# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2b
#=======================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
trans-Cl,P,N-[Fe(PNMe-Ph)₂Cl₂] (2b)
;
_chemical_name_common            'MW trans-FeCl2(PN-Ph)2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H34 Cl2 Fe N4 P2'
_chemical_formula_sum            'C36 H34 Cl2 Fe N4 P2'
_chemical_formula_weight         711.36

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.1491(3)
_cell_length_b                   12.8821(3)
_cell_length_c                   12.8714(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.291(1)
_cell_angle_gamma                90.00
_cell_volume                     1637.75(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9481
_cell_measurement_theta_min      4.494
_cell_measurement_theta_max      29.778

_exptl_crystal_description       plate
_exptl_crystal_colour            light-green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 Kappa APEX-II CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_reflns_number            33383
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         30.04
_reflns_number_total             4749
_reflns_number_gt                3686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_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)+(0.0339P)²+1.0060P] 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         4749
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 0.0000 0.0000 0.0000 0.01013(8) Uani 1 2 d S . .
Cl1 Cl 0.01750(4) -0.11400(3) 0.14643(3) 0.01748(10) Uani 1 1 d . . .
P1 P -0.05777(4) 0.16255(3) 0.10140(3) 0.01108(9) Uani 1 1 d . . .
N1 N 0.19788(13) 0.06432(11) 0.07796(11) 0.0127(3) Uani 1 1 d . . .
N2 N 0.10370(13) 0.21083(11) 0.14323(11) 0.0133(3) Uani 1 1 d . . .
C1 C 0.21686(16) 0.15433(13) 0.13220(12) 0.0114(3) Uani 1 1 d . . .
C2 C 0.34807(16) 0.19118(14) 0.17710(13) 0.0161(3) Uani 1 1 d . . .
H2 H 0.3605 0.2559 0.2134 0.019 Uiso 1 1 calc R . .
C3 C 0.45824(17) 0.13269(15) 0.16805(13) 0.0177(4) Uani 1 1 d . . .
H3 H 0.5473 0.1570 0.1980 0.021 Uiso 1 1 calc R . .
C4 C 0.43909(17) 0.03827(15) 0.11518(14) 0.0191(4) Uani 1 1 d . . .
H4 H 0.5137 -0.0040 0.1092 0.023 Uiso 1 1 calc R . .
C5 C 0.30793(16) 0.00806(14) 0.07167(14) 0.0175(4) Uani 1 1 d . . .
H5 H 0.2940 -0.0564 0.0349 0.021 Uiso 1 1 calc R . .
C6 C -0.13064(16) 0.16163(14) 0.21975(13) 0.0138(3) Uani 1 1 d . . .
C7 C -0.15802(16) 0.06509(14) 0.25917(13) 0.0165(3) Uani 1 1 d . . .
H7 H -0.1409 0.0035 0.2238 0.020 Uiso 1 1 calc R . .
C8 C -0.21033(17) 0.05825(16) 0.35019(14) 0.0210(4) Uani 1 1 d . . .
H8 H -0.2291 -0.0078 0.3762 0.025 Uiso 1 1 calc R . .
C9 C -0.23493(17) 0.14714(16) 0.40267(14) 0.0215(4) Uani 1 1 d . . .
H9 H -0.2671 0.1421 0.4662 0.026 Uiso 1 1 calc R . .
C10 C -0.21242(18) 0.24416(16) 0.36219(14) 0.0216(4) Uani 1 1 d . . .
H10 H -0.2313 0.3053 0.3974 0.026 Uiso 1 1 calc R . .
C11 C -0.16266(17) 0.25213(14) 0.27070(13) 0.0171(4) Uani 1 1 d . . .
H11 H -0.1501 0.3185 0.2423 0.021 Uiso 1 1 calc R . .
C12 C -0.14815(16) 0.27163(13) 0.02678(12) 0.0129(3) Uani 1 1 d . . .
C13 C -0.08316(18) 0.34101(14) -0.02713(14) 0.0175(4) Uani 1 1 d . . .
H13 H 0.0117 0.3352 -0.0206 0.021 Uiso 1 1 calc R . .
C14 C -0.15511(19) 0.41893(14) -0.09061(14) 0.0197(4) Uani 1 1 d . . .
H14 H -0.1089 0.4672 -0.1252 0.024 Uiso 1 1 calc R . .
C15 C -0.29409(19) 0.42623(14) -0.10344(14) 0.0198(4) Uani 1 1 d . . .
H15 H -0.3436 0.4784 -0.1481 0.024 Uiso 1 1 calc R . .
C16 C -0.36043(18) 0.35690(14) -0.05068(14) 0.0195(4) Uani 1 1 d . . .
H16 H -0.4557 0.3619 -0.0590 0.023 Uiso 1 1 calc R . .
C17 C -0.28882(16) 0.28051(13) 0.01389(13) 0.0143(3) Uani 1 1 d . . .
H17 H -0.3352 0.2336 0.0499 0.017 Uiso 1 1 calc R . .
C18 C 0.12899(17) 0.30780(14) 0.20461(14) 0.0180(4) Uani 1 1 d . . .
H18A H 0.1684 0.2918 0.2798 0.027 Uiso 1 1 calc R . .
H18B H 0.0435 0.3451 0.1987 0.027 Uiso 1 1 calc R . .
H18C H 0.1920 0.3512 0.1763 0.027 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
Fe1 N1 2.1910(13) 3 ?
Fe1 N1 2.1910(13) . ?
Fe1 Cl1 2.3637(4) 3 ?
Fe1 Cl1 2.3637(4) . ?
Fe1 P1 2.6046(4) . ?
Fe1 P1 2.6046(4) 3 ?
P1 N2 1.7195(14) . ?
P1 C12 1.8257(17) . ?
P1 C6 1.8400(17) . ?
N1 C1 1.344(2) . ?
N1 C5 1.349(2) . ?
N2 C1 1.394(2) . ?
N2 C18 1.469(2) . ?
C1 C2 1.407(2) . ?
C2 C3 1.375(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(2) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.395(2) . ?
C6 C11 1.412(2) . ?
C7 C8 1.396(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.388(2) . ?
C12 C17 1.404(2) . ?
C13 C14 1.391(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(2) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
N1 Fe1 N1 180.0 3 . ?
N1 Fe1 Cl1 88.67(4) 3 3 ?
N1 Fe1 Cl1 91.33(4) . 3 ?
N1 Fe1 Cl1 91.33(4) 3 . ?
N1 Fe1 Cl1 88.67(4) . . ?
Cl1 Fe1 Cl1 180.0 3 . ?
N1 Fe1 P1 104.20(4) 3 . ?
N1 Fe1 P1 75.80(4) . . ?
Cl1 Fe1 P1 85.167(14) 3 . ?
Cl1 Fe1 P1 94.832(14) . . ?
N1 Fe1 P1 75.80(4) 3 3 ?
N1 Fe1 P1 104.20(4) . 3 ?
Cl1 Fe1 P1 94.833(14) 3 3 ?
Cl1 Fe1 P1 85.168(14) . 3 ?
P1 Fe1 P1 180.0 . 3 ?
N2 P1 C12 102.34(7) . . ?
N2 P1 C6 106.18(7) . . ?
C12 P1 C6 101.04(8) . . ?
N2 P1 Fe1 98.02(5) . . ?
C12 P1 Fe1 119.93(5) . . ?
C6 P1 Fe1 126.11(6) . . ?
C1 N1 C5 118.22(14) . . ?
C1 N1 Fe1 124.81(11) . . ?
C5 N1 Fe1 116.97(11) . . ?
C1 N2 C18 116.91(13) . . ?
C1 N2 P1 121.83(11) . . ?
C18 N2 P1 120.81(11) . . ?
N1 C1 N2 118.69(14) . . ?
N1 C1 C2 120.89(15) . . ?
N2 C1 C2 120.41(15) . . ?
C3 C2 C1 119.45(16) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 119.84(15) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 117.48(16) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.3 . . ?
N1 C5 C4 124.06(17) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C7 C6 C11 118.74(15) . . ?
C7 C6 P1 117.28(13) . . ?
C11 C6 P1 123.96(13) . . ?
C6 C7 C8 120.50(17) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.31(18) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.83(17) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.45(17) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C6 120.04(17) . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
C13 C12 C17 118.42(15) . . ?
C13 C12 P1 121.31(13) . . ?
C17 C12 P1 119.95(13) . . ?
C12 C13 C14 120.86(16) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 120.12(17) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 119.59(16) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.39(16) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C12 120.61(16) . . ?
C16 C17 H17 119.7 . . ?
C12 C17 H17 119.7 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        30.04
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.074
_database_code_depnum_ccdc_archive 'CCDC 981196'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5b
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
cis-P,N-[Fe(PNH-Ph)₃]Br₂ (5b)
;
_chemical_name_common            ?
_chemical_formula_moiety         'C51 H45 Fe N6 P3, 2(Br)'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C51 H45 Br2 Fe1 N6 P3'
_chemical_formula_weight         1050.5
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_Int_Tables_number      43

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 x+1/4,-y+1/4,z+1/4
4 -x+1/4,y+1/4,z+1/4
5 x,y+1/2,z+1/2
6 -x,-y+1/2,z+1/2
7 x+1/4,-y+3/4,z+3/4
8 -x+1/4,y+3/4,z+3/4
9 x+1/2,y,z+1/2
10 -x+1/2,-y,z+1/2
11 x+3/4,-y+1/4,z+3/4
12 -x+3/4,y+1/4,z+3/4
13 x+1/2,y+1/2,z
14 -x+1/2,-y+1/2,z
15 x+3/4,-y+3/4,z+1/4
16 -x+3/4,y+3/4,z+1/4

_cell_length_a                   32.0762(14)
_cell_length_b                   35.738(2)
_cell_length_c                   19.252(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22070(3)

loop_
_jana_cell_twin_matrix_id
_jana_cell_twin_volume_fraction
_jana_cell_twin_matrix_1_1
_jana_cell_twin_matrix_1_2
_jana_cell_twin_matrix_1_3
_jana_cell_twin_matrix_2_1
_jana_cell_twin_matrix_2_2
_jana_cell_twin_matrix_2_3
_jana_cell_twin_matrix_3_1
_jana_cell_twin_matrix_3_2
_jana_cell_twin_matrix_3_3
1 1.008(4) 1 0 0 0 1 0 0 0 1
2 -0.008(4) -1 0 0 0 -1 0 0 0 -1

_cell_formula_units_Z            16
_cell_measurement_reflns_used    5222
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      28.3
_cell_measurement_temperature    100
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.2643
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             8544

_exptl_absorpt_coefficient_mu    1.845
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'clear yellow'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_T_max  0.93

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      100(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 Kappa APEX-II CCD'
_diffrn_measurement_method       'ω- and φ-scans'

_diffrn_reflns_number            43656
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_full        30
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_reduction_process ?


