# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1029372'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;
#2017GuillotICMMO

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C20 H28 Fe N5 O2, F6 Sb '
_chemical_formula_sum            'C20 H28 F6 Fe N5 O2 Sb'
_chemical_melting_point          ?

_exptl_crystal_description       bloc
_exptl_crystal_colour            'pale yellow'

_diffrn_ambient_temperature      100(1)
_chemical_formula_weight         662.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8476 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5870 1.5507 '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 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

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                   10.6202(3)
_cell_length_b                   20.6412(6)
_cell_length_c                   11.6374(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1960(10)
_cell_angle_gamma                90.00
_cell_volume                     2510.79(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      30.35
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8819
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61655
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         30.63
_reflns_number_total             7528
_reflns_number_gt                6041
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0310P)²+5.1661P] 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         7528
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9274(3) 0.70385(13) 0.4757(2) 0.0184(5) Uani 1 1 d . . .
C2 C 1.0012(3) 0.71678(13) 0.5964(2) 0.0184(5) Uani 1 1 d . . .
C3 C 1.0595(4) 0.78265(17) 0.6174(3) 0.0389(9) Uani 1 1 d . . .
H3A H 1.0468 0.8131 0.5528 0.047 Uiso 1 1 calc R . .
H3B H 1.0617 0.8020 0.6937 0.047 Uiso 1 1 calc R . .
C4 C 1.1436(3) 0.72558(19) 0.6093(3) 0.0358(8) Uani 1 1 d . . .
H4A H 1.1965 0.7103 0.6807 0.043 Uiso 1 1 calc R . .
H4B H 1.1817 0.7214 0.5398 0.043 Uiso 1 1 calc R . .
C5 C 0.4869(3) 0.62559(17) 0.6571(3) 0.0347(7) Uani 1 1 d . . .
H5A H 0.4048 0.6043 0.6344 0.042 Uiso 1 1 calc R . .
H5B H 0.4722 0.6667 0.6930 0.042 Uiso 1 1 calc R . .
C6 C 0.5733(3) 0.58371(16) 0.7449(3) 0.0304(7) Uani 1 1 d . . .
H6A H 0.5346 0.5778 0.8137 0.036 Uiso 1 1 calc R . .
H6B H 0.5826 0.5414 0.7111 0.036 Uiso 1 1 calc R . .
C7 C 0.7009(4) 0.66134(16) 0.8728(3) 0.0346(7) Uani 1 1 d . . .
H7A H 0.6824 0.6398 0.9410 0.052 Uiso 1 1 calc R . .
H7B H 0.6366 0.6935 0.8478 0.052 Uiso 1 1 calc R . .
H7C H 0.7832 0.6818 0.8909 0.052 Uiso 1 1 calc R . .
C8 C 0.5187(3) 0.58415(17) 0.4672(3) 0.0376(8) Uani 1 1 d . . .
H8A H 0.5559 0.5449 0.5024 0.056 Uiso 1 1 calc R . .
H8B H 0.5554 0.5940 0.3995 0.056 Uiso 1 1 calc R . .
H8C H 0.4280 0.5786 0.4445 0.056 Uiso 1 1 calc R . .
C9 C 0.7961(3) 0.56313(14) 0.8203(2) 0.0234(6) Uani 1 1 d . . .
H9A H 0.7651 0.5364 0.8780 0.028 Uiso 1 1 calc R . .
H9B H 0.8757 0.5831 0.8574 0.028 Uiso 1 1 calc R . .
C10 C 0.8201(3) 0.52139(14) 0.7207(2) 0.0214(5) Uani 1 1 d . . .
C11 C 0.8548(3) 0.45686(15) 0.7360(3) 0.0275(6) Uani 1 1 d . . .
H11 H 0.8613 0.4373 0.8088 0.033 Uiso 1 1 calc R . .
C12 C 0.8795(3) 0.42206(14) 0.6405(3) 0.0297(7) Uani 1 1 d . . .
H12 H 0.9032 0.3787 0.6484 0.036 Uiso 1 1 calc R . .
C13 C 0.8686(3) 0.45229(14) 0.5342(3) 0.0255(6) Uani 1 1 d . . .
H13 H 0.8851 0.4299 0.4692 0.031 Uiso 1 1 calc R . .
C14 C 0.8325(3) 0.51671(13) 0.5257(2) 0.0200(5) Uani 1 1 d . . .
H14 H 0.8249 0.5370 0.4535 0.024 Uiso 1 1 calc R . .
C15 C 0.4933(3) 0.69836(15) 0.4933(3) 0.0300(7) Uani 1 1 d . . .
H15A H 0.4006 0.6977 0.4811 0.036 Uiso 1 1 calc R . .
H15B H 0.5192 0.7019 0.4177 0.036 Uiso 1 1 calc R . .
C16 C 0.5429(3) 0.75578(15) 0.5679(3) 0.0262(6) Uani 1 1 d . . .
C17 C 0.4728(3) 0.81161(17) 0.5700(3) 0.0355(8) Uani 1 1 d . . .
H17 H 0.3896 0.8142 0.5285 0.043 Uiso 1 1 calc R . .
C18 C 0.5272(4) 0.86373(17) 0.6344(3) 0.0384(8) Uani 1 1 d . . .
H18 H 0.4822 0.9023 0.6354 0.046 Uiso 1 1 calc R . .
