# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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 1541142'
_audit_update_record             
;
2017-03-30 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H63 Fe N9, 2(B F4)'
_chemical_formula_sum            'C48 H63 B2 F8 Fe N9'
_chemical_formula_weight         995.54
_chemical_absolute_configuration rmad

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'
B B 0.0013 0.0007 '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 0.0171 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           Cubic
_symmetry_space_group_name_H-M   P2(1)3
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'

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

_cell_length_a                   17.0031(2)
_cell_length_b                   17.0031(2)
_cell_length_c                   17.0031(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4915.69(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5016
_cell_measurement_theta_min      3.3891
_cell_measurement_theta_max      28.6120

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2088
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7574
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5438
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         25.62
_reflns_number_total             2841
_reflns_number_gt                2657
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0228P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(13)
_refine_ls_number_reflns         2841
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0535
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
B1 B 0.22616(13) 0.27384(13) 0.72616(13) 0.0198(9) Uani 1 3 d S . .
B2 B 0.78876(13) 0.71124(13) 0.28876(13) 0.0189(9) Uani 1 3 d S . .
C1 C 0.06500(10) 0.66436(10) 0.05591(10) 0.0138(4) Uani 1 1 d . . .
C2 C -0.05100(10) 0.64850(10) 0.10904(10) 0.0170(4) Uani 1 1 d . . .
H2 H -0.0946 0.6515 0.1438 0.029(5) Uiso 1 1 calc R . .
C3 C -0.04847(11) 0.60870(11) 0.03928(11) 0.0193(4) Uani 1 1 d . . .
H3 H -0.0901 0.5786 0.0173 0.027(5) Uiso 1 1 calc R . .
C4 C 0.14391(10) 0.68433(10) 0.03384(10) 0.0155(4) Uani 1 1 d . . .
H4 H 0.1773 0.7159 0.0657 0.020(5) Uiso 1 1 calc R . .
C5 C 0.24530(10) 0.67638(10) -0.06354(10) 0.0152(4) Uani 1 1 d . . .
H5 H 0.2384 0.6981 -0.1177 0.019(5) Uiso 1 1 calc R . .
C6 C 0.29735(10) 0.60386(10) -0.07015(10) 0.0145(4) Uani 1 1 d . . .
C7 C 0.30584(11) 0.55287(10) -0.00750(11) 0.0178(4) Uani 1 1 d . . .
H7 H 0.2759 0.5608 0.0390 0.013(5) Uiso 1 1 calc R . .
C8 C 0.35773(11) 0.49024(11) -0.01197(11) 0.0219(4) Uani 1 1 d . . .
H8 H 0.3631 0.4553 0.0313 0.021(5) Uiso 1 1 calc R . .
C9 C 0.40169(11) 0.47853(11) -0.07931(12) 0.0257(5) Uani 1 1 d . . .
H9 H 0.4368 0.4352 -0.0826 0.028(5) Uiso 1 1 calc R . .
