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

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

data_74a_yellow_a
_database_code_depnum_ccdc_archive 'CCDC 1473788'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;
_audit_creation_date             2016-02-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C18 H12 Fe2 O6 P2'
_chemical_formula_sum            'C18 H12 Fe2 O6 P2'
_chemical_formula_weight         497.92
_chemical_melting_point          ?
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'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.2962(6)
_cell_length_b                   14.3680(7)
_cell_length_c                   14.4014(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.111(2)
_cell_angle_gamma                90
_cell_volume                     2013.06(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8670
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.948
_cell_measurement_theta_min      2.529
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1341 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.8868.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.057
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.565
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3652
_reflns_number_total             4084
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4084
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0229
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0336P)²+0.2524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0604
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C12B(H12B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.53029(2) 0.67512(2) 0.65703(2) 0.01790(7) Uani 1 1 d . U . . .
P1A P 0.36143(4) 0.58350(3) 0.66375(3) 0.01913(10) Uani 1 1 d . U . . .
H1A H 0.3656(19) 0.4971(12) 0.6335(13) 0.032(5) Uiso 1 1 d . . . . .
O1A O 0.33439(14) 0.83004(9) 0.60031(12) 0.0446(4) Uani 1 1 d . U . . .
O2A O 0.54662(16) 0.61479(9) 0.46822(10) 0.0406(3) Uani 1 1 d . U . . .
O3A O 0.76508(14) 0.80195(10) 0.72706(10) 0.0448(4) Uani 1 1 d . U . . .
C1A C 0.41072(17) 0.76995(12) 0.62191(13) 0.0265(4) Uani 1 1 d . U . . .
C2A C 0.54170(17) 0.63904(12) 0.54231(13) 0.0255(4) Uani 1 1 d . U . . .
C3A C 0.67497(18) 0.75193(12) 0.70067(12) 0.0267(4) Uani 1 1 d . U . . .
C11A C 0.18204(16) 0.60847(11) 0.59927(12) 0.0218(4) Uani 1 1 d . U . . .
C12A C 0.13958(18) 0.61090(13) 0.49758(13) 0.0306(4) Uani 1 1 d . U . . .
H12A H 0.2050 0.6034 0.4645 0.037 Uiso 1 1 calc R . . . .
C13A C 0.0020(2) 0.62429(14) 0.44360(15) 0.0367(5) Uani 1 1 d . U . . .
H13A H -0.0266 0.6253 0.3738 0.044 Uiso 1 1 calc R . . . .
C14A C -0.09267(18) 0.63601(13) 0.49104(16) 0.0371(5) Uani 1 1 d . U . . .
H14A H -0.1868 0.6453 0.4541 0.045 Uiso 1 1 calc R . . . .
C15A C -0.0516(2) 0.63434(15) 0.59208(17) 0.0422(5) Uani 1 1 d . U . . .
H15A H -0.1174 0.6433 0.6246 0.051 Uiso 1 1 calc R . . . .
C16A C 0.08606(19) 0.61965(13) 0.64700(15) 0.0333(4) Uani 1 1 d . U . . .
H16A H 0.1138 0.6173 0.7167 0.040 Uiso 1 1 calc R . . . .
Fe1B Fe 0.48438(2) 0.61606(2) 0.81669(2) 0.01770(7) Uani 1 1 d . U . . .
P1B P 0.63809(4) 0.56025(3) 0.75346(3) 0.01900(10) Uani 1 1 d . U . . .
H1B H 0.6077(18) 0.4770(12) 0.7145(13) 0.027(5) Uiso 1 1 d . . . . .
O1B O 0.29060(14) 0.75865(10) 0.83589(10) 0.0429(4) Uani 1 1 d . U . . .
O2B O 0.41303(14) 0.44897(9) 0.90385(9) 0.0338(3) Uani 1 1 d . U . . .
O3B O 0.70124(12) 0.68888(8) 0.98902(9) 0.0287(3) Uani 1 1 d . U . . .
C1B C 0.36417(18) 0.70309(13) 0.82740(12) 0.0266(4) Uani 1 1 d . U . . .
C2B C 0.44111(16) 0.51528(12) 0.87119(12) 0.0231(4) Uani 1 1 d . U . . .
C3B C 0.61841(17) 0.66146(11) 0.92119(12) 0.0216(3) Uani 1 1 d . U . . .
C11B C 0.82107(16) 0.54909(12) 0.81578(11) 0.0219(3) Uani 1 1 d . U . . .
C12B C 0.89944(17) 0.62253(12) 0.86807(13) 0.0256(4) Uani 1 1 d . U . . .
H12B H 0.8573 0.6810 0.8699 0.031 Uiso 1 1 calc R . . . .
C13B C 1.03847(19) 0.61094(14) 0.91748(14) 0.0330(4) Uani 1 1 d . U . . .
H13B H 1.0912 0.6613 0.9534 0.040 Uiso 1 1 calc R . . . .
C14B C 1.10073(19) 0.52648(15) 0.91478(14) 0.0387(5) Uani 1 1 d . U . . .
H14B H 1.1960 0.5185 0.9491 0.046 Uiso 1 1 calc R . . . .
C15B C 1.0243(2) 0.45378(15) 0.86223(15) 0.0392(5) Uani 1 1 d . U . . .
H15B H 1.0674 0.3957 0.8601 0.047 Uiso 1 1 calc R . . . .
C16B C 0.88429(18) 0.46443(13) 0.81218(13) 0.0308(4) Uani 1 1 d . U . . .
H16B H 0.8323 0.4140 0.7757 0.037 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A P1A 2.2080(5) . ?
Fe1A C1A 1.7944(18) . ?
Fe1A C2A 1.7717(18) . ?
Fe1A C3A 1.7942(18) . ?
Fe1A Fe1B 2.6348(3) . ?
Fe1A P1B 2.2080(5) . ?
P1A H1A 1.320(18) . ?
P1A C11A 1.8110(16) . ?
P1A Fe1B 2.2015(5) . ?
O1A C1A 1.140(2) . ?
O2A C2A 1.139(2) . ?
O3A C3A 1.136(2) . ?
C11A C12A 1.385(2) . ?
C11A C16A 1.385(3) . ?
C12A H12A 0.9500 . ?
C12A C13A 1.388(3) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.371(3) . ?
C14A H14A 0.9500 . ?
C14A C15A 1.376(3) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.394(3) . ?
C16A H16A 0.9500 . ?
Fe1B P1B 2.2182(5) . ?
Fe1B C1B 1.8011(18) . ?
Fe1B C2B 1.7722(18) . ?
Fe1B C3B 1.7986(17) . ?
P1B H1B 1.315(17) . ?
P1B C11B 1.8093(16) . ?
O1B C1B 1.134(2) . ?
O2B C2B 1.141(2) . ?
O3B C3B 1.136(2) . ?
C11B C12B 1.391(2) . ?
C11B C16B 1.388(2) . ?
C12B H12B 0.9500 . ?
C12B C13B 1.384(2) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.379(3) . ?
C14B H14B 0.9500 . ?
C14B C15B 1.376(3) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.393(3) . ?
C16B H16B 0.9500 . ?

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
P1A Fe1A Fe1B 53.194(12) . . ?
C1A Fe1A P1A 89.29(6) . . ?
C1A Fe1A Fe1B 100.83(6) . . ?
C1A Fe1A P1B 154.42(6) . . ?
C2A Fe1A P1A 99.21(6) . . ?
C2A Fe1A C1A 102.02(8) . . ?
C2A Fe1A C3A 101.87(8) . . ?
C2A Fe1A Fe1B 143.62(6) . . ?
C2A Fe1A P1B 101.22(6) . . ?
C3A Fe1A P1A 157.93(6) . . ?
C3A Fe1A C1A 92.64(8) . . ?
C3A Fe1A Fe1B 104.95(5) . . ?
C3A Fe1A P1B 92.91(5) . . ?
P1B Fe1A P1A 76.565(17) . . ?
P1B Fe1A Fe1B 53.647(13) . . ?
Fe1A P1A H1A 115.8(8) . . ?
C11A P1A Fe1A 123.02(6) . . ?
