# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[hdma]1.5(Fe5F7OwCOO)(Amtetraz)4)
_database_code_depnum_ccdc_archive 'CCDC 1024954'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[hdma]1.5(Fe5F7OwCOO)(Amtetraz)4)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H11 F7 Fe5 N20 O3 1.5-,1.5(C2 H8 N 1+)'
_chemical_formula_sum            'C8 H23 F7 Fe5 N21.50 O3'
_chemical_formula_weight         880.73

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'
F F 0.0171 0.0103 '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   'P 2/m'
_symmetry_space_group_name_Hall  '-P 2y'

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

_cell_length_a                   6.6118(6)
_cell_length_b                   12.4325(11)
_cell_length_c                   8.8075(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.723(3)
_cell_angle_gamma                90.00
_cell_volume                     689.63(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    423
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      23.7

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             438
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16829
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         28.29
_reflns_number_total             1795
_reflns_number_gt                1355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_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)+(0.0497P)²+1.0081P] 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_number_reflns         1795
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1130
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_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 0.5000 0.0000 1.0000 0.0157(2) Uani 1 4 d S . .
Fe2 Fe 1.0000 0.0000 1.0000 0.0141(2) Uani 1 4 d S . .
Fe3 Fe 0.5000 0.36653(6) 0.5000 0.0163(2) Uani 1 2 d S . .
Fe4 Fe 0.0000 0.5000 0.5000 0.0185(3) Uani 1 4 d S . .
F1 F 0.8042(5) 0.0000 1.1388(4) 0.0223(7) Uani 1 2 d S . .
F2 F 0.2183(4) 0.38055(18) 0.5425(3) 0.0273(5) Uani 1 1 d . . .
OW3 O 0.6061(6) 0.5000 0.6660(5) 0.0257(8) Uani 0.75 2 d SP . .
F3 F 0.6061(6) 0.5000 0.6660(5) 0.0257(8) Uani 0.25 2 d SP . .
OW4 O -0.0035(8) 0.5000 0.2577(5) 0.0447(12) Uani 0.75 2 d SP . .
F4 F -0.0035(8) 0.5000 0.2577(5) 0.0447(12) Uani 0.25 2 d SP . .
N1 N 0.7972(5) 0.1250(3) 0.8589(4) 0.0208(7) Uani 1 1 d . . .
N2 N 0.5890(5) 0.1212(3) 0.8501(4) 0.0209(7) Uani 1 1 d . . .
N3 N 0.4812(5) 0.1927(3) 0.7506(4) 0.0233(7) Uani 1 1 d . . .
N4 N 0.6162(5) 0.2471(3) 0.6892(4) 0.0203(7) Uani 1 1 d . . .
C1 C 0.8082(6) 0.2050(3) 0.7593(5) 0.0223(8) Uani 1 1 d . . .
N5 N 0.9897(6) 0.2360(4) 0.7306(6) 0.0520(14) Uani 1 1 d . . .
H5A H 0.9865 0.2863 0.6629 0.062 Uiso 1 1 calc R . .
H5B H 1.1080 0.2054 0.7802 0.062 Uiso 1 1 calc R . .
C4 C 0.176(2) 0.5000 0.2290(18) 0.043(3) Uani 0.50 2 d SP . .
C1A C 0.5000 0.4010(7) 1.0000 0.049(3) Uani 0.75 2 d SP . .
N1A N 0.437(2) 0.5000 0.9086(17) 0.035(3) Uani 0.375 2 d SP . .
C2A C -0.1875(16) 0.0000 0.5031(11) 0.046(3) Uani 0.75 2 d SP . .
N2A N -0.050(4) -0.0477(18) 0.460(2) 0.044(6) Uani 0.1875 1 d P . .


