# 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H16 F0 Fe N6 O2 P0'
_chemical_formula_weight         452.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   9.257(8)
_cell_length_b                   16.127(13)
_cell_length_c                   13.836(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.234(16)
_cell_angle_gamma                90.00
_cell_volume                     2060(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6365
_cell_measurement_theta_min      2.5260
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_process_details   'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17211
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         27.54
_reflns_number_total             4698
_reflns_number_gt                2925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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)+(0.0950P)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_number_reflns         4698
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1779
_refine_ls_wR_factor_gt          0.1639
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_restrained_S_all      0.917
_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 0.09730(5) 0.77882(3) 0.22756(4) 0.02163(18) Uani 1 1 d . . .
C1 C -0.0514(4) 0.8568(2) 0.1923(3) 0.0242(8) Uani 1 1 d . . .
C2 C -0.0492(4) 0.6964(2) 0.2381(3) 0.0243(8) Uani 1 1 d . . .
C3 C 0.3226(4) 0.6444(2) 0.2248(3) 0.0261(8) Uani 1 1 d . . .
H3A H 0.3149 0.6499 0.1577 0.031 Uiso 1 1 calc R . .
C4 C 0.4131(4) 0.5845(2) 0.2655(3) 0.0292(9) Uani 1 1 d . . .
H4A H 0.4656 0.5506 0.2265 0.035 Uiso 1 1 calc R . .
C5 C 0.4256(4) 0.5750(2) 0.3646(3) 0.0326(9) Uani 1 1 d . . .
H5A H 0.4880 0.5356 0.3935 0.039 Uiso 1 1 calc R . .
C6 C 0.3437(4) 0.6252(2) 0.4204(3) 0.0308(9) Uani 1 1 d . . .
H6A H 0.3468 0.6186 0.4873 0.037 Uiso 1 1 calc R . .
C7 C 0.2558(4) 0.6863(2) 0.3740(3) 0.0253(8) Uani 1 1 d . . .
C8 C 0.1722(4) 0.7472(2) 0.4266(3) 0.0236(8) Uani 1 1 d . . .
C9 C 0.1752(4) 0.7523(2) 0.5267(3) 0.0284(8) Uani 1 1 d . . .
H9A H 0.2272 0.7138 0.5654 0.034 Uiso 1 1 calc R . .
C10 C 0.0993(4) 0.8159(2) 0.5685(3) 0.0297(9) Uani 1 1 d . . .
H10A H 0.1009 0.8210 0.6355 0.036 Uiso 1 1 calc R . .
C11 C 0.0219(4) 0.8711(2) 0.5091(3) 0.0282(8) Uani 1 1 d . . .
H11A H -0.0298 0.9139 0.5356 0.034 Uiso 1 1 calc R . .
C12 C 0.0218(4) 0.8623(2) 0.4087(3) 0.0260(8) Uani 1 1 d . . .
H12A H -0.0305 0.8999 0.3690 0.031 Uiso 1 1 calc R . .
C13 C 0.0476(4) 0.6991(2) 0.0343(3) 0.0288(8) Uani 1 1 d . . .
H13A H -0.0227 0.6673 0.0615 0.035 Uiso 1 1 calc R . .
C14 C 0.0726(4) 0.6861(3) -0.0624(3) 0.0322(9) Uani 1 1 d . . .
H14A H 0.0216 0.6454 -0.0982 0.039 Uiso 1 1 calc R . .
C15 C 0.1736(4) 0.7340(2) -0.1045(3) 0.0338(9) Uani 1 1 d . . .
H15A H 0.1897 0.7272 -0.1696 0.041 Uiso 1 1 calc R . .
C16 C 0.2508(4) 0.7923(2) -0.0487(3) 0.0327(9) Uani 1 1 d . . .
H16A H 0.3208 0.8248 -0.0754 0.039 Uiso 1 1 calc R . .
C17 C 0.2223(4) 0.8017(2) 0.0481(3) 0.0253(8) Uani 1 1 d . . .
C18 C 0.2975(4) 0.8616(2) 0.1150(3) 0.0271(8) Uani 1 1 d . . .
C19 C 0.4088(4) 0.9136(3) 0.0884(3) 0.0359(10) Uani 1 1 d . . .
H19A H 0.4409 0.9109 0.0264 0.043 Uiso 1 1 calc R . .
C20 C 0.4707(4) 0.9694(3) 0.1559(3) 0.0373(10) Uani 1 1 d . . .
H20A H 0.5454 1.0044 0.1404 0.045 Uiso 1 1 calc R . .
C21 C 0.4176(4) 0.9712(2) 0.2473(3) 0.0321(9) Uani 1 1 d . . .
H21A H 0.4549 1.0087 0.2937 0.039 Uiso 1 1 calc R . .
C22 C 0.3088(4) 0.9167(2) 0.2687(3) 0.0269(8) Uani 1 1 d . . .
H22A H 0.2755 0.9180 0.3305 0.032 Uiso 1 1 calc R . .
N1 N -0.1450(3) 0.9038(2) 0.1704(2) 0.0314(8) Uani 1 1 d . . .
N2 N -0.1364(3) 0.64554(19) 0.2456(2) 0.0285(7) Uani 1 1 d . . .
N3 N 0.2445(3) 0.69537(18) 0.2771(2) 0.0230(6) Uani 1 1 d . . .
N4 N 0.0956(3) 0.80033(18) 0.3668(2) 0.0219(6) Uani 1 1 d . . .
N5 N 0.1209(3) 0.75605(19) 0.0907(2) 0.0236(7) Uani 1 1 d . . .
N6 N 0.2496(3) 0.86234(17) 0.2047(2) 0.0235(7) Uani 1 1 d . . .
O1 O -0.2750(3) 0.50515(16) 0.16955(19) 0.0318(6) Uiso 1 1 d . . .
O2 O 0.3387(4) 0.99120(19) 0.4893(2) 0.0551(9) Uiso 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
Fe1 C1 1.901(4) . ?
Fe1 C2 1.912(4) . ?
Fe1 N5 1.957(3) . ?
Fe1 N4 1.959(3) . ?
Fe1 N6 1.992(3) . ?
Fe1 N3 2.000(3) . ?
C1 N1 1.174(5) . ?
C2 N2 1.161(5) . ?
C3 N3 1.342(5) . ?
C3 C4 1.372(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.375(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.383(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.402(5) . ?
C6 H6A 0.9300 . ?
C7 N3 1.345(5) . ?
C7 C8 1.476(5) . ?
C8 N4 1.354(4) . ?
C8 C9 1.386(5) . ?
C9 C10 1.393(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.376(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.396(5) . ?
C11 H11A 0.9300 . ?
C12 N4 1.363(5) . ?
C12 H12A 0.9300 . ?
C13 N5 1.354(5) . ?
C13 C14 1.390(6) . ?
C13 H13A 0.9300 . ?
C14 C15 1.375(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.382(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.392(6) . ?
C16 H16A 0.9300 . ?
C17 N5 1.360(5) . ?
C17 C18 1.477(5) . ?
C18 N6 1.349(5) . ?
C18 C19 1.399(5) . ?
C19 C20 1.390(6) . ?
C19 H19A 0.9300 . ?
C20 C21 1.391(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.386(5) . ?
C21 H21A 0.9300 . ?
C22 N6 1.334(4) . ?
C22 H22A 0.9300 . ?

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
C1 Fe1 C2 88.57(16) . . ?
C1 Fe1 N5 90.38(14) . . ?
C2 Fe1 N5 94.25(15) . . ?
C1 Fe1 N4 94.40(14) . . ?
C2 Fe1 N4 89.48(14) . . ?
N5 Fe1 N4 174.01(12) . . ?
C1 Fe1 N6 91.12(15) . . ?
C2 Fe1 N6 175.17(15) . . ?
N5 Fe1 N6 80.93(13) . . ?
N4 Fe1 N6 95.35(12) . . ?
C1 Fe1 N3 174.27(15) . . ?
C2 Fe1 N3 88.59(15) . . ?
N5 Fe1 N3 94.79(13) . . ?
N4 Fe1 N3 80.60(12) . . ?
N6 Fe1 N3 92.13(13) . . ?
N1 C1 Fe1 178.8(3) . . ?
N2 C2 Fe1 178.7(3) . . ?
N3 C3 C4 123.1(4) . . ?
N3 C3 H3A 118.4 . . ?
C4 C3 H3A 118.4 . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
C5 C6 C7 118.6(4) . . ?
C5 C6 H6A 120.7 . . ?
C7 C6 H6A 120.7 . . ?
N3 C7 C6 122.2(4) . . ?
N3 C7 C8 114.4(3) . . ?
C6 C7 C8 123.4(3) . . ?
N4 C8 C9 123.0(3) . . ?
N4 C8 C7 113.0(3) . . ?
C9 C8 C7 124.0(3) . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
C11 C10 C9 119.0(4) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
C10 C11 C12 119.3(4) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
N4 C12 C11 122.3(3) . . ?
N4 C12 H12A 118.9 . . ?
C11 C12 H12A 118.9 . . ?
N5 C13 C14 123.0(4) . . ?
N5 C13 H13A 118.5 . . ?
C14 C13 H13A 118.5 . . ?
C15 C14 C13 119.3(4) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 119.0(4) . . ?
C14 C15 H15A 120.5 . . ?
C16 C15 H15A 120.5 . . ?
C15 C16 C17 119.0(4) . . ?
C15 C16 H16A 120.5 . . ?
C17 C16 H16A 120.5 . . ?
N5 C17 C16 123.0(3) . . ?
N5 C17 C18 113.0(3) . . ?
C16 C17 C18 124.0(4) . . ?
N6 C18 C19 122.4(4) . . ?
N6 C18 C17 114.3(3) . . ?
C19 C18 C17 123.3(4) . . ?
C20 C19 C18 119.1(4) . . ?
C20 C19 H19A 120.4 . . ?
C18 C19 H19A 120.4 . . ?
C19 C20 C21 117.9(4) . . ?
C19 C20 H20A 121.0 . . ?
C21 C20 H20A 121.0 . . ?
C22 C21 C20 119.5(4) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
N6 C22 C21 123.0(4) . . ?
N6 C22 H22A 118.5 . . ?
C21 C22 H22A 118.5 . . ?
C3 N3 C7 117.8(3) . . ?
C3 N3 Fe1 127.4(3) . . ?
C7 N3 Fe1 114.6(2) . . ?
C8 N4 C12 117.4(3) . . ?
C8 N4 Fe1 116.5(3) . . ?
C12 N4 Fe1 126.0(2) . . ?
C13 N5 C17 116.7(3) . . ?
C13 N5 Fe1 126.7(3) . . ?
C17 N5 Fe1 116.6(2) . . ?
C22 N6 C18 118.0(3) . . ?
C22 N6 Fe1 126.9(3) . . ?
C18 N6 Fe1 115.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.611
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 1015599'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H16 N6 O7 Os'
_chemical_formula_weight         666.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   26.832(3)
_cell_length_b                   14.7225(10)
_cell_length_c                   14.7702(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.366(5)
_cell_angle_gamma                90.00
_cell_volume                     5395.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9046
_cell_measurement_theta_min      2.3975
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       prism
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.135
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2576
_exptl_absorpt_coefficient_mu    4.775
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7602
_exptl_absorpt_process_details   'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18205
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5880
_reflns_number_gt                5617
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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)+(0.1126P)²+66.0054P] 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         5880
_refine_ls_number_parameters     325
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1664
_refine_ls_wR_factor_gt          0.1642
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.360929(8) -0.112499(14) 0.949574(16) 0.01395(13) Uani 1 1 d . . .
C1 C 0.2862(3) -0.0708(5) 0.8670(5) 0.0266(14) Uani 1 1 d . . .
C2 C 0.3805(3) -0.1161(4) 0.8327(5) 0.0167(13) Uani 1 1 d . . .
C3 C 0.4624(3) -0.2227(5) 1.0723(5) 0.0222(12) Uani 1 1 d . . .
H3A H 0.4417 -0.2734 1.0438 0.027 Uiso 1 1 calc R . .
C4 C 0.5137(3) -0.2360(5) 1.1394(6) 0.0294(15) Uani 1 1 d . . .
H4A H 0.5271 -0.2945 1.1563 0.035 Uiso 1 1 calc R . .
C5 C 0.5454(3) -0.1614(5) 1.1817(6) 0.0281(15) Uani 1 1 d . . .
H5A H 0.5803 -0.1691 1.2272 0.034 Uiso 1 1 calc R . .
C6 C 0.5242(3) -0.0749(5) 1.1549(5) 0.0260(14) Uani 1 1 d . . .
H6A H 0.5448 -0.0238 1.1823 0.031 Uiso 1 1 calc R . .
C7 C 0.4717(3) -0.0657(4) 1.0867(4) 0.0187(12) Uani 1 1 d . . .
C8 C 0.4443(3) 0.0218(4) 1.0545(5) 0.0207(12) Uani 1 1 d . . .
C9 C 0.4693(4) 0.1055(5) 1.0854(7) 0.0294(18) Uani 1 1 d . . .
H9A H 0.5051 0.1080 1.1284 0.035 Uiso 1 1 calc R . .
C10 C 0.4404(4) 0.1851(5) 1.0515(6) 0.0337(17) Uani 1 1 d . . .
H10A H 0.4566 0.2415 1.0707 0.040 Uiso 1 1 calc R . .
C11 C 0.3875(4) 0.1791(5) 0.9892(6) 0.0337(16) Uani 1 1 d . . .
H11A H 0.3671 0.2314 0.9667 0.040 Uiso 1 1 calc R . .
C12 C 0.3648(3) 0.0950(6) 0.9604(5) 0.0237(14) Uani 1 1 d . . .
H12A H 0.3288 0.0919 0.9182 0.028 Uiso 1 1 calc R . .
C22 C 0.3343(3) -0.0632(5) 1.1304(5) 0.0231(13) Uani 1 1 d . . .
H22A H 0.3438 -0.0042 1.1215 0.028 Uiso 1 1 calc R . .
C21 C 0.3173(3) -0.0806(5) 1.2057(5) 0.0264(14) Uani 1 1 d . . .
H21A H 0.3163 -0.0339 1.2474 0.032 Uiso 1 1 calc R . .
C20 C 0.3019(3) -0.1668(6) 1.2193(5) 0.0287(15) Uani 1 1 d . . .
H20A H 0.2898 -0.1790 1.2693 0.034 Uiso 1 1 calc R . .
C19 C 0.3048(3) -0.2355(5) 1.1571(5) 0.0261(14) Uani 1 1 d . . .
H19A H 0.2954 -0.2947 1.1659 0.031 Uiso 1 1 calc R . .
C18 C 0.3220(2) -0.2151(4) 1.0808(5) 0.0194(12) Uani 1 1 d . . .
C17 C 0.3244(2) -0.2818(4) 1.0086(5) 0.0206(12) Uani 1 1 d . . .
C16 C 0.3137(3) -0.3740(5) 1.0136(6) 0.0286(16) Uani 1 1 d . . .
H16A H 0.3058 -0.3967 1.0653 0.034 Uiso 1 1 calc R . .
C15 C 0.3153(3) -0.4309(5) 0.9405(6) 0.0323(16) Uani 1 1 d . . .
H15A H 0.3085 -0.4927 0.9424 0.039 Uiso 1 1 calc R . .
C14 C 0.3270(3) -0.3950(5) 0.8640(7) 0.0301(17) Uani 1 1 d . . .
H14A H 0.3268 -0.4319 0.8128 0.036 Uiso 1 1 calc R . .
C13 C 0.3388(3) -0.3045(4) 0.8650(5) 0.0239(13) Uani 1 1 d . . .
H13A H 0.3478 -0.2813 0.8146 0.029 Uiso 1 1 calc R . .
N1 N 0.2441(3) -0.0414(6) 0.8264(6) 0.051(2) Uani 1 1 d . . .
N2 N 0.3913(3) -0.1251(4) 0.7641(5) 0.0264(13) Uani 1 1 d . . .
N3 N 0.4407(2) -0.1404(4) 1.0460(4) 0.0175(10) Uani 1 1 d . . .
N4 N 0.3924(2) 0.0163(3) 0.9905(4) 0.0176(10) Uani 1 1 d . . .
N6 N 0.3376(2) -0.1298(4) 1.0682(4) 0.0167(10) Uani 1 1 d . . .
N5 N 0.3379(2) -0.2471(4) 0.9364(4) 0.0186(10) Uani 1 1 d . . .
O1 O 0.0493(2) 0.2085(4) 0.7371(4) 0.0343(12) Uani 1 1 d . . .
O2 O 0.2183(4) -0.1280(7) 0.4183(7) 0.077(3) Uani 1 1 d . . .
O3 O 0.0314(5) 0.1083(5) 0.5674(8) 0.077(3) Uani 1 1 d . . .
O4 O 0.1063(5) 0.0914(7) 0.8831(9) 0.091(3) Uani 1 1 d U . .
O5 O 0.4293(5) 0.4366(8) 0.9621(10) 0.105(4) Uani 1 1 d U . .
O6 O 0.3053(6) 0.3642(10) 0.8494(11) 0.124(5) Uani 1 1 d U . .
O7 O 0.2148(5) 0.3149(8) 0.8901(7) 0.104(4) 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
Os1 C2 1.987(8) . ?
Os1 C1 2.006(7) . ?
Os1 N5 2.064(5) . ?
Os1 N4 2.069(5) . ?
Os1 N6 2.089(6) . ?
Os1 N3 2.112(5) . ?
C1 N1 1.143(10) . ?
C2 N2 1.163(11) . ?
C3 N3 1.337(8) . ?
C3 C4 1.371(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.390(11) . ?
C5 H5A 0.9300 . ?
C6 C7 1.392(9) . ?
C6 H6A 0.9300 . ?
C7 N3 1.371(8) . ?
C7 C8 1.469(9) . ?
C8 N4 1.356(8) . ?
C8 C9 1.393(9) . ?
C9 C10 1.391(12) . ?
C9 H9A 0.9300 . ?
C10 C11 1.368(13) . ?
C10 H10A 0.9300 . ?
C11 C12 1.374(11) . ?
C11 H11A 0.9300 . ?
C12 N4 1.356(9) . ?
C12 H12A 0.9300 . ?
C22 N6 1.369(9) . ?
C22 C21 1.377(9) . ?
C22 H22A 0.9300 . ?
C21 C20 1.373(11) . ?
C21 H21A 0.9300 . ?
C20 C19 1.388(11) . ?
C20 H20A 0.9300 . ?
C19 C18 1.402(9) . ?
C19 H19A 0.9300 . ?
C18 N6 1.360(8) . ?
C18 C17 1.470(9) . ?
C17 N5 1.349(8) . ?
C17 C16 1.395(10) . ?
C16 C15 1.380(12) . ?
C16 H16A 0.9300 . ?
C15 C14 1.388(12) . ?
C15 H15A 0.9300 . ?
C14 C13 1.368(9) . ?
C14 H14A 0.9300 . ?
C13 N5 1.359(8) . ?
C13 H13A 0.9300 . ?