C19 C 0.6502(4) 0.85766(16) 0.6977(3) 0.0353(7) Uani 1 1 d . . .
H19 H 0.6888 0.8919 0.7425 0.042 Uiso 1 1 calc R . .
C20 C 0.7139(3) 0.80010(14) 0.6929(3) 0.0258(6) Uani 1 1 d . . .
H20 H 0.7965 0.7962 0.7351 0.031 Uiso 1 1 calc R . .
N1 N 0.9492(2) 0.68606(11) 0.69084(19) 0.0172(4) Uani 1 1 d . . .
H1A H 0.9477 0.7143 0.7494 0.021 Uiso 1 1 calc R . .
H1B H 0.9974 0.6518 0.7190 0.021 Uiso 1 1 calc R . .
N2 N 0.7013(2) 0.61395(11) 0.7792(2) 0.0213(5) Uani 1 1 d . . .
N3 N 0.5446(2) 0.63755(13) 0.5514(2) 0.0279(5) Uani 1 1 d . . .
N4 N 0.6623(2) 0.74941(12) 0.6301(2) 0.0233(5) Uani 1 1 d . . .
N5 N 0.8081(2) 0.55119(11) 0.6166(2) 0.0192(4) Uani 1 1 d . . .
O1 O 0.82135(19) 0.67376(10) 0.46850(17) 0.0215(4) Uani 1 1 d . . .
O2 O 0.97319(19) 0.72310(10) 0.39106(17) 0.0225(4) Uani 1 1 d . . .
F1 F 0.84738(18) -0.03721(9) 0.62016(18) 0.0357(4) Uani 1 1 d . . .
F2 F 0.67972(19) 0.00811(9) 0.74406(19) 0.0369(4) Uani 1 1 d . . .
F3 F 0.70128(19) 0.12449(10) 0.65738(17) 0.0352(4) Uani 1 1 d . . .
F4 F 0.8716(2) 0.08013(12) 0.5362(2) 0.0515(6) Uani 1 1 d . . .
F5 F 0.6431(2) 0.02476(12) 0.5135(2) 0.0493(6) Uani 1 1 d . . .
F6 F 0.90522(18) 0.06243(10) 0.76364(17) 0.0345(4) Uani 1 1 d . . .
Fe Fe 0.75361(4) 0.654603(18) 0.61620(3) 0.01665(8) Uani 1 1 d . . .
Sb Sb 0.774246(18) 0.043389(10) 0.637509(16) 0.02310(6) 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
C1 O2 1.239(3) . ?
C1 O1 1.276(3) . ?
C1 C2 1.506(4) . ?
C2 N1 1.459(3) . ?
C2 C3 1.496(4) . ?
C2 C4 1.504(4) . ?
C3 C4 1.491(6) . ?
C5 N3 1.489(4) . ?
C5 C6 1.517(5) . ?
C6 N2 1.485(4) . ?
C7 N2 1.465(4) . ?
C8 N3 1.469(4) . ?
C9 N2 1.474(4) . ?
C9 C10 1.502(4) . ?
C10 N5 1.344(3) . ?
C10 C11 1.385(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.371(4) . ?
C13 C14 1.382(4) . ?
C14 N5 1.338(4) . ?
C15 N3 1.483(4) . ?
C15 C16 1.508(5) . ?
C16 N4 1.350(4) . ?
C16 C17 1.375(4) . ?
C17 C18 1.378(5) . ?
C18 C19 1.387(5) . ?
C19 C20 1.373(4) . ?
C20 N4 1.337(4) . ?
N1 Fe 2.203(2) . ?
N2 Fe 2.232(2) . ?
N3 Fe 2.242(3) . ?
N4 Fe 2.203(2) . ?
N5 Fe 2.211(2) . ?
O1 Fe 2.0164(19) . ?
F1 Sb 1.8620(19) . ?
F2 Sb 1.8752(19) . ?
F3 Sb 1.8760(19) . ?
F4 Sb 1.862(2) . ?
F5 Sb 1.860(2) . ?
F6 Sb 1.8765(18) . ?

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 C1 O1 124.7(3) . . ?
O2 C1 C2 118.2(2) . . ?
O1 C1 C2 117.1(2) . . ?
N1 C2 C3 118.2(2) . . ?
N1 C2 C4 119.0(2) . . ?
C3 C2 C4 59.6(2) . . ?
N1 C2 C1 114.9(2) . . ?
C3 C2 C1 116.4(2) . . ?
C4 C2 C1 117.5(2) . . ?
C4 C3 C2 60.5(2) . . ?
C3 C4 C2 59.9(2) . . ?
N3 C5 C6 111.2(3) . . ?
N2 C6 C5 110.9(2) . . ?
N2 C9 C10 110.9(2) . . ?
N5 C10 C11 122.5(3) . . ?
N5 C10 C9 115.5(2) . . ?
C11 C10 C9 122.0(3) . . ?
C10 C11 C12 118.6(3) . . ?
C13 C12 C11 119.3(3) . . ?
C12 C13 C14 118.7(3) . . ?
N5 C14 C13 123.0(3) . . ?
N3 C15 C16 109.9(3) . . ?
N4 C16 C17 122.2(3) . . ?
N4 C16 C15 115.5(3) . . ?
C17 C16 C15 122.3(3) . . ?