_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 F1 2.011(3) . ?
Fe1 F1 2.011(3) 3_657 ?
Fe1 N2 2.199(3) . ?
Fe1 N2 2.199(3) 4 ?
Fe1 N2 2.199(3) 2_657 ?
Fe1 N2 2.199(3) 3_657 ?
Fe2 F1 2.033(3) . ?
Fe2 F1 2.033(3) 3_757 ?
Fe2 N1 2.178(3) . ?
Fe2 N1 2.178(3) 4 ?
Fe2 N1 2.178(3) 2_757 ?
Fe2 N1 2.178(3) 3_757 ?
Fe3 F2 2.016(2) . ?
Fe3 F2 2.016(2) 2_656 ?
Fe3 OW3 2.181(3) . ?
Fe3 F3 2.181(3) 3_666 ?
Fe3 OW3 2.181(3) 3_666 ?
Fe3 N4 2.189(3) 2_656 ?
Fe3 N4 2.189(3) . ?
Fe4 F2 2.025(2) 4_565 ?
Fe4 F2 2.025(2) 2_556 ?
Fe4 F2 2.025(2) 3_566 ?
Fe4 F2 2.025(2) . ?
Fe4 OW4 2.127(5) . ?
Fe4 F4 2.127(5) 3_566 ?
Fe4 OW4 2.127(5) 3_566 ?
OW3 C4 1.459(16) 3_666 ?
OW3 Fe3 2.181(3) 3_666 ?
OW4 C4 1.284(16) . ?
N1 C1 1.343(5) . ?
N1 N2 1.356(4) . ?
N2 N3 1.298(4) . ?
N3 N4 1.357(4) . ?
N4 C1 1.338(5) . ?
C1 N5 1.355(5) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C4 F3 1.459(16) 3_666 ?
C4 OW3 1.459(16) 3_666 ?
C1A N1A 1.460(11) . ?
C1A N1A 1.460(11) 3_667 ?
N1A C1A 1.460(11) 3_667 ?
N1A N1A 1.57(3) 3_667 ?
C2A N2A 1.24(3) . ?
C2A N2A 1.24(3) 4 ?
C2A N2A 1.62(3) 3_556 ?
C2A N2A 1.62(3) 2_556 ?
N2A N2A 0.81(3) 2_556 ?
N2A N2A 1.19(5) 4 ?
N2A N2A 1.44(4) 3_556 ?
N2A C2A 1.62(3) 3_556 ?

