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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1059106'
_audit_update_record             
;
2015-04-13 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H43 F6 Fe2 O2 P S2'
_chemical_formula_weight         708.39

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'
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'
S S 0.1246 0.1234 '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   '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                   12.034(3)
_cell_length_b                   15.336(4)
_cell_length_c                   17.019(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.739(4)
_cell_angle_gamma                90.00
_cell_volume                     3139.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_T_max  0.7672
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7926
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2759
_reflns_number_gt                2383
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0627P)²+12.0628P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2759
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1387
_refine_ls_wR_factor_gt          0.1343
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
P1 P 0.5000 0.5000 0.5000 0.0683(5) Uani 1 2 d S . .
O1 O 0.5898(2) 0.72987(17) 0.76939(16) 0.0493(7) Uani 1 1 d . . .
S1 S 0.54088(9) 0.86534(6) 0.65065(6) 0.0479(3) Uani 1 1 d . . .
Fe1 Fe 0.60431(5) 0.85822(3) 0.77302(3) 0.0413(2) Uani 1 1 d . . .
C1 C 0.6719(3) 0.9752(2) 0.8119(3) 0.0787(17) Uani 1 1 d G . .
C2 C 0.7062(3) 0.9042(3) 0.8711(2) 0.0804(17) Uani 1 1 d G . .
C3 C 0.7636(3) 0.8434(2) 0.8260(2) 0.0700(14) Uani 1 1 d G . .
C4 C 0.7717(3) 0.8772(2) 0.7497(2) 0.0664(13) Uani 1 1 d G . .
C5 C 0.7193(3) 0.9589(2) 0.7477(2) 0.0714(14) Uani 1 1 d G . .
C6 C 0.6160(7) 1.0576(5) 0.8415(6) 0.144(4) Uani 1 1 d . . .
H6A H 0.6717 1.1003 0.8550 0.216 Uiso 1 1 calc R . .
H6B H 0.5742 1.0440 0.8870 0.216 Uiso 1 1 calc R . .
H6C H 0.5669 1.0805 0.8010 0.216 Uiso 1 1 calc R . .
C7 C 0.6822(6) 0.9007(7) 0.9556(4) 0.148(4) Uani 1 1 d . . .
H7A H 0.7430 0.9258 0.9856 0.221 Uiso 1 1 calc R . .
H7B H 0.6725 0.8410 0.9712 0.221 Uiso 1 1 calc R . .
H7C H 0.6155 0.9328 0.9651 0.221 Uiso 1 1 calc R . .
C8 C 0.8142(6) 0.7619(5) 0.8581(5) 0.126(3) Uani 1 1 d . . .
H8A H 0.8875 0.7742 0.8790 0.189 Uiso 1 1 calc R . .
H8B H 0.8186 0.7194 0.8169 0.189 Uiso 1 1 calc R . .
H8C H 0.7692 0.7395 0.8991 0.189 Uiso 1 1 calc R . .
C9 C 0.8355(5) 0.8335(6) 0.6844(5) 0.117(3) Uani 1 1 d . . .
H9A H 0.9110 0.8537 0.6861 0.176 Uiso 1 1 calc R . .
H9B H 0.8012 0.8478 0.6344 0.176 Uiso 1 1 calc R . .
H9C H 0.8343 0.7714 0.6916 0.176 Uiso 1 1 calc R . .
C10 C 0.7160(6) 1.0181(4) 0.6756(5) 0.113(3) Uani 1 1 d . . .
H10A H 0.7774 1.0580 0.6787 0.169 Uiso 1 1 calc R . .
H10B H 0.6475 1.0502 0.6738 0.169 Uiso 1 1 calc R . .
H10C H 0.7209 0.9832 0.6290 0.169 Uiso 1 1 calc R . .
C11 C 0.5604(5) 0.7649(3) 0.5946(3) 0.0680(13) Uani 1 1 d . . .
H11A H 0.6171 0.7292 0.6205 0.082 Uiso 1 1 calc R . .
H11B H 0.4916 0.7320 0.5920 0.082 Uiso 1 1 calc R . .
C12 C 0.5953(6) 0.7877(5) 0.5125(3) 0.098(2) Uani 1 1 d . . .
H12A H 0.6054 0.7351 0.4830 0.147 Uiso 1 1 calc R . .
H12B H 0.6639 0.8196 0.5154 0.147 Uiso 1 1 calc R . .
H12C H 0.5388 0.8228 0.4871 0.147 Uiso 1 1 calc R . .
C13 C 0.5000 0.6921(4) 0.7500 0.0527(15) Uani 1 2 d S . .
C14 C 0.5000 0.5946(5) 0.7500 0.095(3) Uani 1 2 d S . .
H14A H 0.4274 0.5737 0.7344 0.143 Uiso 0.50 1 calc PR . .
H14B H 0.5190 0.5737 0.8019 0.143 Uiso 0.50 1 calc PR . .
H14C H 0.5535 0.5737 0.7138 0.143 Uiso 0.50 1 calc PR . .
F1 F 0.4722(4) 0.5560(4) 0.4267(3) 0.165(2) Uani 1 1 d . . .
F2 F 0.4331(4) 0.5670(3) 0.5496(3) 0.1403(18) Uani 1 1 d . . .
F3 F 0.6100(3) 0.5524(3) 0.5156(4) 0.1444(19) 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
P1 F1 1.542(4) . ?
P1 F1 1.542(4) 5_666 ?
P1 F3 1.565(4) 5_666 ?
P1 F3 1.565(4) . ?
P1 F2 1.568(4) 5_666 ?
P1 F2 1.568(4) . ?
O1 C13 1.261(4) . ?
O1 Fe1 1.977(3) . ?
S1 C11 1.830(5) . ?
S1 Fe1 2.1990(13) . ?
S1 Fe1 2.2114(12) 2_656 ?
Fe1 C1 2.070(3) . ?
Fe1 C4 2.085(3) . ?
Fe1 C3 2.106(4) . ?
Fe1 C5 2.127(3) . ?
Fe1 C2 2.160(4) . ?
Fe1 S1 2.2114(12) 2_656 ?
Fe1 Fe1 2.6071(13) 2_656 ?
C1 C5 1.272(2) . ?
C1 C6 1.524(7) . ?
C1 C2 1.532(3) . ?
C2 C3 1.404(3) . ?
C2 C7 1.477(7) . ?
C3 C4 1.404(3) . ?
C3 C8 1.487(7) . ?
C4 C5 1.404(3) . ?
C4 C9 1.525(7) . ?
C5 C10 1.526(7) . ?
C11 C12 1.511(7) . ?
C13 O1 1.261(4) 2_656 ?
C13 C14 1.496(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 P1 F1 180.0(2) . 5_666 ?
F1 P1 F3 89.2(3) . 5_666 ?
F1 P1 F3 90.8(3) 5_666 5_666 ?
F1 P1 F3 90.8(3) . . ?
F1 P1 F3 89.2(3) 5_666 . ?
F3 P1 F3 180.0(3) 5_666 . ?
F1 P1 F2 91.8(3) . 5_666 ?
F1 P1 F2 88.2(3) 5_666 5_666 ?
F3 P1 F2 91.0(3) 5_666 5_666 ?
F3 P1 F2 89.0(3) . 5_666 ?
F1 P1 F2 88.2(3) . . ?
F1 P1 F2 91.8(3) 5_666 . ?
F3 P1 F2 89.0(3) 5_666 . ?
F3 P1 F2 91.0(3) . . ?
F2 P1 F2 180.0(3) 5_666 . ?
C13 O1 Fe1 122.6(3) . . ?
C11 S1 Fe1 113.92(17) . . ?
C11 S1 Fe1 112.40(18) . 2_656 ?
Fe1 S1 Fe1 72.47(4) . 2_656 ?
O1 Fe1 C1 155.03(15) . . ?
O1 Fe1 C4 102.57(13) . . ?
C1 Fe1 C4 64.39(12) . . ?
O1 Fe1 C3 89.08(13) . . ?
C1 Fe1 C3 67.27(12) . . ?
C4 Fe1 C3 39.13(8) . . ?
O1 Fe1 C5 140.73(14) . . ?
C1 Fe1 C5 35.26(7) . . ?
C4 Fe1 C5 38.92(8) . . ?
C3 Fe1 C5 64.90(12) . . ?
O1 Fe1 C2 113.39(14) . . ?
C1 Fe1 C2 42.41(8) . . ?
C4 Fe1 C2 64.66(12) . . ?
C3 Fe1 C2 38.39(7) . . ?
C5 Fe1 C2 63.98(12) . . ?
O1 Fe1 S1 89.55(8) . . ?
C1 Fe1 S1 112.40(13) . . ?
C4 Fe1 S1 97.04(11) . . ?
C3 Fe1 S1 134.12(11) . . ?
C5 Fe1 S1 88.94(12) . . ?
C2 Fe1 S1 152.67(11) . . ?
O1 Fe1 S1 89.83(9) . 2_656 ?
C1 Fe1 S1 94.54(11) . 2_656 ?
C4 Fe1 S1 152.85(11) . 2_656 ?
C3 Fe1 S1 118.62(12) . 2_656 ?
C5 Fe1 S1 127.85(12) . 2_656 ?
C2 Fe1 S1 88.29(11) . 2_656 ?
S1 Fe1 S1 107.23(4) . 2_656 ?
O1 Fe1 Fe1 84.69(8) . 2_656 ?
C1 Fe1 Fe1 117.46(11) . 2_656 ?
C4 Fe1 Fe1 150.45(11) . 2_656 ?
C3 Fe1 Fe1 169.87(10) . 2_656 ?
C5 Fe1 Fe1 124.45(10) . 2_656 ?