C11A P1A H1A 98.9(8) . . ?
C11A P1A Fe1B 128.81(6) . . ?
Fe1B P1A Fe1A 73.386(15) . . ?
Fe1B P1A H1A 117.4(8) . . ?
O1A C1A Fe1A 179.39(17) . . ?
O2A C2A Fe1A 178.58(17) . . ?
O3A C3A Fe1A 178.59(16) . . ?
C12A C11A P1A 117.59(13) . . ?
C12A C11A C16A 119.49(16) . . ?
C16A C11A P1A 122.82(14) . . ?
C11A C12A H12A 119.8 . . ?
C11A C12A C13A 120.43(18) . . ?
C13A C12A H12A 119.8 . . ?
C12A C13A H13A 120.0 . . ?
C14A C13A C12A 119.96(19) . . ?
C14A C13A H13A 120.0 . . ?
C13A C14A H14A 119.9 . . ?
C13A C14A C15A 120.14(17) . . ?
C15A C14A H14A 119.9 . . ?
C14A C15A H15A 119.8 . . ?
C14A C15A C16A 120.39(19) . . ?
C16A C15A H15A 119.8 . . ?
C11A C16A C15A 119.59(18) . . ?
C11A C16A H16A 120.2 . . ?
C15A C16A H16A 120.2 . . ?
P1A Fe1B Fe1A 53.420(13) . . ?
P1A Fe1B P1B 76.487(17) . . ?
P1B Fe1B Fe1A 53.290(12) . . ?
C1B Fe1B Fe1A 100.12(6) . . ?
C1B Fe1B P1A 92.70(5) . . ?
C1B Fe1B P1B 152.71(6) . . ?
C2B Fe1B Fe1A 142.43(5) . . ?
C2B Fe1B P1A 97.11(5) . . ?
C2B Fe1B P1B 101.71(5) . . ?
C2B Fe1B C1B 104.47(8) . . ?
C2B Fe1B C3B 99.27(7) . . ?
C3B Fe1B Fe1A 107.80(5) . . ?
C3B Fe1B P1A 161.18(5) . . ?
C3B Fe1B P1B 91.12(5) . . ?
C3B Fe1B C1B 92.13(7) . . ?
Fe1A P1B Fe1B 73.063(15) . . ?
Fe1A P1B H1B 114.3(8) . . ?
Fe1B P1B H1B 113.7(8) . . ?
C11B P1B Fe1A 127.28(6) . . ?
C11B P1B Fe1B 126.55(5) . . ?
C11B P1B H1B 101.2(8) . . ?
O1B C1B Fe1B 178.51(16) . . ?
O2B C2B Fe1B 178.00(15) . . ?
O3B C3B Fe1B 177.93(15) . . ?
C12B C11B P1B 121.78(12) . . ?
C16B C11B P1B 118.95(13) . . ?
C16B C11B C12B 119.27(16) . . ?
C11B C12B H12B 119.8 . . ?
C13B C12B C11B 120.41(16) . . ?
C13B C12B H12B 119.8 . . ?
C12B C13B H13B 119.9 . . ?
C14B C13B C12B 120.22(18) . . ?
C14B C13B H13B 119.9 . . ?
C13B C14B H14B 120.1 . . ?
C15B C14B C13B 119.75(17) . . ?
C15B C14B H14B 120.1 . . ?
C14B C15B H15B 119.7 . . ?
C14B C15B C16B 120.65(17) . . ?
C16B C15B H15B 119.7 . . ?
C11B C16B C15B 119.69(18) . . ?
C11B C16B H16B 120.2 . . ?
C15B C16B H16B 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1A P1A C11A C12A 63.35(15) . . . . ?
Fe1A P1A C11A C16A -120.45(14) . . . . ?
Fe1A P1B C11B C12B 46.86(16) . . . . ?
Fe1A P1B C11B C16B -133.97(12) . . . . ?
P1A C11A C12A C13A 176.25(14) . . . . ?
P1A C11A C16A C15A -176.93(15) . . . . ?
C11A C12A C13A C14A 0.6(3) . . . . ?
C12A C11A C16A C15A -0.8(3) . . . . ?
C12A C13A C14A C15A -0.1(3) . . . . ?
C13A C14A C15A C16A -0.8(3) . . . . ?
C14A C15A C16A C11A 1.2(3) . . . . ?
C16A C11A C12A C13A -0.1(3) . . . . ?
Fe1B P1A C11A C12A 158.24(11) . . . . ?
Fe1B P1A C11A C16A -25.56(18) . . . . ?
Fe1B P1B C11B C12B -49.36(16) . . . . ?
Fe1B P1B C11B C16B 129.80(12) . . . . ?
P1B C11B C12B C13B 178.00(14) . . . . ?
P1B C11B C16B C15B -178.05(14) . . . . ?
C11B C12B C13B C14B 0.4(3) . . . . ?
C12B C11B C16B C15B 1.1(3) . . . . ?
C12B C13B C14B C15B 0.4(3) . . . . ?
C13B C14B C15B C16B -0.4(3) . . . . ?
C14B C15B C16B C11B -0.4(3) . . . . ?
C16B C11B C12B C13B -1.2(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ar50a
_database_code_depnum_ccdc_archive 'CCDC 1473789'
_audit_update_record             
;
2016-04-13 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H15 Fe3 O11 P'
_chemical_formula_sum            'C31 H15 Fe3 O11 P'
_chemical_formula_weight         761.95

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'
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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   8.45114(16)
_cell_length_b                   16.8793(3)
_cell_length_c                   21.7282(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3099.51(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    28199
_cell_measurement_theta_min      2.8482
_cell_measurement_theta_max      30.6348

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7650
_exptl_absorpt_correction_T_max  0.9179
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray micro-source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53905
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         29.50
_reflns_number_total             8534
_reflns_number_gt                8026
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0248P)²+0.4642P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(7)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         8534
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0533
_refine_ls_wR_factor_gt          0.0517
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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 0.71566(3) 0.606352(13) 0.318420(10) 0.02257(5) Uani 1 1 d . . .
Fe2 Fe 0.78333(3) 0.472623(14) 0.257835(10) 0.02536(5) Uani 1 1 d . . .
Fe3 Fe 0.50046(3) 0.532755(14) 0.249374(10) 0.02495(5) Uani 1 1 d . . .
P1 P 0.62089(5) 0.49216(2) 0.334053(18) 0.01998(8) Uani 1 1 d . . .
O1 O 0.99116(16) 0.60992(8) 0.39955(6) 0.0387(3) Uani 1 1 d . . .
O2 O 0.50781(19) 0.71406(9) 0.38686(7) 0.0489(4) Uani 1 1 d . . .
O3 O 0.8377(2) 0.72368(11) 0.23000(8) 0.0675(5) Uani 1 1 d . . .
O4 O 0.97300(19) 0.38102(10) 0.34521(7) 0.0553(4) Uani 1 1 d . . .
O5 O 0.7346(3) 0.32410(10) 0.18993(8) 0.0709(5) Uani 1 1 d . . .
O6 O 1.06421(18) 0.54860(12) 0.20469(8) 0.0667(6) Uani 1 1 d . . .
O7 O 0.70807(18) 0.56364(9) 0.14260(6) 0.0435(3) Uani 1 1 d . . .
O8 O 0.3486(2) 0.42310(14) 0.16268(10) 0.0877(7) Uani 1 1 d . . .
O9 O 0.4099(2) 0.69205(10) 0.20806(9) 0.0605(5) Uani 1 1 d . . .
O10 O 0.22812(16) 0.52139(10) 0.33209(7) 0.0523(4) Uani 1 1 d . . .
O11 O 0.85308(14) 0.42832(7) 0.47308(6) 0.0323(3) Uani 1 1 d . . .
C1 C 0.8836(2) 0.60831(10) 0.36830(8) 0.0266(3) Uani 1 1 d . . .
C2 C 0.5882(2) 0.67160(10) 0.36080(8) 0.0314(4) Uani 1 1 d . . .
C3 C 0.7901(2) 0.67763(11) 0.26320(8) 0.0379(4) Uani 1 1 d . . .