C16 C17 C18 119.2(3) . . ?
C17 C18 C19 118.9(3) . . ?
C20 C19 C18 118.8(3) . . ?
N4 C20 C19 122.8(3) . . ?
C2 N1 Fe 106.70(15) . . ?
C7 N2 C9 109.0(2) . . ?
C7 N2 C6 110.9(3) . . ?
C9 N2 C6 109.2(2) . . ?
C7 N2 Fe 114.52(19) . . ?
C9 N2 Fe 106.58(16) . . ?
C6 N2 Fe 106.46(18) . . ?
C8 N3 C15 108.7(3) . . ?
C8 N3 C5 111.8(3) . . ?
C15 N3 C5 110.2(3) . . ?
C8 N3 Fe 113.5(2) . . ?
C15 N3 Fe 106.40(18) . . ?
C5 N3 Fe 106.03(19) . . ?
C20 N4 C16 118.2(3) . . ?
C20 N4 Fe 126.3(2) . . ?
C16 N4 Fe 115.5(2) . . ?
C14 N5 C10 117.9(2) . . ?
C14 N5 Fe 126.79(18) . . ?
C10 N5 Fe 115.28(18) . . ?
C1 O1 Fe 118.91(17) . . ?
O1 Fe N4 96.69(9) . . ?
O1 Fe N1 79.89(8) . . ?
N4 Fe N1 96.08(9) . . ?
O1 Fe N5 93.35(8) . . ?
N4 Fe N5 167.38(9) . . ?
N1 Fe N5 93.18(8) . . ?
O1 Fe N2 167.94(9) . . ?
N4 Fe N2 95.32(9) . . ?
N1 Fe N2 97.74(8) . . ?
N5 Fe N2 74.90(9) . . ?
O1 Fe N3 103.04(9) . . ?
N4 Fe N3 75.02(9) . . ?
N1 Fe N3 170.83(9) . . ?
N5 Fe N3 95.30(9) . . ?
N2 Fe N3 81.16(10) . . ?
F5 Sb F1 90.03(9) . . ?
F5 Sb F4 90.94(12) . . ?
F1 Sb F4 90.35(10) . . ?
F5 Sb F2 91.02(11) . . ?
F1 Sb F2 90.41(9) . . ?
F4 Sb F2 177.89(10) . . ?
F5 Sb F3 90.64(9) . . ?
F1 Sb F3 179.16(9) . . ?
F4 Sb F3 90.14(10) . . ?
F2 Sb F3 89.07(9) . . ?
F5 Sb F6 179.37(10) . . ?
F1 Sb F6 90.36(9) . . ?
F4 Sb F6 89.55(10) . . ?
F2 Sb F6 88.48(9) . . ?
F3 Sb F6 88.96(9) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.053
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.107
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1029373'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;
#2002GuillotICMMO
#Roux Avenier LCBB  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C20 H28 Fe N6, 2(F6 Sb)'
_chemical_formula_sum            'C20 H28 F12 Fe N6 Sb2'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            red

_diffrn_ambient_temperature      100(1)
_chemical_formula_weight         879.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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'
F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8476 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5870 1.5507 '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 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

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                   17.2217(6)
_cell_length_b                   20.1069(7)
_cell_length_c                   16.9451(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4780(10)
_cell_angle_gamma                90.00
_cell_volume                     5865.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9270
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      33.70
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3408
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            72834
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         33.82
_reflns_number_total             21292
_reflns_number_gt                17682
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0293P)²+10.8234P] 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         21292
_refine_ls_number_parameters     747
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0691
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_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
Sb1 Sb 0.368386(9) 0.437672(7) 0.094510(9) 0.01899(3) Uani 1 1 d . . .
F2 F 0.45126(10) 0.46299(8) 0.16200(10) 0.0348(4) Uani 1 1 d . . .
F5 F 0.28751(11) 0.41155(11) 0.02589(13) 0.0480(5) Uani 1 1 d . . .
F4 F 0.42788(10) 0.36553(8) 0.05973(9) 0.0304(3) Uani 1 1 d . . .
F1 F 0.31138(11) 0.51061(9) 0.13026(12) 0.0402(4) Uani 1 1 d . . .
F6 F 0.32835(12) 0.38479(9) 0.17441(11) 0.0419(4) Uani 1 1 d . . .
F3 F 0.40833(12) 0.49021(9) 0.01395(11) 0.0423(4) Uani 1 1 d . . .
Sb2 Sb 0.280756(9) 0.506452(8) 0.612076(8) 0.01890(3) Uani 1 1 d . . .
F14 F 0.27552(13) 0.58812(9) 0.56000(11) 0.0460(5) Uani 1 1 d . . .
F16 F 0.28548(13) 0.42476(9) 0.66476(12) 0.0470(5) Uani 1 1 d . . .
F13 F 0.26687(10) 0.46242(9) 0.51540(9) 0.0359(4) Uani 1 1 d . . .
F17 F 0.17396(10) 0.50944(9) 0.62480(14) 0.0459(5) Uani 1 1 d . . .
F15 F 0.38826(11) 0.50320(13) 0.59872(14) 0.0587(6) Uani 1 1 d . . .
F18 F 0.29706(15) 0.55139(10) 0.70765(10) 0.0518(6) Uani 1 1 d . . .
