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


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Hui Li'
_publ_contact_author_email       lihui@bit.edu.cn
loop_
_publ_author_name
'Gui-Lei Liu'
'Shu-fang He'
'Shaowen Zhang'
'Hui Li'

data_bo348
_database_code_depnum_ccdc_archive 'CCDC 759722'
#TrackingRef '759722.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H24 Fe N2 Na O12'
_chemical_formula_weight         539.23

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   20.159(17)
_cell_length_b                   12.469(10)
_cell_length_c                   8.897(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.465(15)
_cell_angle_gamma                90.00
_cell_volume                     2199(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7825
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14842
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_sigmaI/netI    0.1186
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.99
_reflns_number_total             4306
_reflns_number_gt                2145
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0869P)^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         4306
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0734
_refine_ls_wR_factor_ref         0.1992
_refine_ls_wR_factor_gt          0.1720
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_restrained_S_all      0.940
_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 0.74821(4) 0.51857(5) 0.27270(10) 0.0378(3) Uani 1 1 d . . .
Na1 Na 0.54931(10) 0.44294(15) 0.6766(2) 0.0371(5) Uani 1 1 d . . .
O1 O 0.83124(18) 0.5109(3) 0.4191(5) 0.0446(10) Uani 1 1 d . . .
O2 O 0.66406(18) 0.5718(3) 0.1303(4) 0.0422(10) Uani 1 1 d . . .
O3 O 0.59045(18) 0.7042(3) 0.0578(4) 0.0400(9) Uani 1 1 d . . .
O4 O 0.7953(2) 0.5161(3) 0.1015(5) 0.0462(11) Uani 1 1 d . . .
O5 O 0.68654(17) 0.4763(2) 0.4288(4) 0.0341(9) Uani 1 1 d . . .
O6 O 0.61650(17) 0.3533(2) 0.4971(4) 0.0341(9) Uani 1 1 d . . .
N1 N 0.7429(2) 0.6810(3) 0.3420(5) 0.0350(11) Uani 1 1 d . . .
N2 N 0.7282(2) 0.3562(3) 0.2260(5) 0.0330(10) Uani 1 1 d . . .
C1 C 0.8673(3) 0.5791(4) 0.5140(7) 0.0412(15) Uani 1 1 d . . .
C2 C 0.9292(3) 0.5467(4) 0.5991(7) 0.0398(14) Uani 1 1 d . . .
H2 H 0.9456 0.4770 0.5824 0.048 Uiso 1 1 calc R . .
C3 C 0.9676(3) 0.6119(4) 0.7066(7) 0.0464(15) Uani 1 1 d . . .
H3 H 1.0093 0.5866 0.7627 0.056 Uiso 1 1 calc R . .
C4 C 0.9448(3) 0.7161(4) 0.7332(7) 0.0438(14) Uani 1 1 d . . .
H4 H 0.9701 0.7608 0.8093 0.053 Uiso 1 1 calc R . .
C5 C 0.8843(3) 0.7522(4) 0.6454(7) 0.0413(15) Uani 1 1 d . . .
H5 H 0.8693 0.8230 0.6601 0.050 Uiso 1 1 calc R . .
C6 C 0.8453(3) 0.6859(4) 0.5355(6) 0.0349(13) Uani 1 1 d . . .
C7 C 0.7839(2) 0.7321(4) 0.4483(6) 0.0320(12) Uani 1 1 d . . .
C8 C 0.6833(3) 0.7388(4) 0.2612(7) 0.0379(14) Uani 1 1 d . . .
H8A H 0.6979 0.8036 0.2119 0.046 Uiso 1 1 calc R . .
H8B H 0.6551 0.7619 0.3355 0.046 Uiso 1 1 calc R . .
C9 C 0.6418(3) 0.6673(4) 0.1404(6) 0.0331(13) Uani 1 1 d . . .
C10 C 0.8307(3) 0.4376(4) 0.0539(7) 0.0417(14) Uani 1 1 d . . .
C11 C 0.8829(3) 0.4615(4) -0.0259(7) 0.0489(16) Uani 1 1 d . . .
H11 H 0.8929 0.5343 -0.0443 0.059 Uiso 1 1 calc R . .
C12 C 0.9201(3) 0.3809(4) -0.0780(6) 0.0413(14) Uani 1 1 d . . .
H12 H 0.9548 0.3985 -0.1329 0.050 Uiso 1 1 calc R . .
C13 C 0.9066(3) 0.2738(4) -0.0500(6) 0.0394(14) Uani 1 1 d . . .
H13 H 0.9321 0.2187 -0.0864 0.047 Uiso 1 1 calc R . .
C14 C 0.8572(3) 0.2478(4) 0.0289(6) 0.0359(13) Uani 1 1 d . . .
H14 H 0.8493 0.1744 0.0482 0.043 Uiso 1 1 calc R . .
C15 C 0.8169(3) 0.3279(4) 0.0838(6) 0.0345(13) Uani 1 1 d . . .
C16 C 0.7648(2) 0.2918(4) 0.1619(6) 0.0324(12) Uani 1 1 d . . .
C17 C 0.6728(3) 0.3110(4) 0.2892(6) 0.0345(13) Uani 1 1 d . . .
H17A H 0.6852 0.2385 0.3303 0.041 Uiso 1 1 calc R . .
H17B H 0.6324 0.3043 0.2078 0.041 Uiso 1 1 calc R . .
C18 C 0.6570(3) 0.3830(4) 0.4162(6) 0.0338(12) Uani 1 1 d . . .
O7 O 0.4398(2) 0.4177(3) 0.5131(4) 0.0380(9) Uani 1 1 d . . .
O8 O 0.5256(2) 0.2840(3) 0.8079(5) 0.0666(14) Uani 1 1 d . . .
H08A H 0.5503 0.2483 0.8817 0.080 Uiso 1 1 d R . .
H08B H 0.4801 0.2884 0.8331 0.080 Uiso 1 1 d R . .
O9 O 0.5018(2) 0.5641(3) 0.8339(5) 0.0714(14) Uani 1 1 d . . .
H09A H 0.5320 0.5931 0.9031 0.086 Uiso 1 1 d R . .
H09B H 0.4656 0.6089 0.7950 0.086 Uiso 1 1 d R . .
O10 O 0.6523(2) 0.4553(3) 0.8483(6) 0.0790(16) Uani 1 1 d . . .
H00A H 0.6820 0.4824 0.8030 0.095 Uiso 1 1 d R . .