_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             15186
_reflns_number_gt                11710
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_gt          0.0780
_refine_ls_R_factor_all          0.0512
_refine_ls_wR_factor_ref         0.0819
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_goodness_of_fit_gt    1.15
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         15186
_refine_ls_number_parameters     581
_refine_ls_number_restraints     3
_refine_ls_number_constraints    169
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0159
_refine_ls_shift/su_mean         0.0007
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  6918 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Br -0.2901 2.4595 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_solution    'SUPERFLIP (Petricek, Dusek, Palatinus, 2006)'
_computing_structure_refinement  'JANA2006 (Petricek, Dusek, Palatinus, 2006)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_mutiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.565919(9) 0.074851(8) 0.109094(16) Uani 0.02750(9) 16 1 d . . .
Br2 Br 0.103553(14) 0.144522(13) 0.06352(2) Uani 0.06447(15) 16 1 d . . .
Fe1 Fe 0.536258(10) 0.247579(9) 0.188636(19) Uani 0.01217(9) 16 1 d . . .
P1 P 0.579126(19) 0.204570(17) 0.14329(4) Uani 0.01357(17) 16 1 d . . .
P2 P 0.500464(19) 0.267310(17) 0.09474(4) Uani 0.01441(18) 16 1 d . . .
P3 P 0.582193(19) 0.294344(17) 0.20067(4) Uani 0.01373(17) 16 1 d . . .
N1 N 0.49536(6) 0.20386(5) 0.19312(11) Uani 0.0150(6) 16 1 d . . .
N2 N 0.54912(7) 0.16591(6) 0.15409(12) Uani 0.0176(6) 16 1 d . . .
N3 N 0.49483(6) 0.28091(6) 0.24081(11) Uani 0.0140(6) 16 1 d . . .
N4 N 0.46842(7) 0.29839(6) 0.13315(12) Uani 0.0201(7) 16 1 d . . .
N5 N 0.56144(6) 0.23049(6) 0.28171(11) Uani 0.0146(6) 16 1 d . . .
N6 N 0.60989(6) 0.27842(6) 0.26848(12) Uani 0.0155(6) 16 1 d . . .
C1 C 0.50879(8) 0.16925(7) 0.17601(13) Uani 0.0157(7) 16 1 d . . .
C2 C 0.48357(8) 0.13730(7) 0.18133(15) Uani 0.0203(8) 16 1 d . . .
C3 C 0.44298(9) 0.14162(8) 0.20393(15) Uani 0.0233(8) 16 1 d . . .
C4 C 0.42829(8) 0.17702(8) 0.21995(15) Uani 0.0212(8) 16 1 d . . .
C5 C 0.45488(8) 0.20651(8) 0.21362(14) Uani 0.0184(8) 16 1 d . . .
C6 C 0.62686(8) 0.19286(7) 0.19129(14) Uani 0.0174(7) 16 1 d . . .
C7 C 0.62766(9) 0.16440(7) 0.24060(15) Uani 0.0200(8) 16 1 d . . .
C8 C 0.66402(9) 0.15757(8) 0.27899(16) Uani 0.0265(9) 16 1 d . . .
C9 C 0.69939(9) 0.17873(8) 0.26814(18) Uani 0.0301(9) 16 1 d . . .
C10 C 0.69910(9) 0.20699(8) 0.21803(17) Uani 0.0270(9) 16 1 d . . .
C11 C 0.66310(8) 0.21378(7) 0.18002(16) Uani 0.0216(8) 16 1 d . . .
C12 C 0.59829(7) 0.20093(7) 0.05431(14) Uani 0.0151(7) 16 1 d . . .
C13 C 0.59588(8) 0.16704(7) 0.01792(14) Uani 0.0167(7) 16 1 d . . .
C14 C 0.61368(8) 0.16432(8) -0.04796(14) Uani 0.0194(7) 16 1 d . . .
C15 C 0.63309(8) 0.19470(8) -0.07781(14) Uani 0.0236(8) 16 1 d . . .
C16 C 0.63589(9) 0.22836(8) -0.04214(16) Uani 0.0255(9) 16 1 d . . .
C17 C 0.61861(8) 0.23116(8) 0.02406(16) Uani 0.0236(8) 16 1 d . . .
C18 C 0.46815(8) 0.30189(7) 0.20382(14) Uani 0.0176(7) 16 1 d . . .
C19 C 0.44034(9) 0.32706(8) 0.23583(16) Uani 0.0265(9) 16 1 d . . .
C20 C 0.44036(10) 0.33011(8) 0.30610(17) Uani 0.0314(10) 16 1 d . . .
C21 C 0.46737(9) 0.30810(8) 0.34497(15) Uani 0.0246(8) 16 1 d . . .
C22 C 0.49381(8) 0.28428(7) 0.31081(14) Uani 0.0185(8) 16 1 d . . .
C23 C 0.46536(8) 0.23380(7) 0.05327(14) Uani 0.0172(7) 16 1 d . . .
C24 C 0.42228(9) 0.24041(8) 0.05053(16) Uani 0.0239(8) 16 1 d . . .
C25 C 0.39666(9) 0.21529(9) 0.01591(17) Uani 0.0310(10) 16 1 d . . .
C26 C 0.41302(10) 0.18432(8) -0.01631(17) Uani 0.0298(9) 16 1 d . . .
C27 C 0.45504(10) 0.17760(8) -0.01388(17) Uani 0.0291(9) 16 1 d . . .
C28 C 0.48140(9) 0.20178(7) 0.02142(15) Uani 0.0212(8) 16 1 d . . .
C29 C 0.51746(8) 0.29394(7) 0.01881(14) Uani 0.0170(7) 16 1 d . . .
C30 C 0.51009(8) 0.33247(7) 0.01298(15) Uani 0.0209(8) 16 1 d . . .
C31 C 0.52646(9) 0.35236(8) -0.04339(16) Uani 0.0261(9) 16 1 d . . .
C32 C 0.54932(9) 0.33436(9) -0.09382(16) Uani 0.0295(9) 16 1 d . . .
C33 C 0.55559(9) 0.29607(9) -0.08983(16) Uani 0.0271(9) 16 1 d . . .
C34 C 0.53943(8) 0.27578(8) -0.03403(14) Uani 0.0209(8) 16 1 d . . .
C35 C 0.59603(8) 0.24796(7) 0.30574(14) Uani 0.0153(7) 16 1 d . . .
C36 C 0.61701(8) 0.23653(7) 0.36529(14) Uani 0.0182(7) 16 1 d . . .
C37 C 0.60211(8) 0.20720(7) 0.40321(15) Uani 0.0213(8) 16 1 d . . .
C38 C 0.56534(8) 0.18958(8) 0.38081(15) Uani 0.0209(8) 16 1 d . . .
C39 C 0.54683(8) 0.20149(7) 0.32090(14) Uani 0.0176(7) 16 1 d . . .
C40 C 0.56307(8) 0.34012(7) 0.22990(14) Uani 0.0168(7) 16 1 d . . .
C41 C 0.56905(8) 0.35118(7) 0.29923(15) Uani 0.0192(8) 16 1 d . . .
C42 C 0.55662(8) 0.38704(7) 0.32004(16) Uani 0.0242(8) 16 1 d . . .
C43 C 0.53881(8) 0.41102(8) 0.27343(17) Uani 0.0251(9) 16 1 d . . .
C44 C 0.53192(8) 0.40015(7) 0.20490(17) Uani 0.0245(9) 16 1 d . . .
C45 C 0.54411(8) 0.36457(7) 0.18353(16) Uani 0.0203(8) 16 1 d . . .
C46 C 0.62302(7) 0.30909(7) 0.13981(14) Uani 0.0154(7) 16 1 d . . .
C47 C 0.66533(8) 0.30707(7) 0.15780(16) Uani 0.0223(8) 16 1 d . . .
C48 C 0.69520(9) 0.31649(8) 0.10900(18) Uani 0.0299(9) 16 1 d . . .
C49 C 0.68389(9) 0.32844(8) 0.04281(18) Uani 0.0297(9) 16 1 d . . .
C50 C 0.64236(8) 0.33192(7) 0.02586(16) Uani 0.0225(8) 16 1 d . . .
C51 C 0.61201(8) 0.32248(7) 0.07463(15) Uani 0.0183(7) 16 1 d . . .
H1c2 H 0.494261 0.113022 0.169557 Uiso 0.0244 16 1 d . . .
H1c3 H 0.425078 0.120234 0.208507 Uiso 0.028 16 1 d . . .
H1c4 H 0.400075 0.180664 0.235132 Uiso 0.0254 16 1 d . . .
H1c5 H 0.444295 0.230959 0.224394 Uiso 0.022 16 1 d . . .
H1c7 H 0.603267 0.149405 0.248347 Uiso 0.024 16 1 d . . .
H1c8 H 0.664303 0.13799 0.313121 Uiso 0.0319 16 1 d . . .
H1c9 H 0.724092 0.174059 0.29492 Uiso 0.0361 16 1 d . . .
H1c10 H 0.723696 0.221658 0.2099 Uiso 0.0324 16 1 d . . .
H1c11 H 0.663074 0.233147 0.145459 Uiso 0.0259 16 1 d . . .
H1c13 H 0.582085 0.145855 0.038196 Uiso 0.0201 16 1 d . . .
H1c14 H 0.612383 0.141049 -0.072756 Uiso 0.0233 16 1 d . . .
H1c15 H 0.644745 0.192576 -0.123565 Uiso 0.0284 16 1 d . . .
H1c16 H 0.649589 0.249482 -0.062857 Uiso 0.0306 16 1 d . . .
H1c17 H 0.620768 0.2543 0.04913 Uiso 0.0283 16 1 d . . .
H1c19 H 0.421617 0.341854 0.208293 Uiso 0.0318 16 1 d . . .
H1c20 H 0.421865 0.347344 0.32875 Uiso 0.0376 16 1 d . . .
H1c21 H 0.467509 0.309554 0.394759 Uiso 0.0295 16 1 d . . .
H1c22 H 0.512543 0.269227 0.337864 Uiso 0.0222 16 1 d . . .
H1c24 H 0.410618 0.26215 0.072439 Uiso 0.0287 16 1 d . . .
H1c25 H 0.36713 0.219609 0.014475 Uiso 0.0372 16 1 d . . .
H1c26 H 0.394982 0.167348 -0.040605 Uiso 0.0357 16 1 d . . .
H1c27 H 0.466317 0.155987 -0.036769 Uiso 0.0349 16 1 d . . .
H1c28 H 0.510706 0.196505 0.023951 Uiso 0.0254 16 1 d . . .
H1c30 H 0.493849 0.345187 0.047572 Uiso 0.0251 16 1 d . . .
H1c31 H 0.521691 0.378807 -0.046914 Uiso 0.0314 16 1 d . . .
H1c32 H 0.560916 0.348339 -0.13176 Uiso 0.0355 16 1 d . . .
H1c33 H 0.571085 0.283464 -0.125507 Uiso 0.0325 16 1 d . . .
H1c34 H 0.54344 0.249182 -0.031945 Uiso 0.0251 16 1 d . . .
H1c36 H 0.641914 0.249251 0.37966 Uiso 0.0219 16 1 d . . .
H1c37 H 0.61639 0.198818 0.444179 Uiso 0.0256 16 1 d . . .
H1c38 H 0.553408 0.169468 0.407233 Uiso 0.0251 16 1 d . . .
H1c39 H 0.522164 0.188753 0.305468 Uiso 0.0211 16 1 d . . .
H1c41 H 0.581537 0.334326 0.332008 Uiso 0.0231 16 1 d . . .
H1c42 H 0.560637 0.394805 0.367305 Uiso 0.029 16 1 d . . .
H1c43 H 0.530927 0.435699 0.28811 Uiso 0.0302 16 1 d . . .
H1c44 H 0.518903 0.417023 0.172723 Uiso 0.0294 16 1 d . . .
H1c45 H 0.539383 0.356878 0.136406 Uiso 0.0244 16 1 d . . .
H1c47 H 0.673479 0.29923 0.20352 Uiso 0.0268 16 1 d . . .
H1c48 H 0.724186 0.314753 0.12098 Uiso 0.0359 16 1 d . . .
H1c49 H 0.704973 0.334242 0.009089 Uiso 0.0356 16 1 d . . .
H1c50 H 0.634355 0.340793 -0.01928 Uiso 0.027 16 1 d . . .
H1c51 H 0.583076 0.325266 0.062981 Uiso 0.0219 16 1 d . . .
H1n2 H 0.5572(9) 0.1436(4) 0.1423(18) Uiso 0.030(9) 16 1 d . . .
H1n4 H 0.4517(7) 0.3118(6) 0.1079(12) Uiso 0.012(7) 16 1 d . . .
H1n6 H 0.6299(6) 0.2899(7) 0.2902(15) Uiso 0.025(8) 16 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 Br 0.02658(14) 0.02430(14) 0.03163(17) 0.00861(11) 0.00425(12) -0.00322(12)
Br2 Br 0.0724(3) 0.0794(3) 0.0416(2) 0.0571(2) 0.0265(2) 0.0211(2)
Fe1 Fe 0.01146(15) 0.01257(16) 0.01248(17) -0.00038(12) 0.00151(13)
-0.00146(14)
P1 P 0.0133(3) 0.0130(3) 0.0143(3) -0.0005(2) 0.0016(2) -0.0016(2)
P2 P 0.0142(3) 0.0155(3) 0.0136(3) 0.0007(2) -0.0004(2) -0.0020(2)
P3 P 0.0137(3) 0.0136(3) 0.0139(3) -0.0008(2) 0.0012(2) -0.0019(2)
N1 N 0.0157(10) 0.0167(10) 0.0125(11) -0.0012(8) -0.0012(8) 0.0003(9)
N2 N 0.0191(11) 0.0108(10) 0.0227(13) 0.0005(8) 0.0043(9) -0.0028(9)
N3 N 0.0134(10) 0.0134(10) 0.0153(11) -0.0019(8) 0.0026(8) -0.0022(8)
N4 N 0.0198(11) 0.0229(11) 0.0177(12) 0.0085(9) -0.0011(9) -0.0011(9)
N5 N 0.0157(10) 0.0156(10) 0.0124(11) 0.0002(8) 0.0012(8) -0.0032(8)
N6 N 0.0166(10) 0.0139(10) 0.0159(11) -0.0036(8) -0.0014(8) -0.0018(8)
C1 C 0.0168(12) 0.0180(12) 0.0123(13) -0.0033(9) 0.0009(9) -0.0021(9)
C2 C 0.0257(13) 0.0158(12) 0.0195(14) -0.0030(10) 0.0027(11) -0.0003(11)
C3 C 0.0253(14) 0.0271(14) 0.0176(15) -0.0118(11) 0.0043(11) -0.0023(11)
C4 C 0.0171(13) 0.0270(14) 0.0194(14) -0.0042(10) 0.0015(10) -0.0002(11)
C5 C 0.0196(13) 0.0199(13) 0.0156(14) -0.0019(10) -0.0006(10) 0.0016(10)
C6 C 0.0196(12) 0.0181(12) 0.0144(13) 0.0052(9) -0.0006(10) -0.0051(10)
C7 C 0.0245(14) 0.0161(12) 0.0195(14) 0.0039(10) 0.0005(11) -0.0036(10)
C8 C 0.0377(17) 0.0217(14) 0.0202(16) 0.0130(12) -0.0069(12) -0.0015(12)
C9 C 0.0266(15) 0.0278(15) 0.0359(19) 0.0108(12) -0.0133(13) -0.0143(13)
C10 C 0.0220(14) 0.0256(15) 0.0334(18) 0.0033(11) -0.0056(12) -0.0107(13)
C11 C 0.0224(13) 0.0176(13) 0.0247(16) 0.0010(10) 0.0010(11) -0.0063(11)
C12 C 0.0122(11) 0.0187(12) 0.0145(13) 0.0012(9) 0.0012(9) 0.0008(10)
C13 C 0.0167(12) 0.0198(12) 0.0136(13) 0.0034(10) -0.0043(10) 0.0004(10)
C14 C 0.0220(13) 0.0222(13) 0.0141(13) 0.0108(10) -0.0034(10) -0.0037(10)
C15 C 0.0222(14) 0.0360(16) 0.0127(14) 0.0098(12) 0.0027(10) -0.0006(11)
C16 C 0.0242(14) 0.0264(15) 0.0259(16) 0.0000(11) 0.0079(11) 0.0036(12)
C17 C 0.0264(14) 0.0225(14) 0.0218(15) -0.0005(11) 0.0014(11) -0.0006(12)
C18 C 0.0177(12) 0.0159(12) 0.0191(14) -0.0009(9) 0.0047(10) 0.0005(10)
C19 C 0.0288(15) 0.0261(15) 0.0247(16) 0.0130(12) 0.0078(12) 0.0061(12)
C20 C 0.0387(17) 0.0270(15) 0.0284(18) 0.0138(13) 0.0183(14) 0.0018(13)
C21 C 0.0323(15) 0.0232(14) 0.0182(15) 0.0044(11) 0.0075(12) -0.0007(11)
C22 C 0.0173(12) 0.0202(13) 0.0178(14) -0.0013(10) 0.0035(10) -0.0005(10)
C23 C 0.0189(12) 0.0184(12) 0.0143(13) -0.0043(10) -0.0043(10) 0.0022(10)
C24 C 0.0212(13) 0.0265(14) 0.0241(16) -0.0025(11) -0.0024(11) -0.0004(12)
C25 C 0.0236(15) 0.0373(17) 0.0321(18) -0.0087(12) -0.0080(13) 0.0176(14)
C26 C 0.0383(18) 0.0272(15) 0.0238(16) -0.0174(13) -0.0106(13) 0.0050(12)
C27 C 0.0405(18) 0.0227(15) 0.0240(16) -0.0097(13) -0.0017(13) -0.0057(12)
C28 C 0.0213(13) 0.0226(13) 0.0196(15) -0.0045(11) -0.0012(11) -0.0005(11)
C29 C 0.0151(12) 0.0181(12) 0.0177(14) -0.0031(9) -0.0059(10) 0.0034(10)
C30 C 0.0228(13) 0.0192(13) 0.0207(15) -0.0033(10) -0.0036(11) -0.0004(11)
C31 C 0.0299(15) 0.0189(13) 0.0296(17) -0.0047(11) -0.0111(12) 0.0069(12)
C32 C 0.0272(15) 0.0407(18) 0.0208(16) -0.0119(13) -0.0043(12) 0.0129(13)
C33 C 0.0224(14) 0.0371(17) 0.0218(16) -0.0054(12) 0.0018(11) 0.0013(13)
C34 C 0.0194(13) 0.0245(14) 0.0189(15) -0.0030(10) -0.0027(10) 0.0005(11)
C35 C 0.0156(12) 0.0153(12) 0.0150(13) -0.0004(9) 0.0040(9) -0.0035(10)
C36 C 0.0180(12) 0.0212(13) 0.0155(13) 0.0002(10) -0.0027(10) -0.0033(10)
C37 C 0.0233(14) 0.0238(14) 0.0168(15) 0.0025(11) -0.0027(11) -0.0015(11)
C38 C 0.0261(14) 0.0211(13) 0.0156(14) -0.0014(11) 0.0033(11) 0.0006(10)
C39 C 0.0179(12) 0.0175(12) 0.0173(14) -0.0006(9) 0.0012(10) -0.0006(10)
C40 C 0.0153(12) 0.0135(11) 0.0215(14) -0.0015(9) 0.0038(10) -0.0036(10)
C41 C 0.0184(13) 0.0201(13) 0.0191(14) -0.0017(10) 0.0028(10) -0.0050(11)
C42 C 0.0253(14) 0.0202(13) 0.0270(16) -0.0059(11) 0.0101(12) -0.0083(12)
C43 C 0.0189(13) 0.0174(13) 0.0392(18) -0.0009(10) 0.0135(12) -0.0073(12)
C44 C 0.0179(13) 0.0182(13) 0.0374(19) 0.0026(10) 0.0019(12) 0.0022(12)
C45 C 0.0168(12) 0.0213(13) 0.0228(15) -0.0011(10) 0.0033(11) -0.0026(11)
C46 C 0.0144(12) 0.0128(11) 0.0189(13) -0.0016(9) 0.0030(10) -0.0026(10)
C47 C 0.0213(14) 0.0227(14) 0.0231(15) -0.0002(11) -0.0011(11) 0.0025(11)
C48 C 0.0142(13) 0.0383(17) 0.0371(19) -0.0002(11) 0.0038(12) 0.0118(15)
C49 C 0.0212(14) 0.0307(16) 0.0372(19) 0.0001(12) 0.0098(12) 0.0090(13)
C50 C 0.0247(14) 0.0224(14) 0.0203(15) -0.0053(11) 0.0019(11) 0.0027(11)
C51 C 0.0169(12) 0.0160(12) 0.0220(15) -0.0033(10) 0.0023(10) -0.0017(10)