Sb3 Sb 0.159509(9) 0.254753(7) 0.358191(9) 0.02024(3) Uani 1 1 d . . .
F9 F 0.08795(12) 0.22609(10) 0.43223(12) 0.0474(5) Uani 1 1 d . . .
F10 F 0.17305(12) 0.33430(9) 0.41518(11) 0.0419(4) Uani 1 1 d . . .
F11 F 0.07622(10) 0.29242(9) 0.30030(11) 0.0367(4) Uani 1 1 d . . .
F8 F 0.24132(11) 0.21667(10) 0.41715(11) 0.0418(4) Uani 1 1 d . . .
F7 F 0.22782(9) 0.28482(9) 0.28233(10) 0.0346(4) Uani 1 1 d . . .
F12 F 0.14737(11) 0.17472(8) 0.30342(13) 0.0430(4) Uani 1 1 d . . .
Sb4 Sb 0.177232(10) 0.714786(9) 0.918798(10) 0.02566(4) Uani 1 1 d . . .
F19 F 0.27763(11) 0.72229(11) 0.96301(12) 0.0464(5) Uani 1 1 d . . .
F21 F 0.07993(14) 0.70829(18) 0.86955(19) 0.0908(10) Uani 1 1 d . . .
F20 F 0.22428(15) 0.70972(17) 0.82082(12) 0.0815(10) Uani 1 1 d . . .
F22 F 0.13495(16) 0.71821(11) 1.01844(13) 0.0616(7) Uani 1 1 d . . .
F23 F 0.17346(14) 0.80656(12) 0.9119(2) 0.0807(9) Uani 1 1 d . . .
F24 F 0.18279(17) 0.62266(11) 0.92649(18) 0.0733(8) Uani 1 1 d . . .
Fe5 Fe 0.486366(17) 0.728372(14) 0.231168(17) 0.01275(5) Uani 1 1 d . . .
N4 N 0.43900(10) 0.66053(9) 0.29952(10) 0.0146(3) Uani 1 1 d . . .
N1 N 0.40051(10) 0.72725(9) 0.14540(11) 0.0162(3) Uani 1 1 d . . .
N2 N 0.52805(10) 0.64520(9) 0.17792(10) 0.0155(3) Uani 1 1 d . . .
N3 N 0.53000(10) 0.79487(9) 0.15739(11) 0.0159(3) Uani 1 1 d . . .
N5 N 0.57621(11) 0.73184(9) 0.30293(11) 0.0172(3) Uani 1 1 d . . .
N6 N 0.43994(11) 0.80148(9) 0.28819(11) 0.0173(3) Uani 1 1 d . . .
C100 C 0.47742(13) 0.82120(11) 0.10540(13) 0.0183(4) Uani 1 1 d . . .
C101 C 0.47012(12) 0.59901(10) 0.29482(12) 0.0162(4) Uani 1 1 d . . .
C102 C 0.41669(13) 0.84514(11) 0.32388(13) 0.0182(4) Uani 1 1 d . . .
C103 C 0.46582(13) 0.62199(11) 0.12080(12) 0.0179(4) Uani 1 1 d . . .
H10A H 0.4271 0.5965 0.1484 0.022 Uiso 1 1 calc R . .
H10B H 0.4882 0.5937 0.0810 0.022 Uiso 1 1 calc R . .
C106 C 0.44148(14) 0.54524(11) 0.33634(13) 0.0202(4) Uani 1 1 d . . .
H106 H 0.4633 0.5032 0.3309 0.024 Uiso 1 1 calc R . .
C107 C 0.53755(13) 0.59422(10) 0.24078(13) 0.0176(4) Uani 1 1 d . . .
H10C H 0.5858 0.6016 0.2703 0.021 Uiso 1 1 calc R . .
H10D H 0.5394 0.5502 0.2174 0.021 Uiso 1 1 calc R . .
C108 C 0.37949(12) 0.66974(11) 0.34884(12) 0.0174(4) Uani 1 1 d . . .
H108 H 0.3584 0.7121 0.3533 0.021 Uiso 1 1 calc R . .
C109 C 0.60394(13) 0.81619(11) 0.15458(13) 0.0188(4) Uani 1 1 d . . .
H109 H 0.6399 0.8002 0.1918 0.023 Uiso 1 1 calc R . .
C111 C 0.32152(13) 0.70683(12) 0.16861(14) 0.0217(4) Uani 1 1 d . . .
H11A H 0.3051 0.7341 0.2116 0.033 Uiso 1 1 calc R . .
H11B H 0.3224 0.6611 0.1847 0.033 Uiso 1 1 calc R . .
H11C H 0.2860 0.7122 0.1245 0.033 Uiso 1 1 calc R . .
C112 C 0.38609(15) 0.90031(12) 0.36934(15) 0.0239(4) Uani 1 1 d . . .
H11D H 0.3395 0.8865 0.3946 0.036 Uiso 1 1 calc R . .
H11E H 0.3746 0.9370 0.3347 0.036 Uiso 1 1 calc R . .
H11F H 0.4240 0.9138 0.4087 0.036 Uiso 1 1 calc R . .
C113 C 0.62855(14) 0.73457(11) 0.34554(14) 0.0203(4) Uani 1 1 d . . .
C115 C 0.34866(13) 0.61869(12) 0.39285(13) 0.0200(4) Uani 1 1 d . . .