H00B H 0.6469 0.4965 0.9269 0.095 Uiso 1 1 d R . .
O11 O 0.7559(2) 0.5164(4) 0.7194(6) 0.038(2) Uani 0.648(12) 1 d P . .
H01A H 0.7323 0.4923 0.6376 0.046 Uiso 1 1 d R . .
H01B H 0.7663 0.5162 0.8164 0.046 Uiso 1 1 d R . .
H70A H 0.428(3) 0.348(6) 0.473(7) 0.09(2) Uiso 1 1 d . . .
H70B H 0.390(3) 0.437(5) 0.510(8) 0.10(3) Uiso 1 1 d . . .

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 0.0516(6) 0.0135(4) 0.0518(6) -0.0003(3) 0.0189(4) 0.0025(3)
Na1 0.0482(13) 0.0261(11) 0.0371(13) 0.0010(9) 0.0081(10) 0.0014(9)
O1 0.047(2) 0.0140(19) 0.073(3) -0.0021(18) 0.011(2) 0.0045(15)
O2 0.058(3) 0.0168(19) 0.051(3) -0.0036(16) 0.009(2) 0.0100(16)
O3 0.049(2) 0.023(2) 0.050(3) 0.0041(17) 0.013(2) 0.0048(17)
O4 0.077(3) 0.0177(19) 0.055(3) 0.0084(17) 0.039(2) 0.0095(17)
O5 0.043(2) 0.0211(19) 0.041(2) -0.0051(15) 0.0156(18) 0.0004(15)
O6 0.046(2) 0.0230(19) 0.036(2) -0.0013(15) 0.0140(18) 0.0000(15)
N1 0.043(3) 0.016(2) 0.050(3) 0.006(2) 0.019(2) 0.0072(18)
N2 0.048(3) 0.014(2) 0.038(3) -0.0010(18) 0.013(2) -0.0063(18)
C1 0.052(4) 0.019(3) 0.057(4) 0.007(3) 0.022(3) -0.006(2)
C2 0.041(3) 0.021(3) 0.063(4) 0.006(3) 0.024(3) 0.004(2)
C3 0.036(3) 0.036(3) 0.071(5) 0.013(3) 0.021(3) 0.001(3)
C4 0.051(4) 0.034(3) 0.049(4) 0.000(3) 0.017(3) -0.002(3)
C5 0.050(4) 0.021(3) 0.058(4) 0.000(3) 0.024(3) 0.000(2)
C6 0.044(3) 0.021(3) 0.044(4) 0.001(2) 0.018(3) 0.002(2)
C7 0.037(3) 0.024(3) 0.037(3) 0.003(2) 0.015(3) -0.005(2)
C8 0.052(4) 0.016(3) 0.049(4) 0.000(2) 0.018(3) 0.006(2)
C9 0.041(3) 0.024(3) 0.041(3) 0.007(2) 0.027(3) 0.000(2)
C10 0.058(4) 0.026(3) 0.045(4) 0.000(3) 0.020(3) 0.004(3)
C11 0.072(4) 0.027(3) 0.054(4) 0.009(3) 0.027(3) 0.004(3)
C12 0.048(4) 0.034(3) 0.044(4) 0.006(3) 0.014(3) 0.006(3)
C13 0.049(3) 0.026(3) 0.045(4) -0.005(2) 0.013(3) 0.005(2)
C14 0.047(3) 0.015(3) 0.045(4) -0.003(2) 0.009(3) 0.000(2)
C15 0.057(4) 0.014(3) 0.034(3) -0.002(2) 0.009(3) 0.004(2)
C16 0.035(3) 0.027(3) 0.036(3) 0.003(2) 0.009(2) 0.008(2)
C17 0.052(3) 0.015(3) 0.039(3) -0.004(2) 0.013(3) -0.003(2)
C18 0.046(3) 0.019(3) 0.036(3) 0.001(2) 0.006(3) 0.008(2)
O7 0.048(2) 0.023(2) 0.041(2) -0.0020(17) 0.0039(19) -0.0005(17)
O8 0.061(3) 0.063(3) 0.083(4) 0.043(3) 0.032(3) 0.018(2)
O9 0.079(3) 0.070(3) 0.062(3) -0.020(3) 0.005(3) 0.031(3)
O10 0.074(3) 0.057(3) 0.094(4) -0.040(3) -0.019(3) 0.020(2)
O11 0.053(4) 0.039(4) 0.022(3) -0.004(2) 0.003(3) -0.010(3)

_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 1.927(4) . ?
Fe1 O4 1.936(4) . ?
Fe1 O2 2.035(4) . ?
Fe1 N2 2.091(4) . ?
Fe1 O5 2.092(4) . ?
Fe1 N1 2.125(4) . ?
Na1 O10 2.348(5) . ?
Na1 O9 2.376(4) . ?
Na1 O8 2.393(4) . ?
Na1 O7 2.434(5) . ?
Na1 O7 2.459(4) 3_666 ?
Na1 O6 2.534(4) . ?
Na1 Na1 3.686(5) 3_666 ?
O1 C1 1.319(6) . ?
O2 C9 1.281(6) . ?
O3 C9 1.245(6) . ?
O4 C10 1.327(6) . ?
O5 C18 1.303(6) . ?
O6 C18 1.239(6) . ?
N1 C7 1.304(6) . ?
N1 C8 1.472(6) . ?
N2 C16 1.291(6) . ?
N2 C17 1.452(6) . ?
C1 C2 1.398(8) . ?
C1 C6 1.428(7) . ?
C2 C3 1.380(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.413(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.454(7) . ?
C8 C9 1.524(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.403(7) . ?
C10 C15 1.430(7) . ?
C11 C12 1.383(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.357(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.428(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.434(7) . ?
C17 C18 1.521(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
O7 Na1 2.459(4) 3_666 ?
O7 H70A 0.96(7) . ?
O7 H70B 1.02(7) . ?
O8 H08A 0.8707 . ?
O8 H08B 0.9852 . ?
O9 H09A 0.8609 . ?
O9 H09B 0.9343 . ?
O10 H00A 0.8498 . ?
O10 H00B 0.8893 . ?
O11 H01A 0.8488 . ?
O11 H01B 0.8500 . ?

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 O4 92.37(19) . . ?
O1 Fe1 O2 163.78(14) . . ?
O4 Fe1 O2 89.30(17) . . ?