C10 C 0.39460(11) 0.52985(11) -0.14191(12) 0.0226(5) Uani 1 1 d . . .
H10 H 0.4253 0.5220 -0.1880 0.026(5) Uiso 1 1 calc R . .
C11 C 0.34251(10) 0.59319(11) -0.13775(10) 0.0174(4) Uani 1 1 d . . .
H11 H 0.3379 0.6287 -0.1806 0.009(4) Uiso 1 1 calc R . .
C12 C 0.29038(11) 0.73801(10) -0.01523(11) 0.0191(4) Uani 1 1 d . . .
H12A H 0.2581 0.7854 -0.0096 0.028(5) Uiso 1 1 calc R . .
H12B H 0.3395 0.7514 -0.0422 0.030(5) Uiso 1 1 calc R . .
H12C H 0.3023 0.7166 0.0369 0.013(5) Uiso 1 1 calc R . .
C13 C 0.03954(12) 0.74048(11) 0.18215(10) 0.0189(4) Uani 1 1 d . . .
H13A H 0.0067 0.7880 0.1748 0.025(5) Uiso 1 1 calc R . .
H13B H 0.0953 0.7564 0.1772 0.018(5) Uiso 1 1 calc R . .
C14 C 0.02570(11) 0.70785(11) 0.26466(10) 0.0197(4) Uani 1 1 d . . .
H14A H -0.0273 0.6839 0.2677 0.023(5) Uiso 1 1 calc R . .
H14B H 0.0650 0.6665 0.2763 0.020(5) Uiso 1 1 calc R . .
C15 C 0.03247(12) 0.77386(12) 0.32495(10) 0.0234(5) Uani 1 1 d . . .
H15A H 0.0849 0.7988 0.3200 0.041(6) Uiso 1 1 calc R . .
H15B H -0.0077 0.8144 0.3133 0.024(5) Uiso 1 1 calc R . .
C16 C 0.02157(13) 0.74550(12) 0.40899(11) 0.0285(5) Uani 1 1 d . . .
H16A H -0.0293 0.7189 0.4139 0.057(7) Uiso 1 1 calc R . .
H16B H 0.0232 0.7906 0.4448 0.037(6) Uiso 1 1 calc R . .
H16C H 0.0638 0.7087 0.4225 0.013(5) Uiso 1 1 calc R . .
F1 F 0.28194(6) 0.32021(7) 0.76397(7) 0.0329(3) Uani 1 1 d . . .
F2 F 0.17907(6) 0.32093(6) 0.67907(6) 0.0340(5) Uani 1 3 d S . .
F3 F 0.79784(7) 0.68970(7) 0.21080(6) 0.0374(3) Uani 1 1 d . . .
F4 F 0.83592(6) 0.66408(6) 0.33592(6) 0.0331(5) Uani 1 3 d S . .
Fe1 Fe 0.084555(14) 0.584555(14) -0.084555(14) 0.01205(11) Uani 1 3 d S . .
N1 N 0.02463(8) 0.61957(8) 0.00622(8) 0.0147(3) Uani 1 1 d . . .
N2 N 0.02073(8) 0.68314(9) 0.11961(8) 0.0162(3) Uani 1 1 d . . .
N3 N 0.16573(8) 0.65561(8) -0.03316(8) 0.0125(3) 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
B1 F2 1.387(4) . ?
B1 F1 1.3909(17) . ?
B1 F1 1.3909(17) 6_456 ?
B1 F1 1.3909(17) 12_565 ?
B2 F3 1.3840(17) . ?
B2 F3 1.3840(17) 6_566 ?
B2 F3 1.3840(17) 12_664 ?
B2 F4 1.389(4) . ?
C1 N1 1.329(2) . ?
C1 N2 1.357(2) . ?
C1 C4 1.434(2) . ?
C2 N2 1.366(2) . ?
C2 C3 1.366(3) . ?
C2 H2 0.9500 . ?
C3 N1 1.377(2) . ?
C3 H3 0.9500 . ?
C4 N3 1.294(2) . ?
C4 H4 0.9500 . ?
C5 N3 1.491(2) . ?
C5 C6 1.522(2) . ?
C5 C12 1.536(2) . ?
C5 H5 1.0000 . ?
C6 C7 1.381(2) . ?
C6 C11 1.394(2) . ?
C7 C8 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N2 1.478(2) . ?
C13 C14 1.527(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.524(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.519(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
Fe1 N1 1.9428(14) 8 ?
Fe1 N1 1.9428(14) 11_455 ?
Fe1 N1 1.9429(14) . ?
Fe1 N3 2.0318(15) . ?
Fe1 N3 2.0318(15) 11_455 ?
Fe1 N3 2.0318(15) 8 ?