#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 P1 . . 2.2396(7) ?
Fe1 P2 . . 2.2546(8) ?
Fe1 P3 . . 2.2401(7) ?
Fe1 N1 . . 2.042(2) ?
Fe1 N3 . . 2.048(2) ?
Fe1 N5 . . 2.058(2) ?
P1 N2 . . 1.697(2) ?
P1 C6 . . 1.837(3) ?
P1 C12 . . 1.825(3) ?
P2 N4 . . 1.684(2) ?
P2 C23 . . 1.827(3) ?
P2 C29 . . 1.828(3) ?
P3 N6 . . 1.679(2) ?
P3 C40 . . 1.836(3) ?
P3 C46 . . 1.835(3) ?
N1 C1 . . 1.350(3) ?
N1 C5 . . 1.360(3) ?
N2 C1 . . 1.366(3) ?
N2 H1n2 . . 0.870(18) ?
N3 C18 . . 1.342(3) ?
N3 C22 . . 1.353(4) ?
N4 C18 . . 1.366(4) ?
N4 H1n4 . . 0.87(2) ?
N5 C35 . . 1.354(3) ?
N5 C39 . . 1.365(3) ?
N6 C35 . . 1.377(3) ?
N6 H1n6 . . 0.87(2) ?
C1 C2 . . 1.403(4) ?
C2 C3 . . 1.381(4) ?
C2 H1c2 . . 0.96 ?
C3 C4 . . 1.385(4) ?
C3 H1c3 . . 0.96 ?
C4 C5 . . 1.361(4) ?
C4 H1c4 . . 0.96 ?
C5 H1c5 . . 0.96 ?
C6 C7 . . 1.392(4) ?
C6 C11 . . 1.399(4) ?
C7 C8 . . 1.402(4) ?
C7 H1c7 . . 0.96 ?
C8 C9 . . 1.379(4) ?
C8 H1c8 . . 0.96 ?
C9 C10 . . 1.397(4) ?
C9 H1c9 . . 0.96 ?
C10 C11 . . 1.389(4) ?
C10 H1c10 . . 0.96 ?
C11 H1c11 . . 0.96 ?
C12 C13 . . 1.401(4) ?
C12 C17 . . 1.390(4) ?
C13 C14 . . 1.394(4) ?
C13 H1c13 . . 0.96 ?
C14 C15 . . 1.377(4) ?
C14 H1c14 . . 0.96 ?
C15 C16 . . 1.388(4) ?
C15 H1c15 . . 0.96 ?
C16 C17 . . 1.394(4) ?
C16 H1c16 . . 0.96 ?
C17 H1c17 . . 0.96 ?
C18 C19 . . 1.409(4) ?
C19 C20 . . 1.357(5) ?
C19 H1c19 . . 0.96 ?
C20 C21 . . 1.389(4) ?
C20 H1c20 . . 0.96 ?
C21 C22 . . 1.370(4) ?
C21 H1c21 . . 0.96 ?
C22 H1c22 . . 0.96 ?
C23 C24 . . 1.403(4) ?
C23 C28 . . 1.396(4) ?
C24 C25 . . 1.388(4) ?
C24 H1c24 . . 0.96 ?
C25 C26 . . 1.373(4) ?
C25 H1c25 . . 0.96 ?
C26 C27 . . 1.370(5) ?
C26 H1c26 . . 0.96 ?
C27 C28 . . 1.387(4) ?
C27 H1c27 . . 0.96 ?
C28 H1c28 . . 0.96 ?
C29 C30 . . 1.402(4) ?
C29 C34 . . 1.398(4) ?
C30 C31 . . 1.399(4) ?
C30 H1c30 . . 0.96 ?
C31 C32 . . 1.376(4) ?
C31 H1c31 . . 0.96 ?
C32 C33 . . 1.385(4) ?
C32 H1c32 . . 0.96 ?
C33 C34 . . 1.396(4) ?
C33 H1c33 . . 0.96 ?
C34 H1c34 . . 0.96 ?
C35 C36 . . 1.391(4) ?
C36 C37 . . 1.364(4) ?
C36 H1c36 . . 0.96 ?
C37 C38 . . 1.405(4) ?
C37 H1c37 . . 0.96 ?
C38 C39 . . 1.365(4) ?
C38 H1c38 . . 0.96 ?
C39 H1c39 . . 0.96 ?
C40 C41 . . 1.405(4) ?
C40 C45 . . 1.390(4) ?
C41 C42 . . 1.401(4) ?
C41 H1c41 . . 0.96 ?
C42 C43 . . 1.366(4) ?
C42 H1c42 . . 0.96 ?
C43 C44 . . 1.393(5) ?
C43 H1c43 . . 0.96 ?
C44 C45 . . 1.393(4) ?
C44 H1c44 . . 0.96 ?
C45 H1c45 . . 0.96 ?
C46 C47 . . 1.402(4) ?
C46 C51 . . 1.389(4) ?
C47 C48 . . 1.383(4) ?
C47 H1c47 . . 0.96 ?
C48 C49 . . 1.392(5) ?
C48 H1c48 . . 0.96 ?
C49 C50 . . 1.377(4) ?
C49 H1c49 . . 0.96 ?
C50 C51 . . 1.394(4) ?
C50 H1c50 . . 0.96 ?
C51 H1c51 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Br1 N6 . . 8_644 135.21(5) ?
P1 Fe1 P2 . . . 102.40(3) ?
P1 Fe1 P3 . . . 98.54(3) ?
P1 Fe1 N1 . . . 83.44(6) ?
P1 Fe1 N3 . . . 171.43(6) ?
P1 Fe1 N5 . . . 83.96(6) ?
P2 Fe1 P3 . . . 100.63(3) ?
P2 Fe1 N1 . . . 86.91(6) ?
P2 Fe1 N3 . . . 83.16(6) ?
P2 Fe1 N5 . . . 172.18(6) ?
P3 Fe1 N1 . . . 171.53(7) ?
P3 Fe1 N3 . . . 86.68(6) ?
P3 Fe1 N5 . . . 82.72(6) ?
N1 Fe1 N3 . . . 90.43(8) ?
N1 Fe1 N5 . . . 89.33(8) ?
N3 Fe1 N5 . . . 90.01(8) ?
Fe1 P1 N2 . . . 99.36(8) ?
Fe1 P1 C6 . . . 118.17(9) ?
Fe1 P1 C12 . . . 128.45(8) ?
N2 P1 C6 . . . 103.05(11) ?
N2 P1 C12 . . . 104.37(11) ?
C6 P1 C12 . . . 100.09(12) ?
Fe1 P2 N4 . . . 99.50(9) ?
Fe1 P2 C23 . . . 117.33(9) ?
Fe1 P2 C29 . . . 130.72(8) ?
N4 P2 C23 . . . 104.36(11) ?
N4 P2 C29 . . . 100.94(11) ?
C23 P2 C29 . . . 100.11(12) ?
Fe1 P3 N6 . . . 100.11(8) ?
Fe1 P3 C40 . . . 118.48(8) ?
Fe1 P3 C46 . . . 128.16(9) ?
N6 P3 C40 . . . 103.92(11) ?
N6 P3 C46 . . . 102.49(11) ?
C40 P3 C46 . . . 100.27(11) ?
Fe1 N1 C1 . . . 119.06(16) ?
Fe1 N1 C5 . . . 124.90(17) ?
C1 N1 C5 . . . 116.0(2) ?
Br1 N2 P1 . . . 131.01(10) ?
Br1 N2 C1 . . . 108.15(14) ?
P1 N2 C1 . . . 120.27(17) ?
P1 N2 H1n2 . . . 123.1(19) ?
C1 N2 H1n2 . . . 116.3(19) ?
Fe1 N3 C18 . . . 118.58(17) ?
Fe1 N3 C22 . . . 123.77(16) ?
C18 N3 C22 . . . 117.6(2) ?
Br2 N4 P2 14_555 . . 130.13(11) ?
Br2 N4 C18 14_555 . . 109.73(15) ?
P2 N4 C18 . . . 120.08(18) ?
P2 N4 H1n4 . . . 119.7(15) ?
C18 N4 H1n4 . . . 120.2(15) ?
Fe1 N5 C35 . . . 118.81(16) ?
Fe1 N5 C39 . . . 124.87(17) ?
C35 N5 C39 . . . 116.3(2) ?
Br1 N6 P3 4_655 . . 127.34(10) ?
Br1 N6 C35 4_655 . . 110.24(15) ?
P3 N6 C35 . . . 120.15(17) ?
P3 N6 H1n6 . . . 127.1(18) ?
C35 N6 H1n6 . . . 111.3(18) ?
N1 C1 N2 . . . 117.2(2) ?
N1 C1 C2 . . . 122.9(2) ?
N2 C1 C2 . . . 119.8(2) ?
C1 C2 C3 . . . 118.4(2) ?
C1 C2 H1c2 . . . 120.81 ?
C3 C2 H1c2 . . . 120.81 ?
C2 C3 C4 . . . 119.5(2) ?
C2 C3 H1c3 . . . 120.23 ?
C4 C3 H1c3 . . . 120.23 ?
C3 C4 C5 . . . 118.3(2) ?
C3 C4 H1c4 . . . 120.84 ?
C5 C4 H1c4 . . . 120.84 ?
N1 C5 C4 . . . 124.7(2) ?
N1 C5 H1c5 . . . 117.62 ?
C4 C5 H1c5 . . . 117.63 ?
P1 C6 C7 . . . 121.68(19) ?
P1 C6 C11 . . . 119.5(2) ?
C7 C6 C11 . . . 118.8(2) ?
C6 C7 C8 . . . 120.1(2) ?
C6 C7 H1c7 . . . 119.93 ?
C8 C7 H1c7 . . . 119.93 ?
C7 C8 C9 . . . 120.6(3) ?
C7 C8 H1c8 . . . 119.71 ?
C9 C8 H1c8 . . . 119.7 ?
C8 C9 C10 . . . 119.7(3) ?
C8 C9 H1c9 . . . 120.14 ?
C10 C9 H1c9 . . . 120.15 ?
C9 C10 C11 . . . 119.7(3) ?
C9 C10 H1c10 . . . 120.13 ?
C11 C10 H1c10 . . . 120.13 ?
C6 C11 C10 . . . 121.0(3) ?
C6 C11 H1c11 . . . 119.47 ?
C10 C11 H1c11 . . . 119.48 ?
P1 C12 C13 . . . 120.83(19) ?
P1 C12 C17 . . . 119.7(2) ?
C13 C12 C17 . . . 119.2(2) ?
C12 C13 C14 . . . 119.5(2) ?
C12 C13 H1c13 . . . 120.25 ?
C14 C13 H1c13 . . . 120.25 ?
C13 C14 C15 . . . 120.7(2) ?
C13 C14 H1c14 . . . 119.67 ?
C15 C14 H1c14 . . . 119.67 ?
C14 C15 C16 . . . 120.4(3) ?
C14 C15 H1c15 . . . 119.8 ?
C16 C15 H1c15 . . . 119.8 ?
C15 C16 C17 . . . 119.3(3) ?
C15 C16 H1c16 . . . 120.37 ?
C17 C16 H1c16 . . . 120.37 ?
C12 C17 C16 . . . 120.9(3) ?
C12 C17 H1c17 . . . 119.53 ?
C16 C17 H1c17 . . . 119.53 ?
N3 C18 N4 . . . 118.2(2) ?
N3 C18 C19 . . . 121.9(3) ?
N4 C18 C19 . . . 119.9(2) ?
C18 C19 C20 . . . 119.2(3) ?
C18 C19 H1c19 . . . 120.42 ?
C20 C19 H1c19 . . . 120.42 ?
C19 C20 C21 . . . 119.5(3) ?
C19 C20 H1c20 . . . 120.27 ?
C21 C20 H1c20 . . . 120.27 ?
C20 C21 C22 . . . 118.7(3) ?
C20 C21 H1c21 . . . 120.68 ?
C22 C21 H1c21 . . . 120.67 ?
N3 C22 C21 . . . 123.3(2) ?
N3 C22 H1c22 . . . 118.37 ?
C21 C22 H1c22 . . . 118.37 ?
P2 C23 C24 . . . 120.9(2) ?
P2 C23 C28 . . . 120.12(19) ?
C24 C23 C28 . . . 119.0(2) ?
C23 C24 C25 . . . 119.5(3) ?
C23 C24 H1c24 . . . 120.24 ?
C25 C24 H1c24 . . . 120.25 ?
C24 C25 C26 . . . 120.8(3) ?
C24 C25 H1c25 . . . 119.6 ?
C26 C25 H1c25 . . . 119.6 ?
C25 C26 C27 . . . 120.1(3) ?
C25 C26 H1c26 . . . 119.93 ?
C27 C26 H1c26 . . . 119.93 ?
C26 C27 C28 . . . 120.5(3) ?
C26 C27 H1c27 . . . 119.76 ?
C28 C27 H1c27 . . . 119.76 ?
C23 C28 C27 . . . 120.1(3) ?
C23 C28 H1c28 . . . 119.96 ?
C27 C28 H1c28 . . . 119.96 ?
P2 C29 C30 . . . 121.7(2) ?
P2 C29 C34 . . . 119.40(19) ?
C30 C29 C34 . . . 118.9(2) ?
C29 C30 C31 . . . 119.9(3) ?
C29 C30 H1c30 . . . 120.07 ?
C31 C30 H1c30 . . . 120.07 ?
C30 C31 C32 . . . 120.6(3) ?
C30 C31 H1c31 . . . 119.68 ?
C32 C31 H1c31 . . . 119.68 ?
C31 C32 C33 . . . 120.0(3) ?
C31 C32 H1c32 . . . 120 ?
C33 C32 H1c32 . . . 120 ?
C32 C33 C34 . . . 120.1(3) ?
C32 C33 H1c33 . . . 119.94 ?
C34 C33 H1c33 . . . 119.94 ?
C29 C34 C33 . . . 120.4(3) ?
C29 C34 H1c34 . . . 119.79 ?
C33 C34 H1c34 . . . 119.79 ?
N5 C35 N6 . . . 116.8(2) ?
N5 C35 C36 . . . 122.8(2) ?
N6 C35 C36 . . . 120.4(2) ?
C35 C36 C37 . . . 119.8(2) ?
C35 C36 H1c36 . . . 120.08 ?
C37 C36 H1c36 . . . 120.08 ?
C36 C37 C38 . . . 118.3(3) ?
C36 C37 H1c37 . . . 120.84 ?
C38 C37 H1c37 . . . 120.84 ?
C37 C38 C39 . . . 119.0(2) ?
C37 C38 H1c38 . . . 120.51 ?
C39 C38 H1c38 . . . 120.51 ?
N5 C39 C38 . . . 123.7(2) ?
N5 C39 H1c39 . . . 118.16 ?
C38 C39 H1c39 . . . 118.16 ?
P3 C40 C41 . . . 119.77(19) ?
P3 C40 C45 . . . 120.6(2) ?
C41 C40 C45 . . . 119.5(2) ?
C40 C41 C42 . . . 119.4(2) ?
C40 C41 H1c41 . . . 120.32 ?
C42 C41 H1c41 . . . 120.32 ?
C41 C42 C43 . . . 120.3(3) ?
C41 C42 H1c42 . . . 119.83 ?
C43 C42 H1c42 . . . 119.83 ?
C42 C43 C44 . . . 120.9(3) ?
C42 C43 H1c43 . . . 119.55 ?
C44 C43 H1c43 . . . 119.55 ?
C43 C44 C45 . . . 119.3(3) ?
C43 C44 H1c44 . . . 120.33 ?
C45 C44 H1c44 . . . 120.33 ?
C40 C45 C44 . . . 120.5(3) ?
C40 C45 H1c45 . . . 119.76 ?
C44 C45 H1c45 . . . 119.76 ?
P3 C46 C47 . . . 121.2(2) ?
P3 C46 C51 . . . 119.64(19) ?
C47 C46 C51 . . . 119.1(2) ?
C46 C47 C48 . . . 119.3(3) ?
C46 C47 H1c47 . . . 120.33 ?
C48 C47 H1c47 . . . 120.33 ?
C47 C48 C49 . . . 121.1(3) ?
C47 C48 H1c48 . . . 119.47 ?
C49 C48 H1c48 . . . 119.47 ?
C48 C49 C50 . . . 119.8(3) ?
C48 C49 H1c49 . . . 120.11 ?
C50 C49 H1c49 . . . 120.11 ?
C49 C50 C51 . . . 119.6(3) ?
C49 C50 H1c50 . . . 120.2 ?
C51 C50 H1c50 . . . 120.19 ?
C46 C51 C50 . . . 121.0(2) ?
C46 C51 H1c51 . . . 119.52 ?
C50 C51 H1c51 . . . 119.52 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.000 -0.000 -0.072 684 88 ' '
2 -0.000 0.500 0.428 684 88 ' '
3 0.250 0.250 0.178 684 88 ' '
4 0.250 0.750 0.678 684 88 ' '
5 0.500 -0.000 0.428 684 88 ' '
6 0.500 0.500 -0.072 684 88 ' '
7 0.750 0.250 0.678 684 88 ' '
8 0.750 0.750 0.178 684 88 ' '
_platon_squeeze_details          
;
Due to disorder, the solvent molecules in 5b could not be 
resolved and the electron density in the solvent voids 
corresponding to approximately 2.5 MeOH molecules per 
asymmetric unit was removed with procedure SQUEEZE 
of program PLATON.
;