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
C2 Os1 C1 90.8(3) . . ?
C2 Os1 N5 93.5(2) . . ?
C1 Os1 N5 92.4(2) . . ?
C2 Os1 N4 93.7(2) . . ?
C1 Os1 N4 95.7(3) . . ?
N5 Os1 N4 169.0(2) . . ?
C2 Os1 N6 171.2(2) . . ?
C1 Os1 N6 89.8(2) . . ?
N5 Os1 N6 77.7(2) . . ?
N4 Os1 N6 94.9(2) . . ?
C2 Os1 N3 92.6(2) . . ?
C1 Os1 N3 172.7(3) . . ?
N5 Os1 N3 93.9(2) . . ?
N4 Os1 N3 77.6(2) . . ?
N6 Os1 N3 87.8(2) . . ?
N1 C1 Os1 173.8(8) . . ?
N2 C2 Os1 175.0(5) . . ?
N3 C3 C4 123.1(6) . . ?
N3 C3 H3A 118.4 . . ?
C4 C3 H3A 118.4 . . ?
C3 C4 C5 119.2(7) . . ?
C3 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
C4 C5 C6 119.0(7) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
C5 C6 C7 119.1(6) . . ?
C5 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 . . ?
N3 C7 C6 121.1(6) . . ?
N3 C7 C8 114.6(6) . . ?
C6 C7 C8 124.3(6) . . ?
N4 C8 C9 121.3(7) . . ?
N4 C8 C7 115.3(5) . . ?
C9 C8 C7 123.4(7) . . ?
C10 C9 C8 119.7(8) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C11 C10 C9 118.7(7) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
C10 C11 C12 119.4(7) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
N4 C12 C11 123.1(7) . . ?
N4 C12 H12A 118.4 . . ?
C11 C12 H12A 118.4 . . ?
N6 C22 C21 122.4(7) . . ?
N6 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
C20 C21 C22 120.0(7) . . ?
C20 C21 H21A 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C21 C20 C19 118.8(6) . . ?
C21 C20 H20A 120.6 . . ?
C19 C20 H20A 120.6 . . ?
C20 C19 C18 119.6(6) . . ?
C20 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
N6 C18 C19 121.4(6) . . ?
N6 C18 C17 114.6(5) . . ?
C19 C18 C17 124.0(6) . . ?
N5 C17 C16 122.2(6) . . ?
N5 C17 C18 114.8(5) . . ?
C16 C17 C18 123.0(6) . . ?
C15 C16 C17 118.8(7) . . ?
C15 C16 H16A 120.6 . . ?
C17 C16 H16A 120.6 . . ?
C16 C15 C14 119.2(7) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
C13 C14 C15 119.1(7) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
N5 C13 C14 122.7(7) . . ?
N5 C13 H13A 118.6 . . ?
C14 C13 H13A 118.6 . . ?
C3 N3 C7 118.4(6) . . ?
C3 N3 Os1 126.2(4) . . ?
C7 N3 Os1 115.4(4) . . ?
C12 N4 C8 117.7(6) . . ?
C12 N4 Os1 125.2(5) . . ?
C8 N4 Os1 117.1(4) . . ?
C18 N6 C22 117.8(6) . . ?
C18 N6 Os1 115.7(4) . . ?
C22 N6 Os1 126.3(5) . . ?
C17 N5 C13 117.9(6) . . ?
C17 N5 Os1 116.7(4) . . ?
C13 N5 Os1 125.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         3.527
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.263
_database_code_depnum_ccdc_archive 'CCDC 1015600'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H40 F6 Fe2 N10 O4 P'
_chemical_formula_weight         1017.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   16.088(8)
_cell_length_b                   13.258(6)
_cell_length_c                   21.990(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.196(9)
_cell_angle_gamma                90.00
_cell_volume                     4456(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    13155
_cell_measurement_theta_min      2.0639
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2084
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8825
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55592
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7825
_reflns_number_gt                4989
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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. 
The atoms of c24  c25 c26 c27 c39 c41 f5 c28 and f2 are abnormal, 
so the following least-squares restraint is used in the refinement, isor 
0.01 c24 c25 c26 c27 c39 c41 f5 c28 f2.
 The Delta(F^2)/esd of the Most Disagreeable Reflections is too strong, so 
these points and the points in low angles are omited in the refinement.
omit -2 50
omit -1 1 1
omit -1 1 2
omit -3 1 1
omit -4 1 2
omit  0 2 4



;