O1 Fe1 N2 101.45(15) . . ?
O4 Fe1 N2 86.15(15) . . ?
O2 Fe1 N2 94.77(16) . . ?
O1 Fe1 O5 94.98(17) . . ?
O4 Fe1 O5 162.47(14) . . ?
O2 Fe1 O5 88.07(16) . . ?
N2 Fe1 O5 76.81(14) . . ?
O1 Fe1 N1 86.26(16) . . ?
O4 Fe1 N1 107.52(15) . . ?
O2 Fe1 N1 77.86(16) . . ?
N2 Fe1 N1 164.17(16) . . ?
O5 Fe1 N1 88.85(14) . . ?
O10 Na1 O9 88.75(17) . . ?
O10 Na1 O8 88.19(18) . . ?
O9 Na1 O8 95.85(18) . . ?
O10 Na1 O7 174.96(18) . . ?
O9 Na1 O7 90.89(17) . . ?
O8 Na1 O7 86.85(15) . . ?
O10 Na1 O7 102.79(17) . 3_666 ?
O9 Na1 O7 92.91(17) . 3_666 ?
O8 Na1 O7 166.11(17) . 3_666 ?
O7 Na1 O7 82.25(15) . 3_666 ?
O10 Na1 O6 85.90(16) . . ?
O9 Na1 O6 166.04(16) . . ?
O8 Na1 O6 96.86(15) . . ?
O7 Na1 O6 95.55(15) . . ?
O7 Na1 O6 75.78(14) 3_666 . ?
O10 Na1 Na1 143.65(16) . 3_666 ?
O9 Na1 Na1 92.53(15) . 3_666 ?
O8 Na1 Na1 127.70(15) . 3_666 ?
O7 Na1 Na1 41.39(10) . 3_666 ?
O7 Na1 Na1 40.86(10) 3_666 3_666 ?
O6 Na1 Na1 84.26(12) . 3_666 ?
C1 O1 Fe1 135.2(3) . . ?
C9 O2 Fe1 121.5(4) . . ?
C10 O4 Fe1 129.2(3) . . ?
C18 O5 Fe1 119.0(3) . . ?
C18 O6 Na1 135.9(3) . . ?
C7 N1 C8 118.0(4) . . ?
C7 N1 Fe1 128.1(4) . . ?
C8 N1 Fe1 113.9(3) . . ?
C16 N2 C17 118.1(4) . . ?
C16 N2 Fe1 125.8(3) . . ?
C17 N2 Fe1 115.7(3) . . ?
O1 C1 C2 119.6(5) . . ?
O1 C1 C6 122.6(5) . . ?
C2 C1 C6 117.7(5) . . ?
C3 C2 C1 122.6(5) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 121.3(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 119.6(5) . . ?
C5 C6 C7 116.9(5) . . ?
C1 C6 C7 123.5(5) . . ?
N1 C7 C6 124.0(5) . . ?
N1 C8 C9 110.6(4) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O3 C9 O2 124.5(5) . . ?
O3 C9 C8 119.4(4) . . ?
O2 C9 C8 116.0(5) . . ?
O4 C10 C11 120.1(5) . . ?
O4 C10 C15 120.8(5) . . ?
C11 C10 C15 119.1(5) . . ?
C12 C11 C10 121.1(5) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.1(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.4(5) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 121.7(5) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C10 117.5(5) . . ?
C14 C15 C16 117.3(4) . . ?
C10 C15 C16 125.1(4) . . ?
N2 C16 C15 123.1(5) . . ?
N2 C17 C18 109.8(4) . . ?
N2 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
N2 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
O6 C18 O5 123.8(4) . . ?
O6 C18 C17 120.3(4) . . ?
O5 C18 C17 115.9(4) . . ?
Na1 O7 Na1 97.75(15) . 3_666 ?
Na1 O7 H70A 119(4) . . ?
Na1 O7 H70A 116(4) 3_666 . ?
Na1 O7 H70B 139(4) . . ?
Na1 O7 H70B 91(4) 3_666 . ?
H70A O7 H70B 92(5) . . ?
Na1 O8 H08A 130.8 . . ?
Na1 O8 H08B 110.0 . . ?
H08A O8 H08B 106.6 . . ?
Na1 O9 H09A 112.3 . . ?
Na1 O9 H09B 122.2 . . ?
H09A O9 H09B 114.7 . . ?
Na1 O10 H00A 109.5 . . ?
Na1 O10 H00B 109.2 . . ?
H00A O10 H00B 109.9 . . ?
H01A O11 H01B 149.9 . . ?

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
O4 Fe1 O1 C1 105.9(5) . . . . ?
O2 Fe1 O1 C1 10.3(9) . . . . ?
N2 Fe1 O1 C1 -167.5(5) . . . . ?
O5 Fe1 O1 C1 -90.0(5) . . . . ?
N1 Fe1 O1 C1 -1.5(5) . . . . ?
O1 Fe1 O2 C9 -14.8(8) . . . . ?
O4 Fe1 O2 C9 -110.9(4) . . . . ?
N2 Fe1 O2 C9 163.1(4) . . . . ?
O5 Fe1 O2 C9 86.5(4) . . . . ?
N1 Fe1 O2 C9 -2.8(3) . . . . ?
O1 Fe1 O4 C10 67.2(5) . . . . ?
O2 Fe1 O4 C10 -128.9(5) . . . . ?
N2 Fe1 O4 C10 -34.1(5) . . . . ?
O5 Fe1 O4 C10 -47.6(8) . . . . ?
N1 Fe1 O4 C10 154.1(5) . . . . ?
O1 Fe1 O5 C18 -110.1(4) . . . . ?
O4 Fe1 O5 C18 4.3(7) . . . . ?
O2 Fe1 O5 C18 85.9(4) . . . . ?
N2 Fe1 O5 C18 -9.5(4) . . . . ?
N1 Fe1 O5 C18 163.8(4) . . . . ?
O10 Na1 O6 C18 -74.3(5) . . . . ?
O9 Na1 O6 C18 -6.6(10) . . . . ?
O8 Na1 O6 C18 -162.0(5) . . . . ?
O7 Na1 O6 C18 110.6(5) . . . . ?
O7 Na1 O6 C18 30.0(5) 3_666 . . . ?
Na1 Na1 O6 C18 70.7(5) 3_666 . . . ?
O1 Fe1 N1 C7 -2.9(4) . . . . ?
O4 Fe1 N1 C7 -94.2(5) . . . . ?