C2 Fe1 Fe1 138.71(11) . 2_656 ?
S1 Fe1 Fe1 53.98(3) . 2_656 ?
S1 Fe1 Fe1 53.54(4) 2_656 2_656 ?
C5 C1 C6 131.3(5) . . ?
C5 C1 C2 107.8 . . ?
C6 C1 C2 119.0(5) . . ?
C5 C1 Fe1 74.80(13) . . ?
C6 C1 Fe1 130.7(4) . . ?
C2 C1 Fe1 71.92(13) . . ?
C3 C2 C7 128.5(5) . . ?
C3 C2 C1 103.9 . . ?
C7 C2 C1 127.6(5) . . ?
C3 C2 Fe1 68.73(13) . . ?
C7 C2 Fe1 128.1(3) . . ?
C1 C2 Fe1 65.67(13) . . ?
C2 C3 C4 108.0 . . ?
C2 C3 C8 124.1(5) . . ?
C4 C3 C8 127.7(5) . . ?
C2 C3 Fe1 72.87(13) . . ?
C4 C3 Fe1 69.62(13) . . ?
C8 C3 Fe1 127.3(3) . . ?
C5 C4 C3 108.0 . . ?
C5 C4 C9 127.6(4) . . ?
C3 C4 C9 124.2(4) . . ?
C5 C4 Fe1 72.15(13) . . ?
C3 C4 Fe1 71.25(13) . . ?
C9 C4 Fe1 126.0(4) . . ?
C1 C5 C4 111.6 . . ?
C1 C5 C10 124.9(4) . . ?
C4 C5 C10 123.5(4) . . ?
C1 C5 Fe1 69.95(13) . . ?
C4 C5 Fe1 68.93(13) . . ?
C10 C5 Fe1 126.4(4) . . ?
C12 C11 S1 109.3(4) . . ?
O1 C13 O1 125.3(5) 2_656 . ?
O1 C13 C14 117.3(3) 2_656 . ?
O1 C13 C14 117.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.068
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1059107'
_audit_update_record             
;
2015-04-13 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H45 F6 Fe2 O2 P S2'
_chemical_formula_weight         722.42

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'
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'
S S 0.1246 0.1234 '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           Tetragonal
_symmetry_space_group_name_H-M   'P4(1)2(1)2 '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   13.0082(4)
_cell_length_b                   13.0082(4)
_cell_length_c                   38.517(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6517.6(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7218
_exptl_absorpt_correction_T_max  0.8146
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44596
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5745
_reflns_number_gt                4899
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0879P)²+2.6986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_number_reflns         5745
_refine_ls_number_parameters     355
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1355
_refine_ls_wR_factor_gt          0.1290
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.004
_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
P1 P 0.99399(17) 0.98932(16) 0.13169(5) 0.0985(6) Uani 1 1 d . . .
Fe1 Fe 0.56268(5) 0.94890(5) 0.018256(15) 0.05246(18) Uani 1 1 d . . .
Fe2 Fe 0.40048(5) 1.01939(5) 0.050620(16) 0.05603(19) Uani 1 1 d . . .
S1 S 0.40009(9) 0.91985(9) 0.00455(3) 0.0571(3) Uani 1 1 d . . .
S2 S 0.56155(10) 1.03306(10) 0.06805(3) 0.0630(3) Uani 1 1 d . . .
O1 O 0.5582(3) 1.0811(2) -0.00710(8) 0.0649(8) Uani 1 1 d . . .
O2 O 0.4194(3) 1.1416(3) 0.02065(9) 0.0675(9) Uani 1 1 d . . .
C1 C 0.6646(3) 0.8424(3) 0.04108(9) 0.0742(14) Uani 1 1 d G . .
C2 C 0.5951(3) 0.7898(3) 0.01895(11) 0.0750(15) Uani 1 1 d G . .
C3 C 0.6091(3) 0.8277(3) -0.01531(10) 0.0740(14) Uani 1 1 d G . .
C4 C 0.6872(3) 0.9039(3) -0.01431(9) 0.0677(13) Uani 1 1 d G . .
C5 C 0.7215(3) 0.9129(3) 0.02058(9) 0.0692(13) Uani 1 1 d G . .
C6 C 0.6826(6) 0.8179(6) 0.07839(15) 0.105(2) Uani 1 1 d . . .
H6A H 0.7343 0.7655 0.0802 0.157 Uiso 1 1 calc R . .
H6B H 0.6198 0.7938 0.0887 0.157 Uiso 1 1 calc R . .
H6C H 0.7054 0.8786 0.0903 0.157 Uiso 1 1 calc R . .
C7 C 0.5230(7) 0.7047(5) 0.0297(2) 0.118(3) Uani 1 1 d . . .
H7A H 0.5573 0.6396 0.0276 0.176 Uiso 1 1 calc R . .
H7B H 0.4633 0.7054 0.0151 0.176 Uiso 1 1 calc R . .
H7C H 0.5025 0.7148 0.0534 0.176 Uiso 1 1 calc R . .
C8 C 0.5573(6) 0.7885(5) -0.04808(17) 0.103(2) Uani 1 1 d . . .
H8A H 0.5966 0.7327 -0.0575 0.155 Uiso 1 1 calc R . .
H8B H 0.5533 0.8430 -0.0648 0.155 Uiso 1 1 calc R . .
H8C H 0.4893 0.7649 -0.0426 0.155 Uiso 1 1 calc R . .
C9 C 0.7250(5) 0.9638(6) -0.04416(16) 0.097(2) Uani 1 1 d . . .
H9A H 0.7814 0.9281 -0.0548 0.146 Uiso 1 1 calc R . .
H9B H 0.7478 1.0301 -0.0363 0.146 Uiso 1 1 calc R . .
H9C H 0.6706 0.9723 -0.0607 0.146 Uiso 1 1 calc R . .
C10 C 0.8040(5) 0.9836(6) 0.0329(2) 0.101(2) Uani 1 1 d . . .
H10A H 0.8693 0.9495 0.0314 0.151 Uiso 1 1 calc R . .
H10B H 0.7909 1.0027 0.0566 0.151 Uiso 1 1 calc R . .
H10C H 0.8050 1.0441 0.0186 0.151 Uiso 1 1 calc R . .
C11 C 0.2765(4) 1.0936(4) 0.07522(15) 0.104(2) Uani 1 1 d G . .
C12 C 0.2403(3) 1.0054(5) 0.05842(12) 0.105(3) Uani 1 1 d G . .
C13 C 0.2897(4) 0.9201(4) 0.07303(12) 0.0922(19) Uani 1 1 d G . .
C14 C 0.3565(4) 0.9557(4) 0.09886(10) 0.0774(15) Uani 1 1 d G . .
C15 C 0.3483(4) 1.0629(4) 0.10025(12) 0.098(2) Uani 1 1 d G . .
C16 C 0.2424(9) 1.2015(8) 0.0671(3) 0.224(8) Uani 1 1 d . . .
H16A H 0.1847 1.2191 0.0814 0.337 Uiso 1 1 calc R . .
H16B H 0.2230 1.2058 0.0431 0.337 Uiso 1 1 calc R . .
H16C H 0.2979 1.2483 0.0715 0.337 Uiso 1 1 calc R . .
C17 C 0.1582(6) 0.9972(12) 0.0307(2) 0.180(6) Uani 1 1 d . . .
H17A H 0.0919 0.9923 0.0415 0.270 Uiso 1 1 calc R . .
H17B H 0.1703 0.9370 0.0169 0.270 Uiso 1 1 calc R . .
H17C H 0.1604 1.0571 0.0162 0.270 Uiso 1 1 calc R . .
C18 C 0.2645(7) 0.8086(8) 0.0648(2) 0.159(5) Uani 1 1 d . . .
H18A H 0.2098 0.7855 0.0796 0.239 Uiso 1 1 calc R . .
H18B H 0.3243 0.7668 0.0686 0.239 Uiso 1 1 calc R . .
H18C H 0.2436 0.8030 0.0409 0.239 Uiso 1 1 calc R . .
C19 C 0.4155(7) 0.8876(8) 0.1225(2) 0.142(4) Uani 1 1 d . . .
H19A H 0.3747 0.8720 0.1426 0.213 Uiso 1 1 calc R . .
H19B H 0.4775 0.9216 0.1296 0.213 Uiso 1 1 calc R . .
H19C H 0.4326 0.8250 0.1106 0.213 Uiso 1 1 calc R . .
C20 C 0.4039(8) 1.1273(10) 0.1272(2) 0.177(5) Uani 1 1 d . . .
H20A H 0.3619 1.1334 0.1476 0.266 Uiso 1 1 calc R . .
H20B H 0.4173 1.1944 0.1179 0.266 Uiso 1 1 calc R . .
H20C H 0.4677 1.0947 0.1332 0.266 Uiso 1 1 calc R . .
C21 C 0.3589(5) 0.9864(5) -0.03492(13) 0.0803(16) Uani 1 1 d . . .
H21A H 0.3246 1.0501 -0.0288 0.096 Uiso 1 1 calc R . .
H21B H 0.4184 1.0031 -0.0490 0.096 Uiso 1 1 calc R . .
C22 C 0.2855(6) 0.9178(6) -0.05558(18) 0.113(2) Uani 1 1 d . . .
H22A H 0.2645 0.9528 -0.0763 0.169 Uiso 1 1 calc R . .
H22B H 0.2261 0.9025 -0.0417 0.169 Uiso 1 1 calc R . .
H22C H 0.3198 0.8550 -0.0617 0.169 Uiso 1 1 calc R . .
C23 C 0.6120(4) 1.1651(5) 0.06557(16) 0.0806(16) Uani 1 1 d . . .
H23A H 0.6530 1.1731 0.0447 0.097 Uiso 1 1 calc R . .