H115 H 0.3078 0.6267 0.4264 0.024 Uiso 1 1 calc R . .
C116 C 0.62840(14) 0.86094(12) 0.09846(14) 0.0233(4) Uani 1 1 d . . .
H116 H 0.6803 0.8736 0.0970 0.028 Uiso 1 1 calc R . .
C118 C 0.57470(16) 0.88672(12) 0.04441(15) 0.0273(5) Uani 1 1 d . . .
H118 H 0.5899 0.9167 0.0060 0.033 Uiso 1 1 calc R . .
C121 C 0.42862(13) 0.68191(11) 0.08237(12) 0.0185(4) Uani 1 1 d . . .
H12D H 0.4661 0.7049 0.0504 0.022 Uiso 1 1 calc R . .
H12E H 0.3854 0.6682 0.0483 0.022 Uiso 1 1 calc R . .
C122 C 0.37985(14) 0.55519(12) 0.38606(13) 0.0213(4) Uani 1 1 d . . .
H122 H 0.3596 0.5199 0.4145 0.026 Uiso 1 1 calc R . .
C128 C 0.60244(13) 0.65175(12) 0.13690(13) 0.0202(4) Uani 1 1 d . . .
H12K H 0.6416 0.6682 0.1732 0.030 Uiso 1 1 calc R . .
H12L H 0.5961 0.6822 0.0936 0.030 Uiso 1 1 calc R . .
H12M H 0.6179 0.6091 0.1173 0.030 Uiso 1 1 calc R . .
C129 C 0.69672(16) 0.73791(14) 0.39827(17) 0.0296(5) Uani 1 1 d . . .
H12N H 0.7141 0.6937 0.4107 0.044 Uiso 1 1 calc R . .
H12O H 0.6835 0.7605 0.4460 0.044 Uiso 1 1 calc R . .
H12P H 0.7374 0.7618 0.3728 0.044 Uiso 1 1 calc R . .
C130 C 0.39642(13) 0.79597(11) 0.11363(14) 0.0196(4) Uani 1 1 d . . .
H13A H 0.3682 0.8244 0.1492 0.023 Uiso 1 1 calc R . .
H13B H 0.3695 0.7961 0.0627 0.023 Uiso 1 1 calc R . .
C139 C 0.49803(15) 0.86694(12) 0.04869(15) 0.0247(5) Uani 1 1 d . . .
H139 H 0.4607 0.8842 0.0138 0.030 Uiso 1 1 calc R . .
Fe6 Fe 0.026783(17) 0.515076(15) 0.248048(17) 0.01390(5) Uani 1 1 d . . .
N9 N 0.05556(11) 0.46663(10) 0.15226(11) 0.0187(3) Uani 1 1 d . . .
N7 N 0.07687(11) 0.59213(9) 0.19013(12) 0.0210(4) Uani 1 1 d . . .
N12 N -0.07550(11) 0.53049(9) 0.20096(11) 0.0171(3) Uani 1 1 d . . .
N11 N -0.01939(12) 0.43636(9) 0.29396(11) 0.0188(3) Uani 1 1 d . . .
N8 N 0.13118(12) 0.50466(11) 0.30493(13) 0.0254(4) Uani 1 1 d . . .
N10 N 0.00321(12) 0.56469(10) 0.34546(12) 0.0203(4) Uani 1 1 d . . .
C104 C 0.05974(15) 0.40056(11) 0.14275(14) 0.0222(4) Uani 1 1 d . . .
H104 H 0.0454 0.3731 0.1841 0.027 Uiso 1 1 calc R . .
C110 C -0.05786(15) 0.39312(11) 0.31279(13) 0.0215(4) Uani 1 1 d . . .
C114 C 0.11367(17) 0.50048(15) 0.39032(16) 0.0331(6) Uani 1 1 d . . .
H11G H 0.1601 0.5100 0.4220 0.040 Uiso 1 1 calc R . .
H11H H 0.0961 0.4560 0.4032 0.040 Uiso 1 1 calc R . .
C117 C -0.13854(13) 0.53250(12) 0.17902(13) 0.0197(4) Uani 1 1 d . . .
C119 C -0.05529(14) 0.60760(12) 0.35661(14) 0.0218(4) Uani 1 1 d . . .
H119 H -0.0893 0.6169 0.3146 0.026 Uiso 1 1 calc R . .
C120 C 0.04900(16) 0.65986(12) 0.20835(17) 0.0294(5) Uani 1 1 d . . .
H12A H 0.0646 0.6714 0.2614 0.044 Uiso 1 1 calc R . .
H12B H -0.0066 0.6611 0.2031 0.044 Uiso 1 1 calc R . .
H12C H 0.0710 0.6911 0.1723 0.044 Uiso 1 1 calc R . .
C123 C 0.08457(17) 0.37155(13) 0.07378(15) 0.0279(5) Uani 1 1 d . . .
H123 H 0.0856 0.3255 0.0685 0.033 Uiso 1 1 calc R . .
C124 C -0.21963(14) 0.53499(14) 0.15178(16) 0.0277(5) Uani 1 1 d . . .
H12F H -0.2514 0.5496 0.1941 0.042 Uiso 1 1 calc R . .
H12G H -0.2360 0.4915 0.1349 0.042 Uiso 1 1 calc R . .
H12H H -0.2248 0.5655 0.1084 0.042 Uiso 1 1 calc R . .