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
F2 B1 F1 109.46(16) . . ?
F2 B1 F1 109.47(16) . 6_456 ?
F1 B1 F1 109.48(16) . 6_456 ?
F2 B1 F1 109.47(16) . 12_565 ?
F1 B1 F1 109.48(16) . 12_565 ?
F1 B1 F1 109.48(16) 6_456 12_565 ?
F3 B2 F3 109.32(16) . 6_566 ?
F3 B2 F3 109.31(16) . 12_664 ?
F3 B2 F3 109.32(16) 6_566 12_664 ?
F3 B2 F4 109.63(16) . . ?
F3 B2 F4 109.63(16) 6_566 . ?
F3 B2 F4 109.63(16) 12_664 . ?
N1 C1 N2 110.85(15) . . ?
N1 C1 C4 116.92(15) . . ?
N2 C1 C4 132.23(16) . . ?
N2 C2 C3 107.43(16) . . ?
N2 C2 H2 126.3 . . ?
C3 C2 H2 126.3 . . ?
C2 C3 N1 108.45(17) . . ?
C2 C3 H3 125.8 . . ?
N1 C3 H3 125.8 . . ?
N3 C4 C1 114.16(16) . . ?
N3 C4 H4 122.9 . . ?
C1 C4 H4 122.9 . . ?
N3 C5 C6 111.19(13) . . ?
N3 C5 C12 115.42(14) . . ?
C6 C5 C12 107.58(14) . . ?
N3 C5 H5 107.4 . . ?
C6 C5 H5 107.4 . . ?
C12 C5 H5 107.4 . . ?
C7 C6 C11 119.78(16) . . ?
C7 C6 C5 120.82(16) . . ?
C11 C6 C5 119.12(16) . . ?
C6 C7 C8 120.46(18) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.05(18) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.02(17) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 120.23(18) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C6 C11 C10 119.44(17) . . ?
C6 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C5 C12 H12A 109.5 . . ?
C5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 112.84(14) . . ?
N2 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N2 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 109.80(15) . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C16 C15 C14 112.93(16) . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 Fe1 N1 89.28(6) 8 11_455 ?
N1 Fe1 N1 89.29(6) 8 . ?
N1 Fe1 N1 89.28(6) 11_455 . ?
N1 Fe1 N3 169.51(6) 8 . ?
N1 Fe1 N3 92.21(6) 11_455 . ?
N1 Fe1 N3 80.35(6) . . ?
N1 Fe1 N3 92.21(6) 8 11_455 ?
N1 Fe1 N3 80.35(6) 11_455 11_455 ?
N1 Fe1 N3 169.50(6) . 11_455 ?
N3 Fe1 N3 98.28(5) . 11_455 ?
N1 Fe1 N3 80.35(6) 8 8 ?
N1 Fe1 N3 169.50(6) 11_455 8 ?
N1 Fe1 N3 92.22(6) . 8 ?
N3 Fe1 N3 98.28(5) . 8 ?
N3 Fe1 N3 98.28(5) 11_455 8 ?
C1 N1 C3 106.48(15) . . ?
C1 N1 Fe1 114.20(11) . . ?
C3 N1 Fe1 139.18(13) . . ?
C1 N2 C2 106.78(15) . . ?
C1 N2 C13 127.56(15) . . ?
C2 N2 C13 124.91(15) . . ?
C4 N3 C5 118.42(15) . . ?
C4 N3 Fe1 114.10(12) . . ?
C5 N3 Fe1 127.48(11) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.62
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.029
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1541143'
_audit_update_record             
;
2017-03-30 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H63 Fe N9, 2(B F4)'
_chemical_formula_sum            'C48 H63 B2 F8 Fe N9'
_chemical_formula_weight         995.54
_chemical_absolute_configuration rmad

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'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R3   '
_symmetry_space_group_name_Hall  'R3   '

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

_cell_length_a                   12.6436(16)
_cell_length_b                   12.6436(16)
_cell_length_c                   28.035(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3881.3(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2356
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.26

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1566
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9054
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'