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
F1 Fe1 F1 180.0 . 3_657 ?
F1 Fe1 N2 87.93(11) . . ?
F1 Fe1 N2 92.07(11) 3_657 . ?
F1 Fe1 N2 87.93(11) . 4 ?
F1 Fe1 N2 92.07(11) 3_657 4 ?
N2 Fe1 N2 86.54(17) . 4 ?
F1 Fe1 N2 92.07(11) . 2_657 ?
F1 Fe1 N2 87.93(11) 3_657 2_657 ?
N2 Fe1 N2 93.46(17) . 2_657 ?
N2 Fe1 N2 180.000(1) 4 2_657 ?
F1 Fe1 N2 92.07(11) . 3_657 ?
F1 Fe1 N2 87.93(11) 3_657 3_657 ?
N2 Fe1 N2 179.999(1) . 3_657 ?
N2 Fe1 N2 93.45(17) 4 3_657 ?
N2 Fe1 N2 86.55(17) 2_657 3_657 ?
F1 Fe2 F1 179.999(1) . 3_757 ?
F1 Fe2 N1 87.07(11) . . ?
F1 Fe2 N1 92.93(11) 3_757 . ?
F1 Fe2 N1 87.07(11) . 4 ?
F1 Fe2 N1 92.93(11) 3_757 4 ?
N1 Fe2 N1 91.04(17) . 4 ?
F1 Fe2 N1 92.93(11) . 2_757 ?
F1 Fe2 N1 87.07(11) 3_757 2_757 ?
N1 Fe2 N1 88.96(17) . 2_757 ?
N1 Fe2 N1 180.0 4 2_757 ?
F1 Fe2 N1 92.93(11) . 3_757 ?
F1 Fe2 N1 87.07(11) 3_757 3_757 ?
N1 Fe2 N1 180.00(12) . 3_757 ?
N1 Fe2 N1 88.96(17) 4 3_757 ?
N1 Fe2 N1 91.04(17) 2_757 3_757 ?
F2 Fe3 F2 170.08(14) . 2_656 ?
F2 Fe3 OW3 86.36(13) . . ?
F2 Fe3 OW3 86.09(12) 2_656 . ?
F2 Fe3 F3 86.10(12) . 3_666 ?
F2 Fe3 F3 86.36(13) 2_656 3_666 ?
OW3 Fe3 F3 80.94(16) . 3_666 ?
F2 Fe3 OW3 86.10(12) . 3_666 ?
F2 Fe3 OW3 86.36(13) 2_656 3_666 ?
OW3 Fe3 OW3 80.94(16) . 3_666 ?
F3 Fe3 OW3 0.0(2) 3_666 3_666 ?
F2 Fe3 N4 94.02(11) . 2_656 ?
F2 Fe3 N4 92.71(11) 2_656 2_656 ?
OW3 Fe3 N4 173.15(12) . 2_656 ?
F3 Fe3 N4 92.26(12) 3_666 2_656 ?
OW3 Fe3 N4 92.26(12) 3_666 2_656 ?
F2 Fe3 N4 92.71(11) . . ?
F2 Fe3 N4 94.02(11) 2_656 . ?
OW3 Fe3 N4 92.26(12) . . ?
F3 Fe3 N4 173.15(12) 3_666 . ?
OW3 Fe3 N4 173.15(12) 3_666 . ?
N4 Fe3 N4 94.55(17) 2_656 . ?
F2 Fe4 F2 180.0 4_565 2_556 ?
F2 Fe4 F2 85.65(13) 4_565 3_566 ?
F2 Fe4 F2 94.35(13) 2_556 3_566 ?
F2 Fe4 F2 94.35(13) 4_565 . ?
F2 Fe4 F2 85.65(13) 2_556 . ?
F2 Fe4 F2 180.0 3_566 . ?
F2 Fe4 OW4 88.56(11) 4_565 . ?
F2 Fe4 OW4 91.44(11) 2_556 . ?
F2 Fe4 OW4 91.44(11) 3_566 . ?
F2 Fe4 OW4 88.56(11) . . ?
F2 Fe4 F4 91.44(11) 4_565 3_566 ?
F2 Fe4 F4 88.56(11) 2_556 3_566 ?
F2 Fe4 F4 88.56(11) 3_566 3_566 ?
F2 Fe4 F4 91.44(11) . 3_566 ?
OW4 Fe4 F4 179.999(1) . 3_566 ?
F2 Fe4 OW4 91.44(11) 4_565 3_566 ?
F2 Fe4 OW4 88.56(11) 2_556 3_566 ?
F2 Fe4 OW4 88.56(11) 3_566 3_566 ?
F2 Fe4 OW4 91.44(11) . 3_566 ?
OW4 Fe4 OW4 179.999(1) . 3_566 ?
F4 Fe4 OW4 0.0(3) 3_566 3_566 ?
Fe1 F1 Fe2 109.69(14) . . ?
Fe3 F2 Fe4 132.53(12) . . ?
C4 OW3 Fe3 118.6(3) 3_666 3_666 ?
C4 OW3 Fe3 118.6(3) 3_666 . ?
Fe3 OW3 Fe3 99.06(16) 3_666 . ?
C4 OW4 Fe4 117.9(7) . . ?
C1 N1 N2 104.2(3) . . ?
C1 N1 Fe2 139.0(3) . . ?
N2 N1 Fe2 116.5(2) . . ?
N3 N2 N1 110.7(3) . . ?
N3 N2 Fe1 133.0(3) . . ?
N1 N2 Fe1 116.2(2) . . ?
N2 N3 N4 108.5(3) . . ?
C1 N4 N3 105.6(3) . . ?
C1 N4 Fe3 132.9(3) . . ?
N3 N4 Fe3 121.4(2) . . ?
N4 C1 N1 111.0(3) . . ?
N4 C1 N5 124.9(4) . . ?
N1 C1 N5 124.0(4) . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
OW4 C4 F3 132.0(12) . 3_666 ?
OW4 C4 OW3 132.0(12) . 3_666 ?
F3 C4 OW3 0.0(3) 3_666 3_666 ?
N1A C1A N1A 65.1(10) . 3_667 ?
C1A N1A C1A 114.9(10) 3_667 . ?
C1A N1A N1A 57.5(5) 3_667 3_667 ?
C1A N1A N1A 57.5(5) . 3_667 ?
N2A C2A N2A 57(2) . 4 ?
N2A C2A N2A 58.6(16) . 3_556 ?
N2A C2A N2A 29.2(14) 4 3_556 ?
N2A C2A N2A 29.2(14) . 2_556 ?
N2A C2A N2A 58.6(16) 4 2_556 ?
N2A C2A N2A 43.0(17) 3_556 2_556 ?
N2A N2A N2A 89.999(2) 2_556 4 ?
N2A N2A C2A 103(4) 2_556 . ?
N2A N2A C2A 61.3(12) 4 . ?
N2A N2A N2A 55.7(15) 2_556 3_556 ?
N2A N2A N2A 34.3(15) 4 3_556 ?
C2A N2A N2A 74(2) . 3_556 ?
N2A N2A C2A 48(3) 2_556 3_556 ?
N2A N2A C2A 68.5(8) 4 3_556 ?
C2A N2A C2A 121.4(16) . 3_556 ?
N2A N2A C2A 47.2(16) 3_556 3_556 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.137
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[hdma](Fe5F8Ow2(amtetraz)4)
_database_code_depnum_ccdc_archive 'CCDC 1024955'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[hdma](Fe5F8Ow2(amtetraz)4)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 F8 Fe5 N20 O2 1-,C2 H8 N 1+'
_chemical_formula_sum            'C6 H20 F8 Fe5 N21 O2'
_chemical_formula_weight         849.68