C4 C 0.8971(2) 0.41788(12) 0.31329(9) 0.0346(4) Uani 1 1 d . . .
C5 C 0.7534(3) 0.38222(12) 0.21480(9) 0.0429(5) Uani 1 1 d . . .
C6 C 0.9544(2) 0.52050(14) 0.22556(9) 0.0410(5) Uani 1 1 d . . .
C7 C 0.6750(2) 0.53863(12) 0.19076(8) 0.0315(4) Uani 1 1 d . . .
C8 C 0.4057(2) 0.46554(15) 0.19637(10) 0.0469(5) Uani 1 1 d . . .
C9 C 0.4487(2) 0.63096(12) 0.22385(9) 0.0387(4) Uani 1 1 d . . .
C10 C 0.3359(2) 0.52581(13) 0.30142(8) 0.0341(4) Uani 1 1 d . . .
C11 C 0.53506(17) 0.42236(9) 0.38704(7) 0.0189(3) Uani 1 1 d . . .
C12 C 0.4571(2) 0.35646(9) 0.35970(7) 0.0252(3) Uani 1 1 d . . .
H12 H 0.4589 0.3500 0.3163 0.030 Uiso 1 1 calc R . .
C13 C 0.3801(2) 0.30269(9) 0.39543(8) 0.0259(3) Uani 1 1 d . . .
H13 H 0.3275 0.2592 0.3768 0.031 Uiso 1 1 calc R . .
C14 C 0.37783(17) 0.31114(9) 0.46025(7) 0.0209(3) Uani 1 1 d . . .
C15 C 0.2983(2) 0.25546(9) 0.49781(8) 0.0276(3) Uani 1 1 d . . .
H15 H 0.2442 0.2123 0.4793 0.033 Uiso 1 1 calc R . .
C16 C 0.2986(2) 0.26314(10) 0.56012(8) 0.0322(4) Uani 1 1 d . . .
H16 H 0.2447 0.2254 0.5849 0.039 Uiso 1 1 calc R . .
C17 C 0.3782(2) 0.32664(10) 0.58797(8) 0.0316(4) Uani 1 1 d . . .
H17 H 0.3784 0.3313 0.6315 0.038 Uiso 1 1 calc R . .
C18 C 0.45577(19) 0.38212(9) 0.55316(7) 0.0243(3) Uani 1 1 d . . .
H18 H 0.5089 0.4248 0.5727 0.029 Uiso 1 1 calc R . .
C19 C 0.45707(16) 0.37613(8) 0.48805(7) 0.0179(3) Uani 1 1 d . . .
C20 C 0.53699(16) 0.43285(8) 0.45019(7) 0.0174(3) Uani 1 1 d . . .
C21 C 0.61960(17) 0.50084(8) 0.48037(7) 0.0179(3) Uani 1 1 d . . .
C22 C 0.53356(18) 0.56861(8) 0.50055(7) 0.0196(3) Uani 1 1 d . . .
C23 C 0.36892(19) 0.57779(10) 0.48900(8) 0.0258(3) Uani 1 1 d . . .
H23 H 0.3134 0.5379 0.4669 0.031 Uiso 1 1 calc R . .
C24 C 0.2897(2) 0.64349(10) 0.50940(8) 0.0322(4) Uani 1 1 d . . .
H24 H 0.1795 0.6485 0.5016 0.039 Uiso 1 1 calc R . .
C25 C 0.3691(2) 0.70360(11) 0.54165(9) 0.0367(4) Uani 1 1 d . . .
H25 H 0.3129 0.7491 0.5552 0.044 Uiso 1 1 calc R . .
C26 C 0.5270(2) 0.69656(10) 0.55351(9) 0.0336(4) Uani 1 1 d . . .
H26 H 0.5798 0.7373 0.5757 0.040 Uiso 1 1 calc R . .
C27 C 0.6133(2) 0.62969(9) 0.53336(7) 0.0248(3) Uani 1 1 d . . .
C28 C 0.7772(2) 0.62140(9) 0.54502(7) 0.0277(3) Uani 1 1 d . . .
H28 H 0.8317 0.6622 0.5665 0.033 Uiso 1 1 calc R . .
C29 C 0.8586(2) 0.55589(10) 0.52600(8) 0.0266(3) Uani 1 1 d . . .
H29 H 0.9683 0.5511 0.5347 0.032 Uiso 1 1 calc R . .
C30 C 0.77976(18) 0.49529(8) 0.49352(7) 0.0216(3) Uani 1 1 d . . .
C31 C 1.0146(2) 0.41631(12) 0.48921(12) 0.0466(5) Uani 1 1 d . . .
H31A H 1.0492 0.3643 0.4745 0.070 Uiso 1 1 calc R . .
H31B H 1.0260 0.4187 0.5341 0.070 Uiso 1 1 calc R . .
H31C H 1.0797 0.4577 0.4702 0.070 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.7863(17) . yes
Fe1 C2 1.7948(19) . yes
Fe1 C3 1.8119(18) . yes
Fe1 P1 2.1147(4) . yes
Fe1 Fe3 2.6649(3) . yes
Fe1 Fe2 2.6749(3) . yes
Fe2 C4 1.7970(19) . yes
Fe2 C6 1.799(2) . yes
Fe2 C5 1.807(2) . yes
Fe2 C7 2.0501(18) . yes
Fe2 P1 2.1762(4) . yes
Fe2 Fe3 2.6036(3) . yes
Fe3 C10 1.7961(18) . yes
Fe3 C9 1.802(2) . yes
Fe3 C8 1.804(2) . yes
Fe3 C7 1.9515(17) . yes
Fe3 P1 2.2115(4) . yes
P1 C11 1.7999(15) . yes
O1 C1 1.135(2) . ?
O2 C2 1.138(2) . ?
O3 C3 1.134(2) . ?
O4 C4 1.131(2) . ?
O5 C5 1.131(2) . ?
O6 C6 1.137(2) . ?
O7 C7 1.162(2) . ?
O8 C8 1.132(3) . ?
O9 C9 1.135(2) . ?
O10 C10 1.131(2) . ?
O11 C30 1.3636(19) . ?
O11 C31 1.424(2) . ?
C11 C20 1.384(2) . ?
C11 C12 1.423(2) . ?
C12 C13 1.360(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.416(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.415(2) . ?
C14 C19 1.420(2) . ?
C15 C16 1.360(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.403(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.418(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.432(2) . ?
C20 C21 1.4948(19) . ?
C21 C30 1.387(2) . ?
C21 C22 1.425(2) . ?
C22 C23 1.422(2) . ?
C22 C27 1.423(2) . ?
C23 C24 1.369(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.404(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.364(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.413(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.416(3) . ?
C28 C29 1.366(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.410(2) . ?
C29 H29 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 98.88(8) . . ?
C1 Fe1 C3 96.53(8) . . ?
C2 Fe1 C3 98.08(9) . . ?
C1 Fe1 P1 102.73(5) . . ?
C2 Fe1 P1 104.45(6) . . ?
C3 Fe1 P1 147.47(6) . . ?
C1 Fe1 Fe3 153.20(5) . . ?
C2 Fe1 Fe3 99.51(6) . . ?
C3 Fe1 Fe3 100.00(6) . . ?
P1 Fe1 Fe3 53.635(13) . . ?
C1 Fe1 Fe2 98.30(5) . . ?
C2 Fe1 Fe2 153.98(6) . . ?
C3 Fe1 Fe2 99.22(6) . . ?
P1 Fe1 Fe2 52.474(13) . . ?
Fe3 Fe1 Fe2 58.364(9) . . ?
C4 Fe2 C6 93.59(8) . . ?
C4 Fe2 C5 89.29(9) . . ?
C6 Fe2 C5 106.86(10) . . ?
C4 Fe2 C7 174.18(8) . . ?
C6 Fe2 C7 80.64(8) . . ?
C5 Fe2 C7 91.65(9) . . ?
C4 Fe2 P1 84.55(6) . . ?
C6 Fe2 P1 137.36(8) . . ?
C5 Fe2 P1 115.69(7) . . ?
C7 Fe2 P1 100.19(5) . . ?
C4 Fe2 Fe3 137.63(6) . . ?