# start Validation Reply Form

_vrf_PLAT605_5b                  
;
PROBLEM: 
PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of .        656 A**3  
RESPONSE: 
Crystals from methanol / diethyl ether by vapour diffusion.
Due to disorder, the solvent molecules in 5b could not be 
resolved and the electron density in the solvent voids 
corresponding to approximately 2.5 MeOH molecules per 
asymmetric unit was removed with procedure SQUEEZE 
of program PLATON.
;
_database_code_depnum_ccdc_archive 'CCDC 981197'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6
#=======================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
[Fe(PN-Ph)2(CH3CN)2](BF4)2.solv
;
_chemical_name_common            '1466 xx4 [Fe(PN-Ph)2(AN)2](BF4)2.solv'
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Fe N6 P2, 2(B F4)'
_chemical_formula_sum            'C38 H36 B2 F8 Fe N6 P2'
_chemical_formula_weight         868.14

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'
P P 0.1023 0.0942 '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  '
_symmetry_space_group_name_Hall  '-P 1  '

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

_cell_length_a                   10.7266(13)
_cell_length_b                   20.317(3)
_cell_length_c                   21.130(3)
_cell_angle_alpha                64.129(2)
_cell_angle_beta                 83.943(2)
_cell_angle_gamma                89.942(2)
_cell_volume                     4115.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7606
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      30.08

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
Platy red crystals from acetonitrile / diethyl ether.
The compound is a disordered solvate with 
an estimated solvent content of about 1/2 acetontrile
molecule per complex. 
Prior to final refinement the disordered solvent 
was removed from the data with procedure SQUEEZE of
program PLATON. The 3 most significant solvent peaks were
C1S     0.2064    0.7788    0.4238
C2S     0.0906    0.7714    0.4698
C3S    -0.0309    0.7624    0.5103
and were thought to represent essentially acetonitrile (one
molecule per two Fe-complexes !!). According to program
PLATON the solvent cavities (2 symmetry equivalent per unit cell)
are located at x,y,z = 0.062, 0.736, 0.486 and -x,-y,-z.
The solvent accessible volume per cavity is 166 A^3 and 332 A^3 
per unit cell.
In the final refinement soft SADI 0.005 restraints were used for
the B-F and the F-F distances of the BF4 groups and a 
DELU 0.002 0.002 restraint was used for their Uij.
;