_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)+(0.1299P)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_number_reflns         7825
_refine_ls_number_parameters     595
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.2429
_refine_ls_wR_factor_gt          0.2127
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.053
_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 0.76947(5) 0.60040(6) 0.08703(3) 0.0461(3) Uani 1 1 d . . .
Fe2 Fe 0.72291(5) 0.29735(6) 0.21151(4) 0.0471(3) Uani 1 1 d . . .
C1 C 0.7398(4) 0.4803(4) 0.1194(3) 0.0484(14) Uani 1 1 d . . .
C2 C 0.7712(4) 0.6625(4) 0.1647(3) 0.0464(13) Uani 1 1 d . . .
C3 C 0.7620(4) 0.8034(5) 0.0242(3) 0.0656(18) Uani 1 1 d . . .
H3A H 0.7016 0.7949 0.0091 0.079 Uiso 1 1 calc R . .
C4 C 0.7973(5) 0.8912(5) 0.0097(4) 0.077(2) Uani 1 1 d . . .
H4A H 0.7613 0.9405 -0.0152 0.092 Uiso 1 1 calc R . .
C5 C 0.8860(5) 0.9054(5) 0.0321(4) 0.085(2) Uani 1 1 d . . .
H5A H 0.9112 0.9639 0.0225 0.101 Uiso 1 1 calc R . .
C6 C 0.9366(5) 0.8313(5) 0.0690(4) 0.0725(19) Uani 1 1 d . . .
H6A H 0.9968 0.8402 0.0854 0.087 Uiso 1 1 calc R . .
C7 C 0.8993(4) 0.7438(5) 0.0819(3) 0.0570(15) Uani 1 1 d . . .
C8 C 0.9464(4) 0.6585(5) 0.1224(3) 0.0534(15) Uani 1 1 d . . .
C9 C 1.0362(4) 0.6602(6) 0.1533(3) 0.0671(18) Uani 1 1 d . . .
H9A H 1.0698 0.7161 0.1507 0.081 Uiso 1 1 calc R . .
C10 C 1.0751(5) 0.5731(6) 0.1893(3) 0.075(2) Uani 1 1 d . . .
H10A H 1.1347 0.5716 0.2115 0.090 Uiso 1 1 calc R . .
C11 C 1.0231(5) 0.4919(5) 0.1904(3) 0.0670(18) Uani 1 1 d . . .
H11A H 1.0473 0.4338 0.2127 0.080 Uiso 1 1 calc R . .
C12 C 0.9354(4) 0.4967(5) 0.1585(3) 0.0618(17) Uani 1 1 d . . .
H12A H 0.9010 0.4412 0.1604 0.074 Uiso 1 1 calc R . .
C13 C 0.5878(4) 0.6711(5) 0.0707(4) 0.0684(18) Uani 1 1 d . . .
H13A H 0.6096 0.6937 0.1127 0.082 Uiso 1 1 calc R . .
C14 C 0.5009(5) 0.6844(5) 0.0398(4) 0.072(2) Uani 1 1 d . . .
H14A H 0.4663 0.7182 0.0601 0.086 Uiso 1 1 calc R . .
C15 C 0.4648(5) 0.6485(6) -0.0204(4) 0.077(2) Uani 1 1 d . . .
H15A H 0.4051 0.6547 -0.0416 0.092 Uiso 1 1 calc R . .
C16 C 0.5189(5) 0.6029(5) -0.0490(3) 0.070(2) Uani 1 1 d . . .
H16A H 0.4965 0.5789 -0.0907 0.084 Uiso 1 1 calc R . .
C17 C 0.6089(4) 0.5920(5) -0.0156(3) 0.0603(17) Uani 1 1 d . . .
C18 C 0.6753(5) 0.5428(5) -0.0411(3) 0.0633(18) Uani 1 1 d . . .
C19 C 0.6555(6) 0.5034(6) -0.1015(4) 0.084(2) Uani 1 1 d . . .
H19A H 0.5991 0.5069 -0.1301 0.101 Uiso 1 1 calc R . .
C20 C 0.7210(6) 0.4592(7) -0.1179(4) 0.097(3) Uani 1 1 d . . .
H20A H 0.7096 0.4330 -0.1589 0.116 Uiso 1 1 calc R . .
C21 C 0.8049(7) 0.4519(7) -0.0750(4) 0.103(3) Uani 1 1 d . . .
H21A H 0.8498 0.4211 -0.0864 0.124 Uiso 1 1 calc R . .
C22 C 0.8192(5) 0.4930(5) -0.0132(3) 0.0708(19) Uani 1 1 d . . .
H22A H 0.8746 0.4878 0.0167 0.085 Uiso 1 1 calc R . .
C23 C 0.9124(4) 0.2522(5) 0.2374(4) 0.076(2) Uani 1 1 d . . .
C24 C 0.9752(5) 0.1922(6) 0.2206(5) 0.100(3) Uani 1 1 d U . .
H24A H 0.9567 0.1461 0.1873 0.119 Uiso 1 1 calc R . .
C25 C 1.0662(6) 0.2020(8) 0.2543(6) 0.119(3) Uani 1 1 d U . .
H25A H 1.1070 0.1647 0.2418 0.143 Uiso 1 1 calc R . .
C26 C 1.0914(7) 0.2634(9) 0.3025(6) 0.122(4) Uani 1 1 d U . .
H26A H 1.1507 0.2665 0.3254 0.147 Uiso 1 1 calc R . .
C27 C 1.0331(6) 0.3254(7) 0.3215(5) 0.110(3) Uani 1 1 d U . .
H27A H 1.0540 0.3687 0.3562 0.132 Uiso 1 1 calc R . .
C28 C 0.9414(5) 0.3217(6) 0.2871(4) 0.088(3) Uani 1 1 d U . .
C29 C 0.8858(6) 0.3891(6) 0.3078(4) 0.084(3) Uani 1 1 d . . .
H29A H 0.9130 0.4325 0.3414 0.101 Uiso 1 1 calc R . .
C30 C 0.7529(6) 0.4637(6) 0.3120(4) 0.098(3) Uani 1 1 d . . .
H30A H 0.7477 0.4347 0.3512 0.118 Uiso 1 1 calc R . .
H30B H 0.7844 0.5270 0.3228 0.118 Uiso 1 1 calc R . .
C31 C 0.6674(6) 0.4824(6) 0.2684(4) 0.095(3) Uani 1 1 d . . .
H31A H 0.6708 0.5315 0.2366 0.114 Uiso 1 1 calc R . .
H31B H 0.6298 0.5095 0.2914 0.114 Uiso 1 1 calc R . .
C32 C 0.5514(5) 0.3623(5) 0.2301(3) 0.0666(18) Uani 1 1 d . . .
H32A H 0.5192 0.4021 0.2494 0.080 Uiso 1 1 calc R . .
C33 C 0.5087(4) 0.2731(5) 0.1931(3) 0.0539(15) Uani 1 1 d . . .
C34 C 0.4216(4) 0.2538(6) 0.1905(3) 0.0687(19) Uani 1 1 d . . .
H34A H 0.3952 0.2963 0.2127 0.082 Uiso 1 1 calc R . .
C35 C 0.3747(5) 0.1757(6) 0.1570(4) 0.084(2) Uani 1 1 d . . .
H35A H 0.3177 0.1639 0.1569 0.101 Uiso 1 1 calc R . .
C36 C 0.4131(5) 0.1137(6) 0.1227(4) 0.086(3) Uani 1 1 d . . .
H36A H 0.3814 0.0600 0.0995 0.103 Uiso 1 1 calc R . .
C37 C 0.4979(4) 0.1301(5) 0.1225(3) 0.0654(18) Uani 1 1 d . . .
H37A H 0.5222 0.0882 0.0986 0.078 Uiso 1 1 calc R . .
C38 C 0.5474(4) 0.2094(4) 0.1578(3) 0.0521(15) Uani 1 1 d . . .
C39 C 0.2327(16) 0.830(2) 0.0511(13) 0.357(15) Uani 1 1 d U . .
H39A H 0.2842 0.8625 0.0786 0.536 Uiso 1 1 calc R . .
H39B H 0.2250 0.7661 0.0688 0.536 Uiso 1 1 calc R . .
H39C H 0.1826 0.8721 0.0475 0.536 Uiso 1 1 calc R . .
C40 C 0.3089(11) 0.8639(9) -0.0250(6) 0.128(4) Uani 1 1 d . . .
H40A H 0.3094 0.8591 -0.0671 0.153 Uiso 1 1 calc R . .
C41 C 0.1738(13) 0.7775(15) -0.0612(10) 0.249(9) Uani 1 1 d U . .
H41A H 0.1834 0.7749 -0.1021 0.373 Uiso 1 1 calc R . .
H41B H 0.1244 0.8200 -0.0640 0.373 Uiso 1 1 calc R . .
H41C H 0.1626 0.7108 -0.0487 0.373 Uiso 1 1 calc R . .
C42 C 1.1409(7) 0.2865(8) 0.1146(5) 0.123(4) Uani 1 1 d . . .
H42A H 1.1902 0.2955 0.0994 0.185 Uiso 1 1 calc R . .
H42B H 1.1338 0.2161 0.1220 0.185 Uiso 1 1 calc R . .
H42C H 1.1504 0.3230 0.1539 0.185 Uiso 1 1 calc R . .
C43 C 1.0645(7) 0.3231(8) 0.0683(5) 0.099(3) Uani 1 1 d . . .
N1 N 0.7224(3) 0.4070(4) 0.1419(2) 0.0552(13) Uani 1 1 d . . .
N2 N 0.7761(3) 0.7016(3) 0.2130(2) 0.0536(12) Uani 1 1 d . . .
N3 N 0.8121(3) 0.7287(3) 0.0596(2) 0.0512(12) Uani 1 1 d . . .
N4 N 0.8960(3) 0.5779(4) 0.1242(2) 0.0514(12) Uani 1 1 d . . .
N5 N 0.6432(3) 0.6285(4) 0.0455(2) 0.0553(13) Uani 1 1 d . . .
N6 N 0.7579(3) 0.5378(4) 0.0031(2) 0.0528(12) Uani 1 1 d . . .
N7 N 0.8014(4) 0.3956(4) 0.2844(3) 0.0695(17) Uani 1 1 d . . .
N8 N 0.6308(4) 0.3877(4) 0.2370(3) 0.0646(15) Uani 1 1 d . . .
N9 N 0.2432(8) 0.8142(9) -0.0186(5) 0.138(4) Uani 1 1 d . . .
N10 N 1.0046(6) 0.3535(8) 0.0319(5) 0.130(3) Uani 1 1 d . . .
O1 O 0.8287(3) 0.2396(3) 0.2034(2) 0.0674(12) Uani 1 1 d . . .
O2 O 0.6283(2) 0.2239(3) 0.15442(17) 0.0466(9) Uani 1 1 d . . .
O3 O 0.3678(7) 0.9128(7) 0.0046(6) 0.175(4) Uani 1 1 d . . .
O4 O 0.9281(9) 0.4243(11) 0.4561(6) 0.272(6) Uani 1 1 d . . .
P1 P 0.18368(15) 0.9573(2) 0.17925(14) 0.1055(9) Uani 1 1 d . . .
F1 F 0.1012(4) 0.9537(6) 0.2022(4) 0.174(3) Uani 1 1 d . . .
F2 F 0.2436(5) 0.9242(7) 0.2463(4) 0.204(4) Uani 1 1 d U . .
F3 F 0.1284(4) 1.0053(6) 0.1170(3) 0.167(3) Uani 1 1 d . . .
F4 F 0.1684(4) 0.8460(5) 0.1569(4) 0.161(3) Uani 1 1 d . . .
F5 F 0.2673(4) 0.9627(5) 0.1565(4) 0.165(3) Uani 1 1 d U . .
F6 F 0.2056(4) 1.0699(5) 0.2084(4) 0.148(2) 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
Fe1 C1 1.867(6) . ?
Fe1 C2 1.889(6) . ?
Fe1 N4 1.965(5) . ?
Fe1 N6 1.978(5) . ?
Fe1 N5 1.985(5) . ?
Fe1 N3 1.996(5) . ?
Fe2 O2 1.911(4) . ?
Fe2 O1 1.924(5) . ?
Fe2 N2 2.086(5) 2_645 ?
Fe2 N1 2.109(5) . ?
Fe2 N8 2.113(6) . ?
Fe2 N7 2.144(5) . ?
C1 N1 1.163(7) . ?
C2 N2 1.162(7) . ?
C3 N3 1.359(7) . ?
C3 C4 1.376(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.369(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.368(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.377(9) . ?
C6 H6A 0.9300 . ?
C7 N3 1.349(8) . ?
C7 C8 1.492(9) . ?
C8 N4 1.348(7) . ?
C8 C9 1.392(9) . ?
C9 C10 1.428(10) . ?
C9 H9A 0.9300 . ?
C10 C11 1.368(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.368(9) . ?
C11 H11A 0.9300 . ?
C12 N4 1.353(8) . ?
C12 H12A 0.9300 . ?
C13 N5 1.315(8) . ?
C13 C14 1.362(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.357(10) . ?
C14 H14A 0.9300 . ?
C15 C16 1.365(10) . ?
C15 H15A 0.9300 . ?
C16 C17 1.411(9) . ?
C16 H16A 0.9300 . ?
C17 N5 1.370(8) . ?
C17 C18 1.504(10) . ?
C18 C19 1.369(10) . ?
C18 N6 1.382(8) . ?
C19 C20 1.348(12) . ?
C19 H19A 0.9300 . ?
C20 C21 1.388(12) . ?
C20 H20A 0.9300 . ?
C21 C22 1.414(10) . ?
C21 H21A 0.9300 . ?
C22 N6 1.294(8) . ?
C22 H22A 0.9300 . ?
C23 O1 1.331(8) . ?
C23 C28 1.395(12) . ?
C23 C24 1.422(11) . ?
C24 C25 1.425(12) . ?
C24 H24A 0.9300 . ?
C25 C26 1.297(15) . ?
C25 H25A 0.9300 . ?
C26 C27 1.407(15) . ?
C26 H26A 0.9300 . ?
C27 C28 1.434(11) . ?
C27 H27A 0.9300 . ?
C28 C29 1.436(12) . ?
C29 N7 1.296(9) . ?
C29 H29A 0.9300 . ?
C30 C31 1.432(11) . ?
C30 N7 1.445(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 N8 1.465(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 N8 1.283(8) . ?
C32 C33 1.478(9) . ?
C32 H32A 0.9300 . ?
C33 C34 1.407(9) . ?
C33 C38 1.416(9) . ?
C34 C35 1.356(11) . ?
C34 H34A 0.9300 . ?
C35 C36 1.383(11) . ?
C35 H35A 0.9300 . ?
C36 C37 1.383(9) . ?
C36 H36A 0.9300 . ?
C37 C38 1.399(8) . ?
C37 H37A 0.9300 . ?
C38 O2 1.341(7) . ?
C39 N9 1.61(3) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 O3 1.164(14) . ?
C40 N9 1.290(15) . ?
C40 H40A 0.9300 . ?
C41 N9 1.306(18) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.414(12) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 N10 1.119(11) . ?
N2 Fe2 2.086(5) 2_655 ?
P1 F3 1.520(6) . ?
P1 F4 1.551(7) . ?
P1 F2 1.552(8) . ?
P1 F1 1.561(6) . ?
P1 F5 1.576(7) . ?
P1 F6 1.619(7) . ?

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
C1 Fe1 C2 87.7(2) . . ?
C1 Fe1 N4 93.8(2) . . ?
C2 Fe1 N4 88.2(2) . . ?
C1 Fe1 N6 92.1(2) . . ?
C2 Fe1 N6 175.6(2) . . ?
N4 Fe1 N6 96.2(2) . . ?
C1 Fe1 N5 89.3(2) . . ?
C2 Fe1 N5 93.4(2) . . ?
N4 Fe1 N5 176.5(2) . . ?
N6 Fe1 N5 82.2(2) . . ?
C1 Fe1 N3 174.4(2) . . ?
C2 Fe1 N3 89.6(2) . . ?
N4 Fe1 N3 81.2(2) . . ?
N6 Fe1 N3 91.0(2) . . ?
N5 Fe1 N3 95.7(2) . . ?
O2 Fe2 O1 106.42(19) . . ?
O2 Fe2 N2 91.09(17) . 2_645 ?
O1 Fe2 N2 92.5(2) . 2_645 ?
O2 Fe2 N1 93.02(17) . . ?
O1 Fe2 N1 90.6(2) . . ?
N2 Fe2 N1 173.94(19) 2_645 . ?
O2 Fe2 N8 88.99(19) . . ?
O1 Fe2 N8 164.6(2) . . ?
N2 Fe2 N8 88.1(2) 2_645 . ?
N1 Fe2 N8 87.6(2) . . ?
O2 Fe2 N7 164.5(2) . . ?
O1 Fe2 N7 88.8(2) . . ?
N2 Fe2 N7 85.30(19) 2_645 . ?
N1 Fe2 N7 89.56(19) . . ?
N8 Fe2 N7 75.8(2) . . ?
N1 C1 Fe1 177.4(5) . . ?
N2 C2 Fe1 177.1(5) . . ?
N3 C3 C4 122.4(6) . . ?
N3 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C6 C5 C4 118.4(6) . . ?
C6 C5 H5A 120.8 . . ?
C4 C5 H5A 120.8 . . ?
C5 C6 C7 120.7(7) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
N3 C7 C6 121.4(6) . . ?
N3 C7 C8 112.4(5) . . ?
C6 C7 C8 126.2(6) . . ?
N4 C8 C9 122.7(6) . . ?
N4 C8 C7 114.9(5) . . ?
C9 C8 C7 122.4(6) . . ?
C8 C9 C10 117.8(7) . . ?
C8 C9 H9A 121.1 . . ?
C10 C9 H9A 121.1 . . ?
C11 C10 C9 118.8(6) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
N4 C12 C11 123.5(7) . . ?
N4 C12 H12A 118.2 . . ?
C11 C12 H12A 118.2 . . ?
N5 C13 C14 124.8(7) . . ?
N5 C13 H13A 117.6 . . ?
C14 C13 H13A 117.6 . . ?
C15 C14 C13 120.1(8) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C14 C15 C16 117.7(7) . . ?
C14 C15 H15A 121.1 . . ?
C16 C15 H15A 121.1 . . ?
C15 C16 C17 120.2(7) . . ?
C15 C16 H16A 119.9 . . ?
C17 C16 H16A 119.9 . . ?
N5 C17 C16 120.6(7) . . ?
N5 C17 C18 113.8(6) . . ?
C16 C17 C18 125.6(6) . . ?
C19 C18 N6 123.1(8) . . ?
C19 C18 C17 123.5(7) . . ?
N6 C18 C17 113.4(5) . . ?
C20 C19 C18 117.4(8) . . ?
C20 C19 H19A 121.3 . . ?
C18 C19 H19A 121.3 . . ?
C19 C20 C21 121.6(8) . . ?
C19 C20 H20A 119.2 . . ?
C21 C20 H20A 119.2 . . ?
C20 C21 C22 117.3(9) . . ?
C20 C21 H21A 121.4 . . ?
C22 C21 H21A 121.4 . . ?
N6 C22 C21 122.2(8) . . ?
N6 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
O1 C23 C28 123.7(7) . . ?
O1 C23 C24 117.5(8) . . ?
C28 C23 C24 118.8(8) . . ?
C23 C24 C25 120.9(10) . . ?
C23 C24 H24A 119.6 . . ?
C25 C24 H24A 119.6 . . ?
C26 C25 C24 119.4(12) . . ?
C26 C25 H25A 120.3 . . ?
C24 C25 H25A 120.3 . . ?
C25 C26 C27 122.9(11) . . ?
C25 C26 H26A 118.6 . . ?
C27 C26 H26A 118.6 . . ?
C26 C27 C28 119.7(10) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
C23 C28 C27 118.3(10) . . ?
C23 C28 C29 124.8(7) . . ?
C27 C28 C29 116.9(9) . . ?
N7 C29 C28 126.5(7) . . ?
N7 C29 H29A 116.7 . . ?
C28 C29 H29A 116.7 . . ?
C31 C30 N7 111.0(6) . . ?
C31 C30 H30A 109.4 . . ?
N7 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
N7 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C30 C31 N8 109.1(6) . . ?
C30 C31 H31A 109.9 . . ?
N8 C31 H31A 109.9 . . ?
C30 C31 H31B 109.9 . . ?
N8 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
N8 C32 C33 123.4(6) . . ?
N8 C32 H32A 118.3 . . ?
C33 C32 H32A 118.3 . . ?
C34 C33 C38 118.1(6) . . ?
C34 C33 C32 117.0(6) . . ?
C38 C33 C32 124.8(6) . . ?
C35 C34 C33 122.5(7) . . ?
C35 C34 H34A 118.7 . . ?
C33 C34 H34A 118.7 . . ?
C34 C35 C36 118.9(7) . . ?
C34 C35 H35A 120.5 . . ?
C36 C35 H35A 120.5 . . ?
C37 C36 C35 121.1(7) . . ?
C37 C36 H36A 119.4 . . ?
C35 C36 H36A 119.4 . . ?
C36 C37 C38 120.5(7) . . ?
C36 C37 H37A 119.8 . . ?
C38 C37 H37A 119.8 . . ?
O2 C38 C37 118.0(6) . . ?
O2 C38 C33 123.1(5) . . ?
C37 C38 C33 118.8(6) . . ?
N9 C39 H39A 109.5 . . ?
N9 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N9 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O3 C40 N9 140.9(16) . . ?
O3 C40 H40A 109.6 . . ?
N9 C40 H40A 109.6 . . ?
N9 C41 H41A 109.5 . . ?
N9 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N9 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C43 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N10 C43 C42 178.9(14) . . ?
C1 N1 Fe2 159.6(5) . . ?
C2 N2 Fe2 168.6(4) . 2_655 ?
C7 N3 C3 117.6(5) . . ?
C7 N3 Fe1 115.6(4) . . ?
C3 N3 Fe1 126.6(4) . . ?
C8 N4 C12 117.7(5) . . ?
C8 N4 Fe1 114.9(4) . . ?
C12 N4 Fe1 126.7(5) . . ?
C13 N5 C17 116.5(6) . . ?
C13 N5 Fe1 128.1(4) . . ?
C17 N5 Fe1 115.2(5) . . ?
C22 N6 C18 118.3(6) . . ?
C22 N6 Fe1 126.4(4) . . ?
C18 N6 Fe1 115.2(5) . . ?
C29 N7 C30 120.7(7) . . ?
C29 N7 Fe2 123.8(6) . . ?
C30 N7 Fe2 115.1(5) . . ?
C32 N8 C31 121.3(6) . . ?
C32 N8 Fe2 125.1(5) . . ?
C31 N8 Fe2 113.5(5) . . ?
C40 N9 C41 131.2(15) . . ?
C40 N9 C39 111.6(14) . . ?
C41 N9 C39 114.3(16) . . ?
C23 O1 Fe2 131.9(5) . . ?
C38 O2 Fe2 128.6(4) . . ?
F3 P1 F4 97.0(5) . . ?
F3 P1 F2 171.7(5) . . ?
F4 P1 F2 91.3(5) . . ?
F3 P1 F1 89.2(4) . . ?
F4 P1 F1 90.4(4) . . ?
F2 P1 F1 91.3(5) . . ?
F3 P1 F5 90.8(4) . . ?
F4 P1 F5 90.5(4) . . ?
F2 P1 F5 88.6(5) . . ?
F1 P1 F5 179.1(5) . . ?
F3 P1 F6 88.0(4) . . ?
F4 P1 F6 175.0(4) . . ?
F2 P1 F6 83.7(4) . . ?
F1 P1 F6 90.1(4) . . ?
F5 P1 F6 89.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.086
_database_code_depnum_ccdc_archive 'CCDC 1015601'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H44 F6 Fe2 N10 O5 P'
_chemical_formula_weight         1097.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   16.747(7)
_cell_length_b                   13.494(5)
_cell_length_c                   22.504(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.667(7)
_cell_angle_gamma                90.00
_cell_volume                     4897(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9103
_cell_measurement_theta_min      3.2726
_cell_measurement_theta_max      27.5555