H23B H 0.5554 1.2136 0.0645 0.097 Uiso 1 1 calc R . .
C24 C 0.6770(6) 1.1868(7) 0.09711(18) 0.111(2) Uani 1 1 d . . .
H24A H 0.7029 1.2559 0.0959 0.167 Uiso 1 1 calc R . .
H24B H 0.7336 1.1395 0.0978 0.167 Uiso 1 1 calc R . .
H24C H 0.6361 1.1790 0.1177 0.167 Uiso 1 1 calc R . .
C25 C 0.4906(4) 1.1484(4) -0.00153(13) 0.0659(12) Uani 1 1 d . A .
C26 C 0.4964(8) 1.2460(6) -0.0226(3) 0.131(3) Uani 1 1 d U . .
H26A H 0.5626 1.2457 -0.0343 0.157 Uiso 1 1 d R A .
H26B H 0.4445 1.2409 -0.0406 0.157 Uiso 1 1 d R . .
C27 C 0.4840(18) 1.3382(14) -0.0077(5) 0.190(7) Uani 0.618(15) 1 d PU A 1
H27A H 0.4876 1.3910 -0.0251 0.285 Uiso 0.618(15) 1 calc PR A 1
H27B H 0.5373 1.3489 0.0092 0.285 Uiso 0.618(15) 1 calc PR A 1
H27C H 0.4182 1.3408 0.0036 0.285 Uiso 0.618(15) 1 calc PR A 1
C27' C 0.535(3) 1.265(2) -0.0463(9) 0.189(9) Uani 0.382(15) 1 d PU A 2
H27D H 0.5083 1.3282 -0.0554 0.284 Uiso 0.382(15) 1 calc PR A 2
H27E H 0.5255 1.2110 -0.0629 0.284 Uiso 0.382(15) 1 calc PR A 2
H27F H 0.6076 1.2731 -0.0417 0.284 Uiso 0.382(15) 1 calc PR A 2
F1 F 0.9001(10) 1.0440(15) 0.1344(3) 0.370(11) Uani 1 1 d . . .
F2 F 1.0590(14) 1.0718(10) 0.1431(4) 0.366(9) Uani 1 1 d . . .
F3 F 1.0907(11) 0.9361(11) 0.1260(4) 0.332(8) Uani 1 1 d . . .
F4 F 0.9406(14) 0.9024(11) 0.1201(4) 0.354(9) Uani 1 1 d . . .
F5 F 0.9846(7) 0.9590(11) 0.16741(17) 0.281(6) Uani 1 1 d . . .
F6 F 1.0038(10) 1.0311(10) 0.0950(2) 0.270(5) 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
P1 F4 1.400(8) . ?
P1 F1 1.418(8) . ?
P1 F2 1.435(10) . ?
P1 F5 1.436(7) . ?
P1 F3 1.453(9) . ?
P1 F6 1.520(8) . ?
Fe1 O1 1.978(3) . ?
Fe1 C1 2.109(4) . ?
Fe1 C2 2.113(4) . ?
Fe1 C5 2.120(4) . ?
Fe1 C3 2.126(4) . ?
Fe1 C4 2.131(4) . ?
Fe1 S2 2.2084(13) . ?
Fe1 S1 2.2124(13) . ?
Fe1 Fe2 2.6166(9) . ?
Fe2 O2 1.980(3) . ?
Fe2 C11 2.105(4) . ?
Fe2 C15 2.106(4) . ?
Fe2 C14 2.113(4) . ?
Fe2 C12 2.114(4) . ?
Fe2 C13 2.118(4) . ?
Fe2 S1 2.1968(13) . ?
Fe2 S2 2.2073(14) . ?
S1 C21 1.830(5) . ?
S2 C23 1.841(6) . ?
O1 C25 1.260(6) . ?
O2 C25 1.263(6) . ?
C1 C2 1.419(3) . ?
C1 C5 1.419(3) . ?
C1 C6 1.491(7) . ?
C2 C3 1.421(3) . ?
C2 C7 1.509(8) . ?
C3 C4 1.420(3) . ?
C3 C8 1.519(7) . ?
C4 C5 1.421(3) . ?
C4 C9 1.474(7) . ?
C5 C10 1.491(7) . ?
C11 C12 1.399(3) . ?
C11 C15 1.401(3) . ?
C11 C16 1.504(10) . ?
C12 C13 1.400(3) . ?
C12 C17 1.513(9) . ?
C13 C14 1.399(3) . ?
C13 C18 1.522(10) . ?
C14 C15 1.400(3) . ?
C14 C19 1.484(9) . ?
C15 C20 1.517(9) . ?
C21 C22 1.530(8) . ?
C23 C24 1.507(8) . ?
C25 C26 1.511(8) . ?
C26 C27' 1.07(3) . ?
C26 C27 1.340(19) . ?

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
F4 P1 F1 90.0(11) . . ?
F4 P1 F2 173.6(11) . . ?
F1 P1 F2 96.3(10) . . ?
F4 P1 F5 92.5(8) . . ?
F1 P1 F5 89.6(7) . . ?
F2 P1 F5 87.8(8) . . ?
F4 P1 F3 89.8(10) . . ?
F1 P1 F3 175.4(7) . . ?
F2 P1 F3 83.8(11) . . ?
F5 P1 F3 95.0(7) . . ?
F4 P1 F6 91.9(8) . . ?
F1 P1 F6 87.8(7) . . ?
F2 P1 F6 88.1(8) . . ?
F5 P1 F6 175.0(8) . . ?
F3 P1 F6 87.6(6) . . ?
O1 Fe1 C1 142.65(16) . . ?
O1 Fe1 C2 149.73(15) . . ?
C1 Fe1 C2 39.27(8) . . ?
O1 Fe1 C5 103.95(15) . . ?
C1 Fe1 C5 39.21(8) . . ?
C2 Fe1 C5 65.73(12) . . ?
O1 Fe1 C3 110.63(14) . . ?
C1 Fe1 C3 65.68(12) . . ?
C2 Fe1 C3 39.17(8) . . ?
C5 Fe1 C3 65.51(12) . . ?
O1 Fe1 C4 88.30(14) . . ?
C1 Fe1 C4 65.61(12) . . ?
C2 Fe1 C4 65.58(12) . . ?
C5 Fe1 C4 39.05(8) . . ?
C3 Fe1 C4 38.97(8) . . ?
O1 Fe1 S2 89.88(10) . . ?
C1 Fe1 S2 88.16(11) . . ?
C2 Fe1 S2 118.43(12) . . ?
C5 Fe1 S2 94.55(11) . . ?
C3 Fe1 S2 153.84(11) . . ?
C4 Fe1 S2 130.73(11) . . ?
O1 Fe1 S1 90.16(11) . . ?
C1 Fe1 S1 126.01(12) . . ?
C2 Fe1 S1 91.50(12) . . ?
C5 Fe1 S1 154.67(11) . . ?
C3 Fe1 S1 89.97(11) . . ?
C4 Fe1 S1 122.64(11) . . ?
S2 Fe1 S1 106.59(5) . . ?
O1 Fe1 Fe2 84.67(10) . . ?
C1 Fe1 Fe2 122.57(10) . . ?
C2 Fe1 Fe2 119.87(11) . . ?
C5 Fe1 Fe2 147.46(10) . . ?
C3 Fe1 Fe2 141.11(11) . . ?
C4 Fe1 Fe2 171.80(10) . . ?
S2 Fe1 Fe2 53.64(4) . . ?
S1 Fe1 Fe2 53.32(4) . . ?
O2 Fe2 C11 89.40(17) . . ?
O2 Fe2 C15 110.70(18) . . ?
C11 Fe2 C15 38.85(10) . . ?
O2 Fe2 C14 149.43(17) . . ?
C11 Fe2 C14 64.95(15) . . ?
C15 Fe2 C14 38.75(10) . . ?
O2 Fe2 C12 105.95(19) . . ?
C11 Fe2 C12 38.74(10) . . ?
C15 Fe2 C12 64.93(15) . . ?
C14 Fe2 C12 64.79(15) . . ?
O2 Fe2 C13 144.23(19) . . ?
C11 Fe2 C13 64.85(15) . . ?
C15 Fe2 C13 64.84(15) . . ?
C14 Fe2 C13 38.62(9) . . ?
C12 Fe2 C13 38.63(10) . . ?
O2 Fe2 S1 90.14(11) . . ?
C11 Fe2 S1 129.2(2) . . ?
C15 Fe2 S1 152.99(14) . . ?
C14 Fe2 S1 118.59(15) . . ?
C12 Fe2 S1 93.54(17) . . ?
C13 Fe2 S1 88.18(13) . . ?
O2 Fe2 S2 89.69(12) . . ?
C11 Fe2 S2 123.6(2) . . ?
C15 Fe2 S2 90.47(15) . . ?
C14 Fe2 S2 91.22(13) . . ?
C12 Fe2 S2 154.12(14) . . ?
C13 Fe2 S2 124.81(16) . . ?
S1 Fe2 S2 107.18(5) . . ?
O2 Fe2 Fe1 84.45(10) . . ?
C11 Fe2 Fe1 173.21(16) . . ?
C15 Fe2 Fe1 141.86(16) . . ?
C14 Fe2 Fe1 119.99(13) . . ?
C12 Fe2 Fe1 146.37(18) . . ?
C13 Fe2 Fe1 121.94(15) . . ?
S1 Fe2 Fe1 53.88(4) . . ?
S2 Fe2 Fe1 53.68(4) . . ?
C21 S1 Fe2 113.1(2) . . ?
C21 S1 Fe1 113.42(19) . . ?
Fe2 S1 Fe1 72.80(4) . . ?
C23 S2 Fe2 113.4(2) . . ?