C126 C 0.07423(15) 0.50609(12) 0.09056(14) 0.0239(5) Uani 1 1 d . . .
C127 C 0.16229(15) 0.58767(14) 0.2065(2) 0.0341(6) Uani 1 1 d . . .
H12I H 0.1852 0.5551 0.1719 0.041 Uiso 1 1 calc R . .
H12J H 0.1865 0.6304 0.1971 0.041 Uiso 1 1 calc R . .
C132 C -0.06667(16) 0.63842(14) 0.42850(15) 0.0298(5) Uani 1 1 d . . .
H132 H -0.1077 0.6680 0.4344 0.036 Uiso 1 1 calc R . .
C133 C 0.10132(19) 0.48039(14) 0.02082(16) 0.0337(6) Uani 1 1 d . . .
H133 H 0.1150 0.5085 -0.0201 0.040 Uiso 1 1 calc R . .
C134 C -0.10843(18) 0.33822(13) 0.33509(17) 0.0314(6) Uani 1 1 d . . .
H13C H -0.1516 0.3553 0.3635 0.047 Uiso 1 1 calc R . .
H13D H -0.0797 0.3075 0.3680 0.047 Uiso 1 1 calc R . .
H13E H -0.1272 0.3157 0.2884 0.047 Uiso 1 1 calc R . .
C135 C 0.05132(16) 0.55040(14) 0.40758(15) 0.0286(5) Uani 1 1 d . . .
C136 C 0.17514(16) 0.56764(15) 0.2906(2) 0.0359(6) Uani 1 1 d . . .
H13F H 0.1571 0.6025 0.3253 0.043 Uiso 1 1 calc R . .
H13G H 0.2301 0.5607 0.3015 0.043 Uiso 1 1 calc R . .
C140 C 0.06258(17) 0.57925(12) 0.10471(15) 0.0278(5) Uani 1 1 d . . .
H14A H 0.0984 0.6049 0.0737 0.033 Uiso 1 1 calc R . .
H14B H 0.0100 0.5921 0.0894 0.033 Uiso 1 1 calc R . .
C142 C 0.0433(2) 0.57972(17) 0.48100(16) 0.0400(7) Uani 1 1 d . . .
H142 H 0.0774 0.5693 0.5226 0.048 Uiso 1 1 calc R . .
C144 C 0.10785(18) 0.41208(14) 0.01279(16) 0.0322(6) Uani 1 1 d . . .
H144 H 0.1276 0.3937 -0.0329 0.039 Uiso 1 1 calc R . .
C146 C 0.17884(16) 0.44661(14) 0.28304(18) 0.0321(6) Uani 1 1 d . . .
H14C H 0.2240 0.4442 0.3174 0.048 Uiso 1 1 calc R . .
H14D H 0.1946 0.4512 0.2294 0.048 Uiso 1 1 calc R . .
H14E H 0.1488 0.4067 0.2882 0.048 Uiso 1 1 calc R . .
C150 C -0.0164(2) 0.62471(17) 0.49132(17) 0.0391(7) Uani 1 1 d . . .
H150 H -0.0225 0.6455 0.5398 0.047 Uiso 1 1 calc R . .


_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
Sb1 F5 1.8667(18) . ?
Sb1 F6 1.8675(16) . ?
Sb1 F3 1.8711(16) . ?
Sb1 F1 1.8742(16) . ?
Sb1 F2 1.8762(16) . ?
Sb1 F4 1.8795(15) . ?
Sb2 F17 1.8583(17) . ?
Sb2 F14 1.8653(17) . ?
Sb2 F18 1.8694(17) . ?
Sb2 F16 1.8703(18) . ?
Sb2 F13 1.8720(15) . ?
Sb2 F15 1.8722(19) . ?
Sb3 F7 1.8654(16) . ?
Sb3 F12 1.8667(17) . ?
Sb3 F8 1.8700(17) . ?
Sb3 F9 1.8722(17) . ?
Sb3 F11 1.8764(16) . ?
Sb3 F10 1.8798(17) . ?
Sb4 F23 1.850(2) . ?
Sb4 F22 1.8572(19) . ?
Sb4 F21 1.857(2) . ?
Sb4 F24 1.859(2) . ?
Sb4 F20 1.869(2) . ?
Sb4 F19 1.8726(18) . ?
Fe5 N6 1.9426(19) . ?
Fe5 N5 1.9444(19) . ?
Fe5 N4 1.9790(18) . ?
Fe5 N3 1.9910(18) . ?
Fe5 N2 2.0395(18) . ?
Fe5 N1 2.0465(18) . ?
N4 C101 1.351(3) . ?
N4 C108 1.352(3) . ?
N1 C111 1.484(3) . ?
N1 C130 1.484(3) . ?
N1 C121 1.494(3) . ?
N2 C128 1.479(3) . ?
N2 C107 1.484(3) . ?
N2 C103 1.500(3) . ?
N3 C109 1.346(3) . ?
N3 C100 1.355(3) . ?
N5 C113 1.141(3) . ?
N6 C102 1.144(3) . ?
C100 C139 1.383(3) . ?
C100 C130 1.494(3) . ?
C101 C106 1.388(3) . ?
C101 C107 1.500(3) . ?
C102 C112 1.457(3) . ?
C103 C121 1.505(3) . ?
C106 C122 1.387(3) . ?