O2 Fe1 N1 C7 -179.6(4) . . . . ?
N2 Fe1 N1 C7 117.0(7) . . . . ?
O5 Fe1 N1 C7 92.1(4) . . . . ?
O1 Fe1 N1 C8 179.7(3) . . . . ?
O4 Fe1 N1 C8 88.4(3) . . . . ?
O2 Fe1 N1 C8 3.0(3) . . . . ?
N2 Fe1 N1 C8 -60.4(8) . . . . ?
O5 Fe1 N1 C8 -85.2(3) . . . . ?
O1 Fe1 N2 C16 -64.3(5) . . . . ?
O4 Fe1 N2 C16 27.3(4) . . . . ?
O2 Fe1 N2 C16 116.3(4) . . . . ?
O5 Fe1 N2 C16 -156.8(5) . . . . ?
N1 Fe1 N2 C16 177.6(6) . . . . ?
O1 Fe1 N2 C17 107.6(4) . . . . ?
O4 Fe1 N2 C17 -160.7(4) . . . . ?
O2 Fe1 N2 C17 -71.8(4) . . . . ?
O5 Fe1 N2 C17 15.1(3) . . . . ?
N1 Fe1 N2 C17 -10.4(9) . . . . ?
Fe1 O1 C1 C2 -175.7(4) . . . . ?
Fe1 O1 C1 C6 5.0(8) . . . . ?
O1 C1 C2 C3 -176.2(5) . . . . ?
C6 C1 C2 C3 3.1(8) . . . . ?
C1 C2 C3 C4 -0.5(8) . . . . ?
C2 C3 C4 C5 -2.1(8) . . . . ?
C3 C4 C5 C6 2.0(8) . . . . ?
C4 C5 C6 C1 0.6(8) . . . . ?
C4 C5 C6 C7 -178.8(5) . . . . ?
O1 C1 C6 C5 176.2(5) . . . . ?
C2 C1 C6 C5 -3.1(8) . . . . ?
O1 C1 C6 C7 -4.4(8) . . . . ?
C2 C1 C6 C7 176.3(5) . . . . ?
C8 N1 C7 C6 -178.9(4) . . . . ?
Fe1 N1 C7 C6 3.8(7) . . . . ?
C5 C6 C7 N1 179.5(5) . . . . ?
C1 C6 C7 N1 0.1(8) . . . . ?
C7 N1 C8 C9 179.3(4) . . . . ?
Fe1 N1 C8 C9 -3.0(5) . . . . ?
Fe1 O2 C9 O3 -179.4(4) . . . . ?
Fe1 O2 C9 C8 1.8(6) . . . . ?
N1 C8 C9 O3 -177.9(4) . . . . ?
N1 C8 C9 O2 0.9(6) . . . . ?
Fe1 O4 C10 C11 -152.9(5) . . . . ?
Fe1 O4 C10 C15 26.6(8) . . . . ?
O4 C10 C11 C12 -179.3(6) . . . . ?
C15 C10 C11 C12 1.2(9) . . . . ?
C10 C11 C12 C13 -0.8(9) . . . . ?
C11 C12 C13 C14 -0.3(9) . . . . ?
C12 C13 C14 C15 1.0(9) . . . . ?
C13 C14 C15 C10 -0.6(8) . . . . ?
C13 C14 C15 C16 178.2(5) . . . . ?
O4 C10 C15 C14 180.0(5) . . . . ?
C11 C10 C15 C14 -0.5(8) . . . . ?
O4 C10 C15 C16 1.3(9) . . . . ?
C11 C10 C15 C16 -179.2(6) . . . . ?
C17 N2 C16 C15 174.3(5) . . . . ?
Fe1 N2 C16 C15 -13.9(8) . . . . ?
C14 C15 C16 N2 175.0(5) . . . . ?
C10 C15 C16 N2 -6.4(9) . . . . ?
C16 N2 C17 C18 154.5(5) . . . . ?
Fe1 N2 C17 C18 -18.1(5) . . . . ?
Na1 O6 C18 O5 14.7(8) . . . . ?
Na1 O6 C18 C17 -162.9(3) . . . . ?
Fe1 O5 C18 O6 -175.6(4) . . . . ?
Fe1 O5 C18 C17 2.1(6) . . . . ?
N2 C17 C18 O6 -171.8(5) . . . . ?
N2 C17 C18 O5 10.3(6) . . . . ?
O10 Na1 O7 Na1 179(100) . . . 3_666 ?
O9 Na1 O7 Na1 92.81(18) . . . 3_666 ?
O8 Na1 O7 Na1 -171.38(17) . . . 3_666 ?
O7 Na1 O7 Na1 0.0 3_666 . . 3_666 ?
O6 Na1 O7 Na1 -74.79(15) . . . 3_666 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.109

# Attachment '759723.cif'

data_bo358
_database_code_depnum_ccdc_archive 'CCDC 759723'
#TrackingRef '759723.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H18.50 Fe N O8.75'
_chemical_formula_weight         420.67

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.582(2)
_cell_length_b                   13.473(3)
_cell_length_c                   14.861(3)
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 75.51(3)
_cell_angle_gamma                69.66(3)
_cell_volume                     1914.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needlelike
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             870
_exptl_absorpt_coefficient_mu    0.833
_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      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15699
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8412
_reflns_number_gt                6536
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1497P)^2^+3.5084P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8412
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0910
_refine_ls_wR_factor_ref         0.2808
_refine_ls_wR_factor_gt          0.2615
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.012
_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 0.06183(8) 0.51651(6) 1.08209(5) 0.0301(2) Uani 1 1 d . . .
Fe2 Fe 0.05382(8) -0.05091(6) 0.39432(5) 0.0299(2) Uani 1 1 d . . .
O2 O 0.1269(4) -0.0105(3) 0.4994(2) 0.0289(8) Uani 1 1 d . . .
O18 O -0.0450(4) 0.6004(3) 0.9934(3) 0.0297(8) Uani 1 1 d . . .
N2 N 0.2506(5) 0.4717(3) 0.9748(3) 0.0305(9) Uani 1 1 d . . .
O4 O 0.2469(4) -0.1127(3) 0.3213(3) 0.0355(9) Uani 1 1 d . . .
O19 O 0.0607(4) -0.1968(3) 0.4274(3) 0.0365(9) Uani 1 1 d . . .
O1 O -0.0393(4) -0.0487(3) 0.2976(3) 0.0372(9) Uani 1 1 d . . .