C6 Fe2 Fe3 122.36(7) . . ?
C5 Fe2 Fe3 99.45(7) . . ?
C7 Fe2 Fe3 47.78(5) . . ?
P1 Fe2 Fe3 54.230(12) . . ?
C4 Fe2 Fe1 102.61(6) . . ?
C6 Fe2 Fe1 89.11(8) . . ?
C5 Fe2 Fe1 159.58(7) . . ?
C7 Fe2 Fe1 78.21(5) . . ?
P1 Fe2 Fe1 50.412(12) . . ?
Fe3 Fe2 Fe1 60.626(9) . . ?
C10 Fe3 C9 93.77(9) . . ?
C10 Fe3 C8 91.00(9) . . ?
C9 Fe3 C8 105.92(10) . . ?
C10 Fe3 C7 178.13(8) . . ?
C9 Fe3 C7 86.33(9) . . ?
C8 Fe3 C7 87.18(9) . . ?
C10 Fe3 P1 79.18(6) . . ?
C9 Fe3 P1 130.76(7) . . ?
C8 Fe3 P1 122.72(8) . . ?
C7 Fe3 P1 102.17(5) . . ?
C10 Fe3 Fe2 129.86(6) . . ?
C9 Fe3 Fe2 127.11(6) . . ?
C8 Fe3 Fe2 101.97(7) . . ?
C7 Fe3 Fe2 51.08(5) . . ?
P1 Fe3 Fe2 52.979(12) . . ?
C10 Fe3 Fe1 101.79(6) . . ?
C9 Fe3 Fe1 84.85(7) . . ?
C8 Fe3 Fe1 162.83(7) . . ?
C7 Fe3 Fe1 80.08(5) . . ?
P1 Fe3 Fe1 50.353(12) . . ?
Fe2 Fe3 Fe1 61.010(9) . . ?
C11 P1 Fe1 148.43(5) . . ?
C11 P1 Fe2 129.92(5) . . ?
Fe1 P1 Fe2 77.114(15) . . ?
C11 P1 Fe3 123.33(5) . . ?
Fe1 P1 Fe3 76.012(15) . . ?
Fe2 P1 Fe3 72.791(15) . . ?
C30 O11 C31 118.26(14) . . ?
O1 C1 Fe1 179.33(17) . . ?
O2 C2 Fe1 178.71(17) . . ?
O3 C3 Fe1 178.02(18) . . ?
O4 C4 Fe2 175.69(18) . . ?
O5 C5 Fe2 177.38(19) . . ?
O6 C6 Fe2 178.0(2) . . ?
O7 C7 Fe3 141.96(15) . . ?
O7 C7 Fe2 136.89(15) . . ?
Fe3 C7 Fe2 81.14(6) . . ?
O8 C8 Fe3 178.9(2) . . ?
O9 C9 Fe3 177.29(19) . . ?
O10 C10 Fe3 177.06(16) . . ?
C20 C11 C12 121.30(14) . . ?
C20 C11 P1 123.09(11) . . ?
C12 C11 P1 115.55(11) . . ?
C13 C12 C11 120.33(15) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 120.48(14) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 120.90(14) . . ?
C15 C14 C19 119.46(14) . . ?
C13 C14 C19 119.64(14) . . ?
C16 C15 C14 120.68(15) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.20(15) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 120.89(16) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 120.36(15) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 118.40(13) . . ?
C18 C19 C20 121.94(13) . . ?
C14 C19 C20 119.65(13) . . ?
C11 C20 C19 118.60(13) . . ?
C11 C20 C21 122.59(13) . . ?
C19 C20 C21 118.81(13) . . ?
C30 C21 C22 119.27(14) . . ?
C30 C21 C20 119.64(13) . . ?
C22 C21 C20 120.87(13) . . ?
C23 C22 C27 118.20(14) . . ?
C23 C22 C21 122.17(14) . . ?
C27 C22 C21 119.62(14) . . ?
C24 C23 C22 120.64(16) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 120.86(18) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 119.94(17) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 121.03(17) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 121.90(15) . . ?
C26 C27 C22 119.32(16) . . ?
C28 C27 C22 118.78(15) . . ?
C29 C28 C27 121.22(14) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 120.08(15) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
O11 C30 C21 115.62(13) . . ?
O11 C30 C29 123.36(14) . . ?
C21 C30 C29 121.02(14) . . ?
O11 C31 H31A 109.5 . . ?
O11 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O11 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        29.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_carolina8_021byn
_database_code_depnum_ccdc_archive 'CCDC 1473786'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Fe4 O6 P2'
_chemical_formula_sum            'C36 H30 Fe4 O6 P2'
_chemical_formula_weight         843.94

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'
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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   11.8594(16)
_cell_length_b                   12.0460(16)
_cell_length_c                   24.436(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.571(6)
_cell_angle_gamma                90.00
_cell_volume                     3490.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.407
_cell_measurement_theta_max      25.568

_exptl_crystal_description       Plates
_exptl_crystal_colour            'Bright yellow'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39766
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6136
_reflns_number_gt                5014
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'

_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)+(0.0306P)²+1.5102P] 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         6136
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.005
_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 0.79498(3) 0.85368(3) 1.007537(13) 0.02577(9) Uani 1 1 d . . .
C1A C 0.8674(2) 0.8541(2) 1.07221(11) 0.0411(6) Uani 1 1 d . . .
O1A O 0.9151(2) 0.85564(18) 1.11286(8) 0.0682(7) Uani 1 1 d . . .
C2A C 0.6560(2) 0.8974(2) 1.02636(10) 0.0366(6) Uani 1 1 d . . .
O2A O 0.56949(17) 0.92708(18) 1.03849(9) 0.0589(6) Uani 1 1 d . . .
C3A C 0.8540(2) 0.9850(2) 0.99043(10) 0.0321(6) Uani 1 1 d . . .
O3A O 0.89130(16) 1.06979(15) 0.98050(8) 0.0483(5) Uani 1 1 d . . .
Fe2 Fe 0.91772(3) 0.71220(3) 0.950473(14) 0.03030(9) Uani 1 1 d . . .
C1B C 1.0238(2) 0.6726(2) 0.99931(12) 0.0453(7) Uani 1 1 d . . .
O1B O 1.09271(18) 0.6487(2) 1.03001(10) 0.0770(8) Uani 1 1 d . . .
C2B C 0.9013(2) 0.5954(2) 0.90757(11) 0.0434(7) Uani 1 1 d . . .
O2B O 0.8852(2) 0.52114(18) 0.87935(9) 0.0697(7) Uani 1 1 d . . .
C3B C 1.0151(2) 0.7959(2) 0.91271(11) 0.0424(6) Uani 1 1 d . . .
O3B O 1.07748(18) 0.8471(2) 0.88862(10) 0.0727(7) Uani 1 1 d . . .
C1 C 0.5545(2) 0.6669(2) 0.97348(10) 0.0328(6) Uani 1 1 d . . .
C2 C 0.5503(2) 0.73784(19) 0.92804(10) 0.0320(6) Uani 1 1 d . . .
C3 C 0.4541(2) 0.8002(2) 0.91850(13) 0.0464(7) Uani 1 1 d . . .
H3 H 0.4508 0.8486 0.8878 0.056 Uiso 1 1 calc R . .
C4 C 0.3628(2) 0.7929(3) 0.95305(15) 0.0579(9) Uani 1 1 d . . .
H4 H 0.2969 0.8355 0.9459 0.069 Uiso 1 1 calc R . .
C5 C 0.3675(3) 0.7236(3) 0.99794(14) 0.0573(9) Uani 1 1 d . . .
H5 H 0.3047 0.7183 1.0216 0.069 Uiso 1 1 calc R . .
C6 C 0.4635(2) 0.6621(2) 1.00840(12) 0.0459(7) Uani 1 1 d . . .
H6 H 0.4672 0.6160 1.0399 0.055 Uiso 1 1 calc R . .
C7 C 0.6489(2) 0.7446(2) 0.89043(9) 0.0308(5) Uani 1 1 d . . .
H7A H 0.6251 0.7844 0.8568 0.037 Uiso 1 1 calc R . .