C108 C115 1.383(3) . ?
C109 C116 1.383(3) . ?
C113 C129 1.458(3) . ?
C115 C122 1.391(3) . ?
C116 C118 1.385(4) . ?
C118 C139 1.383(4) . ?
Fe6 N12 1.9399(19) . ?
Fe6 N11 1.9428(19) . ?
Fe6 N9 1.9673(19) . ?
Fe6 N10 1.9797(19) . ?
Fe6 N8 2.029(2) . ?
Fe6 N7 2.0376(19) . ?
N9 C104 1.340(3) . ?
N9 C126 1.358(3) . ?
N7 C120 1.479(3) . ?
N7 C140 1.485(3) . ?
N7 C127 1.493(3) . ?
N12 C117 1.139(3) . ?
N11 C110 1.143(3) . ?
N8 C146 1.480(3) . ?
N8 C114 1.488(4) . ?
N8 C136 1.499(4) . ?
N10 C119 1.343(3) . ?
N10 C135 1.354(3) . ?
C104 C123 1.384(3) . ?
C110 C134 1.462(3) . ?
C114 C135 1.504(4) . ?
C117 C124 1.460(3) . ?
C119 C132 1.385(3) . ?
C123 C144 1.384(4) . ?
C126 C133 1.382(3) . ?
C126 C140 1.505(3) . ?
C127 C136 1.491(5) . ?
C132 C150 1.383(4) . ?
C133 C144 1.385(4) . ?
C135 C142 1.387(4) . ?
C142 C150 1.383(4) . ?

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
F5 Sb1 F6 90.45(10) . . ?
F5 Sb1 F3 89.25(10) . . ?
F6 Sb1 F3 179.62(9) . . ?
F5 Sb1 F1 91.88(9) . . ?
F6 Sb1 F1 90.28(8) . . ?
F3 Sb1 F1 89.97(8) . . ?
F5 Sb1 F2 178.72(9) . . ?
F6 Sb1 F2 90.10(9) . . ?
F3 Sb1 F2 90.19(9) . . ?
F1 Sb1 F2 89.27(8) . . ?
F5 Sb1 F4 89.52(8) . . ?
F6 Sb1 F4 90.14(8) . . ?
F3 Sb1 F4 89.62(8) . . ?
F1 Sb1 F4 178.54(8) . . ?
F2 Sb1 F4 89.33(7) . . ?
F17 Sb2 F14 89.45(9) . . ?
F17 Sb2 F18 90.62(10) . . ?
F14 Sb2 F18 89.35(9) . . ?
F17 Sb2 F16 90.23(9) . . ?
F14 Sb2 F16 179.61(10) . . ?
F18 Sb2 F16 90.42(9) . . ?
F17 Sb2 F13 90.71(9) . . ?
F14 Sb2 F13 89.94(9) . . ?
F18 Sb2 F13 178.48(9) . . ?
F16 Sb2 F13 90.30(9) . . ?
F17 Sb2 F15 179.68(10) . . ?
F14 Sb2 F15 90.54(11) . . ?
F18 Sb2 F15 89.69(10) . . ?
F16 Sb2 F15 89.77(11) . . ?
F13 Sb2 F15 88.98(9) . . ?
F7 Sb3 F12 90.08(9) . . ?
F7 Sb3 F8 91.20(8) . . ?
F12 Sb3 F8 89.18(9) . . ?
F7 Sb3 F9 177.89(9) . . ?
F12 Sb3 F9 90.03(10) . . ?
F8 Sb3 F9 90.91(9) . . ?
F7 Sb3 F11 89.78(8) . . ?
F12 Sb3 F11 90.79(8) . . ?
F8 Sb3 F11 179.02(9) . . ?
F9 Sb3 F11 88.11(9) . . ?
F7 Sb3 F10 90.35(8) . . ?
F12 Sb3 F10 178.68(9) . . ?
F8 Sb3 F10 89.55(9) . . ?
F9 Sb3 F10 89.59(9) . . ?
F11 Sb3 F10 90.47(9) . . ?
F23 Sb4 F22 90.39(12) . . ?
F23 Sb4 F21 90.67(14) . . ?
F22 Sb4 F21 92.33(14) . . ?
F23 Sb4 F24 179.00(13) . . ?
F22 Sb4 F24 89.65(11) . . ?
F21 Sb4 F24 90.32(15) . . ?
F23 Sb4 F20 90.76(15) . . ?
F22 Sb4 F20 177.19(13) . . ?
F21 Sb4 F20 90.22(13) . . ?
F24 Sb4 F20 89.16(14) . . ?
F23 Sb4 F19 88.60(11) . . ?
F22 Sb4 F19 90.74(11) . . ?
F21 Sb4 F19 176.85(12) . . ?
F24 Sb4 F19 90.39(12) . . ?
F20 Sb4 F19 86.72(10) . . ?
N6 Fe5 N5 89.59(8) . . ?
N6 Fe5 N4 92.83(8) . . ?
N5 Fe5 N4 89.54(8) . . ?
N6 Fe5 N3 88.34(8) . . ?
N5 Fe5 N3 93.53(8) . . ?
N4 Fe5 N3 176.72(7) . . ?
N6 Fe5 N2 174.05(8) . . ?
N5 Fe5 N2 91.30(7) . . ?