_diffrn_ambient_temperature      100(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 Kappa APEX-II CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_reflns_number            67127
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         30.00
_reflns_number_total             23584
_reflns_number_gt                18402
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0931P)²+4.9505P] 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         23584
_refine_ls_number_parameters     1031
_refine_ls_number_restraints     436
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1649
_refine_ls_wR_factor_gt          0.1574
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.004
_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 0.72203(4) 0.61014(2) 0.25946(2) 0.01355(9) Uani 1 1 d . . .
P1 P 0.65185(7) 0.70216(4) 0.16804(4) 0.01456(14) Uani 1 1 d . . .
P2 P 0.65078(7) 0.52099(4) 0.23798(4) 0.01431(14) Uani 1 1 d . . .
N1 N 0.8036(2) 0.69535(14) 0.26878(13) 0.0159(4) Uani 1 1 d . . .
N2 N 0.7643(2) 0.76722(14) 0.15361(14) 0.0171(4) Uani 1 1 d . . .
H2N H 0.7855 0.8032 0.1112 0.021 Uiso 1 1 calc R . .
N3 N 0.8695(2) 0.60904(13) 0.19316(13) 0.0148(3) Uani 1 1 d . . .
N4 N 0.7434(2) 0.53663(14) 0.16308(13) 0.0170(4) Uani 1 1 d . . .
H4N H 0.7204 0.5221 0.1322 0.020 Uiso 1 1 calc R . .
N5 N 0.8060(3) 0.53899(15) 0.33782(14) 0.0194(4) Uani 1 1 d . . .
N6 N 0.5873(3) 0.60664(14) 0.32836(14) 0.0184(4) Uani 1 1 d . . .
C1 C 0.8209(3) 0.76106(16) 0.21144(16) 0.0153(4) Uani 1 1 d . . .
C2 C 0.8929(3) 0.81904(17) 0.21068(18) 0.0195(5) Uani 1 1 d . . .
H2 H 0.9065 0.8642 0.1693 0.023 Uiso 1 1 calc R . .
C3 C 0.9437(3) 0.80884(18) 0.27169(19) 0.0235(6) Uani 1 1 d . . .
H3 H 0.9936 0.8470 0.2725 0.028 Uiso 1 1 calc R . .
C4 C 0.9214(3) 0.74241(19) 0.33183(18) 0.0241(6) Uani 1 1 d . . .
H4 H 0.9542 0.7349 0.3744 0.029 Uiso 1 1 calc R . .
C5 C 0.8506(3) 0.68756(18) 0.32855(17) 0.0216(5) Uani 1 1 d . . .
H5 H 0.8342 0.6425 0.3699 0.026 Uiso 1 1 calc R . .
C6 C 0.6552(3) 0.70212(16) 0.08235(15) 0.0151(4) Uani 1 1 d . . .
C7 C 0.5462(3) 0.67914(16) 0.06426(16) 0.0174(5) Uani 1 1 d . . .
H7 H 0.4687 0.6715 0.0933 0.021 Uiso 1 1 calc R . .
C8 C 0.5518(3) 0.66758(17) 0.00401(17) 0.0205(5) Uani 1 1 d . . .
H8 H 0.4783 0.6519 -0.0081 0.025 Uiso 1 1 calc R . .
C9 C 0.6655(3) 0.67903(18) -0.03870(17) 0.0229(6) Uani 1 1 d . . .
H9 H 0.6697 0.6698 -0.0792 0.027 Uiso 1 1 calc R . .
C10 C 0.7723(3) 0.70376(18) -0.02267(17) 0.0215(5) Uani 1 1 d . . .
H10 H 0.8486 0.7130 -0.0531 0.026 Uiso 1 1 calc R . .
C11 C 0.7684(3) 0.71523(17) 0.03811(16) 0.0181(5) Uani 1 1 d . . .
H11 H 0.8420 0.7318 0.0493 0.022 Uiso 1 1 calc R . .
C12 C 0.5034(3) 0.74269(18) 0.17835(17) 0.0192(5) Uani 1 1 d . . .
C13 C 0.4948(3) 0.81844(19) 0.1453(2) 0.0256(6) Uani 1 1 d . . .
H13 H 0.5658 0.8487 0.1167 0.031 Uiso 1 1 calc R . .
C14 C 0.3834(4) 0.8501(2) 0.1537(2) 0.0330(7) Uani 1 1 d . . .
H14 H 0.3785 0.9018 0.1306 0.040 Uiso 1 1 calc R . .
C15 C 0.2796(4) 0.8068(2) 0.1954(2) 0.0330(7) Uani 1 1 d . . .
H15 H 0.2042 0.8287 0.2021 0.040 Uiso 1 1 calc R . .
C16 C 0.2861(3) 0.7306(2) 0.2278(2) 0.0319(7) Uani 1 1 d . . .
H16 H 0.2146 0.7005 0.2559 0.038 Uiso 1 1 calc R . .
C17 C 0.3976(3) 0.6989(2) 0.2189(2) 0.0261(6) Uani 1 1 d . . .
H17 H 0.4017 0.6471 0.2405 0.031 Uiso 1 1 calc R . .
C18 C 0.8578(3) 0.57350(15) 0.15246(15) 0.0147(4) Uani 1 1 d . . .
C19 C 0.9551(3) 0.57381(18) 0.10220(17) 0.0204(5) Uani 1 1 d . . .
H19 H 0.9433 0.5496 0.0735 0.024 Uiso 1 1 calc R . .
C20 C 1.0677(3) 0.60981(18) 0.09551(18) 0.0234(6) Uani 1 1 d . . .
H20 H 1.1342 0.6119 0.0611 0.028 Uiso 1 1 calc R . .
C21 C 1.0837(3) 0.64336(18) 0.13967(19) 0.0228(6) Uani 1 1 d . . .
H21 H 1.1620 0.6668 0.1371 0.027 Uiso 1 1 calc R . .
C22 C 0.9839(3) 0.64180(17) 0.18686(17) 0.0185(5) Uani 1 1 d . . .
H22 H 0.9953 0.6648 0.2167 0.022 Uiso 1 1 calc R . .
C23 C 0.4933(3) 0.51015(16) 0.21905(16) 0.0160(4) Uani 1 1 d . . .
C24 C 0.3934(3) 0.50177(18) 0.27035(18) 0.0204(5) Uani 1 1 d . . .
H24 H 0.4087 0.5061 0.3119 0.024 Uiso 1 1 calc R . .
C25 C 0.2716(3) 0.48722(19) 0.2613(2) 0.0246(6) Uani 1 1 d . . .
H25 H 0.2040 0.4822 0.2963 0.030 Uiso 1 1 calc R . .
C26 C 0.2491(3) 0.47998(19) 0.2011(2) 0.0267(6) Uani 1 1 d . . .
H26 H 0.1662 0.4690 0.1953 0.032 Uiso 1 1 calc R . .
C27 C 0.3476(3) 0.48875(18) 0.14911(18) 0.0247(6) Uani 1 1 d . . .
H27 H 0.3317 0.4840 0.1079 0.030 Uiso 1 1 calc R . .
C28 C 0.4693(3) 0.50449(16) 0.15759(16) 0.0195(5) Uani 1 1 d . . .
H28 H 0.5362 0.5114 0.1217 0.023 Uiso 1 1 calc R . .
C29 C 0.6792(3) 0.42643(16) 0.29934(16) 0.0174(4) Uani 1 1 d . . .
C30 C 0.7647(4) 0.38562(19) 0.27945(19) 0.0255(6) Uani 1 1 d . . .
H30 H 0.8116 0.4070 0.2339 0.031 Uiso 1 1 calc R . .
C31 C 0.7817(4) 0.3131(2) 0.3265(2) 0.0331(7) Uani 1 1 d . . .
H31 H 0.8387 0.2849 0.3123 0.040 Uiso 1 1 calc R . .
C32 C 0.7159(5) 0.2822(2) 0.3934(2) 0.0361(8) Uani 1 1 d . . .
H32 H 0.7287 0.2331 0.4256 0.043 Uiso 1 1 calc R . .
C33 C 0.6308(4) 0.3232(2) 0.4136(2) 0.0322(7) Uani 1 1 d . . .
H33 H 0.5851 0.3019 0.4595 0.039 Uiso 1 1 calc R . .
C34 C 0.6124(4) 0.39499(18) 0.36683(18) 0.0259(6) Uani 1 1 d . . .
H34 H 0.5541 0.4228 0.3808 0.031 Uiso 1 1 calc R . .
C35 C 0.8477(3) 0.4958(2) 0.38378(19) 0.0278(7) Uani 1 1 d . . .
C36 C 0.8984(5) 0.4393(3) 0.4451(3) 0.0558(15) Uani 1 1 d . . .
H36A H 0.8757 0.4483 0.4867 0.084 Uiso 1 1 calc R . .
H36B H 0.9900 0.4407 0.4355 0.084 Uiso 1 1 calc R . .
H36C H 0.8633 0.3911 0.4541 0.084 Uiso 1 1 calc R . .
C37 C 0.5137(3) 0.6066(2) 0.3717(2) 0.0290(8) Uani 1 1 d . . .
C38 C 0.4184(5) 0.6077(3) 0.4259(3) 0.0565(16) Uani 1 1 d . . .
H38A H 0.3838 0.6563 0.4091 0.085 Uiso 1 1 calc R . .
H38B H 0.4564 0.5966 0.4694 0.085 Uiso 1 1 calc R . .
H38C H 0.3510 0.5709 0.4356 0.085 Uiso 1 1 calc R . .
Fe2 Fe 0.66302(4) 0.10276(2) 0.26829(2) 0.01253(9) Uani 1 1 d . . .
P3 P 0.77922(7) 0.19172(4) 0.17692(4) 0.01413(14) Uani 1 1 d . . .
P4 P 0.74695(7) 0.01073(4) 0.25287(4) 0.01394(14) Uani 1 1 d . . .
N7 N 0.5770(2) 0.19039(13) 0.27239(14) 0.0147(4) Uani 1 1 d . . .
N8 N 0.6789(2) 0.25970(14) 0.15992(14) 0.0170(4) Uani 1 1 d . . .
H8N H 0.6799 0.2958 0.1172 0.020 Uiso 1 1 calc R . .
N9 N 0.5520(2) 0.09932(13) 0.19930(13) 0.0145(3) Uani 1 1 d . . .
N10 N 0.6983(3) 0.02713(15) 0.17415(14) 0.0175(4) Uani 1 1 d . . .
H10N H 0.7407 0.0138 0.1440 0.021 Uiso 1 1 calc R . .
N11 N 0.5434(2) 0.03336(14) 0.34629(13) 0.0164(4) Uani 1 1 d . . .
N12 N 0.7669(2) 0.10405(14) 0.33658(14) 0.0167(4) Uani 1 1 d . . .
C39 C 0.5952(3) 0.25670(16) 0.21527(16) 0.0150(4) Uani 1 1 d . . .
C40 C 0.5328(3) 0.31886(17) 0.21208(18) 0.0194(5) Uani 1 1 d . . .
H40 H 0.5453 0.3642 0.1707 0.023 Uiso 1 1 calc R . .
C41 C 0.4530(3) 0.31246(18) 0.27034(19) 0.0221(5) Uani 1 1 d . . .
H41 H 0.4093 0.3534 0.2696 0.027 Uiso 1 1 calc R . .
C42 C 0.4371(3) 0.24525(18) 0.33035(19) 0.0227(6) Uani 1 1 d . . .
H42 H 0.3844 0.2403 0.3714 0.027 Uiso 1 1 calc R . .
C43 C 0.4993(3) 0.18579(17) 0.32941(17) 0.0191(5) Uani 1 1 d . . .
H43 H 0.4870 0.1400 0.3703 0.023 Uiso 1 1 calc R . .
C44 C 0.9261(3) 0.22772(17) 0.18880(16) 0.0172(4) Uani 1 1 d . . .
C45 C 1.0122(3) 0.1816(2) 0.22995(19) 0.0237(6) Uani 1 1 d . . .
H45 H 0.9966 0.1300 0.2509 0.028 Uiso 1 1 calc R . .
C46 C 1.1216(3) 0.2112(2) 0.2405(2) 0.0298(6) Uani 1 1 d . . .
H46 H 1.1791 0.1796 0.2694 0.036 Uiso 1 1 calc R . .
C47 C 1.1465(3) 0.2865(2) 0.2092(2) 0.0308(7) Uani 1 1 d . . .
H47 H 1.2203 0.3063 0.2169 0.037 Uiso 1 1 calc R . .
C48 C 1.0628(3) 0.3328(2) 0.1663(2) 0.0296(6) Uani 1 1 d . . .
H48 H 1.0807 0.3843 0.1437 0.035 Uiso 1 1 calc R . .
C49 C 0.9529(3) 0.30367(18) 0.15660(19) 0.0234(6) Uani 1 1 d . . .
H49 H 0.8955 0.3356 0.1279 0.028 Uiso 1 1 calc R . .
C50 C 0.8111(3) 0.19219(16) 0.09070(16) 0.0158(4) Uani 1 1 d . . .
C51 C 0.7160(3) 0.20644(17) 0.04660(17) 0.0185(5) Uani 1 1 d . . .
H51 H 0.6383 0.2232 0.0584 0.022 Uiso 1 1 calc R . .
C52 C 0.7354(3) 0.19598(18) -0.01460(17) 0.0226(5) Uani 1 1 d . . .
H52 H 0.6710 0.2059 -0.0447 0.027 Uiso 1 1 calc R . .
C53 C 0.8497(3) 0.17085(18) -0.03162(17) 0.0240(6) Uani 1 1 d . . .
H53 H 0.8619 0.1623 -0.0725 0.029 Uiso 1 1 calc R . .
C54 C 0.9451(3) 0.15848(18) 0.01121(18) 0.0227(5) Uani 1 1 d . . .
H54 H 1.0232 0.1423 -0.0009 0.027 Uiso 1 1 calc R . .
C55 C 0.9265(3) 0.16980(17) 0.07187(17) 0.0187(5) Uani 1 1 d . . .
H55 H 0.9926 0.1623 0.1006 0.022 Uiso 1 1 calc R . .
C56 C 0.5873(3) 0.06283(16) 0.16002(16) 0.0154(4) Uani 1 1 d . . .
C57 C 0.5173(3) 0.06167(17) 0.10847(17) 0.0209(5) Uani 1 1 d . . .
H57 H 0.5450 0.0362 0.0815 0.025 Uiso 1 1 calc R . .
C58 C 0.4076(3) 0.09798(18) 0.09742(18) 0.0239(6) Uani 1 1 d . . .
H58 H 0.3599 0.0992 0.0615 0.029 Uiso 1 1 calc R . .
C59 C 0.3669(3) 0.13296(18) 0.13929(19) 0.0229(5) Uani 1 1 d . . .
H59 H 0.2899 0.1569 0.1334 0.028 Uiso 1 1 calc R . .
C60 C 0.4402(3) 0.13218(17) 0.18920(17) 0.0183(5) Uani 1 1 d . . .
H60 H 0.4116 0.1556 0.2179 0.022 Uiso 1 1 calc R . .
C61 C 0.9146(3) -0.00037(15) 0.24362(16) 0.0156(4) Uani 1 1 d . . .
C62 C 0.9819(3) 0.00189(17) 0.18271(18) 0.0208(5) Uani 1 1 d . . .
H62 H 0.9405 0.0110 0.1423 0.025 Uiso 1 1 calc R . .
C63 C 1.1111(3) -0.0093(2) 0.1809(2) 0.0288(6) Uani 1 1 d . . .
H63 H 1.1568 -0.0083 0.1394 0.035 Uiso 1 1 calc R . .
C64 C 1.1721(3) -0.0218(2) 0.2392(2) 0.0301(7) Uani 1 1 d . . .
H64 H 1.2595 -0.0297 0.2377 0.036 Uiso 1 1 calc R . .
C65 C 1.1068(3) -0.0230(2) 0.2998(2) 0.0292(6) Uani 1 1 d . . .
H65 H 1.1497 -0.0305 0.3393 0.035 Uiso 1 1 calc R . .
C66 C 0.9783(3) -0.01310(18) 0.30283(18) 0.0210(5) Uani 1 1 d . . .
H66 H 0.9333 -0.0149 0.3448 0.025 Uiso 1 1 calc R . .
C67 C 0.6889(3) -0.08356(16) 0.31152(16) 0.0154(4) Uani 1 1 d . . .
C68 C 0.6246(3) -0.12501(18) 0.28586(19) 0.0234(6) Uani 1 1 d . . .
H68 H 0.6070 -0.1036 0.2380 0.028 Uiso 1 1 calc R . .
C69 C 0.5861(4) -0.1978(2) 0.3305(2) 0.0304(7) Uani 1 1 d . . .
H69 H 0.5435 -0.2258 0.3125 0.036 Uiso 1 1 calc R . .
C70 C 0.6094(4) -0.22936(19) 0.4000(2) 0.0295(7) Uani 1 1 d . . .
H70 H 0.5841 -0.2791 0.4299 0.035 Uiso 1 1 calc R . .
C71 C 0.6705(3) -0.18757(19) 0.42636(19) 0.0265(6) Uani 1 1 d . . .
H71 H 0.6855 -0.2089 0.4746 0.032 Uiso 1 1 calc R . .
C72 C 0.7097(3) -0.11503(18) 0.38261(17) 0.0228(6) Uani 1 1 d . . .
H72 H 0.7505 -0.0869 0.4011 0.027 Uiso 1 1 calc R . .
C73 C 0.4840(3) -0.01278(19) 0.39203(18) 0.0235(6) Uani 1 1 d . . .
C74 C 0.4121(4) -0.0746(3) 0.4497(3) 0.0473(12) Uani 1 1 d . . .
H74A H 0.3553 -0.0967 0.4302 0.071 Uiso 1 1 calc R . .
H74B H 0.3632 -0.0574 0.4810 0.071 Uiso 1 1 calc R . .
H74C H 0.4697 -0.1110 0.4767 0.071 Uiso 1 1 calc R . .
C75 C 0.8293(3) 0.10754(17) 0.37553(17) 0.0198(5) Uani 1 1 d . . .
C76 C 0.9159(4) 0.1135(2) 0.4217(2) 0.0312(8) Uani 1 1 d . . .
H76A H 1.0023 0.1114 0.4025 0.047 Uiso 1 1 calc R . .
H76B H 0.8977 0.0730 0.4691 0.047 Uiso 1 1 calc R . .
H76C H 0.9060 0.1602 0.4245 0.047 Uiso 1 1 calc R . .
B1 B 0.7652(3) 0.96537(15) 0.02010(15) 0.0277(6) Uani 1 1 d DU . .
F11 F 0.77532(19) 0.89605(9) 0.02224(10) 0.0224(4) Uani 1 1 d DU . .
F12 F 0.7774(3) 0.95966(14) 0.08695(11) 0.0465(7) Uani 1 1 d DU . .
F13 F 0.6488(3) 0.99038(17) 0.00153(18) 0.0668(9) Uani 1 1 d DU . .
F14 F 0.8579(4) 1.01285(15) -0.02873(15) 0.0784(11) Uani 1 1 d DU . .
B2 B 0.7436(3) 0.45699(14) 0.03154(14) 0.0204(5) Uani 1 1 d DU . .
F21 F 0.7718(2) 0.44183(11) 0.09940(10) 0.0337(5) Uani 1 1 d DU . .
F22 F 0.72110(19) 0.39041(9) 0.02942(10) 0.0245(4) Uani 1 1 d DU . .
F23 F 0.8426(2) 0.49541(12) -0.01823(12) 0.0404(6) Uani 1 1 d DU . .
F24 F 0.6375(2) 0.49678(15) 0.01848(13) 0.0469(6) Uani 1 1 d DU . .
B3 B 0.7779(3) 0.92289(18) 0.53730(16) 0.0394(7) Uani 1 1 d DU . .
F31 F 0.8012(3) 0.9600(2) 0.57651(16) 0.0777(10) Uani 1 1 d DU . .
F32 F 0.8622(2) 0.94858(12) 0.47640(10) 0.0328(5) Uani 1 1 d DU . .
F33 F 0.6564(2) 0.93317(18) 0.51973(13) 0.0561(8) Uani 1 1 d DU . .
F34 F 0.7944(3) 0.84900(14) 0.57680(17) 0.0793(10) Uani 1 1 d DU . .
B4 B 0.7469(3) 0.57307(18) 0.52780(16) 0.0407(8) Uani 1 1 d DU . .
F41 F 0.7796(3) 0.51214(13) 0.58520(12) 0.0487(6) Uani 1 1 d DU . .
F42 F 0.8489(3) 0.62176(17) 0.49487(16) 0.0798(12) Uani 1 1 d DU . .
F43 F 0.7053(5) 0.5521(2) 0.47898(16) 0.126(2) Uani 1 1 d DU . .
F44 F 0.6525(4) 0.6066(2) 0.5501(2) 0.139(2) Uani 1 1 d DU . .