H7B H 0.6703 0.6683 0.8796 0.037 Uiso 1 1 calc R . .
C8 C 0.6563(2) 0.5962(2) 0.98460(10) 0.0343(6) Uani 1 1 d . . .
H8A H 0.6760 0.5569 0.9504 0.041 Uiso 1 1 calc R . .
H8B H 0.6360 0.5392 1.0120 0.041 Uiso 1 1 calc R . .
P5 P 0.77588(5) 0.81531(5) 0.91948(2) 0.02492(14) Uani 1 1 d . . .
P6 P 0.78317(5) 0.67126(5) 1.00978(2) 0.02810(14) Uani 1 1 d . . .
C9 C 0.80296(19) 0.92320(19) 0.86727(9) 0.0288(5) Uani 1 1 d . . .
H9A H 0.8705 0.9663 0.8784 0.035 Uiso 1 1 calc R . .
H9B H 0.8195 0.8866 0.8320 0.035 Uiso 1 1 calc R . .
Fe3 Fe 0.70121(3) 1.13664(3) 0.810053(15) 0.03909(11) Uani 1 1 d . . .
C11C C 0.7062(2) 1.00106(19) 0.85931(9) 0.0287(5) Uani 1 1 d . . .
C12C C 0.6175(2) 0.9921(2) 0.81992(11) 0.0405(6) Uani 1 1 d . . .
H12C H 0.6095 0.9346 0.7935 0.049 Uiso 1 1 calc R . .
C13C C 0.5434(2) 1.0824(2) 0.82649(11) 0.0446(7) Uani 1 1 d . . .
H13C H 0.4776 1.0970 0.8052 0.054 Uiso 1 1 calc R . .
C14C C 0.5838(2) 1.1466(2) 0.86990(11) 0.0469(7) Uani 1 1 d . . .
H14C H 0.5498 1.2123 0.8835 0.056 Uiso 1 1 calc R . .
C15C C 0.6841(2) 1.0974(2) 0.89034(10) 0.0399(6) Uani 1 1 d . . .
H15C H 0.7289 1.1246 0.9199 0.048 Uiso 1 1 calc R . .
C16C C 0.8536(4) 1.1532(5) 0.7744(2) 0.0975(16) Uani 1 1 d . . .
H16C H 0.9188 1.1095 0.7816 0.117 Uiso 1 1 calc R . .
C17C C 0.7707(5) 1.1293(4) 0.73467(18) 0.1006(16) Uani 1 1 d . . .
H17C H 0.7697 1.0668 0.7109 0.121 Uiso 1 1 calc R . .
C18C C 0.6922(4) 1.2115(4) 0.73622(16) 0.0892(13) Uani 1 1 d . . .
H18C H 0.6270 1.2158 0.7134 0.107 Uiso 1 1 calc R . .
C19C C 0.7219(4) 1.2883(3) 0.7764(2) 0.0862(13) Uani 1 1 d . . .
H19C H 0.6812 1.3535 0.7856 0.103 Uiso 1 1 calc R . .
C20C C 0.8253(4) 1.2509(4) 0.8016(2) 0.1018(15) Uani 1 1 d . . .
H20C H 0.8659 1.2856 0.8306 0.122 Uiso 1 1 calc R . .
Fe4 Fe 0.72475(3) 0.53354(3) 1.191092(14) 0.04040(11) Uani 1 1 d . . .
C10 C 0.8171(2) 0.5921(2) 1.07309(9) 0.0343(6) Uani 1 1 d . . .
H10A H 0.8394 0.5157 1.0630 0.041 Uiso 1 1 calc R . .
H10B H 0.8822 0.6275 1.0918 0.041 Uiso 1 1 calc R . .
C11D C 0.7203(2) 0.5866(2) 1.11189(9) 0.0337(6) Uani 1 1 d . . .
C12D C 0.6472(2) 0.4944(2) 1.11921(11) 0.0484(7) Uani 1 1 d . . .
H12D H 0.6517 0.4252 1.1006 0.058 Uiso 1 1 calc R . .
C13D C 0.5665(3) 0.5236(3) 1.15899(13) 0.0606(9) Uani 1 1 d . . .
H13D H 0.5074 0.4774 1.1717 0.073 Uiso 1 1 calc R . .
C14D C 0.5887(3) 0.6323(3) 1.17645(12) 0.0568(8) Uani 1 1 d . . .
H14D H 0.5473 0.6723 1.2031 0.068 Uiso 1 1 calc R . .
C15D C 0.6831(2) 0.6720(2) 1.14762(11) 0.0442(7) Uani 1 1 d . . .
H15D H 0.7161 0.7435 1.1514 0.053 Uiso 1 1 calc R . .
C16D C 0.8860(3) 0.4978(6) 1.21086(16) 0.0955(17) Uani 1 1 d . . .
H16D H 0.9485 0.5068 1.1873 0.115 Uiso 1 1 calc R . .
C17D C 0.8192(6) 0.4036(4) 1.2154(2) 0.1062(18) Uani 1 1 d . . .
H17D H 0.8271 0.3366 1.1954 0.127 Uiso 1 1 calc R . .
C18D C 0.7395(4) 0.4258(5) 1.2545(2) 0.0997(15) Uani 1 1 d . . .
H18D H 0.6824 0.3761 1.2663 0.120 Uiso 1 1 calc R . .
C19D C 0.7559(4) 0.5286(5) 1.27279(15) 0.0966(16) Uani 1 1 d . . .
H19D H 0.7119 0.5639 1.3000 0.116 Uiso 1 1 calc R . .
C20D C 0.8449(4) 0.5758(4) 1.2469(2) 0.0922(14) Uani 1 1 d . . .
H20D H 0.8761 0.6519 1.2534 0.111 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C3A 1.781(3) . ?
Fe1 C1A 1.791(3) . ?
Fe1 C2A 1.794(3) . ?
Fe1 P6 2.2026(7) . ?
Fe1 P5 2.2103(7) . ?
Fe1 Fe2 2.6473(5) . ?
C1A O1A 1.138(3) . ?
C2A O2A 1.129(3) . ?
C3A O3A 1.140(3) . ?
Fe2 C2B 1.764(3) . ?
Fe2 C1B 1.790(3) . ?
Fe2 C3B 1.795(3) . ?
Fe2 P5 2.2182(7) . ?
Fe2 P6 2.2217(7) . ?
C1B O1B 1.140(3) . ?
C2B O2B 1.144(3) . ?
C3B O3B 1.133(3) . ?
C1 C6 1.383(4) . ?
C1 C2 1.402(3) . ?
C1 C8 1.500(4) . ?
C2 C3 1.383(4) . ?
C2 C7 1.497(3) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 P5 1.864(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 P6 1.855(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
P5 C9 1.851(2) . ?
P6 C10 1.858(2) . ?
C9 C11C 1.493(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
Fe3 C19C 2.019(3) . ?
Fe3 C18C 2.019(3) . ?
Fe3 C12C 2.020(3) . ?
Fe3 C16C 2.024(4) . ?
Fe3 C13C 2.027(3) . ?
Fe3 C17C 2.027(4) . ?
Fe3 C20C 2.027(4) . ?
Fe3 C11C 2.029(2) . ?
Fe3 C15C 2.030(2) . ?
Fe3 C14C 2.032(3) . ?
C11C C15C 1.412(3) . ?
C11C C12C 1.423(3) . ?
C12C C13C 1.409(4) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.394(4) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.415(4) . ?
C14C H14C 0.9500 . ?
C15C H15C 0.9500 . ?
C16C C20C 1.395(6) . ?
C16C C17C 1.405(6) . ?
C16C H16C 0.9500 . ?
C17C C18C 1.360(6) . ?
C17C H17C 0.9500 . ?
C18C C19C 1.392(6) . ?
C18C H18C 0.9500 . ?
C19C C20C 1.439(6) . ?
C19C H19C 0.9500 . ?
C20C H20C 0.9500 . ?
Fe4 C17D 2.011(4) . ?
Fe4 C16D 2.014(4) . ?
Fe4 C20D 2.027(4) . ?
Fe4 C18D 2.027(4) . ?
Fe4 C19D 2.027(4) . ?