_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  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8614
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.70
_reflns_number_total             3791
_reflns_number_gt                2809
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.1280P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_number_reflns         3791
_refine_ls_number_parameters     210
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0687
_refine_ls_wR_factor_ref         0.1982
_refine_ls_wR_factor_gt          0.1818
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.057
_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
C1 C 0.1164(4) 0.4316(4) 0.27826(15) 0.0446(9) Uani 1 1 d . . .
C2 C 0.1174(5) 0.5434(5) 0.2210(2) 0.0629(13) Uani 1 1 d . . .
H2 H 0.1409 0.6097 0.2007 0.075 Uiso 1 1 calc R . .
C3 C 0.0169(5) 0.4342(5) 0.2156(2) 0.0638(13) Uani 1 1 d . . .
H3 H -0.0409 0.4112 0.1915 0.077 Uiso 1 1 calc R . .
C4 C -0.0837(5) 0.2376(5) 0.2622(2) 0.0705(14) Uani 1 1 d . . .
H4A H -0.1553 0.2406 0.2727 0.085 Uiso 1 1 calc R . .
H4B H -0.0594 0.2027 0.2878 0.085 Uiso 1 1 calc R . .
C5 C -0.1162(6) 0.1571(5) 0.2196(2) 0.0695(14) Uani 1 1 d . . .
H5A H -0.0453 0.1515 0.2103 0.083 Uiso 1 1 calc R . .
H5B H -0.1351 0.1953 0.1935 0.083 Uiso 1 1 calc R . .
C6 C -0.2223(6) 0.0298(5) 0.2263(2) 0.0777(16) Uani 1 1 d . . .
H6A H -0.2024 -0.0098 0.2515 0.093 Uiso 1 1 calc R . .
H6B H -0.2927 0.0351 0.2366 0.093 Uiso 1 1 calc R . .
C7 C -0.2548(7) -0.0458(6) 0.1836(3) 0.091(2) Uani 1 1 d . . .
H7A H -0.3232 -0.1251 0.1904 0.136 Uiso 1 1 calc R . .
H7B H -0.1866 -0.0541 0.1738 0.136 Uiso 1 1 calc R . .
H7C H -0.2761 -0.0082 0.1585 0.136 Uiso 1 1 calc R . .
C8 C 0.1554(4) 0.4012(4) 0.32240(16) 0.0472(9) Uani 1 1 d . . .
H8 H 0.1134 0.3229 0.3352 0.057 Uiso 1 1 calc R . .
C9 C 0.2915(4) 0.4608(5) 0.38812(16) 0.0540(11) Uani 1 1 d . . .
H9 H 0.2971 0.5215 0.4112 0.065 Uiso 1 1 calc R . .
C10 C 0.4194(4) 0.4803(4) 0.38246(17) 0.0511(10) Uani 1 1 d . . .
C11 C 0.4509(5) 0.4346(5) 0.3436(2) 0.0638(13) Uani 1 1 d . . .
H11 H 0.3939 0.3934 0.3197 0.077 Uiso 1 1 calc R . .
C12 C 0.5667(7) 0.4499(6) 0.3402(3) 0.084(2) Uani 1 1 d . . .
H12 H 0.5878 0.4199 0.3138 0.100 Uiso 1 1 calc R . .
C13 C 0.6505(6) 0.5089(8) 0.3754(3) 0.091(2) Uani 1 1 d . . .
H13 H 0.7283 0.5188 0.3730 0.109 Uiso 1 1 calc R . .
C14 C 0.6201(6) 0.5531(8) 0.4140(3) 0.086(2) Uani 1 1 d . . .
H14 H 0.6770 0.5930 0.4381 0.103 Uiso 1 1 calc R . .
C15 C 0.5042(5) 0.5387(5) 0.41751(18) 0.0624(12) Uani 1 1 d . . .