_exptl_crystal_description       Prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2500
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2252
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_process_details   'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37512
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         27.50
_reflns_number_total             11222
_reflns_number_gt                7108
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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. 
The atoms of f2a f4a f3a and f5 are abnormal, so the following least-squares
 restraint is used in the refinement, isor 0.01 f2a f4a f3a f5.
 The C34-C36 (f1-f4) group is disorder, so the following process is used in the refinement. 
PART   1
C34A  1   0.68741   0.05814  -0.19277  21.00000   0.09299   0.05825 =
       0.05944   0.01993   0.01700  -0.00460
AFIX  23
H34A  2   0.64943   0.00608  -0.18844  21.00000  -1.20000
H34B  2   0.70275   0.09611  -0.15478  21.00000  -1.20000
AFIX   0
PART   2
C34B  1   0.68036   0.02245  -0.22190 -21.00000   0.08289   0.05321 =
       0.07329   0.01630   0.02480  -0.01333
AFIX  23
H34C  2   0.64829  -0.00527  -0.19588 -21.00000  -1.20000
H34D  2   0.67888  -0.02304  -0.25555 -21.00000  -1.20000
AFIX   0
PART   1
C35A  1   0.76486   0.01341  -0.20651  21.00000   0.10033   0.03368 =
       0.07924   0.00856   0.02302   0.01338
AFIX  23
H35A  2   0.79953  -0.01943  -0.17034  21.00000  -1.20000
H35B  2   0.74963  -0.03395  -0.24011  21.00000  -1.20000
AFIX   0
PART   2
C35B  1   0.76486   0.04214  -0.18666 -21.00000   0.08183   0.03242 =
       0.07638   0.02563   0.02229   0.02015
AFIX  23
H35C  2   0.79374  -0.01997  -0.17434 -21.00000  -1.20000
H35D  2   0.76475   0.07879  -0.14960 -21.00000  -1.20000
AFIX   0
PART   0
PART   1
F1    9   0.47453   0.05201   0.20417  21.00000   0.15762   0.17186 =
       0.18671  -0.04014   0.05670  -0.00597
F2    9   0.45022   0.13613   0.27082  21.00000   0.11972   0.17342 =
       0.15172  -0.01998   0.04683   0.00934
F3    9   0.47734   0.23430   0.20896  21.00000   0.19065   0.17020 =
       0.16215   0.00496   0.00063   0.03513
PART   2
F1A   9   0.46143   0.21779   0.25969 -21.00000   0.18603   0.18732 =
       0.24288  -0.00614   0.08876   0.04925
F2A   9   0.47136   0.12255   0.18538 -21.00000   0.11138   0.14796 =
       0.12812   0.02135   0.00611   0.00715
F3A   9   0.46458   0.03744   0.26074 -21.00000   0.17238   0.16711 =
       0.16234   0.03770   0.01918  -0.04755
PART   0
The bond lengths of P-F group in hexafluorophosphate anion p1(f1f2f3f4f5f6)and 
p1(f1af2af3af4a) are abnormal, so the following process is used in the refinement. 
dfix 1.58 0.01 p1 f1 p1 f2 p1 f3 p1 f4 p1 f5 p1 f6 p1 f1a p1 f2a p1 f3a p1 f4a

;

_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)+(0.0524P)²+5.5848P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11222
_refine_ls_number_parameters     704
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1570
_refine_ls_wR_factor_gt          0.1300
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.75370(3) -0.10314(4) -0.41571(2) 0.03864(15) Uani 1 1 d . . .
Fe2 Fe 0.73096(3) 0.19833(4) -0.28255(2) 0.04116(15) Uani 1 1 d . . .
C1 C 0.7299(2) 0.0163(3) -0.38004(17) 0.0421(9) Uani 1 1 d . . .
C2 C 0.7488(2) -0.1664(3) -0.34202(18) 0.0428(9) Uani 1 1 d . . .
C26 C 0.8123(3) 0.0051(3) -0.5136(2) 0.0632(12) Uani 1 1 d . . .
H26A H 0.8657 0.0043 -0.4873 0.076 Uiso 1 1 calc R . .
C25 C 0.7985(4) 0.0508(4) -0.5719(2) 0.0783(15) Uani 1 1 d . . .
H25A H 0.8427 0.0787 -0.5837 0.094 Uiso 1 1 calc R . .
C24 C 0.7205(4) 0.0542(4) -0.6109(2) 0.0796(16) Uani 1 1 d . . .
H24A H 0.7112 0.0850 -0.6492 0.095 Uiso 1 1 calc R . .
C22 C 0.6548(3) 0.0112(4) -0.5931(2) 0.0658(13) Uani 1 1 d . . .
C23 C 0.6736(3) -0.0340(3) -0.53493(17) 0.0498(10) Uani 1 1 d . . .
C21 C 0.5697(4) 0.0097(4) -0.6295(2) 0.0788(16) Uani 1 1 d . . .
H21A H 0.5554 0.0412 -0.6676 0.095 Uiso 1 1 calc R . .
C20 C 0.5107(4) -0.0359(4) -0.6098(2) 0.0784(16) Uani 1 1 d . . .
H20A H 0.4565 -0.0352 -0.6348 0.094 Uiso 1 1 calc R . .
C18 C 0.5283(3) -0.0857(3) -0.5517(2) 0.0594(12) Uani 1 1 d . . .
C19 C 0.6105(2) -0.0820(3) -0.51425(18) 0.0483(10) Uani 1 1 d . . .
C17 C 0.4711(3) -0.1380(4) -0.5287(3) 0.0686(14) Uani 1 1 d . . .
H17A H 0.4162 -0.1434 -0.5521 0.082 Uiso 1 1 calc R . .
C16 C 0.4957(3) -0.1805(4) -0.4728(3) 0.0675(13) Uani 1 1 d . . .
H16A H 0.4578 -0.2153 -0.4573 0.081 Uiso 1 1 calc R . .
C15 C 0.5777(2) -0.1723(3) -0.4380(2) 0.0562(11) Uani 1 1 d . . .
H15A H 0.5932 -0.2020 -0.3993 0.067 Uiso 1 1 calc R . .
C14 C 0.9169(3) -0.0148(3) -0.3467(2) 0.0589(11) Uani 1 1 d . . .
H14A H 0.8885 0.0420 -0.3408 0.071 Uiso 1 1 calc R . .
C13 C 1.0027(3) -0.0192(4) -0.3200(2) 0.0687(13) Uani 1 1 d . . .
H13A H 1.0303 0.0342 -0.2973 0.082 Uiso 1 1 calc R . .
C12 C 1.0456(3) -0.1025(4) -0.3273(2) 0.0691(13) Uani 1 1 d . . .
H12A H 1.1024 -0.1063 -0.3092 0.083 Uiso 1 1 calc R . .
C10 C 1.0038(2) -0.1817(4) -0.3620(2) 0.0560(11) Uani 1 1 d . . .
C11 C 0.9181(2) -0.1711(3) -0.38771(17) 0.0442(9) Uani 1 1 d . . .
C9 C 1.0415(3) -0.2728(4) -0.3723(2) 0.0724(14) Uani 1 1 d . . .
H9A H 1.0983 -0.2812 -0.3558 0.087 Uiso 1 1 calc R . .
C8 C 0.9967(3) -0.3462(4) -0.4053(2) 0.0743(15) Uani 1 1 d . . .
H8A H 1.0231 -0.4048 -0.4107 0.089 Uiso 1 1 calc R . .
C6 C 0.9101(3) -0.3371(3) -0.4323(2) 0.0578(11) Uani 1 1 d . . .
C7 C 0.8714(2) -0.2490(3) -0.42296(17) 0.0458(9) Uani 1 1 d . . .
C5 C 0.8592(3) -0.4104(4) -0.4680(2) 0.0726(14) Uani 1 1 d . . .
H5A H 0.8817 -0.4704 -0.4759 0.087 Uiso 1 1 calc R . .
C4 C 0.7763(3) -0.3926(3) -0.4911(2) 0.0730(14) Uani 1 1 d . . .
H4A H 0.7423 -0.4404 -0.5149 0.088 Uiso 1 1 calc R . .
C3 C 0.7428(3) -0.3030(3) -0.4790(2) 0.0564(11) Uani 1 1 d . . .
H3A H 0.6862 -0.2922 -0.4954 0.068 Uiso 1 1 calc R . .
C27 C 0.5653(2) 0.2851(3) -0.32967(18) 0.0476(10) Uani 1 1 d . A .
C28 C 0.5159(3) 0.3572(3) -0.3675(2) 0.0634(12) Uani 1 1 d . . .
H28A H 0.5390 0.3976 -0.3921 0.076 Uiso 1 1 calc R . .
C29 C 0.4343(3) 0.3688(5) -0.3687(3) 0.0876(18) Uani 1 1 d . . .
H29A H 0.4029 0.4178 -0.3934 0.105 Uiso 1 1 calc R . .
C30 C 0.3978(3) 0.3086(5) -0.3337(3) 0.094(2) Uani 1 1 d . . .
H30A H 0.3421 0.3167 -0.3353 0.113 Uiso 1 1 calc R . .
C31 C 0.4439(3) 0.2375(4) -0.2968(3) 0.0816(16) Uani 1 1 d . . .
H31A H 0.4192 0.1968 -0.2735 0.098 Uiso 1 1 calc R . .
C32 C 0.5283(3) 0.2251(3) -0.2936(2) 0.0542(10) Uani 1 1 d . . .
C33 C 0.5714(3) 0.1470(3) -0.2538(2) 0.0604(12) Uani 1 1 d . A .
H33A H 0.5415 0.1106 -0.2320 0.073 Uiso 1 1 calc R . .
C34A C 0.6874(8) 0.0581(13) -0.1928(8) 0.071(4) Uani 0.62(3) 1 d P A 1
H34A H 0.6494 0.0061 -0.1884 0.085 Uiso 0.62(3) 1 calc PR A 1
H34B H 0.7028 0.0961 -0.1548 0.085 Uiso 0.62(3) 1 calc PR A 1
C34B C 0.6804(13) 0.0224(18) -0.2219(16) 0.069(6) Uani 0.38(3) 1 d P A 2
H34C H 0.6483 -0.0053 -0.1959 0.083 Uiso 0.38(3) 1 calc PR A 2
H34D H 0.6789 -0.0230 -0.2556 0.083 Uiso 0.38(3) 1 calc PR A 2
C35A C 0.7649(15) 0.0134(13) -0.2065(10) 0.071(4) Uani 0.62(3) 1 d P A 1
H35A H 0.7995 -0.0194 -0.1703 0.086 Uiso 0.62(3) 1 calc PR A 1
H35B H 0.7496 -0.0339 -0.2401 0.086 Uiso 0.62(3) 1 calc PR A 1
C35B C 0.765(2) 0.042(2) -0.1867(16) 0.063(6) Uani 0.38(3) 1 d P A 2
H35C H 0.7937 -0.0200 -0.1743 0.076 Uiso 0.38(3) 1 calc PR A 2
H35D H 0.7648 0.0788 -0.1496 0.076 Uiso 0.38(3) 1 calc PR A 2
C36 C 0.8872(3) 0.1073(3) -0.2061(2) 0.0640(12) Uani 1 1 d . A .
H36A H 0.9154 0.0620 -0.1768 0.077 Uiso 1 1 calc R . .
C37 C 0.9365(3) 0.1794(3) -0.2275(2) 0.0594(12) Uani 1 1 d . . .
C38 C 1.0229(3) 0.1781(4) -0.2010(3) 0.0852(17) Uani 1 1 d . . .
H42A H 1.0451 0.1328 -0.1697 0.102 Uiso 1 1 calc R . .
C39 C 1.0742(4) 0.2404(5) -0.2193(4) 0.100(2) Uani 1 1 d . . .
H41A H 1.1310 0.2381 -0.2005 0.120 Uiso 1 1 calc R . .
C40 C 1.0431(3) 0.3072(5) -0.2656(3) 0.0884(19) Uani 1 1 d . . .
H40A H 1.0789 0.3495 -0.2786 0.106 Uiso 1 1 calc R . .
C41 C 0.9583(3) 0.3121(4) -0.2934(2) 0.0664(13) Uani 1 1 d . . .
H39A H 0.9378 0.3579 -0.3246 0.080 Uiso 1 1 calc R . .
C42 C 0.9029(2) 0.2481(3) -0.27450(19) 0.0517(10) Uani 1 1 d . A .
C43 C 0.7210(5) -0.2392(6) -0.0448(3) 0.138(3) Uani 1 1 d . . .
H43A H 0.7350 -0.2410 -0.0834 0.207 Uiso 1 1 calc R . .
H43B H 0.6651 -0.2160 -0.0514 0.207 Uiso 1 1 calc R . .
H43C H 0.7258 -0.3045 -0.0273 0.207 Uiso 1 1 calc R . .
C44 C 0.7648(6) -0.1617(6) 0.0552(3) 0.141(3) Uani 1 1 d . . .
H44A H 0.8053 -0.1163 0.0787 0.211 Uiso 1 1 calc R . .
H44B H 0.7707 -0.2247 0.0758 0.211 Uiso 1 1 calc R . .
H44C H 0.7102 -0.1361 0.0515 0.211 Uiso 1 1 calc R . .
C45 C 0.8339(5) -0.1309(6) -0.0217(5) 0.124(3) Uani 1 1 d . . .
H45A H 0.8370 -0.1410 -0.0619 0.149 Uiso 1 1 calc R . .
C46 C 0.0123(5) 0.1745(6) -0.4521(4) 0.141(3) Uani 1 1 d . . .
H46A H -0.0411 0.2015 -0.4728 0.211 Uiso 1 1 calc R . .
H46B H 0.0061 0.1269 -0.4220 0.211 Uiso 1 1 calc R . .
H46C H 0.0357 0.1428 -0.4817 0.211 Uiso 1 1 calc R . .
C47 C 0.1506(4) 0.2309(6) -0.3870(4) 0.137(3) Uani 1 1 d . . .
H47A H 0.1786 0.2908 -0.3700 0.206 Uiso 1 1 calc R . .
H47B H 0.1794 0.2006 -0.4137 0.206 Uiso 1 1 calc R . .
H47C H 0.1494 0.1861 -0.3541 0.206 Uiso 1 1 calc R . .
C48 C 0.0409(4) 0.3473(5) -0.4256(3) 0.0935(18) Uani 1 1 d . . .
H48A H 0.0792 0.3956 -0.4071 0.112 Uiso 1 1 calc R . .
N1 N 0.7169(2) 0.0868(3) -0.35494(15) 0.0508(8) Uani 1 1 d . . .
N2 N 0.7502(2) -0.2051(3) -0.29613(16) 0.0566(9) Uani 1 1 d . . .
N6 N 0.7517(2) -0.0366(2) -0.49530(14) 0.0462(8) Uani 1 1 d . . .
N5 N 0.63530(19) -0.1241(2) -0.45747(14) 0.0443(7) Uani 1 1 d . . .
N4 N 0.87427(18) -0.0886(2) -0.38038(14) 0.0437(7) Uani 1 1 d . . .
N3 N 0.78820(19) -0.2322(2) -0.44505(14) 0.0446(7) Uani 1 1 d . . .
N7 N 0.6476(2) 0.1240(3) -0.24617(17) 0.0572(9) Uani 1 1 d . . .
N8 N 0.8081(2) 0.0998(3) -0.22392(15) 0.0538(9) Uani 1 1 d . . .
N9 N 0.7766(3) -0.1734(3) -0.00320(19) 0.0704(11) Uani 1 1 d . . .
N10 N 0.0668(3) 0.2539(4) -0.4216(2) 0.0880(14) Uani 1 1 d . . .
O1 O 0.64339(16) 0.2767(2) -0.33106(12) 0.0486(7) Uani 1 1 d . . .
O2 O 0.82337(16) 0.2545(2) -0.30345(13) 0.0538(7) Uani 1 1 d . . .
O3 O 0.8874(3) -0.0744(5) 0.0147(4) 0.165(3) Uani 1 1 d . . .
O4 O -0.0291(4) 0.3746(4) -0.4515(3) 0.1374(19) Uani 1 1 d . . .
O5 O 1.0666(3) -0.0838(4) 0.0521(2) 0.1361(18) Uani 1 1 d . . .
P1 P 0.23077(7) 0.53197(10) -0.28585(6) 0.0648(3) Uani 1 1 d D . .
F1 F 0.1679(7) 0.5214(11) -0.3505(5) 0.123(5) Uani 0.50 1 d PD B 1
F2 F 0.1585(5) 0.5447(7) -0.2532(4) 0.101(3) Uani 0.50 1 d PD B 1
F3 F 0.2972(5) 0.5475(7) -0.2216(4) 0.107(3) Uani 0.50 1 d PD B 1
F4 F 0.3048(5) 0.5206(10) -0.3165(4) 0.095(3) Uani 0.50 1 d PD B 1
F1A F 0.2099(10) 0.4902(11) -0.3531(4) 0.149(5) Uani 0.50 1 d PD B 2
F2A F 0.1354(4) 0.5311(8) -0.2926(6) 0.110(3) Uani 0.50 1 d PDU B 2
F3A F 0.3240(5) 0.5300(11) -0.2841(6) 0.111(4) Uani 0.50 1 d PDU B 2
F4A F 0.2517(10) 0.5690(10) -0.2185(4) 0.157(5) Uani 0.50 1 d PDU B 2
F5 F 0.22726(19) 0.6457(2) -0.30350(19) 0.1121(12) Uani 1 1 d DU B .
F6 F 0.2340(2) 0.4187(2) -0.26737(19) 0.1098(12) Uani 1 1 d D B .