Fe4 C13D 2.030(3) . ?
Fe4 C12D 2.030(3) . ?
Fe4 C14D 2.034(3) . ?
Fe4 C15D 2.036(3) . ?
Fe4 C11D 2.038(2) . ?
C10 C11D 1.497(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11D C15D 1.422(4) . ?
C11D C12D 1.422(4) . ?
C12D C13D 1.415(4) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.401(5) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.412(4) . ?
C14D H14D 0.9500 . ?
C15D H15D 0.9500 . ?
C16D C20D 1.379(6) . ?
C16D C17D 1.389(7) . ?
C16D H16D 0.9500 . ?
C17D C18D 1.376(7) . ?
C17D H17D 0.9500 . ?
C18D C19D 1.331(7) . ?
C18D H18D 0.9500 . ?
C19D C20D 1.361(6) . ?
C19D H19D 0.9500 . ?
C20D H20D 1.0000 . ?

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
C3A Fe1 C1A 91.05(11) . . ?
C3A Fe1 C2A 99.44(11) . . ?
C1A Fe1 C2A 101.92(12) . . ?
C3A Fe1 P6 156.48(8) . . ?
C1A Fe1 P6 90.63(8) . . ?
C2A Fe1 P6 103.15(8) . . ?
C3A Fe1 P5 89.65(8) . . ?
C1A Fe1 P5 154.58(10) . . ?
C2A Fe1 P5 103.03(8) . . ?
P6 Fe1 P5 79.03(2) . . ?
C3A Fe1 Fe2 103.20(8) . . ?
C1A Fe1 Fe2 101.85(9) . . ?
C2A Fe1 Fe2 146.62(8) . . ?
P6 Fe1 Fe2 53.58(2) . . ?
P5 Fe1 Fe2 53.425(19) . . ?
O1A C1A Fe1 178.6(3) . . ?
O2A C2A Fe1 178.5(2) . . ?
O3A C3A Fe1 178.6(2) . . ?
C2B Fe2 C1B 104.86(13) . . ?
C2B Fe2 C3B 102.13(13) . . ?
C1B Fe2 C3B 92.34(12) . . ?
C2B Fe2 P5 99.48(9) . . ?
C1B Fe2 P5 154.47(10) . . ?
C3B Fe2 P5 89.97(8) . . ?
C2B Fe2 P6 97.75(9) . . ?
C1B Fe2 P6 90.61(9) . . ?
C3B Fe2 P6 158.42(9) . . ?
P5 Fe2 P6 78.46(3) . . ?
C2B Fe2 Fe1 140.20(9) . . ?
C1B Fe2 Fe1 101.94(10) . . ?
C3B Fe2 Fe1 105.61(9) . . ?
P5 Fe2 Fe1 53.151(19) . . ?
P6 Fe2 Fe1 52.92(2) . . ?
O1B C1B Fe2 178.8(3) . . ?
O2B C2B Fe2 176.6(3) . . ?
O3B C3B Fe2 178.8(3) . . ?
C6 C1 C2 119.5(3) . . ?
C6 C1 C8 119.7(2) . . ?
C2 C1 C8 120.8(2) . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 C7 121.0(2) . . ?
C1 C2 C7 119.9(2) . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C2 C7 P5 115.11(16) . . ?
C2 C7 H7A 108.5 . . ?
P5 C7 H7A 108.5 . . ?
C2 C7 H7B 108.5 . . ?
P5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C1 C8 P6 115.61(16) . . ?
C1 C8 H8A 108.4 . . ?
P6 C8 H8A 108.4 . . ?
C1 C8 H8B 108.4 . . ?
P6 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C9 P5 C7 101.74(11) . . ?
C9 P5 Fe1 120.48(8) . . ?
C7 P5 Fe1 122.73(8) . . ?
C9 P5 Fe2 119.49(8) . . ?
C7 P5 Fe2 118.76(8) . . ?
Fe1 P5 Fe2 73.42(2) . . ?
C8 P6 C10 101.20(11) . . ?
C8 P6 Fe1 121.97(8) . . ?
C10 P6 Fe1 121.29(9) . . ?
C8 P6 Fe2 118.50(8) . . ?
C10 P6 Fe2 120.42(8) . . ?
Fe1 P6 Fe2 73.50(2) . . ?
C11C C9 P5 113.10(15) . . ?
C11C C9 H9A 109.0 . . ?
P5 C9 H9A 109.0 . . ?
C11C C9 H9B 109.0 . . ?
P5 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C19C Fe3 C18C 40.35(16) . . ?
C19C Fe3 C12C 152.92(16) . . ?
C18C Fe3 C12C 118.02(16) . . ?
C19C Fe3 C16C 67.86(18) . . ?
C18C Fe3 C16C 67.12(19) . . ?
C12C Fe3 C16C 125.32(19) . . ?
C19C Fe3 C13C 119.25(15) . . ?
C18C Fe3 C13C 106.26(16) . . ?
C12C Fe3 C13C 40.76(11) . . ?
C16C Fe3 C13C 161.4(2) . . ?
C19C Fe3 C17C 67.53(19) . . ?
C18C Fe3 C17C 39.29(17) . . ?
C12C Fe3 C17C 105.98(17) . . ?
C16C Fe3 C17C 40.57(19) . . ?
C13C Fe3 C17C 123.4(2) . . ?
C19C Fe3 C20C 41.66(17) . . ?
C18C Fe3 C20C 68.77(19) . . ?
C12C Fe3 C20C 162.87(19) . . ?
C16C Fe3 C20C 40.27(18) . . ?
C13C Fe3 C20C 155.8(2) . . ?
C17C Fe3 C20C 68.6(2) . . ?
C19C Fe3 C11C 165.14(17) . . ?
C18C Fe3 C11C 152.93(16) . . ?
C12C Fe3 C11C 41.15(10) . . ?
C16C Fe3 C11C 108.27(14) . . ?
C13C Fe3 C11C 69.18(10) . . ?
C17C Fe3 C11C 119.59(15) . . ?
C20C Fe3 C11C 126.15(17) . . ?
C19C Fe3 C15C 128.14(17) . . ?
C18C Fe3 C15C 164.30(17) . . ?
C12C Fe3 C15C 68.29(11) . . ?
C16C Fe3 C15C 122.49(17) . . ?
C13C Fe3 C15C 68.41(11) . . ?
C17C Fe3 C15C 155.96(17) . . ?
C20C Fe3 C15C 109.64(17) . . ?
C11C Fe3 C15C 40.72(10) . . ?
C19C Fe3 C14C 109.06(15) . . ?
C18C Fe3 C14C 125.89(17) . . ?
C12C Fe3 C14C 67.91(12) . . ?
C16C Fe3 C14C 157.6(2) . . ?
C13C Fe3 C14C 40.17(11) . . ?
C17C Fe3 C14C 160.7(2) . . ?
C20C Fe3 C14C 122.45(19) . . ?
C11C Fe3 C14C 68.69(10) . . ?
C15C Fe3 C14C 40.76(10) . . ?
C15C C11C C12C 106.6(2) . . ?
C15C C11C C9 126.4(2) . . ?
C12C C11C C9 127.0(2) . . ?
C15C C11C Fe3 69.67(14) . . ?
C12C C11C Fe3 69.09(14) . . ?
C9 C11C Fe3 126.91(16) . . ?
C13C C12C C11C 108.8(2) . . ?
C13C C12C Fe3 69.86(16) . . ?
C11C C12C Fe3 69.76(14) . . ?
C13C C12C H12C 125.6 . . ?
C11C C12C H12C 125.6 . . ?
Fe3 C12C H12C 126.3 . . ?
C14C C13C C12C 107.7(2) . . ?
C14C C13C Fe3 70.14(16) . . ?
C12C C13C Fe3 69.38(15) . . ?
C14C C13C H13C 126.1 . . ?
C12C C13C H13C 126.1 . . ?
Fe3 C13C H13C 125.9 . . ?
C13C C14C C15C 108.6(2) . . ?
C13C C14C Fe3 69.70(16) . . ?
C15C C14C Fe3 69.54(15) . . ?
C13C C14C H14C 125.7 . . ?