H15 H 0.4839 0.5691 0.4440 0.075 Uiso 1 1 calc R . .
C16 C 0.2094(5) 0.3362(6) 0.4101(2) 0.0798(18) Uani 1 1 d . . .
H16A H 0.1318 0.3283 0.4179 0.120 Uiso 1 1 calc R . .
H16B H 0.2467 0.3277 0.4386 0.120 Uiso 1 1 calc R . .
H16C H 0.1977 0.2737 0.3877 0.120 Uiso 1 1 calc R . .
Fe1 Fe 0.3333 0.6667 0.30315(4) 0.0446(3) Uani 1 3 d S . .
N1 N 0.0159(4) 0.3627(4) 0.25268(14) 0.0561(10) Uani 1 1 d . . .
N2 N 0.1797(4) 0.5435(3) 0.26018(14) 0.0470(8) Uani 1 1 d . . .
N3 N 0.2494(3) 0.4864(4) 0.34282(13) 0.0459(8) Uani 1 1 d . . .
B2 B 0.6667 0.3333 0.1906(3) 0.037(2) Uiso 0.769(14) 3 d SPDU . 3
F3 F 0.6667 0.3333 0.2383(4) 0.143(5) Uiso 0.769(14) 3 d SPDU . 3
F4 F 0.7754(7) 0.4167(9) 0.1701(3) 0.157(3) Uiso 0.769(14) 1 d PDU . 3
B2' B 0.6667 0.3333 0.1672(9) 0.102(8) Uiso 0.231(14) 3 d SPDU . 4
F3' F 0.6667 0.3333 0.1188(9) 0.212(18) Uiso 0.231(14) 3 d SPDU . 4
F4' F 0.5504(8) 0.2915(17) 0.1832(6) 0.084(6) Uiso 0.231(14) 1 d PDU . 4
B1 B 1.0000 0.0000 0.3367(6) 0.117(6) Uiso 0.637(14) 3 d SPDU . 1
F1 F 0.9755(9) 0.0878(8) 0.3518(3) 0.134(4) Uiso 0.637(14) 1 d PDU . 1
F2 F 1.0000 0.0000 0.2882(6) 0.176(6) Uiso 0.637(14) 3 d SPDU . 1
B1' B 1.0000 0.0000 0.3427(8) 0.128(7) Uiso 0.363(14) 3 d SPDU . 2
F1' F 1.0574(18) 0.1167(8) 0.3259(6) 0.162(7) Uiso 0.363(14) 1 d PDU . 2
F2' F 1.0000 0.0000 0.3912(8) 0.173(11) Uiso 0.363(14) 3 d SPDU . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.329(6) . ?
C1 N1 1.334(6) . ?
C1 C8 1.453(6) . ?
C2 C3 1.337(8) . ?
C2 N2 1.351(6) . ?
C2 H2 0.9300 . ?
C3 N1 1.373(7) . ?
C3 H3 0.9300 . ?
C4 N1 1.472(7) . ?
C4 C5 1.487(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.505(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.457(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N3 1.273(6) . ?
C8 H8 0.9300 . ?
C9 N3 1.475(6) . ?
C9 C16 1.518(8) . ?
C9 C10 1.516(7) . ?
C9 H9 0.9800 . ?
C10 C15 1.367(7) . ?
C10 C11 1.382(7) . ?
C11 C12 1.381(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.365(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.358(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
Fe1 N2 2.151(4) . ?
Fe1 N2 2.151(4) 3_565 ?
Fe1 N2 2.151(4) 2_665 ?
Fe1 N3 2.267(4) 3_565 ?
Fe1 N3 2.267(4) 2_665 ?
Fe1 N3 2.267(4) . ?
B2 F3 1.336(8) . ?
B2 F4 1.372(7) . ?
B2 F4 1.372(7) 2_655 ?
B2 F4 1.372(7) 3_665 ?
B2' F3' 1.358(9) . ?
B2' F4' 1.365(8) 3_665 ?
B2' F4' 1.365(8) 2_655 ?
B2' F4' 1.365(8) . ?
B1 F1 1.361(7) 3_765 ?
B1 F1 1.361(7) 2_645 ?
B1 F1 1.361(7) . ?
B1 F2 1.361(9) . ?
B1' F2' 1.359(9) . ?
B1' F1' 1.362(8) 3_765 ?
B1' F1' 1.362(8) 2_645 ?
B1' F1' 1.362(8) . ?