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'
F F 0.0171 0.0103 '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   'P 2/m'
_symmetry_space_group_name_Hall  '-P 2y'

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

_cell_length_a                   6.6687(7)
_cell_length_b                   12.2450(10)
_cell_length_c                   9.0305(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.439(6)
_cell_angle_gamma                90.00
_cell_volume                     690.99(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2132
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      28.9



_exptl_crystal_description       'small platelets'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             421
_exptl_absorpt_coefficient_mu    2.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   '(SHELX76; Sheldrick, 2008)'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 APEXII'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16982
_diffrn_reflns_av_R_equivalents  0.1477
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         30.61
_reflns_number_total             2206
_reflns_number_gt                1269
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          Twin

_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)+(0.1354P)²+2.5109P] 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_number_reflns         2206
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.2614
_refine_ls_wR_factor_gt          0.2212
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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 0.5000 0.0000 0.0000 0.0423(10) Uani 1 4 d S . .
Fe2 Fe 0.0000 0.0000 0.0000 0.0410(10) Uani 1 4 d S . .
Fe3 Fe 0.5000 0.36593(9) 0.5000 0.0232(4) Uani 1 2 d S . .
Fe4 Fe 0.0000 0.5000 0.5000 0.0274(6) Uani 1 4 d S . .
F1 F 0.190(2) 0.0000 -0.1361(7) 0.0397(18) Uani 1 2 d S . .
F2 F 0.2041(9) 0.3842(4) 0.5206(12) 0.065(2) Uani 1 1 d . . .
F3 F 0.587(2) 0.5000 0.6606(9) 0.044(2) Uani 0.50 2 d SP . .
OW3 O 0.587(2) 0.5000 0.6606(9) 0.044(2) Uani 0.50 2 d SP . .
F4 F 0.044(2) 0.5000 0.7241(12) 0.075(5) Uani 0.50 2 d SP . .
OW4 O 0.044(2) 0.5000 0.7241(12) 0.075(5) Uani 0.50 2 d SP . .
N1 N 0.209(2) 0.1248(7) 0.1406(12) 0.054(4) Uani 1 1 d . . .
N2 N 0.418(2) 0.1234(7) 0.1468(10) 0.059(4) Uani 1 1 d . . .
N3 N 0.522(2) 0.1964(7) 0.2489(11) 0.055(3) Uani 1 1 d . . .
N4 N 0.399(2) 0.2479(4) 0.3127(8) 0.046(2) Uani 1 1 d . . .
N5 N -0.0029(16) 0.2336(8) 0.2700(16) 0.071(4) Uani 1 1 d . . .
H5A H -0.1210 0.2011 0.2185 0.085 Uiso 1 1 calc R . .
H5B H -0.0007 0.2840 0.3370 0.085 Uiso 1 1 calc R . .
C1 C 0.204(2) 0.2018(8) 0.2425(12) 0.050(4) Uani 1 1 d . . .
C1A C 0.5000 0.401(3) 0.0000 0.044(7) Uiso 0.50 2 d SP . .
N1A N 0.457(8) 0.5000 -0.107(6) 0.036(10) Uiso 0.25 2 d SP . .
C2A C 0.185(3) 0.0000 -0.503(4) 0.027(4) Uiso 0.50 2 d SP . .
N2A N 0.003(11) 0.044(4) -0.446(6) 0.030(12) Uiso 0.125 1 d P . .