O3 O 0.1123(4) 0.6283(3) 1.1259(3) 0.0355(9) Uani 1 1 d . . .
N1 N 0.0521(5) 0.1023(4) 0.3635(3) 0.0328(10) Uani 1 1 d . . .
O21 O 0.1575(4) 0.4117(3) 1.1561(3) 0.0374(9) Uani 1 1 d . . .
C59 C -0.1787(5) 0.6810(4) 1.0307(4) 0.0319(11) Uani 1 1 d . . .
H59 H -0.1697 0.7301 1.0752 0.038 Uiso 1 1 calc R . .
C30 C 0.2069(6) 0.7623(4) 1.1310(4) 0.0349(12) Uani 1 1 d . . .
H30A H 0.1387 0.7936 1.1862 0.042 Uiso 1 1 calc R . .
C29 C 0.3377(5) 0.5205(4) 0.9556(4) 0.0323(11) Uani 1 1 d . . .
H29A H 0.4171 0.4912 0.9060 0.039 Uiso 1 1 calc R . .
C28 C 0.2047(6) 0.0571(5) 0.4658(4) 0.0327(11) Uani 1 1 d . . .
H28A H 0.2252 0.0861 0.5186 0.039 Uiso 1 1 calc R . .
C27 C 0.3199(6) 0.6179(4) 1.0064(4) 0.0318(11) Uani 1 1 d . . .
C26 C 0.4822(6) -0.1307(5) 0.2604(4) 0.0374(13) Uani 1 1 d . . .
H26A H 0.4909 -0.1818 0.2148 0.045 Uiso 1 1 calc R . .
C25 C -0.0601(6) 0.0152(5) 0.2307(4) 0.0361(12) Uani 1 1 d . . .
C24 C -0.1121(6) -0.0128(5) 0.1595(4) 0.0403(13) Uani 1 1 d . . .
H24A H -0.1298 -0.0758 0.1605 0.048 Uiso 1 1 calc R . .
C23 C 0.2768(6) 0.3742(4) 0.9155(4) 0.0328(12) Uani 1 1 d . . .
H23 H 0.3745 0.3268 0.9047 0.039 Uiso 1 1 calc R . .
C22 C 0.3411(6) -0.0037(4) 0.3941(4) 0.0330(11) Uani 1 1 d . . .
C21 C 0.0216(6) 0.1492(5) 0.2933(4) 0.0359(12) Uani 1 1 d . . .
H21A H 0.0361 0.2132 0.2843 0.043 Uiso 1 1 calc R . .
C20 C 0.3528(6) -0.0821(4) 0.3261(4) 0.0342(12) Uani 1 1 d . . .
C19 C 0.4075(6) 0.7625(5) 1.0108(4) 0.0380(13) Uani 1 1 d . . .
H19A H 0.4706 0.7951 0.9845 0.046 Uiso 1 1 calc R . .
C18 C -0.2982(6) 0.8525(4) 0.9724(4) 0.0364(13) Uani 1 1 d . . .
H18A H -0.3005 0.8854 1.0281 0.044 Uiso 1 1 calc R . .
C17 C 0.2469(6) 0.4078(4) 0.8233(4) 0.0328(12) Uani 1 1 d . . .
C16 C -0.2354(6) 0.7441(4) 0.9553(4) 0.0348(12) Uani 1 1 d . . .
C15 C -0.0342(6) 0.1112(5) 0.2261(4) 0.0365(12) Uani 1 1 d . . .
C14 C 0.2249(6) 0.3058(4) 1.1326(4) 0.0383(13) Uani 1 1 d . . .
C13 C -0.3581(6) 0.9145(5) 0.9091(5) 0.0428(14) Uani 1 1 d . . .
H13A H -0.4002 0.9879 0.9223 0.051 Uiso 1 1 calc R . .
C12 C 0.2890(7) 0.2429(5) 1.1946(4) 0.0418(14) Uani 1 1 d . . .
H12 H 0.2877 0.2746 1.2506 0.050 Uiso 1 1 calc R . .
C11 C 0.4165(6) 0.6688(5) 0.9693(4) 0.0361(12) Uani 1 1 d . . .
H11A H 0.4876 0.6375 0.9153 0.043 Uiso 1 1 calc R . .
C10 C 0.2099(6) 0.6684(4) 1.0879(4) 0.0317(11) Uani 1 1 d . . .
C9 C 0.1144(6) 0.1479(4) 0.4235(4) 0.0335(12) Uani 1 1 d . . .
H9 H 0.1723 0.1838 0.3856 0.040 Uiso 1 1 calc R . .
C8 C 0.5973(7) -0.1049(5) 0.2616(4) 0.0437(14) Uani 1 1 d . . .
H8A H 0.6823 -0.1390 0.2177 0.052 Uiso 1 1 calc R . .
C7 C -0.3547(7) 0.8660(5) 0.8258(5) 0.0428(14) Uani 1 1 d . . .
H7 H -0.3967 0.9068 0.7835 0.051 Uiso 1 1 calc R . .
C4 C -0.0597(6) 0.1736(6) 0.1525(4) 0.0439(14) Uani 1 1 d . . .
H4A H -0.0413 0.2364 0.1490 0.053 Uiso 1 1 calc R . .
C3 C -0.1365(7) 0.0491(6) 0.0906(4) 0.0445(15) Uani 1 1 d . . .
H3A H -0.1710 0.0282 0.0451 0.053 Uiso 1 1 calc R . .
C2 C -0.1117(7) 0.1432(6) 0.0853(4) 0.0481(16) Uani 1 1 d . . .
H2A H -0.1298 0.1855 0.0372 0.058 Uiso 1 1 calc R . .
C1 C 0.3026(6) 0.8091(5) 1.0932(4) 0.0371(13) Uani 1 1 d . . .
H1A H 0.2976 0.8718 1.1226 0.045 Uiso 1 1 calc R . .
C51 C 0.4588(6) 0.0214(5) 0.3930(4) 0.0364(12) Uani 1 1 d . . .
H51A H 0.4511 0.0731 0.4377 0.044 Uiso 1 1 calc R . .
C52 C 0.5860(6) -0.0274(5) 0.3287(4) 0.0415(14) Uani 1 1 d . . .
H52A H 0.6626 -0.0091 0.3299 0.050 Uiso 1 1 calc R . .
C55 C 0.0058(7) -0.2287(5) 0.5027(4) 0.0400(13) Uani 1 1 d . . .