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
N2 C1 N1 111.1(4) . . ?
N2 C1 C8 120.2(4) . . ?
N1 C1 C8 128.6(4) . . ?
C3 C2 N2 110.2(5) . . ?
C3 C2 H2 124.9 . . ?
N2 C2 H2 124.9 . . ?
C2 C3 N1 106.6(4) . . ?
C2 C3 H3 126.7 . . ?
N1 C3 H3 126.7 . . ?
N1 C4 C5 112.7(5) . . ?
N1 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 115.1(5) . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C7 C6 C5 114.0(6) . . ?
C7 C6 H6A 108.7 . . ?
C5 C6 H6A 108.7 . . ?
C7 C6 H6B 108.7 . . ?
C5 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C1 117.1(4) . . ?
N3 C8 H8 121.4 . . ?
C1 C8 H8 121.4 . . ?
N3 C9 C16 116.3(4) . . ?
N3 C9 C10 110.3(4) . . ?
C16 C9 C10 109.4(4) . . ?
N3 C9 H9 106.8 . . ?
C16 C9 H9 106.8 . . ?
C10 C9 H9 106.8 . . ?
C15 C10 C11 118.7(5) . . ?
C15 C10 C9 119.8(4) . . ?
C11 C10 C9 121.4(5) . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.4(6) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 119.9(6) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0(7) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 120.8(6) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C9 C16 H16A 109.5 . . ?
C9 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C9 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 Fe1 N2 91.68(15) . 3_565 ?
N2 Fe1 N2 91.68(15) . 2_665 ?
N2 Fe1 N2 91.68(15) 3_565 2_665 ?
N2 Fe1 N3 96.41(13) . 3_565 ?
N2 Fe1 N3 75.37(13) 3_565 3_565 ?
N2 Fe1 N3 164.87(12) 2_665 3_565 ?
N2 Fe1 N3 164.87(12) . 2_665 ?
N2 Fe1 N3 96.41(13) 3_565 2_665 ?
N2 Fe1 N3 75.37(13) 2_665 2_665 ?
N3 Fe1 N3 97.99(12) 3_565 2_665 ?
N2 Fe1 N3 75.37(13) . . ?
N2 Fe1 N3 164.87(12) 3_565 . ?
N2 Fe1 N3 96.41(13) 2_665 . ?
N3 Fe1 N3 97.99(12) 3_565 . ?
N3 Fe1 N3 97.99(12) 2_665 . ?
C1 N1 C3 106.5(4) . . ?
C1 N1 C4 128.9(4) . . ?
C3 N1 C4 124.4(4) . . ?
C1 N2 C2 105.6(4) . . ?
C1 N2 Fe1 113.7(3) . . ?
C2 N2 Fe1 140.5(3) . . ?
C8 N3 C9 119.2(4) . . ?
C8 N3 Fe1 113.6(3) . . ?
C9 N3 Fe1 127.2(3) . . ?
F3 B2 F4 114.7(4) . . ?
F3 B2 F4 114.7(4) . 2_655 ?
F4 B2 F4 103.7(5) . 2_655 ?
F3 B2 F4 114.7(4) . 3_665 ?
F4 B2 F4 103.7(5) . 3_665 ?
F4 B2 F4 103.7(5) 2_655 3_665 ?
F3' B2' F4' 109.1(8) . 3_665 ?
F3' B2' F4' 109.1(8) . 2_655 ?
F4' B2' F4' 109.8(8) 3_665 2_655 ?
F3' B2' F4' 109.1(8) . . ?
F4' B2' F4' 109.8(8) 3_665 . ?
F4' B2' F4' 109.8(8) 2_655 . ?
F1 B1 F1 110.8(6) 3_765 2_645 ?
F1 B1 F1 110.8(6) 3_765 . ?
F1 B1 F1 110.8(6) 2_645 . ?
F1 B1 F2 108.1(7) 3_765 . ?
F1 B1 F2 108.1(7) 2_645 . ?
F1 B1 F2 108.1(7) . . ?
F2' B1' F1' 110.2(8) . 3_765 ?
F2' B1' F1' 110.2(8) . 2_645 ?
F1' B1' F1' 108.7(8) 3_765 2_645 ?
F2' B1' F1' 110.2(8) . . ?
F1' B1' F1' 108.7(8) 3_765 . ?
F1' B1' F1' 108.7(8) 2_645 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.70
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.065
