O2 Na1 Fe1 42.30(8) 36 25 ?
O2 Na1 Fe1 42.30(8) 35 25 ?
O2 Na1 Fe1 42.30(8) 25 25 ?
Fe1 Na1 Fe1 180.0 . 25 ?
N1 O1 Fe1 114.5(3) . . ?
C1 O2 Fe1 112.6(3) . . ?
C1 O2 Na1 146.6(3) . . ?
Fe1 O2 Na1 87.72(11) . . ?
C1 N1 O1 114.0(4) . . ?
C1 N1 H1 123.0 . . ?
O1 N1 H1 123.0 . . ?
C4 N2 C5 117.1(5) . . ?
N1 C1 O2 121.2(5) . . ?
N1 C1 C2 119.9(4) . . ?
O2 C1 C2 118.9(4) . . ?
C6 C2 C3 117.4(5) . . ?
C6 C2 C1 123.4(5) . . ?
C3 C2 C1 119.2(4) . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
N2 C4 C3 123.2(5) . . ?
N2 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
N2 C5 C6 123.4(5) . . ?
N2 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C2 C6 C5 119.2(5) . . ?
C2 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.143

# 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 0.137 0.238 0.251 1744 436 ' '
2 -0.143 0.732 0.752 1744 436 ' '
_platon_squeeze_details          
;
The crystal under investigation was diffracting only weakly due to partial lost
of solvent. The solvent/anion system was heavily disordered and could not be
resolved unambiguously. Therefore, the contribution of the missing
molecules and anions to the calculated structure factors was taken into account
with the BYPASS algorithm (van der Sluis & Spek, 1990), implemented as the
SQUEEZE option in PLATON (Spek, 2003). The missing molecules and anions were
not taken into account in unit cell content.
;

# start Validation Reply Form
_vrf_PUBL601_GLOBAL              
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 1744.00 A**3
RESPONSE: The disordered solvent/anion molecules could not be resolved
unambiguously. Therefore, the contribution of the missing
molecules and anions to the calculated structure factors was taken into account
with the BYPASS algorithm (van der Sluis & Spek, 1990), implemented as the
SQUEEZE option in PLATON (Spek, 2003). The missing molecules and anions were
not taken into account in unit cell content.
;
# end Validation Reply Form