O6 O 0.1197(4) 0.4415(3) 0.8184(3) 0.0365(9) Uani 1 1 d . . .
O11 O 0.3605(5) 0.6611(4) 0.3099(5) 0.0727(17) Uani 1 1 d . . .
H11D H 0.3261 0.7285 0.3134 0.087 Uiso 1 1 d R . .
H11E H 0.4489 0.6414 0.2904 0.087 Uiso 1 1 d R . .
O22 O 0.0521(7) -0.3214(4) 0.5207(4) 0.084(2) Uani 1 1 d . . .
O5 O 0.9183(7) 0.7269(6) 0.3001(4) 0.103(3) Uani 1 1 d . . .
H5C H 0.9758 0.6976 0.2480 0.124 Uiso 1 1 d R . .
H5D H 0.8779 0.6846 0.3232 0.124 Uiso 1 1 d R . .
O12 O 0.3240(7) 0.7947(6) 0.5362(6) 0.106(3) Uani 1 1 d . . .
H12C H 0.2705 0.8533 0.5234 0.127 Uiso 1 1 d R . .
H12A H 0.3021 0.7436 0.5201 0.127 Uiso 1 1 d R . .
O7 O 0.3298(7) 0.6101(6) 0.4733(5) 0.097(2) Uani 1 1 d . . .
H7C H 0.2497 0.6068 0.4776 0.116 Uiso 1 1 d R . .
H7D H 0.3924 0.5523 0.4453 0.116 Uiso 1 1 d R . .
O8 O 0.1976(8) 0.3948(5) 0.6326(4) 0.101(3) Uani 1 1 d . . .
H8D H 0.2438 0.3974 0.6705 0.122 Uiso 1 1 d R . .
H8E H 0.1353 0.4434 0.6146 0.122 Uiso 1 1 d R . .
O9 O 0.3848(10) 0.2486(7) 0.5597(5) 0.045(2) Uani 0.50 1 d P . .
H9C H 0.3173 0.3014 0.5874 0.054 Uiso 0.50 1 d PR . .
H9D H 0.4690 0.2380 0.5302 0.054 Uiso 0.50 1 d PR . .
O15 O 0.3456(4) 0.4030(4) 0.7550(3) 0.0452(11) Uani 1 1 d . . .
O16 O 0.3328(12) 0.4801(8) 0.2417(8) 0.067(3) Uani 0.50 1 d P . .
H16C H 0.2930 0.5375 0.2200 0.080 Uiso 0.50 1 d PR . .
H16D H 0.3006 0.4343 0.2275 0.080 Uiso 0.50 1 d PR . .
O17 O 1.0029(15) 0.5441(8) 0.6522(7) 0.124(8) Uani 0.50 1 d P . .
H17C H 0.9513 0.5696 0.7068 0.149 Uiso 0.50 1 d PR . .
H17D H 1.0074 0.5952 0.6196 0.149 Uiso 0.50 1 d PR . .
O23 O 0.4050(13) 0.7309(18) 0.7222(8) 0.136(8) Uani 0.50 1 d P . .
H23C H 0.3829 0.7484 0.6717 0.164 Uiso 0.50 1 d PR . .
H23D H 0.4607 0.6767 0.7395 0.164 Uiso 0.50 1 d PR . .
O24 O 0.248(2) 0.4443(16) 0.4574(13) 0.058(5) Uani 0.25 1 d P . .
H24E H 0.1969 0.4329 0.4256 0.070 Uiso 0.25 1 d PR . .
H24C H 0.2325 0.4287 0.5137 0.070 Uiso 0.25 1 d PR . .
O25 O 0.398(3) 0.5323(16) 0.6044(13) 0.063(6) Uani 0.25 1 d P . .
H25A H 0.3861 0.5909 0.6328 0.076 Uiso 0.25 1 d PR . .
H25B H 0.3316 0.5087 0.6204 0.076 Uiso 0.25 1 d PR . .

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 0.0274(4) 0.0286(4) 0.0305(4) -0.0053(3) 0.0031(3) -0.0130(3)
Fe2 0.0290(4) 0.0370(4) 0.0220(4) -0.0022(3) -0.0022(3) -0.0130(3)
O2 0.0290(18) 0.0325(18) 0.0237(17) -0.0015(14) -0.0014(14) -0.0132(15)
O18 0.0229(17) 0.0275(17) 0.0332(19) -0.0031(15) 0.0017(15) -0.0088(14)
N2 0.028(2) 0.030(2) 0.031(2) -0.0044(18) 0.0010(18) -0.0130(18)
O4 0.0289(19) 0.044(2) 0.0307(19) -0.0081(16) 0.0021(16) -0.0161(17)
O19 0.039(2) 0.036(2) 0.031(2) -0.0055(16) 0.0009(16) -0.0161(17)
O1 0.037(2) 0.047(2) 0.0280(19) 0.0023(17) -0.0039(16) -0.0180(18)
O3 0.035(2) 0.037(2) 0.033(2) -0.0059(16) 0.0005(16) -0.0178(17)
N1 0.029(2) 0.044(3) 0.024(2) 0.0019(19) -0.0044(18) -0.012(2)
O21 0.041(2) 0.0288(19) 0.036(2) -0.0027(16) -0.0023(17) -0.0099(17)
C59 0.029(3) 0.027(2) 0.033(3) -0.007(2) 0.005(2) -0.012(2)
C30 0.042(3) 0.031(3) 0.032(3) 0.004(2) -0.011(2) -0.012(2)
C29 0.026(3) 0.036(3) 0.033(3) -0.001(2) -0.001(2) -0.013(2)
C28 0.029(3) 0.040(3) 0.027(3) -0.001(2) -0.002(2) -0.015(2)
C27 0.027(3) 0.033(3) 0.038(3) 0.003(2) -0.007(2) -0.015(2)
C26 0.034(3) 0.044(3) 0.031(3) -0.002(2) -0.002(2) -0.014(2)
C25 0.028(3) 0.055(3) 0.025(2) 0.006(2) -0.003(2) -0.016(2)
C24 0.035(3) 0.058(4) 0.027(3) 0.000(3) -0.003(2) -0.020(3)
C23 0.027(3) 0.029(3) 0.036(3) -0.006(2) 0.003(2) -0.011(2)