_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 N6 1.918(3) . ?
Fe1 N5 1.966(3) . ?
Fe1 N3 2.006(2) . ?
Fe1 N1 2.034(2) . ?
Fe1 P2 2.2056(8) . ?
Fe1 P1 2.2241(9) . ?
P1 N2 1.693(3) . ?
P1 C6 1.808(3) . ?
P1 C12 1.828(3) . ?
P2 N4 1.680(3) . ?
P2 C23 1.812(3) . ?
P2 C29 1.837(3) . ?
N1 C1 1.351(4) . ?
N1 C5 1.354(4) . ?
N2 C1 1.379(4) . ?
N2 H2N 0.8800 . ?
N3 C18 1.357(4) . ?
N3 C22 1.363(4) . ?
N4 C18 1.383(4) . ?
N4 H4N 0.8800 . ?
N5 C35 1.123(5) . ?
N6 C37 1.145(4) . ?
C1 C2 1.403(4) . ?
C2 C3 1.385(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C11 1.401(4) . ?
C6 C7 1.408(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.393(5) . ?
C12 C17 1.394(5) . ?
C13 C14 1.388(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.407(4) . ?
C19 C20 1.374(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.395(4) . ?
C23 C28 1.403(4) . ?
C24 C25 1.390(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.393(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.388(4) . ?
C29 C34 1.395(4) . ?
C30 C31 1.397(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.381(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.391(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(5) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.463(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.459(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
Fe2 N12 1.923(3) . ?
Fe2 N11 1.970(3) . ?
Fe2 N9 2.001(2) . ?
Fe2 N7 2.036(2) . ?
Fe2 P4 2.2089(8) . ?
Fe2 P3 2.2359(9) . ?
P3 N8 1.686(3) . ?
P3 C50 1.814(3) . ?
P3 C44 1.824(3) . ?
P4 N10 1.688(3) . ?
P4 C61 1.813(3) . ?
P4 C67 1.833(3) . ?
N7 C39 1.357(4) . ?
N7 C43 1.358(4) . ?
N8 C39 1.376(4) . ?
N8 H8N 0.8800 . ?
N9 C56 1.361(4) . ?
N9 C60 1.363(4) . ?
N10 C56 1.384(4) . ?
N10 H10N 0.8800 . ?
N11 C73 1.140(4) . ?
N12 C75 1.139(4) . ?
C39 C40 1.408(4) . ?
C40 C41 1.379(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.395(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.386(4) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.394(5) . ?
C44 C49 1.404(4) . ?
C45 C46 1.401(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.388(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.392(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.393(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C55 1.396(4) . ?
C50 C51 1.399(4) . ?
C51 C52 1.394(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.400(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.388(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.392(4) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.395(4) . ?
C57 C58 1.375(5) . ?
C57 H57 0.9500 . ?
C58 C59 1.395(5) . ?
C58 H58 0.9500 . ?
C59 C60 1.375(4) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.390(4) . ?
C61 C66 1.413(4) . ?
C62 C63 1.404(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.381(6) . ?
C63 H63 0.9500 . ?
C64 C65 1.384(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.392(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C72 1.395(4) . ?
C67 C68 1.400(4) . ?
C68 C69 1.396(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.374(6) . ?
C69 H69 0.9500 . ?
C70 C71 1.397(5) . ?
C70 H70 0.9500 . ?
C71 C72 1.390(5) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C74 1.457(5) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.456(5) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
B1 F13 1.378(3) . ?
B1 F14 1.378(3) . ?
B1 F12 1.386(3) . ?
B1 F11 1.394(3) . ?
B2 F23 1.376(3) . ?
B2 F24 1.376(3) . ?
B2 F22 1.395(3) . ?
B2 F21 1.396(3) . ?
B3 F31 1.381(3) . ?
B3 F33 1.383(3) . ?
B3 F32 1.384(3) . ?
B3 F34 1.385(3) . ?
B4 F44 1.375(3) . ?
B4 F42 1.379(3) . ?
B4 F41 1.380(3) . ?
B4 F43 1.388(3) . ?