_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 F1 2.001(11) . ?
Fe1 F1 2.001(11) 3_655 ?
Fe1 N2 2.201(11) 3_655 ?
Fe1 N2 2.201(11) 4 ?
Fe1 N2 2.201(11) 2_655 ?
Fe1 N2 2.201(11) . ?
Fe2 F1 2.051(12) . ?
Fe2 F1 2.051(12) 3 ?
Fe2 N1 2.157(10) . ?
Fe2 N1 2.157(10) 3 ?
Fe2 N1 2.157(10) 4 ?
Fe2 N1 2.157(10) 2 ?
Fe3 F2 2.058(6) 2_656 ?
Fe3 F2 2.058(6) . ?
Fe3 F3 2.132(5) . ?
Fe3 OW3 2.132(5) 3_666 ?
Fe3 F3 2.132(5) 3_666 ?
Fe3 N4 2.146(6) . ?
Fe3 N4 2.146(6) 2_656 ?
Fe4 F2 1.929(5) . ?
Fe4 F2 1.930(5) 4_565 ?
Fe4 F2 1.930(5) 2_556 ?
Fe4 F2 1.930(5) 3_566 ?
Fe4 OW4 1.940(10) 3_566 ?
Fe4 F4 1.940(10) 3_566 ?
Fe4 F4 1.940(10) . ?
F3 Fe3 2.132(5) 3_666 ?
N1 C1 1.325(14) . ?
N1 N2 1.377(16) . ?
N2 N3 1.299(11) . ?
N3 N4 1.319(17) . ?
N4 C1 1.352(17) . ?
N5 C1 1.537(19) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?