C15C C14C H14C 125.7 . . ?
Fe3 C14C H14C 126.6 . . ?
C11C C15C C14C 108.3(2) . . ?
C11C C15C Fe3 69.61(13) . . ?
C14C C15C Fe3 69.71(14) . . ?
C11C C15C H15C 125.8 . . ?
C14C C15C H15C 125.8 . . ?
Fe3 C15C H15C 126.4 . . ?
C20C C16C C17C 109.4(4) . . ?
C20C C16C Fe3 70.0(2) . . ?
C17C C16C Fe3 69.8(2) . . ?
C20C C16C H16C 125.3 . . ?
C17C C16C H16C 125.3 . . ?
Fe3 C16C H16C 126.5 . . ?
C18C C17C C16C 107.8(5) . . ?
C18C C17C Fe3 70.0(2) . . ?
C16C C17C Fe3 69.6(2) . . ?
C18C C17C H17C 126.1 . . ?
C16C C17C H17C 126.1 . . ?
Fe3 C17C H17C 125.9 . . ?
C17C C18C C19C 109.5(5) . . ?
C17C C18C Fe3 70.7(2) . . ?
C19C C18C Fe3 69.8(2) . . ?
C17C C18C H18C 125.2 . . ?
C19C C18C H18C 125.2 . . ?
Fe3 C18C H18C 125.8 . . ?
C18C C19C C20C 107.6(4) . . ?
C18C C19C Fe3 69.8(2) . . ?
C20C C19C Fe3 69.5(2) . . ?
C18C C19C H19C 126.2 . . ?
C20C C19C H19C 126.2 . . ?
Fe3 C19C H19C 126.1 . . ?
C16C C20C C19C 105.6(4) . . ?
C16C C20C Fe3 69.7(2) . . ?
C19C C20C Fe3 68.8(2) . . ?
C16C C20C H20C 127.2 . . ?
C19C C20C H20C 127.2 . . ?
Fe3 C20C H20C 125.8 . . ?
C17D Fe4 C16D 40.36(19) . . ?
C17D Fe4 C20D 67.10(19) . . ?
C16D Fe4 C20D 39.92(18) . . ?
C17D Fe4 C18D 39.83(19) . . ?
C16D Fe4 C18D 66.77(18) . . ?
C20D Fe4 C18D 65.97(19) . . ?
C17D Fe4 C19D 65.82(18) . . ?
C16D Fe4 C19D 66.06(17) . . ?
C20D Fe4 C19D 39.23(18) . . ?
C18D Fe4 C19D 38.33(19) . . ?
C17D Fe4 C13D 125.3(2) . . ?
C16D Fe4 C13D 162.1(2) . . ?
C20D Fe4 C13D 156.3(2) . . ?
C18D Fe4 C13D 109.25(17) . . ?
C19D Fe4 C13D 122.51(18) . . ?
C17D Fe4 C12D 108.75(16) . . ?
C16D Fe4 C12D 125.37(18) . . ?
C20D Fe4 C12D 161.7(2) . . ?
C18D Fe4 C12D 123.2(2) . . ?
C19D Fe4 C12D 157.2(2) . . ?
C13D Fe4 C12D 40.79(12) . . ?
C17D Fe4 C14D 161.1(2) . . ?
C16D Fe4 C14D 156.5(2) . . ?
C20D Fe4 C14D 121.51(19) . . ?
C18D Fe4 C14D 124.83(19) . . ?
C19D Fe4 C14D 109.08(15) . . ?
C13D Fe4 C14D 40.33(13) . . ?
C12D Fe4 C14D 68.39(13) . . ?
C17D Fe4 C15D 157.4(2) . . ?
C16D Fe4 C15D 121.68(19) . . ?
C20D Fe4 C15D 108.08(15) . . ?
C18D Fe4 C15D 160.4(2) . . ?
C19D Fe4 C15D 125.36(19) . . ?
C13D Fe4 C15D 68.16(13) . . ?
C12D Fe4 C15D 68.49(12) . . ?
C14D Fe4 C15D 40.62(12) . . ?
C17D Fe4 C11D 122.29(18) . . ?
C16D Fe4 C11D 108.08(13) . . ?
C20D Fe4 C11D 124.81(18) . . ?
C18D Fe4 C11D 158.0(2) . . ?
C19D Fe4 C11D 161.2(2) . . ?
C13D Fe4 C11D 68.68(11) . . ?
C12D Fe4 C11D 40.91(10) . . ?
C14D Fe4 C11D 68.68(11) . . ?
C15D Fe4 C11D 40.85(10) . . ?
C11D C10 P6 112.91(17) . . ?
C11D C10 H10A 109.0 . . ?
P6 C10 H10A 109.0 . . ?
C11D C10 H10B 109.0 . . ?
P6 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C15D C11D C12D 107.1(2) . . ?
C15D C11D C10 126.9(2) . . ?
C12D C11D C10 125.9(2) . . ?
C15D C11D Fe4 69.47(14) . . ?
C12D C11D Fe4 69.25(14) . . ?
C10 C11D Fe4 127.04(17) . . ?
C13D C12D C11D 108.0(3) . . ?
C13D C12D Fe4 69.60(17) . . ?
C11D C12D Fe4 69.84(15) . . ?
C13D C12D H12D 126.0 . . ?
C11D C12D H12D 126.0 . . ?
Fe4 C12D H12D 126.1 . . ?
C14D C13D C12D 108.4(3) . . ?
C14D C13D Fe4 69.96(18) . . ?
C12D C13D Fe4 69.61(17) . . ?
C14D C13D H13D 125.8 . . ?
C12D C13D H13D 125.8 . . ?
Fe4 C13D H13D 126.2 . . ?
C13D C14D C15D 108.2(3) . . ?
C13D C14D Fe4 69.71(18) . . ?
C15D C14D Fe4 69.76(16) . . ?
C13D C14D H14D 125.9 . . ?
C15D C14D H14D 125.9 . . ?
Fe4 C14D H14D 126.2 . . ?
C14D C15D C11D 108.3(3) . . ?
C14D C15D Fe4 69.62(16) . . ?
C11D C15D Fe4 69.68(14) . . ?
C14D C15D H15D 125.9 . . ?
C11D C15D H15D 125.9 . . ?
Fe4 C15D H15D 126.4 . . ?
C20D C16D C17D 107.4(4) . . ?
C20D C16D Fe4 70.5(2) . . ?
C17D C16D Fe4 69.7(2) . . ?
C20D C16D H16D 126.3 . . ?
C17D C16D H16D 126.3 . . ?
Fe4 C16D H16D 125.1 . . ?
C18D C17D C16D 107.1(4) . . ?
C18D C17D Fe4 70.7(2) . . ?
C16D C17D Fe4 69.9(2) . . ?
C18D C17D H17D 126.4 . . ?
C16D C17D H17D 126.4 . . ?
Fe4 C17D H17D 124.5 . . ?
C19D C18D C17D 108.3(5) . . ?
C19D C18D Fe4 70.8(2) . . ?
C17D C18D Fe4 69.5(2) . . ?
C19D C18D H18D 125.9 . . ?
C17D C18D H18D 125.9 . . ?
Fe4 C18D H18D 125.4 . . ?
C18D C19D C20D 110.1(4) . . ?
C18D C19D Fe4 70.8(2) . . ?
C20D C19D Fe4 70.4(2) . . ?
C18D C19D H19D 124.9 . . ?
C20D C19D H19D 124.9 . . ?
Fe4 C19D H19D 125.5 . . ?
C19D C20D C16D 107.0(4) . . ?
C19D C20D Fe4 70.4(2) . . ?
C16D C20D Fe4 69.5(2) . . ?
C19D C20D H20D 126.5 . . ?
C16D C20D H20D 126.5 . . ?
Fe4 C20D H20D 126.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3A Fe1 C1A O1A -29(12) . . . . ?
C2A Fe1 C1A O1A -129(12) . . . . ?
P6 Fe1 C1A O1A 128(12) . . . . ?
P5 Fe1 C1A O1A 62(12) . . . . ?
Fe2 Fe1 C1A O1A 75(12) . . . . ?