C23 S2 Fe1 114.5(2) . . ?
Fe2 S2 Fe1 72.68(4) . . ?
C25 O1 Fe1 122.7(3) . . ?
C25 O2 Fe2 122.8(3) . . ?
C2 C1 C5 108.1 . . ?
C2 C1 C6 125.2(4) . . ?
C5 C1 C6 126.3(4) . . ?
C2 C1 Fe1 70.51(14) . . ?
C5 C1 Fe1 70.81(14) . . ?
C6 C1 Fe1 129.9(3) . . ?
C1 C2 C3 108.0 . . ?
C1 C2 C7 125.8(5) . . ?
C3 C2 C7 126.2(5) . . ?
C1 C2 Fe1 70.22(14) . . ?
C3 C2 Fe1 70.92(13) . . ?
C7 C2 Fe1 126.7(4) . . ?
C4 C3 C2 108.0 . . ?
C4 C3 C8 125.1(4) . . ?
C2 C3 C8 126.7(4) . . ?
C4 C3 Fe1 70.69(14) . . ?
C2 C3 Fe1 69.91(13) . . ?
C8 C3 Fe1 128.9(3) . . ?
C3 C4 C5 108.0 . . ?
C3 C4 C9 125.9(4) . . ?
C5 C4 C9 126.1(4) . . ?
C3 C4 Fe1 70.34(14) . . ?
C5 C4 Fe1 70.07(13) . . ?
C9 C4 Fe1 124.6(3) . . ?
C1 C5 C4 108.0 . . ?
C1 C5 C10 126.7(4) . . ?
C4 C5 C10 125.3(4) . . ?
C1 C5 Fe1 69.98(13) . . ?
C4 C5 Fe1 70.88(14) . . ?
C10 C5 Fe1 125.4(4) . . ?
C12 C11 C15 108.0 . . ?
C12 C11 C16 124.7(8) . . ?
C15 C11 C16 127.3(8) . . ?
C12 C11 Fe2 70.94(17) . . ?
C15 C11 Fe2 70.60(16) . . ?
C16 C11 Fe2 124.0(5) . . ?
C11 C12 C13 108.0 . . ?
C11 C12 C17 128.4(7) . . ?
C13 C12 C17 123.5(7) . . ?
C11 C12 Fe2 70.32(17) . . ?
C13 C12 Fe2 70.88(16) . . ?
C17 C12 Fe2 127.0(4) . . ?
C14 C13 C12 108.0 . . ?
C14 C13 C18 126.7(6) . . ?
C12 C13 C18 124.9(6) . . ?
C14 C13 Fe2 70.50(16) . . ?
C12 C13 Fe2 70.50(16) . . ?
C18 C13 Fe2 130.0(4) . . ?
C13 C14 C15 108.0 . . ?
C13 C14 C19 124.0(6) . . ?
C15 C14 C19 127.6(6) . . ?
C13 C14 Fe2 70.89(17) . . ?
C15 C14 Fe2 70.34(17) . . ?
C19 C14 Fe2 129.2(4) . . ?
C14 C15 C11 108.0 . . ?
C14 C15 C20 122.7(7) . . ?
C11 C15 C20 129.2(7) . . ?
C14 C15 Fe2 70.91(16) . . ?
C11 C15 Fe2 70.55(16) . . ?
C20 C15 Fe2 128.0(4) . . ?
C22 C21 S1 109.8(4) . . ?
C24 C23 S2 109.4(5) . . ?
O1 C25 O2 125.4(4) . . ?
O1 C25 C26 117.2(5) . . ?
O2 C25 C26 117.4(5) . . ?
C27' C26 C27 102.4(19) . . ?
C27' C26 C25 132.5(18) . . ?
C27 C26 C25 121.0(11) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.063
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1059108'
_audit_update_record             
;
2015-04-13 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H47 F6 Fe2 O2 P S2'
_chemical_formula_weight         784.49

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'
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'
S S 0.1246 0.1234 '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   'P2(1)/c  '

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

_cell_length_a                   15.844(3)
_cell_length_b                   13.974(2)
_cell_length_c                   16.746(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.737(3)
_cell_angle_gamma                90.00
_cell_volume                     3511.1(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7503
_exptl_absorpt_correction_T_max  0.8173
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18590
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6178
_reflns_number_gt                4818
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0911P)²+0.9995P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6178
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
P1 P 0.29184(9) -0.13918(10) 0.53440(8) 0.0673(3) Uani 1 1 d . . .
Fe1 Fe 0.73239(3) -0.16479(3) 1.14347(3) 0.03260(16) Uani 1 1 d . . .
Fe2 Fe 0.85311(3) -0.03133(3) 1.16136(3) 0.03197(16) Uani 1 1 d . . .
S2 S 0.87181(6) -0.18574(6) 1.14599(5) 0.0350(2) Uani 1 1 d . . .
S1 S 0.71957(6) -0.01378(6) 1.17489(5) 0.0383(2) Uani 1 1 d . . .
O1 O 0.69625(15) -0.13112(17) 1.02232(13) 0.0389(6) Uani 1 1 d . . .
O2 O 0.80006(15) -0.01708(17) 1.03812(13) 0.0382(5) Uani 1 1 d . . .
C1 C 0.74807(17) -0.26551(19) 1.24168(15) 0.0459(9) Uani 1 1 d G . .
C2 C 0.72441(17) -0.31498(18) 1.16364(16) 0.0432(8) Uani 1 1 d G . .
C3 C 0.64007(16) -0.28067(18) 1.11264(15) 0.0441(9) Uani 1 1 d G . .
C4 C 0.61160(16) -0.20998(19) 1.15915(16) 0.0464(9) Uani 1 1 d G . .
C5 C 0.67835(17) -0.20061(19) 1.23891(15) 0.0479(9) Uani 1 1 d G . .
C6 C 0.8296(3) -0.2837(4) 1.3147(3) 0.0689(13) Uani 1 1 d . . .
H6A H 0.8177 -0.3332 1.3494 0.103 Uiso 1 1 calc R . .
H6B H 0.8465 -0.2262 1.3472 0.103 Uiso 1 1 calc R . .
H6C H 0.8772 -0.3036 1.2945 0.103 Uiso 1 1 calc R . .
C7 C 0.7754(3) -0.3968(3) 1.1430(3) 0.0691(13) Uani 1 1 d . . .
H7A H 0.7558 -0.4559 1.1605 0.104 Uiso 1 1 calc R . .
H7B H 0.8379 -0.3884 1.1721 0.104 Uiso 1 1 calc R . .
H7C H 0.7652 -0.3984 1.0833 0.104 Uiso 1 1 calc R . .
C8 C 0.5892(3) -0.3148(3) 1.0261(3) 0.0655(12) Uani 1 1 d . . .
H8A H 0.5521 -0.3678 1.0299 0.098 Uiso 1 1 calc R . .
H8B H 0.6302 -0.3348 0.9978 0.098 Uiso 1 1 calc R . .
H8C H 0.5527 -0.2638 0.9950 0.098 Uiso 1 1 calc R . .
C9 C 0.5236(3) -0.1588(4) 1.1297(4) 0.0766(15) Uani 1 1 d . . .
H9A H 0.4799 -0.1952 1.1453 0.115 Uiso 1 1 calc R . .
H9B H 0.5049 -0.1517 1.0695 0.115 Uiso 1 1 calc R . .
H9C H 0.5297 -0.0967 1.1556 0.115 Uiso 1 1 calc R . .
C10 C 0.6715(4) -0.1435(4) 1.3123(3) 0.0764(15) Uani 1 1 d . . .
H10A H 0.6432 -0.1814 1.3443 0.115 Uiso 1 1 calc R . .
H10B H 0.6368 -0.0870 1.2921 0.115 Uiso 1 1 calc R . .
H10C H 0.7301 -0.1256 1.3476 0.115 Uiso 1 1 calc R . .
C11 C 0.88735(17) 0.10390(17) 1.22169(15) 0.0423(8) Uani 1 1 d G . .
C12 C 0.91507(17) 0.02971(18) 1.28236(14) 0.0427(9) Uani 1 1 d G . .
C13 C 0.97640(16) -0.02912(17) 1.25916(15) 0.0426(9) Uani 1 1 d G . .
C14 C 0.98659(16) 0.00872(18) 1.18417(16) 0.0457(9) Uani 1 1 d G . .
C15 C 0.93156(17) 0.09093(18) 1.16101(15) 0.0423(8) Uani 1 1 d G . .
C16 C 0.8299(3) 0.1863(3) 1.2274(3) 0.0646(12) Uani 1 1 d . . .
H16A H 0.8665 0.2369 1.2593 0.097 Uiso 1 1 calc R . .
H16B H 0.7882 0.1662 1.2548 0.097 Uiso 1 1 calc R . .
H16C H 0.7981 0.2089 1.1717 0.097 Uiso 1 1 calc R . .
C17 C 0.8875(3) 0.0183(3) 1.3594(2) 0.0660(13) Uani 1 1 d . . .
H17A H 0.9273 0.0540 1.4051 0.099 Uiso 1 1 calc R . .
H17B H 0.8897 -0.0481 1.3745 0.099 Uiso 1 1 calc R . .
H17C H 0.8279 0.0418 1.3481 0.099 Uiso 1 1 calc R . .
C18 C 1.0298(3) -0.1082(3) 1.3123(3) 0.0716(13) Uani 1 1 d . . .
H18A H 1.0835 -0.0823 1.3512 0.107 Uiso 1 1 calc R . .
H18B H 1.0448 -0.1545 1.2767 0.107 Uiso 1 1 calc R . .
H18C H 0.9954 -0.1384 1.3431 0.107 Uiso 1 1 calc R . .