C22 0.032(3) 0.037(3) 0.026(3) -0.001(2) -0.002(2) -0.011(2)
C21 0.034(3) 0.040(3) 0.033(3) 0.005(2) -0.003(2) -0.016(2)
C20 0.035(3) 0.034(3) 0.028(3) -0.002(2) -0.002(2) -0.011(2)
C19 0.034(3) 0.040(3) 0.045(3) 0.006(3) -0.009(2) -0.020(2)
C18 0.030(3) 0.030(3) 0.045(3) -0.004(2) 0.004(2) -0.015(2)
C17 0.030(3) 0.026(2) 0.036(3) -0.006(2) 0.005(2) -0.013(2)
C16 0.031(3) 0.031(3) 0.039(3) -0.001(2) 0.001(2) -0.014(2)
C15 0.030(3) 0.047(3) 0.030(3) 0.006(2) -0.006(2) -0.013(2)
C14 0.037(3) 0.032(3) 0.041(3) -0.002(2) 0.004(2) -0.016(2)
C13 0.037(3) 0.027(3) 0.056(4) 0.005(3) 0.002(3) -0.012(2)
C12 0.044(3) 0.043(3) 0.034(3) 0.007(2) 0.001(3) -0.019(3)
C11 0.033(3) 0.037(3) 0.042(3) 0.002(2) -0.008(2) -0.019(2)
C10 0.032(3) 0.031(3) 0.032(3) 0.000(2) -0.007(2) -0.012(2)
C9 0.033(3) 0.037(3) 0.028(3) -0.004(2) -0.001(2) -0.015(2)
C8 0.036(3) 0.054(4) 0.036(3) -0.002(3) 0.003(2) -0.019(3)
C7 0.040(3) 0.040(3) 0.045(3) 0.010(3) -0.002(3) -0.016(3)
C4 0.035(3) 0.059(4) 0.036(3) 0.009(3) -0.007(2) -0.017(3)
C3 0.038(3) 0.064(4) 0.034(3) 0.003(3) -0.014(3) -0.019(3)
C2 0.044(4) 0.068(4) 0.035(3) 0.010(3) -0.015(3) -0.020(3)
C1 0.045(3) 0.034(3) 0.040(3) 0.004(2) -0.014(3) -0.022(3)
C51 0.036(3) 0.044(3) 0.030(3) 0.000(2) -0.007(2) -0.017(3)
C52 0.032(3) 0.057(4) 0.038(3) 0.000(3) -0.005(2) -0.022(3)
C55 0.046(3) 0.031(3) 0.034(3) -0.002(2) 0.002(3) -0.011(2)
O6 0.031(2) 0.041(2) 0.033(2) -0.0063(16) 0.0055(16) -0.0169(17)
O11 0.040(3) 0.050(3) 0.119(5) 0.001(3) -0.011(3) -0.012(2)
O22 0.112(5) 0.037(3) 0.058(3) 0.008(2) 0.021(3) -0.003(3)
O5 0.085(5) 0.149(7) 0.076(4) -0.064(4) 0.028(3) -0.076(5)
O12 0.064(4) 0.110(6) 0.121(6) 0.054(5) -0.013(4) -0.009(4)
O7 0.063(4) 0.107(5) 0.077(4) 0.012(4) 0.015(3) -0.002(4)
O8 0.110(5) 0.066(4) 0.058(4) 0.015(3) 0.019(3) 0.025(4)
O9 0.052(5) 0.049(5) 0.022(4) 0.003(3) -0.004(4) -0.008(4)
O15 0.032(2) 0.056(3) 0.039(2) 0.003(2) 0.0088(18) -0.0176(19)
O16 0.103(9) 0.056(6) 0.080(7) 0.003(5) -0.064(7) -0.048(6)
O17 0.157(13) 0.051(6) 0.044(6) 0.030(5) 0.065(7) 0.045(7)
O23 0.055(7) 0.30(3) 0.036(6) 0.021(10) -0.009(5) -0.050(11)
O24 0.059(12) 0.056(12) 0.037(10) -0.001(8) -0.011(9) 0.005(9)
O25 0.117(18) 0.070(13) 0.051(11) 0.051(10) -0.048(12) -0.075(14)

_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 O3 1.926(4) . ?
Fe1 O21 1.947(4) . ?
Fe1 O6 2.005(4) 2_567 ?
Fe1 O18 2.017(4) 2_567 ?
Fe1 O18 2.037(4) . ?
Fe1 N2 2.113(4) . ?
Fe2 O1 1.931(4) . ?
Fe2 O4 1.938(4) . ?
Fe2 O19 2.007(4) . ?
Fe2 O2 2.056(4) . ?
Fe2 O2 2.056(4) 2_556 ?
Fe2 N1 2.110(5) . ?
O2 C28 1.440(6) . ?
O2 Fe2 2.056(4) 2_556 ?
O18 C59 1.424(6) . ?
O18 Fe1 2.017(4) 2_567 ?
N2 C29 1.286(7) . ?
N2 C23 1.484(7) . ?
O4 C20 1.338(7) . ?
O19 C55 1.274(7) . ?
O1 C25 1.324(7) . ?
O3 C10 1.331(6) . ?
N1 C21 1.272(7) . ?
N1 C9 1.477(7) . ?
O21 C14 1.354(7) . ?
C59 C16 1.523(8) . ?
C59 C23 1.547(7) 2_567 ?
C30 C1 1.378(8) . ?
C30 C10 1.404(7) . ?
C29 C27 1.444(7) . ?
C28 C9 1.514(8) . ?
C28 C22 1.516(7) . ?
C27 C11 1.423(7) . ?
C27 C10 1.425(7) . ?
C26 C8 1.382(9) . ?
C26 C20 1.402(7) . ?
C25 C15 1.410(9) . ?
C25 C24 1.415(8) . ?
C24 C3 1.339(9) . ?
C23 C17 1.517(8) . ?
C23 C59 1.547(7) 2_567 ?
C22 C51 1.395(8) . ?
C22 C20 1.415(8) . ?
C21 C15 1.454(8) . ?
C19 C11 1.369(8) . ?
C19 C1 1.400(8) . ?
C18 C16 1.372(7) . ?
C18 C13 1.383(9) . ?
C17 O15 1.244(6) . ?
C17 O6 1.284(7) . ?
C16 C14 1.430(8) 2_567 ?
C15 C4 1.403(8) . ?
C14 C12 1.394(9) . ?
C14 C16 1.430(8) 2_567 ?
C13 C7 1.386(9) . ?