_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 C2 1.886(4) . ?
Fe1 C1 1.890(4) . ?
Fe1 N4 1.970(3) . ?
Fe1 N5 1.972(3) . ?
Fe1 N6 1.996(3) . ?
Fe1 N3 2.002(3) . ?
Fe2 O2 1.893(3) . ?
Fe2 O1 1.896(3) . ?
Fe2 N7 2.060(4) . ?
Fe2 N8 2.063(3) . ?
Fe2 N2 2.152(4) 2_654 ?
Fe2 N1 2.183(3) . ?
C1 N1 1.157(5) . ?
C2 N2 1.152(5) . ?
C26 N6 1.320(5) . ?
C26 C25 1.410(7) . ?
C26 H26A 0.9300 . ?
C25 C24 1.364(7) . ?
C25 H25A 0.9300 . ?
C24 C22 1.395(7) . ?
C24 H24A 0.9300 . ?
C22 C23 1.401(6) . ?
C22 C21 1.439(7) . ?
C23 N6 1.369(5) . ?
C23 C19 1.421(6) . ?
C21 C20 1.336(8) . ?
C21 H21A 0.9300 . ?
C20 C18 1.430(7) . ?
C20 H20A 0.9300 . ?
C18 C17 1.396(7) . ?
C18 C19 1.408(5) . ?
C19 N5 1.357(5) . ?
C17 C16 1.342(7) . ?
C17 H17A 0.9300 . ?
C16 C15 1.390(6) . ?
C16 H16A 0.9300 . ?
C15 N5 1.332(5) . ?
C15 H15A 0.9300 . ?
C14 N4 1.336(5) . ?
C14 C13 1.400(6) . ?
C14 H14A 0.9300 . ?
C13 C12 1.368(7) . ?
C13 H13A 0.9300 . ?
C12 C10 1.395(6) . ?
C12 H12A 0.9300 . ?
C10 C11 1.402(5) . ?
C10 C9 1.429(6) . ?
C11 N4 1.368(5) . ?
C11 C7 1.418(5) . ?
C9 C8 1.340(7) . ?
C9 H9A 0.9300 . ?
C8 C6 1.418(6) . ?
C8 H8A 0.9300 . ?
C6 C7 1.397(5) . ?
C6 C5 1.408(6) . ?
C7 N3 1.367(5) . ?
C5 C4 1.365(6) . ?
C5 H5A 0.9300 . ?
C4 C3 1.391(6) . ?
C4 H4A 0.9300 . ?
C3 N3 1.328(5) . ?
C3 H3A 0.9300 . ?
C27 O1 1.321(4) . ?
C27 C32 1.404(6) . ?
C27 C28 1.406(6) . ?
C28 C29 1.370(7) . ?
C28 H28A 0.9300 . ?
C29 C30 1.383(8) . ?
C29 H29A 0.9300 . ?
C30 C31 1.363(8) . ?
C30 H30A 0.9300 . ?
C31 C32 1.406(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.445(6) . ?
C33 N7 1.278(5) . ?
C33 H33A 0.9300 . ?
C34A N7 1.499(11) . ?
C34A C35A 1.54(3) . ?
C34A H34A 0.9700 . ?
C34A H34B 0.9700 . ?
C34B C35B 1.45(5) . ?
C34B N7 1.522(19) . ?
C34B H34C 0.9700 . ?
C34B H34D 0.9700 . ?
C35A N8 1.48(2) . ?
C35A H35A 0.9700 . ?
C35A H35B 0.9700 . ?
C35B N8 1.47(3) . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
C36 N8 1.280(5) . ?
C36 C37 1.439(7) . ?
C36 H36A 0.9300 . ?
C37 C42 1.405(6) . ?
C37 C38 1.408(6) . ?
C38 C39 1.344(8) . ?
C38 H42A 0.9300 . ?
C39 C40 1.371(9) . ?
C39 H41A 0.9300 . ?
C40 C41 1.389(7) . ?
C40 H40A 0.9300 . ?
C41 C42 1.414(6) . ?
C41 H39A 0.9300 . ?
C42 O2 1.319(5) . ?
C43 N9 1.435(7) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 N9 1.390(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 N9 1.281(8) . ?
C45 O3 1.287(9) . ?
C45 H45A 0.9300 . ?
C46 N10 1.454(8) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 N10 1.444(7) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 O4 1.216(7) . ?
C48 N10 1.328(7) . ?
C48 H48A 0.9300 . ?
N2 Fe2 2.152(4) 2_644 ?
P1 F4A 1.544(8) . ?
P1 F3A 1.551(7) . ?
P1 F1 1.555(8) . ?
P1 F2A 1.562(7) . ?
P1 F1A 1.563(8) . ?
P1 F6 1.581(3) . ?
P1 F4 1.581(7) . ?
P1 F3 1.582(6) . ?
P1 F5 1.583(3) . ?
P1 F2 1.586(6) . ?