C19 C 1.0477(3) -0.0294(4) 1.1398(3) 0.0724(14) Uani 1 1 d . . .
H19A H 1.1050 0.0007 1.1620 0.109 Uiso 1 1 calc R . .
H19B H 1.0232 -0.0162 1.0806 0.109 Uiso 1 1 calc R . .
H19C H 1.0542 -0.0973 1.1484 0.109 Uiso 1 1 calc R . .
C20 C 0.9209(3) 0.1521(3) 1.0850(3) 0.0617(11) Uani 1 1 d . . .
H20A H 0.9634 0.2034 1.0994 0.093 Uiso 1 1 calc R . .
H20B H 0.8617 0.1782 1.0657 0.093 Uiso 1 1 calc R . .
H20C H 0.9306 0.1141 1.0410 0.093 Uiso 1 1 calc R . .
C23 C 0.8785(3) -0.2176(3) 1.0418(2) 0.0489(9) Uani 1 1 d . . .
H23A H 0.8217 -0.2430 1.0069 0.059 Uiso 1 1 calc R . .
H23B H 0.8916 -0.1608 1.0145 0.059 Uiso 1 1 calc R . .
C24 C 0.9505(3) -0.2912(3) 1.0508(3) 0.0715(13) Uani 1 1 d . . .
H24A H 0.9534 -0.3075 0.9960 0.107 Uiso 1 1 calc R . .
H24B H 0.9371 -0.3475 1.0773 0.107 Uiso 1 1 calc R . .
H24C H 1.0068 -0.2655 1.0847 0.107 Uiso 1 1 calc R . .
C21 C 0.6440(3) 0.0574(3) 1.0896(3) 0.0567(10) Uani 1 1 d . . .
H21A H 0.6782 0.0959 1.0628 0.068 Uiso 1 1 calc R . .
H21B H 0.6054 0.0153 1.0474 0.068 Uiso 1 1 calc R . .
C22 C 0.5885(4) 0.1215(4) 1.1258(4) 0.0958(19) Uani 1 1 d . . .
H22A H 0.5489 0.1590 1.0814 0.144 Uiso 1 1 calc R . .
H22B H 0.6270 0.1633 1.1672 0.144 Uiso 1 1 calc R . .
H22C H 0.5544 0.0830 1.1518 0.144 Uiso 1 1 calc R . .
C25 C 0.7325(2) -0.0641(2) 0.9943(2) 0.0359(8) Uani 1 1 d . . .
C26 C 0.6926(2) -0.0360(3) 0.9044(2) 0.0396(8) Uani 1 1 d . . .
C27 C 0.7151(3) 0.0500(3) 0.8752(2) 0.0549(10) Uani 1 1 d . . .
H27A H 0.7583 0.0889 0.9114 0.066 Uiso 1 1 calc R . .
C28 C 0.6742(3) 0.0787(3) 0.7928(3) 0.0661(12) Uani 1 1 d . . .
H28A H 0.6909 0.1361 0.7741 0.079 Uiso 1 1 calc R . .
C29 C 0.6086(3) 0.0235(3) 0.7377(2) 0.0567(11) Uani 1 1 d . . .
C30 C 0.5871(3) -0.0608(3) 0.7671(2) 0.0577(11) Uani 1 1 d . . .
H30A H 0.5441 -0.0996 0.7305 0.069 Uiso 1 1 calc R . .
C31 C 0.6272(3) -0.0909(3) 0.8495(2) 0.0491(9) Uani 1 1 d . . .
H31A H 0.6098 -0.1483 0.8678 0.059 Uiso 1 1 calc R . .
C32 C 0.5606(3) 0.0575(4) 0.6494(3) 0.0873(17) Uani 1 1 d . . .
H32A H 0.5173 0.0106 0.6205 0.131 Uiso 1 1 calc R . .
H32B H 0.6028 0.0667 0.6198 0.131 Uiso 1 1 calc R . .
H32C H 0.5311 0.1170 0.6517 0.131 Uiso 1 1 calc R . .
F1 F 0.2647(5) -0.0356(3) 0.5425(4) 0.189(3) Uani 1 1 d . . .
F2 F 0.3224(4) -0.1433(5) 0.6283(3) 0.219(3) Uani 1 1 d . . .
F3 F 0.3137(4) -0.2445(3) 0.5199(3) 0.173(2) Uani 1 1 d . . .
F4 F 0.2563(4) -0.1318(4) 0.4357(2) 0.1559(18) Uani 1 1 d . . .
F5 F 0.1990(4) -0.1732(4) 0.5335(4) 0.208(3) Uani 1 1 d . . .
F6 F 0.3814(3) -0.1050(5) 0.5323(4) 0.215(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F2 1.491(4) . ?
P1 F6 1.509(4) . ?
P1 F1 1.529(4) . ?
P1 F3 1.549(4) . ?
P1 F5 1.541(5) . ?
P1 F4 1.569(4) . ?
Fe1 O1 1.980(2) . ?
Fe1 C5 2.102(3) . ?
Fe1 C4 2.110(3) . ?
Fe1 C1 2.118(2) . ?
Fe1 C3 2.131(3) . ?
Fe1 C2 2.136(3) . ?
Fe1 S1 2.2001(10) . ?
Fe1 S2 2.2152(10) . ?
Fe1 Fe2 2.6189(7) . ?
Fe2 O2 1.972(2) . ?
Fe2 C14 2.101(3) . ?
Fe2 C13 2.108(2) . ?
Fe2 C15 2.114(3) . ?
Fe2 C12 2.126(2) . ?
Fe2 C11 2.129(3) . ?
Fe2 S2 2.2043(10) . ?
Fe2 S1 2.2128(10) . ?
S2 C23 1.836(3) . ?
S1 C21 1.834(4) . ?
O1 C25 1.265(4) . ?
O2 C25 1.269(4) . ?
C1 C2 1.4184(19) . ?
C1 C5 1.4184(19) . ?
C1 C6 1.488(5) . ?
C2 C3 1.4183(19) . ?
C2 C7 1.503(5) . ?
C3 C4 1.4185(19) . ?
C3 C8 1.492(4) . ?
C4 C5 1.4184(19) . ?
C4 C9 1.503(5) . ?
C5 C10 1.498(5) . ?
C11 C15 1.4188(18) . ?
C11 C12 1.4188(18) . ?
C11 C16 1.489(5) . ?
C12 C13 1.4189(18) . ?
C12 C17 1.498(4) . ?
C13 C14 1.4189(18) . ?
C13 C18 1.498(4) . ?
C14 C15 1.4188(18) . ?
C14 C19 1.496(5) . ?
C15 C20 1.498(5) . ?
C23 C24 1.507(5) . ?
C21 C22 1.512(6) . ?
C25 C26 1.485(4) . ?
C26 C31 1.378(5) . ?
C26 C27 1.388(5) . ?
C27 C28 1.382(5) . ?
C28 C29 1.382(6) . ?
C29 C30 1.361(6) . ?
C29 C32 1.506(5) . ?
C30 C31 1.387(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 P1 F6 92.7(4) . . ?
F2 P1 F1 87.0(3) . . ?
F6 P1 F1 89.8(3) . . ?
F2 P1 F3 96.6(3) . . ?
F6 P1 F3 92.2(3) . . ?
F1 P1 F3 175.8(3) . . ?
F2 P1 F5 89.1(4) . . ?
F6 P1 F5 178.2(4) . . ?
F1 P1 F5 89.9(3) . . ?
F3 P1 F5 88.0(3) . . ?
F2 P1 F4 177.5(3) . . ?
F6 P1 F4 88.7(3) . . ?
F1 P1 F4 90.9(3) . . ?
F3 P1 F4 85.4(3) . . ?
F5 P1 F4 89.5(3) . . ?
O1 Fe1 C5 141.40(10) . . ?
O1 Fe1 C4 102.90(10) . . ?
C5 Fe1 C4 39.36(6) . . ?
O1 Fe1 C1 151.28(10) . . ?
C5 Fe1 C1 39.28(6) . . ?
C4 Fe1 C1 65.75(9) . . ?
O1 Fe1 C3 88.98(10) . . ?
C5 Fe1 C3 65.66(9) . . ?
C4 Fe1 C3 39.07(6) . . ?
C1 Fe1 C3 65.38(9) . . ?
O1 Fe1 C2 112.54(10) . . ?
C5 Fe1 C2 65.57(9) . . ?
C4 Fe1 C2 65.43(9) . . ?
C1 Fe1 C2 38.95(6) . . ?
C3 Fe1 C2 38.82(5) . . ?
O1 Fe1 S1 89.92(8) . . ?
C5 Fe1 S1 87.43(8) . . ?
C4 Fe1 S1 95.75(8) . . ?
C1 Fe1 S1 116.65(8) . . ?
C3 Fe1 S1 132.67(8) . . ?
C2 Fe1 S1 152.87(8) . . ?
O1 Fe1 S2 90.53(7) . . ?
C5 Fe1 S2 126.97(8) . . ?
C4 Fe1 S2 153.74(8) . . ?
C1 Fe1 S2 91.72(8) . . ?
C3 Fe1 S2 120.45(8) . . ?
C2 Fe1 S2 88.65(7) . . ?
S1 Fe1 S2 106.88(4) . . ?
O1 Fe1 Fe2 84.73(7) . . ?
C5 Fe1 Fe2 122.93(7) . . ?
C4 Fe1 Fe2 148.99(7) . . ?
C1 Fe1 Fe2 119.03(7) . . ?
C3 Fe1 Fe2 171.08(7) . . ?
C2 Fe1 Fe2 139.45(7) . . ?
S1 Fe1 Fe2 53.82(3) . . ?
S2 Fe1 Fe2 53.47(3) . . ?