C12 C7 1.383(9) 2_567 ?
C9 C55 1.532(7) 2_556 ?
C8 C52 1.397(9) . ?
C7 C12 1.383(9) 2_567 ?
C4 C2 1.379(9) . ?
C3 C2 1.379(10) . ?
C51 C52 1.378(8) . ?
C55 O22 1.229(8) . ?
C55 C9 1.532(7) 2_556 ?
O6 Fe1 2.005(4) 2_567 ?

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
O3 Fe1 O21 94.42(18) . . ?
O3 Fe1 O6 93.37(16) . 2_567 ?
O21 Fe1 O6 91.92(17) . 2_567 ?
O3 Fe1 O18 165.60(15) . 2_567 ?
O21 Fe1 O18 89.85(16) . 2_567 ?
O6 Fe1 O18 100.23(15) 2_567 2_567 ?
O3 Fe1 O18 97.35(16) . . ?
O21 Fe1 O18 168.17(16) . . ?
O6 Fe1 O18 88.60(16) 2_567 . ?
O18 Fe1 O18 78.43(16) 2_567 . ?
O3 Fe1 N2 87.67(17) . . ?
O21 Fe1 N2 88.95(18) . . ?
O6 Fe1 N2 178.59(17) 2_567 . ?
O18 Fe1 N2 78.66(16) 2_567 . ?
O18 Fe1 N2 90.32(16) . . ?
O1 Fe2 O4 99.86(17) . . ?
O1 Fe2 O19 94.63(17) . . ?
O4 Fe2 O19 89.02(17) . . ?
O1 Fe2 O2 164.83(17) . . ?
O4 Fe2 O2 87.33(16) . . ?
O19 Fe2 O2 98.86(16) . . ?
O1 Fe2 O2 95.30(16) . 2_556 ?
O4 Fe2 O2 164.75(16) . 2_556 ?
O19 Fe2 O2 88.17(15) . 2_556 ?
O2 Fe2 O2 78.30(16) . 2_556 ?
O1 Fe2 N1 87.87(18) . . ?
O4 Fe2 N1 90.22(18) . . ?
O19 Fe2 N1 177.48(17) . . ?
O2 Fe2 N1 78.70(16) . . ?
O2 Fe2 N1 91.94(16) 2_556 . ?
C28 O2 Fe2 109.3(3) . . ?
C28 O2 Fe2 118.5(3) . 2_556 ?
Fe2 O2 Fe2 101.70(16) . 2_556 ?
C59 O18 Fe1 110.4(3) . 2_567 ?
C59 O18 Fe1 119.4(3) . . ?
Fe1 O18 Fe1 101.57(16) 2_567 . ?
C29 N2 C23 119.4(4) . . ?
C29 N2 Fe1 127.5(4) . . ?
C23 N2 Fe1 113.1(3) . . ?
C20 O4 Fe2 127.3(3) . . ?
C55 O19 Fe2 131.4(4) . . ?
C25 O1 Fe2 131.6(4) . . ?
C10 O3 Fe1 132.5(3) . . ?
C21 N1 C9 119.4(5) . . ?
C21 N1 Fe2 126.5(4) . . ?
C9 N1 Fe2 113.4(3) . . ?
C14 O21 Fe1 127.6(4) . . ?
O18 C59 C16 112.2(4) . . ?
O18 C59 C23 107.2(4) . 2_567 ?
C16 C59 C23 112.0(5) . 2_567 ?
C1 C30 C10 121.5(5) . . ?
N2 C29 C27 124.0(5) . . ?
O2 C28 C9 108.1(4) . . ?
O2 C28 C22 111.4(4) . . ?
C9 C28 C22 110.3(4) . . ?
C11 C27 C10 118.2(5) . . ?
C11 C27 C29 117.0(5) . . ?
C10 C27 C29 124.8(5) . . ?
C8 C26 C20 121.8(6) . . ?
O1 C25 C15 123.8(5) . . ?
O1 C25 C24 119.0(6) . . ?
C15 C25 C24 117.3(5) . . ?
C3 C24 C25 121.6(6) . . ?
N2 C23 C17 107.8(4) . . ?
N2 C23 C59 107.0(4) . 2_567 ?
C17 C23 C59 112.3(5) . 2_567 ?
C51 C22 C20 118.6(5) . . ?
C51 C22 C28 118.7(5) . . ?
C20 C22 C28 122.6(5) . . ?
N1 C21 C15 125.4(5) . . ?
O4 C20 C26 118.2(5) . . ?
O4 C20 C22 123.5(5) . . ?
C26 C20 C22 118.3(5) . . ?
C11 C19 C1 119.5(5) . . ?
C16 C18 C13 121.9(6) . . ?
O15 C17 O6 121.9(6) . . ?
O15 C17 C23 119.4(5) . . ?
O6 C17 C23 118.7(5) . . ?
C18 C16 C14 119.0(6) . 2_567 ?
C18 C16 C59 118.7(5) . . ?
C14 C16 C59 122.3(5) 2_567 . ?
C4 C15 C25 119.6(6) . . ?
C4 C15 C21 117.0(6) . . ?
C25 C15 C21 123.4(5) . . ?
O21 C14 C12 119.5(6) . . ?
O21 C14 C16 122.1(6) . 2_567 ?
C12 C14 C16 118.3(5) . 2_567 ?
C18 C13 C7 119.3(6) . . ?
C7 C12 C14 121.0(6) 2_567 . ?
C19 C11 C27 121.8(5) . . ?
O3 C10 C30 119.0(5) . . ?
O3 C10 C27 122.4(5) . . ?
C30 C10 C27 118.6(5) . . ?
N1 C9 C28 107.7(4) . . ?
N1 C9 C55 107.6(5) . 2_556 ?
C28 C9 C55 112.6(5) . 2_556 ?
C26 C8 C52 120.0(6) . . ?
C12 C7 C13 120.2(6) 2_567 . ?
C2 C4 C15 120.9(6) . . ?
C24 C3 C2 121.7(6) . . ?
C4 C2 C3 118.9(6) . . ?
C30 C1 C19 120.3(5) . . ?
C52 C51 C22 122.7(5) . . ?
C51 C52 C8 118.6(6) . . ?
O22 C55 O19 122.0(6) . . ?
O22 C55 C9 118.7(5) . 2_556 ?
O19 C55 C9 119.2(5) . 2_556 ?
C17 O6 Fe1 131.5(4) . 2_567 ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         1.609
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.142