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
C2 Fe1 C1 87.03(16) . . ?
C2 Fe1 N4 88.47(14) . . ?
C1 Fe1 N4 93.10(14) . . ?
C2 Fe1 N5 94.45(15) . . ?
C1 Fe1 N5 91.39(14) . . ?
N4 Fe1 N5 174.77(13) . . ?
C2 Fe1 N6 176.67(15) . . ?
C1 Fe1 N6 92.46(14) . . ?
N4 Fe1 N6 94.85(13) . . ?
N5 Fe1 N6 82.27(14) . . ?
C2 Fe1 N3 88.94(15) . . ?
C1 Fe1 N3 173.89(14) . . ?
N4 Fe1 N3 82.20(13) . . ?
N5 Fe1 N3 93.50(13) . . ?
N6 Fe1 N3 91.83(13) . . ?
O2 Fe2 O1 101.00(12) . . ?
O2 Fe2 N7 168.83(13) . . ?
O1 Fe2 N7 89.90(14) . . ?
O2 Fe2 N8 90.23(14) . . ?
O1 Fe2 N8 168.77(14) . . ?
N7 Fe2 N8 78.87(15) . . ?
O2 Fe2 N2 90.79(13) . 2_654 ?
O1 Fe2 N2 93.14(13) . 2_654 ?
N7 Fe2 N2 86.12(14) . 2_654 ?
N8 Fe2 N2 86.37(14) . 2_654 ?
O2 Fe2 N1 91.23(13) . . ?
O1 Fe2 N1 92.52(12) . . ?
N7 Fe2 N1 90.73(14) . . ?
N8 Fe2 N1 87.47(13) . . ?
N2 Fe2 N1 173.52(13) 2_654 . ?
N1 C1 Fe1 176.1(3) . . ?
N2 C2 Fe1 176.5(4) . . ?
N6 C26 C25 122.0(5) . . ?
N6 C26 H26A 119.0 . . ?
C25 C26 H26A 119.0 . . ?
C24 C25 C26 120.1(5) . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C25 C24 C22 119.6(5) . . ?
C25 C24 H24A 120.2 . . ?
C22 C24 H24A 120.2 . . ?
C24 C22 C23 117.0(5) . . ?
C24 C22 C21 125.4(5) . . ?
C23 C22 C21 117.6(5) . . ?
N6 C23 C22 123.6(4) . . ?
N6 C23 C19 116.0(3) . . ?
C22 C23 C19 120.3(4) . . ?
C20 C21 C22 121.7(5) . . ?
C20 C21 H21A 119.1 . . ?
C22 C21 H21A 119.1 . . ?
C21 C20 C18 122.1(5) . . ?
C21 C20 H20A 118.9 . . ?
C18 C20 H20A 118.9 . . ?
C17 C18 C19 117.0(4) . . ?
C17 C18 C20 125.8(5) . . ?
C19 C18 C20 117.2(5) . . ?
N5 C19 C18 123.3(4) . . ?
N5 C19 C23 115.7(3) . . ?
C18 C19 C23 121.0(4) . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C16 C15 120.0(5) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
N5 C15 C16 123.2(4) . . ?
N5 C15 H15A 118.4 . . ?
C16 C15 H15A 118.4 . . ?
N4 C14 C13 122.8(4) . . ?
N4 C14 H14A 118.6 . . ?
C13 C14 H14A 118.6 . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 H13A 120.2 . . ?
C14 C13 H13A 120.2 . . ?
C13 C12 C10 119.8(4) . . ?
C13 C12 H12A 120.1 . . ?
C10 C12 H12A 120.1 . . ?
C12 C10 C11 117.1(4) . . ?
C12 C10 C9 125.0(4) . . ?
C11 C10 C9 118.0(4) . . ?
N4 C11 C10 123.8(4) . . ?
N4 C11 C7 116.0(3) . . ?
C10 C11 C7 120.2(4) . . ?
C8 C9 C10 121.3(4) . . ?
C8 C9 H9A 119.4 . . ?
C10 C9 H9A 119.4 . . ?
C9 C8 C6 121.9(4) . . ?
C9 C8 H8A 119.0 . . ?
C6 C8 H8A 119.0 . . ?
C7 C6 C5 116.7(4) . . ?
C7 C6 C8 118.1(4) . . ?
C5 C6 C8 125.2(4) . . ?
N3 C7 C6 123.8(4) . . ?
N3 C7 C11 115.8(3) . . ?
C6 C7 C11 120.5(4) . . ?
C4 C5 C6 119.4(4) . . ?
C4 C5 H5A 120.3 . . ?
C6 C5 H5A 120.3 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
N3 C3 C4 122.6(4) . . ?
N3 C3 H3A 118.7 . . ?
C4 C3 H3A 118.7 . . ?
O1 C27 C32 124.0(4) . . ?
O1 C27 C28 118.0(4) . . ?
C32 C27 C28 118.0(4) . . ?
C29 C28 C27 120.7(5) . . ?
C29 C28 H28A 119.6 . . ?
C27 C28 H28A 119.6 . . ?
C28 C29 C30 121.0(5) . . ?
C28 C29 H29A 119.5 . . ?
C30 C29 H29A 119.5 . . ?
C31 C30 C29 119.7(5) . . ?
C31 C30 H30A 120.2 . . ?
C29 C30 H30A 120.2 . . ?
C30 C31 C32 120.7(6) . . ?
C30 C31 H31A 119.6 . . ?
C32 C31 H31A 119.6 . . ?
C27 C32 C31 119.8(5) . . ?
C27 C32 C33 123.7(4) . . ?
C31 C32 C33 116.5(5) . . ?
N7 C33 C32 125.0(4) . . ?
N7 C33 H33A 117.5 . . ?
C32 C33 H33A 117.5 . . ?
N7 C34A C35A 106.8(13) . . ?
N7 C34A H34A 110.4 . . ?
C35A C34A H34A 110.4 . . ?
N7 C34A H34B 110.4 . . ?
C35A C34A H34B 110.4 . . ?
H34A C34A H34B 108.6 . . ?
C35B C34B N7 104(2) . . ?
C35B C34B H34C 111.0 . . ?
N7 C34B H34C 111.0 . . ?
C35B C34B H34D 111.0 . . ?
N7 C34B H34D 111.0 . . ?
H34C C34B H34D 109.0 . . ?
N8 C35A C34A 104.1(14) . . ?
N8 C35A H35A 110.9 . . ?
C34A C35A H35A 110.9 . . ?
N8 C35A H35B 110.9 . . ?
C34A C35A H35B 110.9 . . ?
H35A C35A H35B 108.9 . . ?
C34B C35B N8 110(2) . . ?
C34B C35B H35C 109.6 . . ?
N8 C35B H35C 109.6 . . ?
C34B C35B H35D 109.6 . . ?
N8 C35B H35D 109.6 . . ?
H35C C35B H35D 108.1 . . ?
N8 C36 C37 125.9(4) . . ?
N8 C36 H36A 117.0 . . ?
C37 C36 H36A 117.0 . . ?
C42 C37 C38 118.9(5) . . ?
C42 C37 C36 123.2(4) . . ?
C38 C37 C36 117.8(5) . . ?
C39 C38 C37 122.1(6) . . ?
C39 C38 H42A 118.9 . . ?
C37 C38 H42A 118.9 . . ?
C38 C39 C40 120.1(6) . . ?
C38 C39 H41A 120.0 . . ?
C40 C39 H41A 120.0 . . ?
C39 C40 C41 120.4(6) . . ?
C39 C40 H40A 119.8 . . ?
C41 C40 H40A 119.8 . . ?
C40 C41 C42 120.7(5) . . ?
C40 C41 H39A 119.7 . . ?
C42 C41 H39A 119.7 . . ?
O2 C42 C37 124.1(4) . . ?
O2 C42 C41 118.0(4) . . ?
C37 C42 C41 117.9(4) . . ?
N9 C43 H43A 109.5 . . ?
N9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N9 C44 H44A 109.5 . . ?
N9 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N9 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N9 C45 O3 120.9(8) . . ?
N9 C45 H45A 119.6 . . ?
O3 C45 H45A 119.6 . . ?
N10 C46 H46A 109.5 . . ?
N10 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N10 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N10 C47 H47A 109.5 . . ?
N10 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N10 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O4 C48 N10 125.0(7) . . ?
O4 C48 H48A 117.5 . . ?
N10 C48 H48A 117.5 . . ?
C1 N1 Fe2 159.2(3) . . ?
C2 N2 Fe2 167.2(3) . 2_644 ?
C26 N6 C23 117.7(4) . . ?
C26 N6 Fe1 130.1(3) . . ?
C23 N6 Fe1 112.2(3) . . ?
C15 N5 C19 116.7(3) . . ?
C15 N5 Fe1 129.6(3) . . ?
C19 N5 Fe1 113.7(3) . . ?
C14 N4 C11 116.9(3) . . ?
C14 N4 Fe1 129.5(3) . . ?
C11 N4 Fe1 113.3(2) . . ?
C3 N3 C7 117.4(3) . . ?
C3 N3 Fe1 130.1(3) . . ?
C7 N3 Fe1 112.4(2) . . ?
C33 N7 C34A 117.6(6) . . ?
C33 N7 C34B 121.1(8) . . ?
C34A N7 C34B 30.5(8) . . ?
C33 N7 Fe2 126.0(3) . . ?
C34A N7 Fe2 113.9(5) . . ?
C34B N7 Fe2 111.3(8) . . ?
C36 N8 C35B 119.4(13) . . ?
C36 N8 C35A 121.2(9) . . ?
C35B N8 C35A 23.1(10) . . ?
C36 N8 Fe2 124.5(3) . . ?
C35B N8 Fe2 112.7(12) . . ?
C35A N8 Fe2 114.2(9) . . ?
C45 N9 C44 124.5(7) . . ?
C45 N9 C43 118.5(7) . . ?
C44 N9 C43 117.0(6) . . ?
C48 N10 C47 119.5(6) . . ?
C48 N10 C46 121.1(6) . . ?
C47 N10 C46 119.4(6) . . ?
C27 O1 Fe2 130.6(3) . . ?
C42 O2 Fe2 129.5(3) . . ?
F4A P1 F3A 91.2(7) . . ?
F4A P1 F1 149.9(7) . . ?
F3A P1 F1 116.4(7) . . ?
F4A P1 F2A 93.1(7) . . ?
F3A P1 F2A 175.8(7) . . ?
F1 P1 F2A 59.5(7) . . ?
F4A P1 F1A 177.7(8) . . ?
F3A P1 F1A 88.8(7) . . ?
F1 P1 F1A 31.1(6) . . ?
F2A P1 F1A 87.0(7) . . ?
F4A P1 F6 94.1(6) . . ?
F3A P1 F6 90.8(5) . . ?
F1 P1 F6 97.1(6) . . ?
F2A P1 F6 88.9(4) . . ?
F1A P1 F6 83.6(6) . . ?
F4A P1 F4 117.5(7) . . ?
F3A P1 F4 26.7(5) . . ?
F1 P1 F4 89.8(6) . . ?
F2A P1 F4 149.1(6) . . ?
F1A P1 F4 62.5(7) . . ?
F6 P1 F4 92.6(5) . . ?
F4A P1 F3 30.9(6) . . ?
F3A P1 F3 61.6(5) . . ?
F1 P1 F3 176.8(8) . . ?
F2A P1 F3 122.5(6) . . ?
F1A P1 F3 148.3(7) . . ?
F6 P1 F3 85.5(4) . . ?
F4 P1 F3 88.3(5) . . ?
F4A P1 F5 85.2(6) . . ?
F3A P1 F5 89.5(5) . . ?
F1 P1 F5 83.4(6) . . ?
F2A P1 F5 90.9(4) . . ?
F1A P1 F5 97.1(6) . . ?
F6 P1 F5 179.2(2) . . ?
F4 P1 F5 88.0(5) . . ?
F3 P1 F5 94.0(4) . . ?
F4A P1 F2 60.6(6) . . ?
F3A P1 F2 151.5(6) . . ?
F1 P1 F2 92.0(6) . . ?
F2A P1 F2 32.7(4) . . ?
F1A P1 F2 119.3(7) . . ?
F6 P1 F2 87.6(4) . . ?
F4 P1 F2 178.2(6) . . ?
F3 P1 F2 89.9(5) . . ?
F5 P1 F2 91.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 1015602'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H30 Cl0 F6 Fe N8 O2 Os P'
_chemical_formula_weight         1021.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   27.291(11)
_cell_length_b                   12.386(5)
_cell_length_c                   24.808(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.893(6)
_cell_angle_gamma                90.00
_cell_volume                     8065(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9646
_cell_measurement_theta_min      2.0965
_cell_measurement_theta_max      27.4719

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4008
_exptl_absorpt_coefficient_mu    3.619
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3722
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'RIGAKU/MSC(2004), CrystalClear Version 1.3.6'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30974
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         27.42
_reflns_number_total             9159
_reflns_number_gt                7398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_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. 
 The atoms of c10 c15 c20 p2 f9 f8 f6 f3a f1a f2a f1 f2 f3 f5 are abnormal, so the following 
least-squares restraint is used in the refinement, isor 0.01 c10 c15 c20 p2 f9 f8 f6 f3a f1a f2a f1 f2 f3 f5.
 The c30-C31 and F1-F3 group are disorder, so the following process is used in the refinement. 
PART   1
C30A  1   0.29079   0.19655   0.25501  31.00000   0.07241   0.03057 =
       0.08116  -0.00274   0.02025  -0.00973
AFIX  23
H30A  2   0.29803   0.23699   0.28979  31.00000  -1.20000
H30B  2   0.28317   0.24697   0.22391  31.00000  -1.20000
AFIX   0
C31A  1   0.33558   0.12538   0.25349  31.00000   0.06480   0.04330 =
       0.08458   0.01394   0.01128   0.00120
AFIX  23
H31A  2   0.36422   0.16848   0.24998  31.00000  -1.20000
H31B  2   0.34625   0.08166   0.28711  31.00000  -1.20000
AFIX   0
PART   2
C30B  1   0.29811   0.16458   0.27346 -31.00000   0.10267   0.03756 =
       0.08985   0.01033   0.04306  -0.00682
AFIX  23
H30C  2   0.29619   0.23633   0.28842 -31.00000  -1.20000
H30D  2   0.31780   0.11894   0.30338 -31.00000  -1.20000
AFIX   0
C31B  1   0.32214   0.16904   0.22733 -31.00000   0.07332   0.04341 =
       0.06845  -0.00610   0.01442  -0.00554
AFIX  23
H31C  2   0.35795   0.18748   0.24112 -31.00000  -1.20000
H31D  2   0.30542   0.22196   0.19953 -31.00000  -1.20000
AFIX   0
PART   0
PART   1
F1    9   0.47453   0.05201   0.20417  21.00000   0.15762   0.17186 =
       0.18671  -0.04014   0.05670  -0.00597
F2    9   0.45022   0.13613   0.27082  21.00000   0.11972   0.17342 =
       0.15172  -0.01998   0.04683   0.00934
F3    9   0.47734   0.23430   0.20896  21.00000   0.19065   0.17020 =
       0.16215   0.00496   0.00063   0.03513
PART   2
F1A   9   0.46143   0.21779   0.25969 -21.00000   0.18603   0.18732 =
       0.24288  -0.00614   0.08876   0.04925
F2A   9   0.47136   0.12255   0.18538 -21.00000   0.11138   0.14796 =
       0.12812   0.02135   0.00611   0.00715
F3A   9   0.46458   0.03744   0.26074 -21.00000   0.17238   0.16711 =
       0.16234   0.03770   0.01918  -0.04755
PART   0
The bond lengths of p-F in p1(f1f2f3) p1a(f1af2af3a) and p2(f4f5f6f7f8f9)
are abnormal, so the following process is used in the refinement. 
dfix 3.16 f3a_$1 f1a f2a_$1 f2a  f1a_$1 f3a
dfix 1.58 0.01  p1 f1 p1 f2 p1 f3 p1 f1a p1 f2a p1 f3a
dfix 2.24 f1 f2 f1 f3 f2 f3 f1 f1_$1 f1 f2_$1 f2 f1_$1 f2 f3_$1
dfix 3.16 f3 f1_$1 f1 f3_$1 f2 f2_$1
dfix 2.24 f1a f2a f1a f3a f2a f3a f1a f1a_$1 f1a f2a_$1 f2a f1a_$1
dfix 2.24 f2a f1a_$1 f2a f3a_$1
eqiv $1  1-x, y, 0.5-z+-

;