O2 Fe2 C14 103.25(10) . . ?
O2 Fe2 C13 142.05(10) . . ?
C14 Fe2 C13 39.40(5) . . ?
O2 Fe2 C15 88.22(10) . . ?
C14 Fe2 C15 39.34(5) . . ?
C13 Fe2 C15 65.88(8) . . ?
O2 Fe2 C12 150.21(10) . . ?
C14 Fe2 C12 65.80(8) . . ?
C13 Fe2 C12 39.16(5) . . ?
C15 Fe2 C12 65.57(8) . . ?
O2 Fe2 C11 111.40(10) . . ?
C14 Fe2 C11 65.74(8) . . ?
C13 Fe2 C11 65.61(8) . . ?
C15 Fe2 C11 39.07(5) . . ?
C12 Fe2 C11 38.96(5) . . ?
O2 Fe2 S2 90.27(7) . . ?
C14 Fe2 S2 96.71(7) . . ?
C13 Fe2 S2 88.81(7) . . ?
C15 Fe2 S2 133.60(7) . . ?
C12 Fe2 S2 117.77(7) . . ?
C11 Fe2 S2 154.27(7) . . ?
O2 Fe2 S1 89.76(7) . . ?
C14 Fe2 S1 153.10(8) . . ?
C13 Fe2 S1 126.63(8) . . ?
C15 Fe2 S1 119.55(7) . . ?
C12 Fe2 S1 91.25(7) . . ?
C11 Fe2 S1 87.67(7) . . ?
S2 Fe2 S1 106.81(4) . . ?
O2 Fe2 Fe1 84.38(7) . . ?
C14 Fe2 Fe1 150.02(7) . . ?
C13 Fe2 Fe1 124.04(7) . . ?
C15 Fe2 Fe1 169.66(7) . . ?
C12 Fe2 Fe1 119.44(7) . . ?
C11 Fe2 Fe1 138.74(7) . . ?
S2 Fe2 Fe1 53.85(3) . . ?
S1 Fe2 Fe1 53.37(3) . . ?
C23 S2 Fe2 113.52(13) . . ?
C23 S2 Fe1 112.08(13) . . ?
Fe2 S2 Fe1 72.68(3) . . ?
C21 S1 Fe1 114.90(15) . . ?
C21 S1 Fe2 112.76(14) . . ?
Fe1 S1 Fe2 72.81(3) . . ?
C25 O1 Fe1 122.7(2) . . ?
C25 O2 Fe2 123.4(2) . . ?
C2 C1 C5 108.0 . . ?
C2 C1 C6 125.2(3) . . ?
C5 C1 C6 126.7(3) . . ?
C2 C1 Fe1 71.22(9) . . ?
C5 C1 Fe1 69.75(10) . . ?
C6 C1 Fe1 127.3(2) . . ?
C3 C2 C1 108.0 . . ?
C3 C2 C7 126.2(3) . . ?
C1 C2 C7 125.5(3) . . ?
C3 C2 Fe1 70.42(9) . . ?
C1 C2 Fe1 69.83(9) . . ?
C7 C2 Fe1 130.4(2) . . ?
C2 C3 C4 108.0 . . ?
C2 C3 C8 126.0(3) . . ?
C4 C3 C8 126.0(3) . . ?
C2 C3 Fe1 70.76(9) . . ?
C4 C3 Fe1 69.66(10) . . ?
C8 C3 Fe1 126.3(2) . . ?
C5 C4 C3 108.0 . . ?
C5 C4 C9 126.7(3) . . ?
C3 C4 C9 125.2(3) . . ?
C5 C4 Fe1 69.99(9) . . ?
C3 C4 Fe1 71.27(9) . . ?
C9 C4 Fe1 126.9(3) . . ?
C1 C5 C4 108.0 . . ?
C1 C5 C10 125.1(3) . . ?
C4 C5 C10 126.4(3) . . ?
C1 C5 Fe1 70.97(10) . . ?
C4 C5 Fe1 70.65(9) . . ?
C10 C5 Fe1 130.7(2) . . ?
C15 C11 C12 108.0 . . ?
C15 C11 C16 126.7(3) . . ?
C12 C11 C16 125.0(3) . . ?
C15 C11 Fe2 69.88(9) . . ?
C12 C11 Fe2 70.39(9) . . ?
C16 C11 Fe2 130.4(2) . . ?
C11 C12 C13 108.0 . . ?
C11 C12 C17 125.9(3) . . ?
C13 C12 C17 126.1(3) . . ?
C11 C12 Fe2 70.66(9) . . ?
C13 C12 Fe2 69.74(9) . . ?
C17 C12 Fe2 127.3(2) . . ?
C14 C13 C12 108.0 . . ?
C14 C13 C18 126.7(3) . . ?
C12 C13 C18 124.8(3) . . ?
C14 C13 Fe2 70.02(9) . . ?
C12 C13 Fe2 71.10(9) . . ?
C18 C13 Fe2 131.0(2) . . ?
C15 C14 C13 108.0 . . ?
C15 C14 C19 126.3(3) . . ?
C13 C14 C19 125.6(3) . . ?
C15 C14 Fe2 70.83(9) . . ?
C13 C14 Fe2 70.58(9) . . ?
C19 C14 Fe2 126.1(2) . . ?
C14 C15 C11 108.0 . . ?
C14 C15 C20 125.9(3) . . ?
C11 C15 C20 126.1(3) . . ?
C14 C15 Fe2 69.83(9) . . ?
C11 C15 Fe2 71.05(9) . . ?
C20 C15 Fe2 123.9(2) . . ?
C24 C23 S2 110.1(3) . . ?
C22 C21 S1 109.1(3) . . ?
O1 C25 O2 124.6(3) . . ?
O1 C25 C26 118.4(3) . . ?
O2 C25 C26 117.0(3) . . ?
C31 C26 C27 118.1(3) . . ?
C31 C26 C25 120.8(3) . . ?
C27 C26 C25 120.9(3) . . ?
C28 C27 C26 120.8(4) . . ?
C29 C28 C27 121.0(4) . . ?
C30 C29 C28 117.7(4) . . ?
C30 C29 C32 121.5(4) . . ?
C28 C29 C32 120.8(5) . . ?
C29 C30 C31 122.3(4) . . ?
C26 C31 C30 120.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.070
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_12
_database_code_depnum_ccdc_archive 'CCDC 1059109'
_audit_update_record             
;
2015-04-13 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H47 F6 Fe2 O2 P S2'
_chemical_formula_weight         796.50

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'
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'
S S 0.1246 0.1234 '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   'P2(1)/c  '

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

_cell_length_a                   15.237(2)
_cell_length_b                   14.235(2)
_cell_length_c                   17.525(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.440(8)
_cell_angle_gamma                90.00
_cell_volume                     3645.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_T_max  0.8547
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17495
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6344
_reflns_number_gt                4660
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0690P)²+0.8989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6344
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1278
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
P1 P 0.72916(10) 0.35003(11) 0.96797(9) 0.0799(4) Uani 1 1 d . . .
Fe1 Fe 0.73335(3) 0.81454(3) 1.14904(3) 0.04071(17) Uani 1 1 d . . .
Fe2 Fe 0.85369(3) 0.94899(3) 1.16009(3) 0.03960(16) Uani 1 1 d . . .
S2 S 0.87688(6) 0.79763(6) 1.14532(5) 0.0421(2) Uani 1 1 d . . .
S1 S 0.71515(7) 0.96335(6) 1.17642(6) 0.0490(3) Uani 1 1 d . . .
O1 O 0.69617(17) 0.84393(17) 1.03495(15) 0.0482(6) Uani 1 1 d . . .
O2 O 0.79887(17) 0.96134(17) 1.04387(14) 0.0457(6) Uani 1 1 d . . .
C1 C 0.61031(18) 0.7663(2) 1.16790(18) 0.0577(11) Uani 1 1 d G . .
C2 C 0.6771(2) 0.77799(19) 1.24229(17) 0.0566(10) Uani 1 1 d G . .
C3 C 0.75114(19) 0.71666(19) 1.24429(16) 0.0511(10) Uani 1 1 d G . .
C4 C 0.7301(2) 0.66704(18) 1.17114(17) 0.0515(10) Uani 1 1 d G . .
C5 C 0.64303(19) 0.69769(19) 1.12393(16) 0.0570(11) Uani 1 1 d G . .
C6 C 0.5181(3) 0.8133(4) 1.1403(4) 0.0971(19) Uani 1 1 d . . .
H6A H 0.4738 0.7768 1.1568 0.146 Uiso 1 1 calc R . .
H6B H 0.5000 0.8181 1.0833 0.146 Uiso 1 1 calc R . .
H6C H 0.5218 0.8750 1.1631 0.146 Uiso 1 1 calc R . .
C7 C 0.6653(4) 0.8350(4) 1.3111(3) 0.0873(17) Uani 1 1 d . . .
H7A H 0.6372 0.7968 1.3429 0.131 Uiso 1 1 calc R . .
H7B H 0.6271 0.8883 1.2913 0.131 Uiso 1 1 calc R . .
H7C H 0.7240 0.8561 1.3431 0.131 Uiso 1 1 calc R . .
C8 C 0.8348(3) 0.7033(3) 1.3125(3) 0.0736(13) Uani 1 1 d . . .
H8A H 0.8240 0.6547 1.3467 0.110 Uiso 1 1 calc R . .
H8B H 0.8490 0.7609 1.3419 0.110 Uiso 1 1 calc R . .
H8C H 0.8852 0.6858 1.2928 0.110 Uiso 1 1 calc R . .
C9 C 0.7853(4) 0.5878(3) 1.1521(3) 0.0833(16) Uani 1 1 d . . .