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
F1 Fe1 F1 180.0 . 3_655 ?
F1 Fe1 N2 92.9(4) . 3_655 ?
F1 Fe1 N2 87.1(4) 3_655 3_655 ?
F1 Fe1 N2 87.1(4) . 4 ?
F1 Fe1 N2 92.9(4) 3_655 4 ?
N2 Fe1 N2 93.3(6) 3_655 4 ?
F1 Fe1 N2 92.9(4) . 2_655 ?
F1 Fe1 N2 87.1(4) 3_655 2_655 ?
N2 Fe1 N2 86.7(6) 3_655 2_655 ?
N2 Fe1 N2 180.0(3) 4 2_655 ?
F1 Fe1 N2 87.1(4) . . ?
F1 Fe1 N2 92.9(4) 3_655 . ?
N2 Fe1 N2 179.999(1) 3_655 . ?
N2 Fe1 N2 86.7(6) 4 . ?
N2 Fe1 N2 93.3(6) 2_655 . ?
F1 Fe2 F1 179.999(1) . 3 ?
F1 Fe2 N1 86.9(4) . . ?
F1 Fe2 N1 93.1(4) 3 . ?
F1 Fe2 N1 93.1(4) . 3 ?
F1 Fe2 N1 86.9(4) 3 3 ?
N1 Fe2 N1 180.000(1) . 3 ?
F1 Fe2 N1 86.9(4) . 4 ?
F1 Fe2 N1 93.1(4) 3 4 ?
N1 Fe2 N1 90.2(6) . 4 ?
N1 Fe2 N1 89.8(6) 3 4 ?
F1 Fe2 N1 93.1(4) . 2 ?
F1 Fe2 N1 86.9(4) 3 2 ?
N1 Fe2 N1 89.8(6) . 2 ?
N1 Fe2 N1 90.2(6) 3 2 ?
N1 Fe2 N1 180.0(3) 4 2 ?
F2 Fe3 F2 167.5(3) 2_656 . ?
F2 Fe3 F3 86.4(5) 2_656 . ?
F2 Fe3 F3 84.0(5) . . ?
F2 Fe3 OW3 84.0(5) 2_656 3_666 ?
F2 Fe3 OW3 86.4(5) . 3_666 ?
F3 Fe3 OW3 79.3(3) . 3_666 ?
F2 Fe3 F3 84.0(5) 2_656 3_666 ?
F2 Fe3 F3 86.4(5) . 3_666 ?
F3 Fe3 F3 79.3(3) . 3_666 ?
OW3 Fe3 F3 0.0(10) 3_666 3_666 ?
F2 Fe3 N4 92.8(5) 2_656 . ?
F2 Fe3 N4 95.6(5) . . ?
F3 Fe3 N4 172.0(2) . . ?
OW3 Fe3 N4 92.7(2) 3_666 . ?
F3 Fe3 N4 92.7(2) 3_666 . ?
F2 Fe3 N4 95.6(5) 2_656 2_656 ?
F2 Fe3 N4 92.8(5) . 2_656 ?
F3 Fe3 N4 92.7(2) . 2_656 ?
OW3 Fe3 N4 172.0(2) 3_666 2_656 ?
F3 Fe3 N4 172.0(2) 3_666 2_656 ?
N4 Fe3 N4 95.4(3) . 2_656 ?
F2 Fe4 F2 94.6(3) . 4_565 ?
F2 Fe4 F2 85.4(3) . 2_556 ?
F2 Fe4 F2 180.0 4_565 2_556 ?
F2 Fe4 F2 179.999(1) . 3_566 ?
F2 Fe4 F2 85.4(3) 4_565 3_566 ?
F2 Fe4 F2 94.6(3) 2_556 3_566 ?
F2 Fe4 OW4 86.9(4) . 3_566 ?
F2 Fe4 OW4 86.9(4) 4_565 3_566 ?
F2 Fe4 OW4 93.1(4) 2_556 3_566 ?
F2 Fe4 OW4 93.1(4) 3_566 3_566 ?
F2 Fe4 F4 86.9(4) . 3_566 ?
F2 Fe4 F4 86.9(4) 4_565 3_566 ?
F2 Fe4 F4 93.1(4) 2_556 3_566 ?
F2 Fe4 F4 93.1(4) 3_566 3_566 ?
OW4 Fe4 F4 0.000(2) 3_566 3_566 ?
F2 Fe4 F4 93.1(4) . . ?
F2 Fe4 F4 93.1(4) 4_565 . ?
F2 Fe4 F4 86.9(4) 2_556 . ?
F2 Fe4 F4 86.9(4) 3_566 . ?
OW4 Fe4 F4 180.000(4) 3_566 . ?
F4 Fe4 F4 180.000(4) 3_566 . ?
Fe1 F1 Fe2 110.7(3) . . ?
Fe4 F2 Fe3 137.5(3) . . ?
Fe3 F3 Fe3 100.7(3) 3_666 . ?
C1 N1 N2 104.4(11) . . ?
C1 N1 Fe2 138.3(12) . . ?
N2 N1 Fe2 116.9(8) . . ?
N3 N2 N1 107.7(12) . . ?
N3 N2 Fe1 135.8(12) . . ?
N1 N2 Fe1 116.5(7) . . ?
N2 N3 N4 112.2(13) . . ?
N3 N4 C1 103.8(7) . . ?
N3 N4 Fe3 126.4(9) . . ?
C1 N4 Fe3 129.5(11) . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N1 C1 N4 111.9(14) . . ?
N1 C1 N5 122.1(12) . . ?
N4 C1 N5 126.0(10) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        30.61
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.082
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.231
_exptl_crystal_preparation       'Magnetic properties'