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
N6 Fe1 N5 88.03(12) . . ?
N6 Fe1 N3 175.89(12) . . ?
N5 Fe1 N3 87.87(11) . . ?
N6 Fe1 N1 88.61(10) . . ?
N5 Fe1 N1 91.28(11) . . ?
N3 Fe1 N1 91.18(10) . . ?
N6 Fe1 P2 98.29(8) . . ?
N5 Fe1 P2 90.28(8) . . ?
N3 Fe1 P2 82.03(7) . . ?
N1 Fe1 P2 172.97(8) . . ?
N6 Fe1 P1 95.84(9) . . ?
N5 Fe1 P1 171.28(8) . . ?
N3 Fe1 P1 88.18(8) . . ?
N1 Fe1 P1 81.03(8) . . ?
P2 Fe1 P1 96.86(3) . . ?
N2 P1 C6 102.86(13) . . ?
N2 P1 C12 105.06(14) . . ?
C6 P1 C12 103.98(14) . . ?
N2 P1 Fe1 98.69(10) . . ?
C6 P1 Fe1 121.98(10) . . ?
C12 P1 Fe1 121.17(11) . . ?
N4 P2 C23 104.84(14) . . ?
N4 P2 C29 104.46(14) . . ?
C23 P2 C29 101.09(14) . . ?
N4 P2 Fe1 100.09(9) . . ?
C23 P2 Fe1 125.98(10) . . ?
C29 P2 Fe1 117.91(10) . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Fe1 118.9(2) . . ?
C5 N1 Fe1 122.6(2) . . ?
C1 N2 P1 116.8(2) . . ?
C1 N2 H2N 121.6 . . ?
P1 N2 H2N 121.6 . . ?
C18 N3 C22 117.0(3) . . ?
C18 N3 Fe1 119.6(2) . . ?
C22 N3 Fe1 123.4(2) . . ?
C18 N4 P2 116.5(2) . . ?
C18 N4 H4N 121.8 . . ?
P2 N4 H4N 121.8 . . ?
C35 N5 Fe1 175.9(3) . . ?
C37 N6 Fe1 174.6(3) . . ?
N1 C1 N2 115.8(3) . . ?
N1 C1 C2 122.0(3) . . ?
N2 C1 C2 122.2(3) . . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 122.7(3) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C11 C6 C7 119.6(3) . . ?
C11 C6 P1 120.6(2) . . ?
C7 C6 P1 119.2(2) . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C6 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C6 C11 H11 120.2 . . ?
C13 C12 C17 119.0(3) . . ?
C13 C12 P1 119.9(3) . . ?
C17 C12 P1 121.0(3) . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.6(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 119.9(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C12 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C12 C17 H17 119.8 . . ?
N3 C18 N4 115.9(2) . . ?
N3 C18 C19 122.6(3) . . ?
N4 C18 C19 121.4(3) . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 118.6(3) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
N3 C22 C21 123.5(3) . . ?
N3 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
C24 C23 C28 119.1(3) . . ?
C24 C23 P2 118.2(2) . . ?
C28 C23 P2 122.6(2) . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C26 C25 C24 119.8(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.3(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C23 120.1(3) . . ?
C27 C28 H28 119.9 . . ?
C23 C28 H28 119.9 . . ?
C30 C29 C34 119.6(3) . . ?
C30 C29 P2 121.2(2) . . ?
C34 C29 P2 119.2(2) . . ?
C29 C30 C31 120.0(3) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.3(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 119.7(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C29 120.1(3) . . ?
C33 C34 H34 119.9 . . ?
C29 C34 H34 119.9 . . ?
N5 C35 C36 178.2(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N6 C37 C38 178.9(6) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N12 Fe2 N11 89.40(11) . . ?
N12 Fe2 N9 178.50(11) . . ?
N11 Fe2 N9 89.10(10) . . ?
N12 Fe2 N7 88.01(10) . . ?
N11 Fe2 N7 91.85(10) . . ?
N9 Fe2 N7 92.22(10) . . ?
N12 Fe2 P4 98.12(8) . . ?
N11 Fe2 P4 89.98(8) . . ?
N9 Fe2 P4 81.70(7) . . ?
N7 Fe2 P4 173.62(8) . . ?
N12 Fe2 P3 93.58(8) . . ?
N11 Fe2 P3 172.65(8) . . ?
N9 Fe2 P3 87.93(7) . . ?
N7 Fe2 P3 81.55(7) . . ?
P4 Fe2 P3 96.24(3) . . ?
N8 P3 C50 101.43(14) . . ?
N8 P3 C44 105.59(14) . . ?
C50 P3 C44 103.73(13) . . ?
N8 P3 Fe2 98.75(9) . . ?
C50 P3 Fe2 122.98(10) . . ?
C44 P3 Fe2 120.98(11) . . ?
N10 P4 C61 106.28(14) . . ?
N10 P4 C67 104.27(14) . . ?
C61 P4 C67 101.15(13) . . ?
N10 P4 Fe2 99.57(10) . . ?
C61 P4 Fe2 123.53(10) . . ?
C67 P4 Fe2 119.88(10) . . ?
C39 N7 C43 117.7(3) . . ?
C39 N7 Fe2 119.14(19) . . ?
C43 N7 Fe2 123.2(2) . . ?
C39 N8 P3 117.6(2) . . ?
C39 N8 H8N 121.2 . . ?
P3 N8 H8N 121.2 . . ?
C56 N9 C60 117.1(3) . . ?
C56 N9 Fe2 119.9(2) . . ?
C60 N9 Fe2 123.0(2) . . ?
C56 N10 P4 115.7(2) . . ?
C56 N10 H10N 122.1 . . ?
P4 N10 H10N 122.1 . . ?
C73 N11 Fe2 172.1(3) . . ?
C75 N12 Fe2 177.4(3) . . ?
N7 C39 N8 115.8(2) . . ?
N7 C39 C40 122.6(3) . . ?
N8 C39 C40 121.6(3) . . ?
C41 C40 C39 118.5(3) . . ?
C41 C40 H40 120.8 . . ?
C39 C40 H40 120.8 . . ?
C40 C41 C42 119.4(3) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C43 C42 C41 119.2(3) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
N7 C43 C42 122.6(3) . . ?
N7 C43 H43 118.7 . . ?
C42 C43 H43 118.7 . . ?
C45 C44 C49 118.9(3) . . ?
C45 C44 P3 121.6(2) . . ?
C49 C44 P3 119.5(2) . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C47 C46 C45 120.4(4) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C46 C47 C48 119.8(3) . . ?
C46 C47 H47 120.1 . . ?
C48 C47 H47 120.1 . . ?
C47 C48 C49 119.9(3) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 C44 120.7(3) . . ?
C48 C49 H49 119.6 . . ?
C44 C49 H49 119.6 . . ?
C55 C50 C51 119.7(3) . . ?
C55 C50 P3 119.6(2) . . ?
C51 C50 P3 120.3(2) . . ?
C52 C51 C50 120.0(3) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 119.9(3) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C54 C53 C52 120.1(3) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.0(3) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C54 C55 C50 120.3(3) . . ?
C54 C55 H55 119.9 . . ?
C50 C55 H55 119.9 . . ?
N9 C56 N10 115.5(3) . . ?
N9 C56 C57 122.6(3) . . ?
N10 C56 C57 121.9(3) . . ?
C58 C57 C56 118.9(3) . . ?
C58 C57 H57 120.6 . . ?
C56 C57 H57 120.6 . . ?
C57 C58 C59 119.5(3) . . ?
C57 C58 H58 120.3 . . ?
C59 C58 H58 120.3 . . ?
C60 C59 C58 118.8(3) . . ?
C60 C59 H59 120.6 . . ?
C58 C59 H59 120.6 . . ?
N9 C60 C59 123.0(3) . . ?
N9 C60 H60 118.5 . . ?
C59 C60 H60 118.5 . . ?
C62 C61 C66 119.1(3) . . ?
C62 C61 P4 123.8(3) . . ?
C66 C61 P4 117.0(2) . . ?
C61 C62 C63 120.0(3) . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 120.2(3) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C63 C64 C65 120.5(3) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C64 C65 C66 120.0(4) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 C61 120.2(3) . . ?
C65 C66 H66 119.9 . . ?
C61 C66 H66 119.9 . . ?
C72 C67 C68 119.2(3) . . ?
C72 C67 P4 120.0(2) . . ?
C68 C67 P4 120.9(2) . . ?
C69 C68 C67 120.1(3) . . ?
C69 C68 H68 120.0 . . ?
C67 C68 H68 120.0 . . ?
C70 C69 C68 120.7(3) . . ?
C70 C69 H69 119.7 . . ?
C68 C69 H69 119.7 . . ?
C69 C70 C71 119.4(3) . . ?
C69 C70 H70 120.3 . . ?
C71 C70 H70 120.3 . . ?
C72 C71 C70 120.6(3) . . ?
C72 C71 H71 119.7 . . ?
C70 C71 H71 119.7 . . ?
C71 C72 C67 120.0(3) . . ?
C71 C72 H72 120.0 . . ?
C67 C72 H72 120.0 . . ?
N11 C73 C74 176.9(4) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N12 C75 C76 176.3(4) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
F13 B1 F14 109.9(3) . . ?
F13 B1 F12 109.4(2) . . ?
F14 B1 F12 110.2(2) . . ?
F13 B1 F11 109.0(2) . . ?
F14 B1 F11 109.9(2) . . ?
F12 B1 F11 108.5(2) . . ?
F23 B2 F24 110.3(2) . . ?
F23 B2 F22 109.5(2) . . ?
F24 B2 F22 109.7(2) . . ?
F23 B2 F21 110.4(2) . . ?
F24 B2 F21 109.0(2) . . ?
F22 B2 F21 107.9(2) . . ?
F31 B3 F33 109.8(3) . . ?
F31 B3 F32 109.4(2) . . ?
F33 B3 F32 109.9(2) . . ?
F31 B3 F34 109.2(3) . . ?
F33 B3 F34 110.0(3) . . ?
F32 B3 F34 108.6(2) . . ?
F44 B4 F42 109.6(3) . . ?
F44 B4 F41 109.5(3) . . ?
F42 B4 F41 110.7(3) . . ?
F44 B4 F43 109.3(3) . . ?
F42 B4 F43 108.1(3) . . ?
F41 B4 F43 109.6(3) . . ?