H9A H 0.7664 0.5297 1.1704 0.125 Uiso 1 1 calc R . .
H9B H 0.8490 0.5982 1.1782 0.125 Uiso 1 1 calc R . .
H9C H 0.7759 0.5847 1.0956 0.125 Uiso 1 1 calc R . .
C10 C 0.5952(4) 0.6636(4) 1.0421(3) 0.0901(17) Uani 1 1 d . . .
H10A H 0.5580 0.6102 1.0456 0.135 Uiso 1 1 calc R . .
H10B H 0.6397 0.6458 1.0154 0.135 Uiso 1 1 calc R . .
H10C H 0.5572 0.7127 1.0128 0.135 Uiso 1 1 calc R . .
C11 C 0.88591(19) 1.08161(18) 1.21808(17) 0.0507(9) Uani 1 1 d G . .
C12 C 0.93055(19) 1.07218(18) 1.15762(16) 0.0511(9) Uani 1 1 d G . .
C13 C 0.98927(18) 0.99301(19) 1.17617(18) 0.0535(10) Uani 1 1 d G . .
C14 C 0.98092(19) 0.95352(18) 1.24807(17) 0.0598(11) Uani 1 1 d G . .
C15 C 0.9170(2) 1.0083(2) 1.27399(16) 0.0585(11) Uani 1 1 d G . .
C16 C 0.8248(4) 1.1609(3) 1.2262(4) 0.0847(16) Uani 1 1 d . . .
H16A H 0.8611 1.2109 1.2561 0.127 Uiso 1 1 calc R . .
H16B H 0.7820 1.1393 1.2533 0.127 Uiso 1 1 calc R . .
H16C H 0.7922 1.1836 1.1743 0.127 Uiso 1 1 calc R . .
C17 C 0.9178(3) 1.1341(3) 1.0863(3) 0.0737(13) Uani 1 1 d . . .
H17A H 0.9602 1.1855 1.0991 0.111 Uiso 1 1 calc R . .
H17B H 0.8564 1.1581 1.0706 0.111 Uiso 1 1 calc R . .
H17C H 0.9286 1.0985 1.0433 0.111 Uiso 1 1 calc R . .
C18 C 1.0520(4) 0.9588(4) 1.1299(4) 0.0963(19) Uani 1 1 d . . .
H18A H 1.1101 0.9896 1.1487 0.144 Uiso 1 1 calc R . .
H18B H 1.0257 0.9726 1.0745 0.144 Uiso 1 1 calc R . .
H18C H 1.0602 0.8921 1.1368 0.144 Uiso 1 1 calc R . .
C19 C 1.0392(4) 0.8765(3) 1.2955(3) 0.099(2) Uani 1 1 d . . .
H19A H 1.0934 0.9032 1.3309 0.148 Uiso 1 1 calc R . .
H19B H 1.0561 0.8333 1.2599 0.148 Uiso 1 1 calc R . .
H19C H 1.0054 0.8438 1.3258 0.148 Uiso 1 1 calc R . .
C20 C 0.8902(4) 0.9933(4) 1.3491(3) 0.0949(19) Uani 1 1 d . . .
H20A H 0.9306 1.0283 1.3916 0.142 Uiso 1 1 calc R . .
H20B H 0.8944 0.9277 1.3623 0.142 Uiso 1 1 calc R . .
H20C H 0.8285 1.0144 1.3415 0.142 Uiso 1 1 calc R . .
C23 C 0.8836(3) 0.7661(3) 1.0455(2) 0.0588(11) Uani 1 1 d . . .
H23A H 0.8259 0.7389 1.0152 0.071 Uiso 1 1 calc R . .
H23B H 0.8943 0.8222 1.0180 0.071 Uiso 1 1 calc R . .
C24 C 0.9598(4) 0.6969(4) 1.0509(3) 0.0903(17) Uani 1 1 d . . .
H24A H 0.9622 0.6810 0.9983 0.136 Uiso 1 1 calc R . .
H24B H 0.9488 0.6411 1.0776 0.136 Uiso 1 1 calc R . .
H24C H 1.0169 0.7243 1.0802 0.136 Uiso 1 1 calc R . .
C21 C 0.6380(3) 1.0307(3) 1.0949(3) 0.0698(13) Uani 1 1 d . . .
H21A H 0.6736 1.0731 1.0721 0.084 Uiso 1 1 calc R . .
H21B H 0.6052 0.9880 1.0535 0.084 Uiso 1 1 calc R . .
C22 C 0.5705(4) 1.0863(4) 1.1253(4) 0.1029(19) Uani 1 1 d . . .
H22A H 0.5308 1.1209 1.0822 0.154 Uiso 1 1 calc R . .
H22B H 0.6030 1.1292 1.1657 0.154 Uiso 1 1 calc R . .
H22C H 0.5349 1.0442 1.1472 0.154 Uiso 1 1 calc R . .
C25 C 0.7327(3) 0.9103(3) 1.0059(2) 0.0452(9) Uani 1 1 d . . .
C26 C 0.6897(3) 0.9293(3) 0.9206(2) 0.0489(9) Uani 1 1 d . . .
H26A H 0.6524 0.8832 0.8904 0.059 Uiso 1 1 calc R . .
C27 C 0.7013(3) 1.0085(3) 0.8846(2) 0.0496(9) Uani 1 1 d . . .
H27A H 0.7415 1.0522 0.9153 0.059 Uiso 1 1 calc R . .
C28 C 0.6573(3) 1.0344(3) 0.8015(2) 0.0497(9) Uani 1 1 d . . .
C29 C 0.5896(3) 0.9787(3) 0.7517(2) 0.0596(11) Uani 1 1 d . . .
H29A H 0.5729 0.9221 0.7702 0.072 Uiso 1 1 calc R . .
C30 C 0.5473(3) 1.0075(4) 0.6747(3) 0.0747(14) Uani 1 1 d . . .
H30A H 0.4998 0.9721 0.6424 0.090 Uiso 1 1 calc R . .
C31 C 0.5753(4) 1.0876(5) 0.6463(3) 0.0912(17) Uani 1 1 d . . .
H31A H 0.5491 1.1050 0.5936 0.109 Uiso 1 1 calc R . .
C32 C 0.6412(4) 1.1424(4) 0.6944(3) 0.0951(18) Uani 1 1 d . . .
H32A H 0.6591 1.1974 0.6744 0.114 Uiso 1 1 calc R . .
C33 C 0.6820(3) 1.1176(3) 0.7725(3) 0.0702(13) Uani 1 1 d . . .
H33A H 0.7257 1.1566 0.8054 0.084 Uiso 1 1 calc R . .
F1 F 0.6858(4) 0.3519(4) 0.8774(2) 0.187(2) Uani 1 1 d . . .
F2 F 0.8198(3) 0.3175(4) 0.9565(4) 0.203(3) Uani 1 1 d . . .
F3 F 0.7573(4) 0.4534(3) 0.9654(3) 0.188(2) Uani 1 1 d . . .
F4 F 0.6370(3) 0.3826(4) 0.9784(3) 0.189(2) Uani 1 1 d . . .
F5 F 0.7008(4) 0.2461(3) 0.9720(3) 0.188(2) Uani 1 1 d . . .
F6 F 0.7698(3) 0.3454(4) 1.0595(2) 0.1707(19) 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
P1 F3 1.536(4) . ?
P1 F1 1.537(4) . ?
P1 F2 1.524(4) . ?
P1 F4 1.538(4) . ?
P1 F6 1.549(4) . ?
P1 F5 1.548(4) . ?
Fe1 O1 1.963(3) . ?
Fe1 C1 2.109(3) . ?
Fe1 C2 2.114(3) . ?
Fe1 C5 2.124(3) . ?
Fe1 C3 2.132(3) . ?
Fe1 C4 2.138(3) . ?
Fe1 S1 2.2068(11) . ?
Fe1 S2 2.2194(11) . ?
Fe1 Fe2 2.6195(7) . ?
Fe2 O2 1.978(2) . ?
Fe2 C13 2.100(3) . ?
Fe2 C14 2.109(3) . ?
Fe2 C12 2.116(3) . ?
Fe2 C15 2.130(3) . ?
Fe2 C11 2.134(3) . ?
Fe2 S2 2.2104(10) . ?
Fe2 S1 2.2184(11) . ?
S2 C23 1.836(4) . ?
S1 C21 1.841(4) . ?
O1 C25 1.274(4) . ?
O2 C25 1.268(4) . ?
C1 C2 1.419(2) . ?
C1 C5 1.419(2) . ?
C1 C6 1.507(5) . ?
C2 C3 1.419(2) . ?
C2 C7 1.506(5) . ?
C3 C4 1.419(2) . ?
C3 C8 1.492(5) . ?
C4 C5 1.419(2) . ?
C4 C9 1.501(5) . ?
C5 C10 1.494(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.4182(19) . ?
C11 C15 1.4183(19) . ?
C11 C16 1.496(5) . ?
C12 C13 1.4182(19) . ?
C12 C17 1.497(5) . ?
C13 C14 1.4181(19) . ?
C13 C18 1.499(5) . ?
C14 C15 1.4183(19) . ?
C14 C19 1.505(5) . ?
C15 C20 1.500(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C23 C24 1.506(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C21 C22 1.509(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C25 C26 1.477(5) . ?
C26 C27 1.327(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.468(5) . ?
C27 H27A 0.9300 . ?
C28 C29 1.395(6) . ?
C28 C33 1.383(6) . ?
C29 C30 1.382(6) . ?
C29 H29A 0.9300 . ?
C30 C31 1.360(7) . ?
C30 H30A 0.9300 . ?
C31 C32 1.360(8) . ?
C31 H31A 0.9300 . ?
C32 C33 1.379(7) . ?