_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)+(0.0732P)²+26.4152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9159
_refine_ls_number_parameters     593
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1805
_refine_ls_wR_factor_gt          0.1674
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.164464(12) 0.34298(2) 0.099859(12) 0.05451(13) Uani 1 1 d . . .
Fe1 Fe 0.24675(4) -0.00250(8) 0.19865(5) 0.0527(3) Uani 1 1 d . . .
C1 C 0.1956(3) 0.1983(6) 0.1164(3) 0.0533(16) Uani 1 1 d . . .
C2 C 0.1940(4) 0.3787(6) 0.1795(4) 0.064(2) Uani 1 1 d . . .
C22 C 0.0974(4) 0.2597(8) -0.0136(4) 0.084(3) Uani 1 1 d . . .
H22A H 0.0743 0.2418 0.0064 0.101 Uiso 1 1 calc R . .
C21 C 0.0854(5) 0.2332(10) -0.0715(5) 0.107(4) Uani 1 1 d . . .
H21A H 0.0548 0.1999 -0.0897 0.129 Uiso 1 1 calc R . .
C20 C 0.1210(6) 0.2589(11) -0.0996(6) 0.112(4) Uani 1 1 d U . .
H20A H 0.1146 0.2424 -0.1375 0.134 Uiso 1 1 calc R . .
C19 C 0.1665(5) 0.3093(9) -0.0716(4) 0.089(3) Uani 1 1 d . . .
H19A H 0.1912 0.3256 -0.0898 0.106 Uiso 1 1 calc R . .
C18 C 0.1732(4) 0.3333(6) -0.0175(4) 0.068(2) Uani 1 1 d . . .
C17 C 0.2206(4) 0.3835(7) 0.0168(4) 0.072(2) Uani 1 1 d . . .
C16 C 0.2584(5) 0.4228(9) -0.0079(6) 0.105(4) Uani 1 1 d . . .
H16A H 0.2547 0.4158 -0.0461 0.126 Uiso 1 1 calc R . .
C15 C 0.2999(6) 0.4707(11) 0.0265(7) 0.116(4) Uani 1 1 d U . .
H15A H 0.3244 0.4999 0.0111 0.139 Uiso 1 1 calc R . .
C14 C 0.3068(5) 0.4775(9) 0.0816(8) 0.123(5) Uani 1 1 d . . .
H14A H 0.3369 0.5064 0.1043 0.148 Uiso 1 1 calc R . .
C13 C 0.2686(4) 0.4408(8) 0.1056(5) 0.089(3) Uani 1 1 d . . .
H13A H 0.2729 0.4475 0.1440 0.106 Uiso 1 1 calc R . .
C12 C 0.0846(4) 0.2079(9) 0.1324(5) 0.096(3) Uani 1 1 d . . .
H12A H 0.1064 0.1499 0.1327 0.115 Uiso 1 1 calc R . .
C11 C 0.0396(6) 0.1912(13) 0.1467(8) 0.139(6) Uani 1 1 d . . .
H11A H 0.0298 0.1218 0.1535 0.167 Uiso 1 1 calc R . .
C10 C 0.0098(7) 0.2774(16) 0.1506(8) 0.156(6) Uani 1 1 d U . .
H10A H -0.0196 0.2670 0.1619 0.187 Uiso 1 1 calc R . .
C9 C 0.0223(5) 0.3752(13) 0.1385(7) 0.131(5) Uani 1 1 d . . .
H9A H 0.0026 0.4342 0.1426 0.157 Uiso 1 1 calc R . .
C8 C 0.0654(4) 0.3893(9) 0.1197(5) 0.088(3) Uani 1 1 d . . .
C7 C 0.0815(4) 0.4943(8) 0.1034(5) 0.086(3) Uani 1 1 d . . .
C6 C 0.0545(6) 0.5879(11) 0.1024(6) 0.127(5) Uani 1 1 d . . .
H6A H 0.0240 0.5868 0.1123 0.152 Uiso 1 1 calc R . .
C5 C 0.0721(8) 0.6826(12) 0.0869(7) 0.150(7) Uani 1 1 d . . .
H5A H 0.0541 0.7465 0.0863 0.180 Uiso 1 1 calc R . .
C4 C 0.1165(7) 0.6812(9) 0.0725(7) 0.135(6) Uani 1 1 d . . .
H4A H 0.1290 0.7445 0.0611 0.162 Uiso 1 1 calc R . .
C3 C 0.1432(5) 0.5855(8) 0.0747(5) 0.101(4) Uani 1 1 d . . .
H3A H 0.1741 0.5856 0.0656 0.122 Uiso 1 1 calc R . .
C23 C 0.1525(3) -0.0080(6) 0.2306(4) 0.0609(18) Uani 1 1 d . A .
C24 C 0.1072(3) -0.0648(8) 0.2297(5) 0.087(3) Uani 1 1 d . . .
H24A H 0.0999 -0.1292 0.2099 0.105 Uiso 1 1 calc R . .
C25 C 0.0743(5) -0.0269(12) 0.2575(7) 0.129(5) Uani 1 1 d . . .
H25A H 0.0442 -0.0641 0.2557 0.155 Uiso 1 1 calc R . .
C26 C 0.0853(5) 0.0679(13) 0.2889(8) 0.145(6) Uani 1 1 d . . .
H26A H 0.0632 0.0923 0.3089 0.174 Uiso 1 1 calc R . .
C27 C 0.1280(4) 0.1245(11) 0.2904(6) 0.110(4) Uani 1 1 d . . .
H27A H 0.1342 0.1891 0.3103 0.132 Uiso 1 1 calc R . .
C28 C 0.1636(4) 0.0872(7) 0.2624(4) 0.072(2) Uani 1 1 d . . .
C29 C 0.2103(3) 0.1476(6) 0.2707(4) 0.062(2) Uani 1 1 d . A .
H29A H 0.2141 0.2103 0.2921 0.074 Uiso 1 1 calc R . .
C30A C 0.2908(10) 0.1965(18) 0.2550(12) 0.062(6) Uani 0.54(4) 1 d P A 1
H30A H 0.2980 0.2370 0.2898 0.074 Uiso 0.54(4) 1 calc PR A 1
H30B H 0.2832 0.2470 0.2239 0.074 Uiso 0.54(4) 1 calc PR A 1
C31A C 0.3356(7) 0.1254(16) 0.2535(10) 0.066(6) Uani 0.54(4) 1 d P A 1
H31A H 0.3642 0.1685 0.2500 0.079 Uiso 0.54(4) 1 calc PR A 1
H31B H 0.3462 0.0817 0.2871 0.079 Uiso 0.54(4) 1 calc PR A 1
C30B C 0.2981(15) 0.165(2) 0.2735(16) 0.073(8) Uani 0.46(4) 1 d P A 2
H30C H 0.2962 0.2363 0.2884 0.088 Uiso 0.46(4) 1 calc PR A 2
H30D H 0.3178 0.1189 0.3034 0.088 Uiso 0.46(4) 1 calc PR A 2
C31B C 0.3221(9) 0.169(2) 0.2273(12) 0.063(7) Uani 0.46(4) 1 d P A 2
H31C H 0.3579 0.1875 0.2411 0.075 Uiso 0.46(4) 1 calc PR A 2
H31D H 0.3054 0.2220 0.1995 0.075 Uiso 0.46(4) 1 calc PR A 2
C32 C 0.3471(3) 0.0176(7) 0.1789(4) 0.0630(19) Uani 1 1 d . A .
H32A H 0.3794 0.0482 0.1878 0.076 Uiso 1 1 calc R . .
C33 C 0.3373(3) -0.0688(7) 0.1396(3) 0.0618(19) Uani 1 1 d . . .
C34 C 0.3754(4) -0.0949(8) 0.1134(4) 0.082(3) Uani 1 1 d . . .
H34A H 0.4063 -0.0582 0.1239 0.099 Uiso 1 1 calc R . .
C35 C 0.3679(5) -0.1748(10) 0.0720(6) 0.101(4) Uani 1 1 d . . .
H35A H 0.3930 -0.1897 0.0543 0.122 Uiso 1 1 calc R . .
C36 C 0.3228(5) -0.2305(9) 0.0582(5) 0.096(3) Uani 1 1 d . . .
H36A H 0.3176 -0.2845 0.0312 0.115 Uiso 1 1 calc R . .
C37 C 0.2854(4) -0.2078(7) 0.0834(4) 0.074(2) Uani 1 1 d . . .
H37A H 0.2553 -0.2473 0.0730 0.089 Uiso 1 1 calc R . .
C38 C 0.2906(3) -0.1271(6) 0.1244(3) 0.0587(18) Uani 1 1 d . A .
N1 N 0.2141(3) 0.1132(5) 0.1282(3) 0.0643(17) Uani 1 1 d . . .
N2 N 0.2139(3) 0.4002(6) 0.2257(3) 0.081(2) Uani 1 1 d . . .
N6 N 0.1406(3) 0.3092(5) 0.0131(3) 0.0620(16) Uani 1 1 d . . .
N5 N 0.2252(3) 0.3954(5) 0.0722(3) 0.0668(17) Uani 1 1 d . . .
N4 N 0.0972(3) 0.3052(6) 0.1184(3) 0.0709(18) Uani 1 1 d . . .
N3 N 0.1254(3) 0.4930(6) 0.0895(3) 0.075(2) Uani 1 1 d . . .
N7 N 0.3155(2) 0.0561(5) 0.2027(3) 0.0634(17) Uani 1 1 d . . .
N8 N 0.2467(2) 0.1200(5) 0.2506(3) 0.0559(14) Uani 1 1 d . . .
O1 O 0.1821(2) -0.0484(5) 0.2019(3) 0.0734(16) Uani 1 1 d . . .
O2 O 0.2534(2) -0.1118(4) 0.1474(2) 0.0589(12) Uani 1 1 d . . .
P2 P -0.0207(4) 0.0243(8) 0.0125(4) 0.153(4) Uani 0.50 1 d PDU . 1
F9 F -0.0796(4) 0.002(2) -0.0100(10) 0.233(11) Uani 0.50 1 d PDU . 1
F8 F 0.0379(5) 0.0458(19) 0.0389(9) 0.214(10) Uani 0.50 1 d PDU . 1
F7 F -0.0319(10) 0.1461(12) 0.0224(10) 0.224(12) Uani 0.50 1 d PD . 1
F6 F -0.0311(11) 0.006(2) 0.0705(8) 0.256(13) Uani 0.50 1 d PDU . 1
F5 F -0.0098(8) -0.0993(10) 0.0053(10) 0.195(10) Uani 0.50 1 d PDU . 1
F4 F -0.0162(9) 0.0518(19) -0.0483(6) 0.211(11) Uani 0.50 1 d PD . 1
P1 P 0.5000 0.1361(5) 0.2500 0.1245(19) Uani 1 2 d SD . .
F1 F 0.4745(6) 0.0520(11) 0.2042(4) 0.170(10) Uani 0.45(2) 1 d PDU B 2
F2 F 0.4502(4) 0.1361(14) 0.2708(8) 0.146(9) Uani 0.45(2) 1 d PDU B 2
F3 F 0.4773(7) 0.2343(12) 0.2090(7) 0.184(11) Uani 0.45(2) 1 d PDU B 2
F1A F 0.4614(4) 0.2178(11) 0.2597(7) 0.199(10) Uani 0.55(2) 1 d PDU B 1
F2A F 0.4714(5) 0.1226(11) 0.1854(3) 0.134(7) Uani 0.55(2) 1 d PDU B 1
F3A F 0.4646(6) 0.0374(12) 0.2607(6) 0.173(9) Uani 0.55(2) 1 d PDU B 1


_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
Os1 C2 1.968(9) . ?
Os1 C1 1.978(7) . ?
Os1 N4 2.064(8) . ?
Os1 N5 2.065(7) . ?
Os1 N6 2.114(7) . ?
Os1 N3 2.123(7) . ?
Fe1 O1 1.876(6) . ?
Fe1 O2 1.899(5) . ?
Fe1 N7 1.989(7) . ?
Fe1 N8 1.990(6) . ?
Fe1 N2 2.242(8) 4_545 ?
Fe1 N1 2.248(7) . ?
C1 N1 1.170(10) . ?
C2 N2 1.157(10) . ?
C22 N6 1.332(12) . ?
C22 C21 1.421(14) . ?
C22 H22A 0.9300 . ?
C21 C20 1.379(18) . ?
C21 H21A 0.9300 . ?
C20 C19 1.394(17) . ?
C20 H20A 0.9300 . ?
C19 C18 1.337(13) . ?
C19 H19A 0.9300 . ?
C18 N6 1.353(11) . ?
C18 C17 1.477(14) . ?
C17 N5 1.352(11) . ?
C17 C16 1.422(14) . ?
C16 C15 1.356(18) . ?
C16 H16A 0.9300 . ?
C15 C14 1.330(19) . ?
C15 H15A 0.9300 . ?
C14 C13 1.411(16) . ?
C14 H14A 0.9300 . ?
C13 N5 1.366(12) . ?
C13 H13A 0.9300 . ?
C12 N4 1.326(12) . ?
C12 C11 1.384(16) . ?
C12 H12A 0.9300 . ?
C11 C10 1.36(2) . ?
C11 H11A 0.9300 . ?
C10 C9 1.32(2) . ?
C10 H10A 0.9300 . ?
C9 C8 1.390(16) . ?
C9 H9A 0.9300 . ?
C8 N4 1.363(12) . ?
C8 C7 1.464(15) . ?
C7 N3 1.335(12) . ?
C7 C6 1.370(13) . ?
C6 C5 1.36(2) . ?
C6 H6A 0.9300 . ?
C5 C4 1.35(2) . ?
C5 H5A 0.9300 . ?
C4 C3 1.385(14) . ?
C4 H4A 0.9300 . ?
C3 N3 1.334(13) . ?
C3 H3A 0.9300 . ?
C23 O1 1.313(9) . ?
C23 C28 1.406(12) . ?
C23 C24 1.418(12) . ?
C24 C25 1.359(14) . ?
C24 H24A 0.9300 . ?
C25 C26 1.395(18) . ?
C25 H25A 0.9300 . ?
C26 C27 1.351(17) . ?
C26 H26A 0.9300 . ?
C27 C28 1.417(13) . ?
C27 H27A 0.9300 . ?
C28 C29 1.443(12) . ?
C29 N8 1.276(10) . ?
C29 H29A 0.9300 . ?
C30A N8 1.51(2) . ?
C30A C31A 1.52(4) . ?
C30A H30A 0.9700 . ?
C30A H30B 0.9700 . ?
C31A N7 1.50(2) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C30B C31B 1.47(4) . ?
C30B N8 1.47(4) . ?
C30B H30C 0.9700 . ?
C30B H30D 0.9700 . ?
C31B N7 1.52(2) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C32 N7 1.263(10) . ?
C32 C33 1.423(12) . ?
C32 H32A 0.9300 . ?
C33 C34 1.404(11) . ?
C33 C38 1.423(12) . ?
C34 C35 1.400(15) . ?
C34 H34A 0.9300 . ?
C35 C36 1.369(16) . ?
C35 H35A 0.9300 . ?
C36 C37 1.365(14) . ?
C36 H36A 0.9300 . ?
C37 C38 1.406(12) . ?
C37 H37A 0.9300 . ?
C38 O2 1.308(9) . ?
N2 Fe1 2.242(8) 4 ?
P2 F5 1.40(2) 5 ?
P2 F4 1.48(2) 5 ?
P2 F8 1.51(2) 5 ?
P2 P2 1.55(2) 5 ?
P2 F6 1.556(9) . ?
P2 F7 1.572(9) . ?
P2 F9 1.575(9) . ?
P2 F8 1.576(9) . ?
P2 F5 1.579(9) . ?
P2 F4 1.584(9) . ?
F9 F8 1.62(3) 5 ?
F8 F5 1.33(3) 5 ?
F8 F4 1.39(2) 5 ?
F8 P2 1.51(2) 5 ?
F8 F9 1.62(3) 5 ?
F7 F5 1.59(3) 5 ?
F6 F4 1.69(3) 5 ?
F5 F4 1.26(2) 5 ?
F5 F8 1.33(3) 5 ?
F5 P2 1.40(2) 5 ?
F5 F7 1.59(3) 5 ?
F4 F5 1.26(2) 5 ?
F4 F8 1.39(2) 5 ?
F4 P2 1.48(2) 5 ?
F4 F6 1.69(3) 5 ?
P1 F1A 1.526(7) 2_655 ?
P1 F1A 1.526(7) . ?
P1 F1 1.558(7) . ?
P1 F1 1.558(7) 2_655 ?
P1 F2 1.580(6) . ?
P1 F2 1.580(6) 2_655 ?
P1 F2A 1.588(6) . ?
P1 F2A 1.588(6) 2_655 ?
P1 F3 1.598(8) 2_655 ?
P1 F3 1.598(8) . ?
P1 F3A 1.625(8) . ?
P1 F3A 1.625(8) 2_655 ?