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
N6 Fe1 P1 N2 111.13(12) . . . . ?
N3 Fe1 P1 N2 -68.02(12) . . . . ?
N1 Fe1 P1 N2 23.47(12) . . . . ?
P2 Fe1 P1 N2 -149.76(10) . . . . ?
N6 Fe1 P1 C6 -137.71(14) . . . . ?
N3 Fe1 P1 C6 43.14(14) . . . . ?
N1 Fe1 P1 C6 134.63(14) . . . . ?
P2 Fe1 P1 C6 -38.60(12) . . . . ?
N6 Fe1 P1 C12 -2.43(14) . . . . ?
N3 Fe1 P1 C12 178.42(14) . . . . ?
N1 Fe1 P1 C12 -90.09(14) . . . . ?
P2 Fe1 P1 C12 96.68(12) . . . . ?
N6 Fe1 P2 N4 165.30(13) . . . . ?
N5 Fe1 P2 N4 -106.65(13) . . . . ?
N3 Fe1 P2 N4 -18.84(12) . . . . ?
P1 Fe1 P2 N4 68.35(10) . . . . ?
N6 Fe1 P2 C23 48.52(15) . . . . ?
N5 Fe1 P2 C23 136.57(15) . . . . ?
N3 Fe1 P2 C23 -135.62(15) . . . . ?
P1 Fe1 P2 C23 -48.43(13) . . . . ?
N6 Fe1 P2 C29 -82.29(15) . . . . ?
N5 Fe1 P2 C29 5.76(14) . . . . ?
N3 Fe1 P2 C29 93.57(14) . . . . ?
P1 Fe1 P2 C29 -179.25(12) . . . . ?
N6 Fe1 N1 C1 -117.8(2) . . . . ?
N5 Fe1 N1 C1 154.2(2) . . . . ?
N3 Fe1 N1 C1 66.3(2) . . . . ?
P1 Fe1 N1 C1 -21.7(2) . . . . ?
N6 Fe1 N1 C5 67.6(3) . . . . ?
N5 Fe1 N1 C5 -20.4(3) . . . . ?
N3 Fe1 N1 C5 -108.3(3) . . . . ?
P1 Fe1 N1 C5 163.8(3) . . . . ?
C6 P1 N2 C1 -154.3(2) . . . . ?
C12 P1 N2 C1 97.2(2) . . . . ?
Fe1 P1 N2 C1 -28.5(2) . . . . ?
N5 Fe1 N3 C18 105.7(2) . . . . ?
N1 Fe1 N3 C18 -163.1(2) . . . . ?
P2 Fe1 N3 C18 15.1(2) . . . . ?
P1 Fe1 N3 C18 -82.1(2) . . . . ?
N5 Fe1 N3 C22 -73.5(2) . . . . ?
N1 Fe1 N3 C22 17.7(2) . . . . ?
P2 Fe1 N3 C22 -164.1(2) . . . . ?
P1 Fe1 N3 C22 98.7(2) . . . . ?
C23 P2 N4 C18 156.2(2) . . . . ?
C29 P2 N4 C18 -97.9(2) . . . . ?
Fe1 P2 N4 C18 24.6(2) . . . . ?
C5 N1 C1 N2 -176.0(3) . . . . ?
Fe1 N1 C1 N2 9.2(3) . . . . ?
C5 N1 C1 C2 4.6(4) . . . . ?
Fe1 N1 C1 C2 -170.2(2) . . . . ?
P1 N2 C1 N1 15.7(3) . . . . ?
P1 N2 C1 C2 -164.9(2) . . . . ?
N1 C1 C2 C3 -2.3(5) . . . . ?
N2 C1 C2 C3 178.3(3) . . . . ?
C1 C2 C3 C4 -0.7(5) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C1 N1 C5 C4 -4.0(5) . . . . ?
Fe1 N1 C5 C4 170.6(3) . . . . ?
C3 C4 C5 N1 1.1(5) . . . . ?
N2 P1 C6 C11 34.5(3) . . . . ?
C12 P1 C6 C11 143.9(3) . . . . ?
Fe1 P1 C6 C11 -74.5(3) . . . . ?
N2 P1 C6 C7 -153.9(2) . . . . ?
C12 P1 C6 C7 -44.6(3) . . . . ?
Fe1 P1 C6 C7 97.1(2) . . . . ?
C11 C6 C7 C8 1.8(5) . . . . ?
P1 C6 C7 C8 -169.8(2) . . . . ?
C6 C7 C8 C9 -0.2(5) . . . . ?
C7 C8 C9 C10 -1.8(5) . . . . ?
C8 C9 C10 C11 2.2(5) . . . . ?
C9 C10 C11 C6 -0.6(5) . . . . ?
C7 C6 C11 C10 -1.4(5) . . . . ?
P1 C6 C11 C10 170.1(2) . . . . ?
N2 P1 C12 C13 27.6(3) . . . . ?
C6 P1 C12 C13 -80.1(3) . . . . ?
Fe1 P1 C12 C13 137.8(2) . . . . ?
N2 P1 C12 C17 -152.5(3) . . . . ?
C6 P1 C12 C17 99.7(3) . . . . ?
Fe1 P1 C12 C17 -42.3(3) . . . . ?
C17 C12 C13 C14 1.4(5) . . . . ?
P1 C12 C13 C14 -178.8(3) . . . . ?
C12 C13 C14 C15 0.4(6) . . . . ?
C13 C14 C15 C16 -1.7(6) . . . . ?
C14 C15 C16 C17 1.2(6) . . . . ?
C15 C16 C17 C12 0.6(6) . . . . ?
C13 C12 C17 C16 -1.9(5) . . . . ?
P1 C12 C17 C16 178.3(3) . . . . ?
C22 N3 C18 N4 175.9(3) . . . . ?
Fe1 N3 C18 N4 -3.3(3) . . . . ?
C22 N3 C18 C19 -4.2(4) . . . . ?
Fe1 N3 C18 C19 176.5(2) . . . . ?
P2 N4 C18 N3 -16.3(3) . . . . ?
P2 N4 C18 C19 163.9(2) . . . . ?
N3 C18 C19 C20 1.9(5) . . . . ?
N4 C18 C19 C20 -178.3(3) . . . . ?
C18 C19 C20 C21 1.6(5) . . . . ?
C19 C20 C21 C22 -2.6(5) . . . . ?
C18 N3 C22 C21 3.2(5) . . . . ?
Fe1 N3 C22 C21 -177.6(2) . . . . ?
C20 C21 C22 N3 0.1(5) . . . . ?
N4 P2 C23 C24 -175.3(2) . . . . ?
C29 P2 C23 C24 76.3(3) . . . . ?
Fe1 P2 C23 C24 -60.7(3) . . . . ?
N4 P2 C23 C28 9.5(3) . . . . ?
C29 P2 C23 C28 -98.8(3) . . . . ?
Fe1 P2 C23 C28 124.1(2) . . . . ?
C28 C23 C24 C25 0.7(5) . . . . ?
P2 C23 C24 C25 -174.7(3) . . . . ?
C23 C24 C25 C26 0.8(5) . . . . ?
C24 C25 C26 C27 -1.3(5) . . . . ?
C25 C26 C27 C28 0.3(5) . . . . ?
C26 C27 C28 C23 1.2(5) . . . . ?
C24 C23 C28 C27 -1.7(5) . . . . ?
P2 C23 C28 C27 173.4(2) . . . . ?
N4 P2 C29 C30 1.4(3) . . . . ?
C23 P2 C29 C30 110.1(3) . . . . ?
Fe1 P2 C29 C30 -108.5(3) . . . . ?
N4 P2 C29 C34 -177.8(3) . . . . ?
C23 P2 C29 C34 -69.2(3) . . . . ?
Fe1 P2 C29 C34 72.2(3) . . . . ?
C34 C29 C30 C31 1.2(5) . . . . ?
P2 C29 C30 C31 -178.1(3) . . . . ?
C29 C30 C31 C32 -1.5(6) . . . . ?
C30 C31 C32 C33 1.1(7) . . . . ?
C31 C32 C33 C34 -0.3(7) . . . . ?
C32 C33 C34 C29 0.0(6) . . . . ?
C30 C29 C34 C33 -0.4(5) . . . . ?
P2 C29 C34 C33 178.9(3) . . . . ?
N12 Fe2 P3 N8 -108.05(12) . . . . ?
N9 Fe2 P3 N8 71.95(12) . . . . ?
N7 Fe2 P3 N8 -20.60(12) . . . . ?
P4 Fe2 P3 N8 153.37(10) . . . . ?
N12 Fe2 P3 C50 142.14(14) . . . . ?
N9 Fe2 P3 C50 -37.85(14) . . . . ?
N7 Fe2 P3 C50 -130.40(14) . . . . ?
P4 Fe2 P3 C50 43.56(12) . . . . ?
N12 Fe2 P3 C44 6.13(14) . . . . ?
N9 Fe2 P3 C44 -173.87(13) . . . . ?
N7 Fe2 P3 C44 93.58(14) . . . . ?
P4 Fe2 P3 C44 -92.45(12) . . . . ?
N12 Fe2 P4 N10 -160.18(12) . . . . ?
N11 Fe2 P4 N10 110.43(12) . . . . ?
N9 Fe2 P4 N10 21.33(12) . . . . ?
P3 Fe2 P4 N10 -65.65(10) . . . . ?
N12 Fe2 P4 C61 -43.26(15) . . . . ?
N11 Fe2 P4 C61 -132.65(15) . . . . ?
N9 Fe2 P4 C61 138.25(15) . . . . ?
P3 Fe2 P4 C61 51.27(13) . . . . ?
N12 Fe2 P4 C67 87.17(14) . . . . ?
N11 Fe2 P4 C67 -2.23(14) . . . . ?
N9 Fe2 P4 C67 -91.32(14) . . . . ?
P3 Fe2 P4 C67 -178.30(12) . . . . ?
N12 Fe2 N7 C39 110.8(2) . . . . ?
N11 Fe2 N7 C39 -159.9(2) . . . . ?
N9 Fe2 N7 C39 -70.7(2) . . . . ?
P3 Fe2 N7 C39 16.9(2) . . . . ?
N12 Fe2 N7 C43 -70.6(2) . . . . ?
N11 Fe2 N7 C43 18.8(2) . . . . ?
N9 Fe2 N7 C43 108.0(2) . . . . ?
P3 Fe2 N7 C43 -164.5(2) . . . . ?
C50 P3 N8 C39 153.6(2) . . . . ?
C44 P3 N8 C39 -98.5(2) . . . . ?
Fe2 P3 N8 C39 27.2(2) . . . . ?
N11 Fe2 N9 C56 -106.8(2) . . . . ?
N7 Fe2 N9 C56 161.4(2) . . . . ?
P4 Fe2 N9 C56 -16.7(2) . . . . ?
P3 Fe2 N9 C56 79.9(2) . . . . ?
N11 Fe2 N9 C60 73.1(2) . . . . ?
N7 Fe2 N9 C60 -18.7(2) . . . . ?
P4 Fe2 N9 C60 163.2(2) . . . . ?
P3 Fe2 N9 C60 -100.2(2) . . . . ?
C61 P4 N10 C56 -157.4(2) . . . . ?
C67 P4 N10 C56 96.2(2) . . . . ?
Fe2 P4 N10 C56 -28.1(2) . . . . ?
C43 N7 C39 N8 177.2(3) . . . . ?
Fe2 N7 C39 N8 -4.0(3) . . . . ?
C43 N7 C39 C40 -3.0(4) . . . . ?
Fe2 N7 C39 C40 175.7(2) . . . . ?
P3 N8 C39 N7 -18.0(3) . . . . ?
P3 N8 C39 C40 162.2(2) . . . . ?
N7 C39 C40 C41 2.2(5) . . . . ?
N8 C39 C40 C41 -178.1(3) . . . . ?
C39 C40 C41 C42 0.3(5) . . . . ?
C40 C41 C42 C43 -1.8(5) . . . . ?
C39 N7 C43 C42 1.5(4) . . . . ?
Fe2 N7 C43 C42 -177.2(2) . . . . ?
C41 C42 C43 N7 0.9(5) . . . . ?
N8 P3 C44 C45 153.8(3) . . . . ?
C50 P3 C44 C45 -99.9(3) . . . . ?
Fe2 P3 C44 C45 43.2(3) . . . . ?
N8 P3 C44 C49 -25.4(3) . . . . ?
C50 P3 C44 C49 80.9(3) . . . . ?
Fe2 P3 C44 C49 -136.0(2) . . . . ?
C49 C44 C45 C46 2.0(5) . . . . ?
P3 C44 C45 C46 -177.2(3) . . . . ?
C44 C45 C46 C47 -1.2(5) . . . . ?
C45 C46 C47 C48 -0.7(6) . . . . ?
C46 C47 C48 C49 1.7(6) . . . . ?
C47 C48 C49 C44 -1.0(5) . . . . ?
C45 C44 C49 C48 -0.9(5) . . . . ?
P3 C44 C49 C48 178.3(3) . . . . ?
N8 P3 C50 C55 151.1(2) . . . . ?
C44 P3 C50 C55 41.7(3) . . . . ?
Fe2 P3 C50 C55 -100.5(2) . . . . ?
N8 P3 C50 C51 -36.5(3) . . . . ?
C44 P3 C50 C51 -145.9(2) . . . . ?
Fe2 P3 C50 C51 71.9(3) . . . . ?
C55 C50 C51 C52 2.1(4) . . . . ?
P3 C50 C51 C52 -170.4(2) . . . . ?
C50 C51 C52 C53 0.3(5) . . . . ?
C51 C52 C53 C54 -2.0(5) . . . . ?
C52 C53 C54 C55 1.1(5) . . . . ?
C53 C54 C55 C50 1.3(5) . . . . ?
C51 C50 C55 C54 -2.9(5) . . . . ?
P3 C50 C55 C54 169.6(2) . . . . ?
C60 N9 C56 N10 -177.0(3) . . . . ?
Fe2 N9 C56 N10 3.0(3) . . . . ?
C60 N9 C56 C57 3.5(4) . . . . ?
Fe2 N9 C56 C57 -176.6(2) . . . . ?
P4 N10 C56 N9 19.2(3) . . . . ?
P4 N10 C56 C57 -161.3(2) . . . . ?
N9 C56 C57 C58 -0.9(5) . . . . ?
N10 C56 C57 C58 179.7(3) . . . . ?
C56 C57 C58 C59 -2.0(5) . . . . ?
C57 C58 C59 C60 2.1(5) . . . . ?
C56 N9 C60 C59 -3.5(4) . . . . ?
Fe2 N9 C60 C59 176.6(2) . . . . ?
C58 C59 C60 N9 0.7(5) . . . . ?
N10 P4 C61 C62 -2.4(3) . . . . ?
C67 P4 C61 C62 106.2(3) . . . . ?
Fe2 P4 C61 C62 -116.1(2) . . . . ?
N10 P4 C61 C66 178.6(2) . . . . ?
C67 P4 C61 C66 -72.8(2) . . . . ?
Fe2 P4 C61 C66 64.9(3) . . . . ?
C66 C61 C62 C63 0.8(5) . . . . ?
P4 C61 C62 C63 -178.2(3) . . . . ?
C61 C62 C63 C64 -0.7(5) . . . . ?
C62 C63 C64 C65 -0.4(6) . . . . ?
C63 C64 C65 C66 1.4(6) . . . . ?
C64 C65 C66 C61 -1.3(5) . . . . ?
C62 C61 C66 C65 0.2(5) . . . . ?
P4 C61 C66 C65 179.2(3) . . . . ?
N10 P4 C67 C72 -178.3(3) . . . . ?
C61 P4 C67 C72 71.5(3) . . . . ?
Fe2 P4 C67 C72 -68.2(3) . . . . ?
N10 P4 C67 C68 2.2(3) . . . . ?
C61 P4 C67 C68 -108.0(3) . . . . ?
Fe2 P4 C67 C68 112.3(2) . . . . ?
C72 C67 C68 C69 -2.4(5) . . . . ?
P4 C67 C68 C69 177.0(3) . . . . ?
C67 C68 C69 C70 0.8(6) . . . . ?
C68 C69 C70 C71 0.9(6) . . . . ?
C69 C70 C71 C72 -1.1(6) . . . . ?
C70 C71 C72 C67 -0.6(5) . . . . ?
C68 C67 C72 C71 2.3(5) . . . . ?
P4 C67 C72 C71 -177.2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N F11 0.88 2.01 2.857(3) 160.2 .
N4 H4N F21 0.88 2.09 2.791(3) 136.4 .
N8 H8N F22 0.88 2.01 2.865(3) 163.3 .
N10 H10N F12 0.88 1.97 2.805(3) 158.0 1_545

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.084

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
? ? ? ? ? ? ?

_platon_squeeze_details          
;
Platy red crystals from acetonitrile / diethyl ether.
The compound is a disordered solvate with 
an estimated solvent content of about 1/2 acetontrile
molecule per complex. 
Prior to final refinement the disordered solvent 
was removed from the data with procedure SQUEEZE of
program PLATON. The 3 most significant solvent peaks were
C1S     0.2064    0.7788    0.4238
C2S     0.0906    0.7714    0.4698
C3S    -0.0309    0.7624    0.5103
and were thought to represent essentially acetonitrile (one
molecule per two Fe-complexes !!). According to program
PLATON the solvent cavities (2 symmetry equivalent per unit cell)
are located at x,y,z = 0.062, 0.736, 0.486 and -x,-y,-z.
The solvent accessible volume per cavity is 166 A^3 and 332 A^3 
per unit cell.
;


# start Validation Reply Form

_vrf_PLAT002_6                   
;
PROBLEM: 
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 20
RESPONSE: 
In the final refinement soft SADI 0.005 restraints were used for
the B-F and F-F distances of the BF4 groups in order to compensate
the large displacement parameters of the BF4 fluorine atoms.
;

_vrf_PLAT003_6                   
;
PROBLEM: 
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms  20
RESPONSE: 
A DELU 0.002 0.002 restraint was used for the Uij of the atoms of
the BF4 groups.
;

_vrf_PLAT605_6                   
;
PROBLEM: 
PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of 166 A**3
RESPONSE: 
Platy red crystals from acetonitrile / diethyl ether.
The compound is a disordered solvate with 
an estimated solvent content of about 1/2 acetontrile
molecule per complex. 
Prior to final refinement the disordered solvent 
was removed from the data with procedure SQUEEZE of
program PLATON. The 3 most significant solvent peaks were
C1S     0.2064    0.7788    0.4238
C2S     0.0906    0.7714    0.4698
C3S    -0.0309    0.7624    0.5103
and were thought to represent essentially acetonitrile (one
molecule per two Fe-complexes !!). According to program
PLATON the solvent cavities (2 symmetry equivalent per unit cell)
are located at x,y,z = 0.062, 0.736, 0.486 and -x,-y,-z.
The solvent accessible volume per cavity is 166 A^3 and 332 A^3 
per unit cell. The solvent content is not contained in chemical
formula and quantities derived thereof.
;

# end Validation Reply Form



#===END





_database_code_depnum_ccdc_archive 'CCDC 981198'