C32 H32A 0.9300 . ?
C33 H33A 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
F3 P1 F1 89.7(3) . . ?
F3 P1 F2 90.9(3) . . ?
F1 P1 F2 90.6(3) . . ?
F3 P1 F4 89.3(3) . . ?
F1 P1 F4 88.7(3) . . ?
F2 P1 F4 179.3(3) . . ?
F3 P1 F6 92.2(3) . . ?
F1 P1 F6 177.7(3) . . ?
F2 P1 F6 90.7(3) . . ?
F4 P1 F6 90.0(3) . . ?
F3 P1 F5 179.1(3) . . ?
F1 P1 F5 91.1(3) . . ?
F2 P1 F5 89.5(3) . . ?
F4 P1 F5 90.4(3) . . ?
F6 P1 F5 87.0(3) . . ?
O1 Fe1 C1 102.48(11) . . ?
O1 Fe1 C2 140.96(12) . . ?
C1 Fe1 C2 39.26(6) . . ?
O1 Fe1 C5 88.43(11) . . ?
C1 Fe1 C5 39.16(6) . . ?
C2 Fe1 C5 65.59(9) . . ?
O1 Fe1 C3 150.81(11) . . ?
C1 Fe1 C3 65.54(9) . . ?
C2 Fe1 C3 39.04(6) . . ?
C5 Fe1 C3 65.28(9) . . ?
O1 Fe1 C4 112.28(11) . . ?
C1 Fe1 C4 65.43(9) . . ?
C2 Fe1 C4 65.35(9) . . ?
C5 Fe1 C4 38.88(6) . . ?
C3 Fe1 C4 38.81(6) . . ?
O1 Fe1 S1 89.95(8) . . ?
C1 Fe1 S1 96.12(8) . . ?
C2 Fe1 S1 87.98(8) . . ?
C5 Fe1 S1 133.07(9) . . ?
C3 Fe1 S1 116.94(8) . . ?
C4 Fe1 S1 153.17(8) . . ?
O1 Fe1 S2 89.77(8) . . ?
C1 Fe1 S2 153.69(8) . . ?
C2 Fe1 S2 127.91(9) . . ?
C5 Fe1 S2 119.67(9) . . ?
C3 Fe1 S2 92.53(8) . . ?
C4 Fe1 S2 88.43(8) . . ?
S1 Fe1 S2 107.22(4) . . ?
O1 Fe1 Fe2 85.05(7) . . ?
C1 Fe1 Fe2 149.46(8) . . ?
C2 Fe1 Fe2 123.44(8) . . ?
C5 Fe1 Fe2 170.55(8) . . ?
C3 Fe1 Fe2 119.24(8) . . ?
C4 Fe1 Fe2 139.10(8) . . ?
S1 Fe1 Fe2 53.91(3) . . ?
S2 Fe1 Fe2 53.59(3) . . ?
O2 Fe2 C13 102.96(11) . . ?
O2 Fe2 C14 141.53(11) . . ?
C13 Fe2 C14 39.38(6) . . ?
O2 Fe2 C12 88.86(10) . . ?
C13 Fe2 C12 39.31(6) . . ?
C14 Fe2 C12 65.80(9) . . ?
O2 Fe2 C15 151.26(10) . . ?
C13 Fe2 C15 65.70(9) . . ?
C14 Fe2 C15 39.09(6) . . ?
C12 Fe2 C15 65.43(9) . . ?
O2 Fe2 C11 112.63(11) . . ?
C13 Fe2 C11 65.62(9) . . ?
C14 Fe2 C11 65.47(9) . . ?
C12 Fe2 C11 38.98(6) . . ?
C15 Fe2 C11 38.85(6) . . ?
O2 Fe2 S2 90.06(8) . . ?
C13 Fe2 S2 97.05(8) . . ?
C14 Fe2 S2 88.34(8) . . ?
C12 Fe2 S2 134.24(8) . . ?
C15 Fe2 S2 116.80(8) . . ?
C11 Fe2 S2 153.52(9) . . ?
O2 Fe2 S1 89.12(8) . . ?
C13 Fe2 S1 153.00(8) . . ?
C14 Fe2 S1 127.89(9) . . ?
C12 Fe2 S1 118.60(8) . . ?
C15 Fe2 S1 92.17(9) . . ?
C11 Fe2 S1 87.48(8) . . ?
S2 Fe2 S1 107.12(4) . . ?
O2 Fe2 Fe1 84.61(7) . . ?
C13 Fe2 Fe1 150.38(8) . . ?
C14 Fe2 Fe1 123.76(8) . . ?
C12 Fe2 Fe1 169.71(8) . . ?
C15 Fe2 Fe1 118.74(8) . . ?
C11 Fe2 Fe1 138.02(8) . . ?
S2 Fe2 Fe1 53.91(3) . . ?
S1 Fe2 Fe1 53.50(3) . . ?
C23 S2 Fe2 113.79(14) . . ?
C23 S2 Fe1 112.04(15) . . ?
Fe2 S2 Fe1 72.50(3) . . ?
C21 S1 Fe1 115.02(16) . . ?
C21 S1 Fe2 111.71(15) . . ?
Fe1 S1 Fe2 72.59(3) . . ?
C25 O1 Fe1 122.2(2) . . ?
C25 O2 Fe2 122.1(2) . . ?
C2 C1 C5 108.0 . . ?
C2 C1 C6 127.2(3) . . ?
C5 C1 C6 124.8(3) . . ?
C2 C1 Fe1 70.56(10) . . ?
C5 C1 Fe1 70.99(10) . . ?
C6 C1 Fe1 126.4(3) . . ?
C1 C2 C3 108.0 . . ?
C1 C2 C7 125.6(3) . . ?
C3 C2 C7 125.9(3) . . ?
C1 C2 Fe1 70.18(10) . . ?
C3 C2 Fe1 71.17(10) . . ?
C7 C2 Fe1 130.8(2) . . ?
C4 C3 C2 108.0 . . ?
C4 C3 C8 125.7(3) . . ?
C2 C3 C8 126.2(3) . . ?
C4 C3 Fe1 70.83(10) . . ?
C2 C3 Fe1 69.79(10) . . ?
C8 C3 Fe1 126.9(2) . . ?
C5 C4 C3 108.0 . . ?
C5 C4 C9 126.3(3) . . ?
C3 C4 C9 125.3(3) . . ?
C5 C4 Fe1 70.02(10) . . ?
C3 C4 Fe1 70.36(10) . . ?
C9 C4 Fe1 130.9(2) . . ?
C4 C5 C1 108.0 . . ?
C4 C5 C10 125.5(3) . . ?
C1 C5 C10 126.4(3) . . ?
C4 C5 Fe1 71.10(10) . . ?
C1 C5 Fe1 69.84(10) . . ?
C10 C5 Fe1 124.4(2) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C15 108.0 . . ?
C12 C11 C16 125.8(3) . . ?
C15 C11 C16 125.9(3) . . ?
C12 C11 Fe2 69.80(10) . . ?
C15 C11 Fe2 70.42(10) . . ?
C16 C11 Fe2 130.4(3) . . ?
C13 C12 C11 108.0 . . ?
C13 C12 C17 125.7(3) . . ?
C11 C12 C17 126.3(3) . . ?
C13 C12 Fe2 69.74(10) . . ?
C11 C12 Fe2 71.21(10) . . ?
C17 C12 Fe2 124.3(2) . . ?
C14 C13 C12 108.0 . . ?
C14 C13 C18 125.7(3) . . ?
C12 C13 C18 126.3(3) . . ?
C14 C13 Fe2 70.65(10) . . ?
C12 C13 Fe2 70.95(10) . . ?
C18 C13 Fe2 125.7(3) . . ?
C13 C14 C15 108.0 . . ?
C13 C14 C19 126.3(3) . . ?
C15 C14 C19 125.1(3) . . ?
C13 C14 Fe2 69.97(10) . . ?
C15 C14 Fe2 71.26(10) . . ?
C19 C14 Fe2 131.2(2) . . ?
C11 C15 C14 108.0 . . ?
C11 C15 C20 126.1(3) . . ?
C14 C15 C20 125.8(3) . . ?
C11 C15 Fe2 70.74(10) . . ?
C14 C15 Fe2 69.65(10) . . ?
C20 C15 Fe2 127.1(3) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C24 C23 S2 110.5(3) . . ?
C24 C23 H23A 109.5 . . ?
S2 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
S2 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C21 S1 110.4(4) . . ?
C22 C21 H21A 109.6 . . ?
S1 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
S1 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 C25 O2 126.0(3) . . ?
O1 C25 C26 114.9(3) . . ?
O2 C25 C26 119.0(3) . . ?
C27 C26 C25 123.8(4) . . ?
C27 C26 H26A 118.1 . . ?
C25 C26 H26A 118.1 . . ?
C26 C27 C28 126.9(4) . . ?
C26 C27 H27A 116.6 . . ?
C28 C27 H27A 116.6 . . ?
C29 C28 C33 119.1(4) . . ?
C29 C28 C27 121.9(4) . . ?
C33 C28 C27 119.0(4) . . ?
C28 C29 C30 120.0(4) . . ?
C28 C29 H29A 120.0 . . ?
C30 C29 H29A 120.0 . . ?
C29 C30 C31 119.9(5) . . ?
C29 C30 H30A 120.1 . . ?
C31 C30 H30A 120.1 . . ?
C32 C31 C30 120.5(5) . . ?
C32 C31 H31A 119.8 . . ?
C30 C31 H31A 119.8 . . ?
C31 C32 C33 121.0(5) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C32 C33 C28 119.4(5) . . ?
C32 C33 H33A 120.3 . . ?
C28 C33 H33A 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.065
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