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
C2 Os1 C1 87.7(3) . . ?
C2 Os1 N4 88.4(3) . . ?
C1 Os1 N4 96.1(3) . . ?
C2 Os1 N5 96.7(3) . . ?
C1 Os1 N5 90.9(3) . . ?
N4 Os1 N5 171.5(3) . . ?
C2 Os1 N6 173.7(3) . . ?
C1 Os1 N6 91.6(3) . . ?
N4 Os1 N6 97.9(3) . . ?
N5 Os1 N6 77.0(3) . . ?
C2 Os1 N3 88.8(3) . . ?
C1 Os1 N3 172.5(3) . . ?
N4 Os1 N3 77.2(3) . . ?
N5 Os1 N3 96.1(3) . . ?
N6 Os1 N3 92.6(3) . . ?
O1 Fe1 O2 94.3(2) . . ?
O1 Fe1 N7 173.6(3) . . ?
O2 Fe1 N7 91.9(2) . . ?
O1 Fe1 N8 92.1(3) . . ?
O2 Fe1 N8 173.5(3) . . ?
N7 Fe1 N8 81.8(3) . . ?
O1 Fe1 N2 92.4(3) . 4_545 ?
O2 Fe1 N2 93.8(3) . 4_545 ?
N7 Fe1 N2 85.7(3) . 4_545 ?
N8 Fe1 N2 87.3(3) . 4_545 ?
O1 Fe1 N1 92.8(3) . . ?
O2 Fe1 N1 91.4(2) . . ?
N7 Fe1 N1 88.6(3) . . ?
N8 Fe1 N1 87.0(3) . . ?
N2 Fe1 N1 172.4(3) 4_545 . ?
N1 C1 Os1 177.6(6) . . ?
N2 C2 Os1 176.4(9) . . ?
N6 C22 C21 122.5(11) . . ?
N6 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
C20 C21 C22 117.2(12) . . ?
C20 C21 H21A 121.4 . . ?
C22 C21 H21A 121.4 . . ?
C21 C20 C19 120.4(12) . . ?
C21 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
C18 C19 C20 117.3(12) . . ?
C18 C19 H19A 121.4 . . ?
C20 C19 H19A 121.4 . . ?
C19 C18 N6 125.7(11) . . ?
C19 C18 C17 122.1(10) . . ?
N6 C18 C17 112.1(8) . . ?
N5 C17 C16 121.6(11) . . ?
N5 C17 C18 117.1(8) . . ?
C16 C17 C18 121.2(10) . . ?
C15 C16 C17 117.3(13) . . ?
C15 C16 H16A 121.3 . . ?
C17 C16 H16A 121.3 . . ?
C14 C15 C16 122.3(14) . . ?
C14 C15 H15A 118.9 . . ?
C16 C15 H15A 118.9 . . ?
C15 C14 C13 120.0(13) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
N5 C13 C14 119.7(12) . . ?
N5 C13 H13A 120.2 . . ?
C14 C13 H13A 120.2 . . ?
N4 C12 C11 121.0(12) . . ?
N4 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C10 C11 C12 119.4(15) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C9 C10 C11 120.6(17) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C10 C9 C8 119.2(15) . . ?
C10 C9 H9A 120.4 . . ?
C8 C9 H9A 120.4 . . ?
N4 C8 C9 121.0(11) . . ?
N4 C8 C7 115.5(9) . . ?
C9 C8 C7 123.3(10) . . ?
N3 C7 C6 121.4(11) . . ?
N3 C7 C8 114.8(8) . . ?
C6 C7 C8 123.8(11) . . ?
C5 C6 C7 120.3(13) . . ?
C5 C6 H6A 119.9 . . ?
C7 C6 H6A 119.9 . . ?
C4 C5 C6 118.3(12) . . ?
C4 C5 H5A 120.8 . . ?
C6 C5 H5A 120.8 . . ?
C5 C4 C3 120.0(13) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
N3 C3 C4 121.2(12) . . ?
N3 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
O1 C23 C28 123.7(8) . . ?
O1 C23 C24 117.8(8) . . ?
C28 C23 C24 118.5(8) . . ?
C25 C24 C23 121.1(11) . . ?
C25 C24 H24A 119.4 . . ?
C23 C24 H24A 119.4 . . ?
C24 C25 C26 120.1(11) . . ?
C24 C25 H25A 119.9 . . ?
C26 C25 H25A 119.9 . . ?
C27 C26 C25 120.4(11) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 121.2(12) . . ?
C26 C27 H27A 119.4 . . ?
C28 C27 H27A 119.4 . . ?
C23 C28 C27 118.6(9) . . ?
C23 C28 C29 124.1(7) . . ?
C27 C28 C29 117.2(9) . . ?
N8 C29 C28 123.9(7) . . ?
N8 C29 H29A 118.0 . . ?
C28 C29 H29A 118.0 . . ?
N8 C30A C31A 105.3(17) . . ?
N8 C30A H30A 110.7 . . ?
C31A C30A H30A 110.7 . . ?
N8 C30A H30B 110.7 . . ?
C31A C30A H30B 110.7 . . ?
H30A C30A H30B 108.8 . . ?
N7 C31A C30A 104.1(18) . . ?
N7 C31A H31A 110.9 . . ?
C30A C31A H31A 110.9 . . ?
N7 C31A H31B 110.9 . . ?
C30A C31A H31B 110.9 . . ?
H31A C31A H31B 109.0 . . ?
C31B C30B N8 107(3) . . ?
C31B C30B H30C 110.3 . . ?
N8 C30B H30C 110.3 . . ?
C31B C30B H30D 110.3 . . ?
N8 C30B H30D 110.3 . . ?
H30C C30B H30D 108.5 . . ?
C30B C31B N7 104(2) . . ?
C30B C31B H31C 110.9 . . ?
N7 C31B H31C 110.9 . . ?
C30B C31B H31D 110.9 . . ?
N7 C31B H31D 110.9 . . ?
H31C C31B H31D 108.9 . . ?
N7 C32 C33 125.5(8) . . ?
N7 C32 H32A 117.2 . . ?
C33 C32 H32A 117.2 . . ?
C34 C33 C32 117.8(8) . . ?
C34 C33 C38 118.9(8) . . ?
C32 C33 C38 123.2(7) . . ?
C35 C34 C33 121.6(10) . . ?
C35 C34 H34A 119.2 . . ?
C33 C34 H34A 119.2 . . ?
C36 C35 C34 118.7(10) . . ?
C36 C35 H35A 120.6 . . ?
C34 C35 H35A 120.6 . . ?
C37 C36 C35 121.0(10) . . ?
C37 C36 H36A 119.5 . . ?
C35 C36 H36A 119.5 . . ?
C36 C37 C38 122.5(10) . . ?
C36 C37 H37A 118.7 . . ?
C38 C37 H37A 118.7 . . ?
O2 C38 C37 118.8(8) . . ?
O2 C38 C33 124.0(7) . . ?
C37 C38 C33 117.2(8) . . ?
C1 N1 Fe1 145.1(6) . . ?
C2 N2 Fe1 160.1(7) . 4 ?
C22 N6 C18 116.8(8) . . ?
C22 N6 Os1 125.5(7) . . ?
C18 N6 Os1 117.5(6) . . ?
C17 N5 C13 119.0(9) . . ?
C17 N5 Os1 116.3(6) . . ?
C13 N5 Os1 124.7(7) . . ?
C12 N4 C8 118.4(9) . . ?
C12 N4 Os1 125.1(7) . . ?
C8 N4 Os1 116.3(7) . . ?
C3 N3 C7 118.8(8) . . ?
C3 N3 Os1 125.2(7) . . ?
C7 N3 Os1 115.8(6) . . ?
C32 N7 C31A 118.1(9) . . ?
C32 N7 C31B 121.0(10) . . ?
C31A N7 C31B 32.6(9) . . ?
C32 N7 Fe1 126.4(6) . . ?
C31A N7 Fe1 111.9(8) . . ?
C31B N7 Fe1 111.3(9) . . ?
C29 N8 C30B 120.8(15) . . ?
C29 N8 C30A 119.5(11) . . ?
C30B N8 C30A 23.0(11) . . ?
C29 N8 Fe1 126.6(6) . . ?
C30B N8 Fe1 111.5(14) . . ?
C30A N8 Fe1 112.6(11) . . ?
C23 O1 Fe1 129.3(5) . . ?
C38 O2 Fe1 128.5(5) . . ?
F5 P2 F4 104.1(13) 5 5 ?
F5 P2 F8 100.9(13) 5 5 ?
F4 P2 F8 98.2(13) 5 5 ?
F5 P2 P2 64.4(9) 5 5 ?
F4 P2 P2 62.8(9) 5 5 ?
F8 P2 P2 62.0(8) 5 5 ?
F5 P2 F6 131.7(12) 5 . ?
F4 P2 F6 67.6(11) 5 . ?
F8 P2 F6 127.1(12) 5 . ?
P2 P2 F6 130.5(13) 5 . ?
F5 P2 F7 64.5(11) 5 . ?
F4 P2 F7 130.2(12) 5 . ?
F8 P2 F7 131.0(12) 5 . ?
P2 P2 F7 128.9(12) 5 . ?
F6 P2 F7 84.6(13) . . ?
F5 P2 F9 129.9(12) 5 . ?
F4 P2 F9 124.3(12) 5 . ?
F8 P2 F9 63.3(10) 5 . ?
P2 P2 F9 125.2(11) 5 . ?
F6 P2 F9 82.9(13) . . ?
F7 P2 F9 89.8(13) . . ?
F5 P2 F8 52.7(11) 5 . ?
F4 P2 F8 54.0(10) 5 . ?
F8 P2 F8 119.5(9) 5 . ?
P2 P2 F8 57.6(9) 5 . ?
F6 P2 F8 93.6(10) . . ?
F7 P2 F8 89.5(9) . . ?
F9 P2 F8 176.5(12) . . ?
F5 P2 F5 117.5(10) 5 . ?
F4 P2 F5 48.3(10) 5 . ?
F8 P2 F5 50.9(10) 5 . ?
P2 P2 F5 53.0(9) 5 . ?
F6 P2 F5 92.8(10) . . ?
F7 P2 F5 177.5(12) . . ?
F9 P2 F5 89.9(9) . . ?
F8 P2 F5 90.5(9) . . ?
F5 P2 F4 49.3(10) 5 . ?
F4 P2 F4 119.3(9) 5 . ?
F8 P2 F4 53.5(10) 5 . ?
P2 P2 F4 56.4(9) 5 . ?
F6 P2 F4 173.1(13) . . ?
F7 P2 F4 90.6(9) . . ?
F9 P2 F4 92.1(9) . . ?
F8 P2 F4 91.4(9) . . ?
F5 P2 F4 91.9(9) . . ?
P2 F9 F8 56.3(8) . 5 ?
F5 F8 F4 113.3(15) 5 5 ?
F5 F8 P2 67.4(11) 5 5 ?
F4 F8 P2 66.1(10) 5 5 ?
F5 F8 P2 56.8(10) 5 . ?
F4 F8 P2 59.6(10) 5 . ?
P2 F8 P2 60.5(9) 5 . ?
F5 F8 F9 97.9(17) 5 5 ?
F4 F8 F9 97.9(16) 5 5 ?
P2 F8 F9 60.4(9) 5 5 ?
P2 F8 F9 120.8(13) . 5 ?
P2 F7 F5 52.5(8) . 5 ?
P2 F6 F4 54.2(8) . 5 ?
F4 F5 F8 122.1(17) 5 5 ?
F4 F5 P2 73.1(12) 5 5 ?
F8 F5 P2 70.6(12) 5 5 ?
F4 F5 P2 61.9(11) 5 . ?
F8 F5 P2 61.7(11) 5 . ?
P2 F5 P2 62.5(10) 5 . ?
F4 F5 F7 103.4(17) 5 5 ?
F8 F5 F7 98.4(17) 5 5 ?
P2 F5 F7 63.1(11) 5 5 ?
P2 F5 F7 125.6(14) . 5 ?
F5 F4 F8 115.6(17) 5 5 ?
F5 F4 P2 69.8(11) 5 5 ?
F8 F4 P2 66.4(10) 5 5 ?
F5 F4 P2 57.6(11) 5 . ?
F8 F4 P2 60.4(10) 5 . ?
P2 F4 P2 60.7(9) 5 . ?
F5 F4 F6 99.7(16) 5 5 ?
F8 F4 F6 95.0(15) 5 5 ?
P2 F4 F6 58.2(10) 5 5 ?
P2 F4 F6 118.9(13) . 5 ?
F1A P1 F1A 96.9(10) 2_655 . ?
F1A P1 F1 121.2(9) 2_655 . ?
F1A P1 F1 111.7(9) . . ?
F1A P1 F1 111.7(9) 2_655 2_655 ?
F1A P1 F1 121.2(9) . 2_655 ?
F1 P1 F1 96.1(10) . 2_655 ?
F1A P1 F2 138.0(9) 2_655 . ?
F1A P1 F2 42.0(7) . . ?
F1 P1 F2 89.3(7) . . ?
F1 P1 F2 90.8(6) 2_655 . ?
F1A P1 F2 42.0(7) 2_655 2_655 ?
F1A P1 F2 138.0(9) . 2_655 ?
F1 P1 F2 90.8(6) . 2_655 ?
F1 P1 F2 89.3(7) 2_655 2_655 ?
F2 P1 F2 180.0(15) . 2_655 ?
F1A P1 F2A 94.7(6) 2_655 . ?
F1A P1 F2A 93.4(7) . . ?
F1 P1 F2A 36.4(6) . . ?
F1 P1 F2A 131.6(8) 2_655 . ?
F2 P1 F2A 95.8(9) . . ?
F2 P1 F2A 84.2(9) 2_655 . ?
F1A P1 F2A 93.4(7) 2_655 2_655 ?
F1A P1 F2A 94.7(6) . 2_655 ?
F1 P1 F2A 131.6(8) . 2_655 ?
F1 P1 F2A 36.4(6) 2_655 2_655 ?
F2 P1 F2A 84.2(9) . 2_655 ?
F2 P1 F2A 95.8(9) 2_655 2_655 ?
F2A P1 F2A 167.9(10) . 2_655 ?
F1A P1 F3 55.4(8) 2_655 2_655 ?
F1A P1 F3 63.8(8) . 2_655 ?
F1 P1 F3 172.4(10) . 2_655 ?
F1 P1 F3 91.5(8) 2_655 2_655 ?
F2 P1 F3 90.5(8) . 2_655 ?
F2 P1 F3 89.5(8) 2_655 2_655 ?
F2A P1 F3 136.2(10) . 2_655 ?
F2A P1 F3 55.9(8) 2_655 2_655 ?
F1A P1 F3 63.8(8) 2_655 . ?
F1A P1 F3 55.4(8) . . ?
F1 P1 F3 91.5(8) . . ?
F1 P1 F3 172.4(10) 2_655 . ?
F2 P1 F3 89.5(8) . . ?
F2 P1 F3 90.5(8) 2_655 . ?
F2A P1 F3 55.9(8) . . ?
F2A P1 F3 136.2(10) 2_655 . ?
F3 P1 F3 80.9(15) 2_655 . ?
F1A P1 F3A 172.6(10) 2_655 . ?
F1A P1 F3A 90.3(7) . . ?
F1 P1 F3A 56.7(8) . . ?
F1 P1 F3A 62.9(8) 2_655 . ?
F2 P1 F3A 48.9(8) . . ?
F2 P1 F3A 131.1(11) 2_655 . ?
F2A P1 F3A 86.3(6) . . ?
F2A P1 F3A 84.6(7) 2_655 . ?
F3 P1 F3A 127.7(9) 2_655 . ?
F3 P1 F3A 122.2(9) . . ?
F1A P1 F3A 90.3(7) 2_655 2_655 ?
F1A P1 F3A 172.6(10) . 2_655 ?
F1 P1 F3A 62.9(8) . 2_655 ?
F1 P1 F3A 56.7(8) 2_655 2_655 ?
F2 P1 F3A 131.1(11) . 2_655 ?
F2 P1 F3A 48.9(8) 2_655 2_655 ?
F2A P1 F3A 84.6(7) . 2_655 ?
F2A P1 F3A 86.3(6) 2_655 2_655 ?
F3 P1 F3A 122.2(9) 2_655 2_655 ?
F3 P1 F3A 127.7(9) . 2_655 ?
F3A P1 F3A 82.4(14) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.147
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.136
_database_code_depnum_ccdc_archive 'CCDC 1015603'