N4 Fe5 N2 81.30(7) . . ?
N3 Fe5 N2 97.47(7) . . ?
N6 Fe5 N1 93.58(8) . . ?
N5 Fe5 N1 173.34(8) . . ?
N4 Fe5 N1 96.14(7) . . ?
N3 Fe5 N1 80.73(7) . . ?
N2 Fe5 N1 86.15(7) . . ?
C101 N4 C108 118.04(18) . . ?
C101 N4 Fe5 115.24(14) . . ?
C108 N4 Fe5 126.71(15) . . ?
C111 N1 C130 108.57(17) . . ?
C111 N1 C121 109.68(17) . . ?
C130 N1 C121 108.79(17) . . ?
C111 N1 Fe5 117.73(14) . . ?
C130 N1 Fe5 105.91(13) . . ?
C121 N1 Fe5 105.84(13) . . ?
C128 N2 C107 108.54(17) . . ?
C128 N2 C103 109.73(17) . . ?
C107 N2 C103 108.18(16) . . ?
C128 N2 Fe5 116.99(14) . . ?
C107 N2 Fe5 106.40(13) . . ?
C103 N2 Fe5 106.67(13) . . ?
C109 N3 C100 118.02(19) . . ?
C109 N3 Fe5 127.51(15) . . ?
C100 N3 Fe5 114.46(14) . . ?
C113 N5 Fe5 179.1(2) . . ?
C102 N6 Fe5 176.04(19) . . ?
N3 C100 C139 122.2(2) . . ?
N3 C100 C130 114.61(19) . . ?
C139 C100 C130 123.2(2) . . ?
N4 C101 C106 122.5(2) . . ?
N4 C101 C107 114.15(18) . . ?
C106 C101 C107 123.4(2) . . ?
N6 C102 C112 179.2(2) . . ?
N2 C103 C121 108.62(17) . . ?
C122 C106 C101 118.9(2) . . ?
N2 C107 C101 108.72(17) . . ?
N4 C108 C115 122.6(2) . . ?
N3 C109 C116 122.5(2) . . ?
N5 C113 C129 178.5(3) . . ?
C108 C115 C122 118.8(2) . . ?
C109 C116 C118 119.2(2) . . ?
C139 C118 C116 118.7(2) . . ?
N1 C121 C103 108.74(17) . . ?
C106 C122 C115 119.1(2) . . ?
N1 C130 C100 108.31(17) . . ?
C118 C139 C100 119.4(2) . . ?
N12 Fe6 N11 85.30(8) . . ?
N12 Fe6 N9 89.15(8) . . ?
N11 Fe6 N9 92.37(8) . . ?
N12 Fe6 N10 93.38(8) . . ?
N11 Fe6 N10 88.96(8) . . ?
N9 Fe6 N10 177.23(8) . . ?
N12 Fe6 N8 174.93(8) . . ?
N11 Fe6 N8 95.31(9) . . ?
N9 Fe6 N8 95.85(8) . . ?
N10 Fe6 N8 81.61(8) . . ?
N12 Fe6 N7 94.11(8) . . ?
N11 Fe6 N7 174.32(8) . . ?
N9 Fe6 N7 81.97(8) . . ?
N10 Fe6 N7 96.71(8) . . ?
N8 Fe6 N7 85.78(9) . . ?
C104 N9 C126 118.17(19) . . ?
C104 N9 Fe6 127.26(15) . . ?
C126 N9 Fe6 114.56(15) . . ?
C120 N7 C140 108.5(2) . . ?
C120 N7 C127 109.9(2) . . ?
C140 N7 C127 108.0(2) . . ?
C120 N7 Fe6 117.12(15) . . ?
C140 N7 Fe6 105.98(14) . . ?
C127 N7 Fe6 106.98(16) . . ?
C117 N12 Fe6 170.96(19) . . ?
C110 N11 Fe6 167.8(2) . . ?
C146 N8 C114 109.1(2) . . ?
C146 N8 C136 109.9(2) . . ?
C114 N8 C136 108.7(2) . . ?
C146 N8 Fe6 116.93(17) . . ?
C114 N8 Fe6 105.58(16) . . ?
C136 N8 Fe6 106.32(16) . . ?
C119 N10 C135 118.2(2) . . ?
C119 N10 Fe6 127.70(16) . . ?
C135 N10 Fe6 114.01(16) . . ?
N9 C104 C123 122.6(2) . . ?
N11 C110 C134 178.5(3) . . ?
N8 C114 C135 108.4(2) . . ?
N12 C117 C124 179.4(3) . . ?
N10 C119 C132 122.3(2) . . ?
C144 C123 C104 119.0(2) . . ?
N9 C126 C133 122.1(2) . . ?
N9 C126 C140 114.4(2) . . ?
C133 C126 C140 123.4(2) . . ?
C136 C127 N7 108.4(2) . . ?
C150 C132 C119 119.2(2) . . ?
C126 C133 C144 119.0(2) . . ?
N10 C135 C142 122.3(2) . . ?
N10 C135 C114 114.6(2) . . ?
C142 C135 C114 123.1(2) . . ?
C127 C136 N8 108.7(2) . . ?
N7 C140 C126 107.8(2) . . ?
C150 C142 C135 118.9(3) . . ?
C123 C144 C133 119.0(2) . . ?
C142 C150 C132 119.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.902
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.405
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.114