C3A Fe1 C2A O2A -26(10) . . . . ?
C1A Fe1 C2A O2A 67(10) . . . . ?
P6 Fe1 C2A O2A 160(10) . . . . ?
P5 Fe1 C2A O2A -118(10) . . . . ?
Fe2 Fe1 C2A O2A -159(10) . . . . ?
C1A Fe1 C3A O3A -47(9) . . . . ?
C2A Fe1 C3A O3A 56(9) . . . . ?
P6 Fe1 C3A O3A -141(9) . . . . ?
P5 Fe1 C3A O3A 159(9) . . . . ?
Fe2 Fe1 C3A O3A -149(9) . . . . ?
C3A Fe1 Fe2 C2B -134.21(15) . . . . ?
C1A Fe1 Fe2 C2B 131.86(16) . . . . ?
C2A Fe1 Fe2 C2B -2.7(2) . . . . ?
P6 Fe1 Fe2 C2B 49.96(14) . . . . ?
P5 Fe1 Fe2 C2B -54.69(14) . . . . ?
C3A Fe1 Fe2 C1B 94.23(12) . . . . ?
C1A Fe1 Fe2 C1B 0.30(12) . . . . ?
C2A Fe1 Fe2 C1B -134.28(17) . . . . ?
P6 Fe1 Fe2 C1B -81.60(9) . . . . ?
P5 Fe1 Fe2 C1B 173.75(9) . . . . ?
C3A Fe1 Fe2 C3B -1.65(12) . . . . ?
C1A Fe1 Fe2 C3B -95.58(12) . . . . ?
C2A Fe1 Fe2 C3B 129.83(17) . . . . ?
P6 Fe1 Fe2 C3B -177.48(9) . . . . ?
P5 Fe1 Fe2 C3B 77.87(9) . . . . ?
C3A Fe1 Fe2 P5 -79.52(8) . . . . ?
C1A Fe1 Fe2 P5 -173.45(9) . . . . ?
C2A Fe1 Fe2 P5 51.97(15) . . . . ?
P6 Fe1 Fe2 P5 104.66(3) . . . . ?
C3A Fe1 Fe2 P6 175.82(8) . . . . ?
C1A Fe1 Fe2 P6 81.90(9) . . . . ?
C2A Fe1 Fe2 P6 -52.69(15) . . . . ?
P5 Fe1 Fe2 P6 -104.66(3) . . . . ?
C2B Fe2 C1B O1B 111(16) . . . . ?
C3B Fe2 C1B O1B 7(16) . . . . ?
P5 Fe2 C1B O1B -87(16) . . . . ?
P6 Fe2 C1B O1B -151(16) . . . . ?
Fe1 Fe2 C1B O1B -99(16) . . . . ?
C1B Fe2 C2B O2B 150(4) . . . . ?
C3B Fe2 C2B O2B -114(4) . . . . ?
P5 Fe2 C2B O2B -22(4) . . . . ?
P6 Fe2 C2B O2B 57(4) . . . . ?
Fe1 Fe2 C2B O2B 19(4) . . . . ?
C2B Fe2 C3B O3B -39(14) . . . . ?
C1B Fe2 C3B O3B 66(14) . . . . ?
P5 Fe2 C3B O3B -139(14) . . . . ?
P6 Fe2 C3B O3B 164(100) . . . . ?
Fe1 Fe2 C3B O3B 170(100) . . . . ?
C6 C1 C2 C3 -1.2(3) . . . . ?
C8 C1 C2 C3 178.7(2) . . . . ?
C6 C1 C2 C7 179.2(2) . . . . ?
C8 C1 C2 C7 -0.8(3) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C7 C2 C3 C4 179.4(2) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C4 C5 C6 C1 -1.7(4) . . . . ?
C2 C1 C6 C5 2.1(4) . . . . ?
C8 C1 C6 C5 -177.8(2) . . . . ?
C3 C2 C7 P5 109.5(2) . . . . ?
C1 C2 C7 P5 -70.9(3) . . . . ?
C6 C1 C8 P6 -107.6(2) . . . . ?
C2 C1 C8 P6 72.5(3) . . . . ?
C2 C7 P5 C9 -125.66(18) . . . . ?
C2 C7 P5 Fe1 12.9(2) . . . . ?
C2 C7 P5 Fe2 100.91(18) . . . . ?
C3A Fe1 P5 C9 -8.08(12) . . . . ?
C1A Fe1 P5 C9 -99.8(2) . . . . ?
C2A Fe1 P5 C9 91.53(12) . . . . ?
P6 Fe1 P5 C9 -167.34(9) . . . . ?
Fe2 Fe1 P5 C9 -114.88(9) . . . . ?
C3A Fe1 P5 C7 -139.29(12) . . . . ?
C1A Fe1 P5 C7 129.0(2) . . . . ?
C2A Fe1 P5 C7 -39.68(13) . . . . ?
P6 Fe1 P5 C7 61.45(10) . . . . ?
Fe2 Fe1 P5 C7 113.91(10) . . . . ?
C3A Fe1 P5 Fe2 106.79(8) . . . . ?
C1A Fe1 P5 Fe2 15.08(19) . . . . ?
C2A Fe1 P5 Fe2 -153.59(8) . . . . ?
P6 Fe1 P5 Fe2 -52.47(2) . . . . ?
C2B Fe2 P5 C9 -95.90(13) . . . . ?
C1B Fe2 P5 C9 101.8(2) . . . . ?
C3B Fe2 P5 C9 6.40(13) . . . . ?
P6 Fe2 P5 C9 168.06(9) . . . . ?
Fe1 Fe2 P5 C9 116.08(9) . . . . ?
C2B Fe2 P5 C7 29.33(12) . . . . ?
C1B Fe2 P5 C7 -133.0(2) . . . . ?
C3B Fe2 P5 C7 131.63(13) . . . . ?
P6 Fe2 P5 C7 -66.72(9) . . . . ?
Fe1 Fe2 P5 C7 -118.69(9) . . . . ?
C2B Fe2 P5 Fe1 148.02(9) . . . . ?
C1B Fe2 P5 Fe1 -14.3(2) . . . . ?
C3B Fe2 P5 Fe1 -109.68(9) . . . . ?
P6 Fe2 P5 Fe1 51.97(2) . . . . ?
C1 C8 P6 C10 126.41(18) . . . . ?
C1 C8 P6 Fe1 -12.0(2) . . . . ?
C1 C8 P6 Fe2 -99.57(18) . . . . ?
C3A Fe1 P6 C8 -123.9(2) . . . . ?
C1A Fe1 P6 C8 142.00(13) . . . . ?
C2A Fe1 P6 C8 39.61(13) . . . . ?
P5 Fe1 P6 C8 -61.37(10) . . . . ?
Fe2 Fe1 P6 C8 -113.69(10) . . . . ?
C3A Fe1 P6 C10 105.7(2) . . . . ?
C1A Fe1 P6 C10 11.67(13) . . . . ?
C2A Fe1 P6 C10 -90.73(13) . . . . ?
P5 Fe1 P6 C10 168.29(10) . . . . ?
Fe2 Fe1 P6 C10 115.97(10) . . . . ?
C3A Fe1 P6 Fe2 -10.23(19) . . . . ?
C1A Fe1 P6 Fe2 -104.31(9) . . . . ?
C2A Fe1 P6 Fe2 153.30(8) . . . . ?
P5 Fe1 P6 Fe2 52.32(2) . . . . ?
C2B Fe2 P6 C8 -32.48(13) . . . . ?
C1B Fe2 P6 C8 -137.57(13) . . . . ?
C3B Fe2 P6 C8 124.5(3) . . . . ?
P5 Fe2 P6 C8 65.67(10) . . . . ?
Fe1 Fe2 P6 C8 117.88(10) . . . . ?
C2B Fe2 P6 C10 92.63(13) . . . . ?
C1B Fe2 P6 C10 -12.46(14) . . . . ?
C3B Fe2 P6 C10 -110.4(3) . . . . ?
P5 Fe2 P6 C10 -169.21(10) . . . . ?
Fe1 Fe2 P6 C10 -117.01(10) . . . . ?
C2B Fe2 P6 Fe1 -150.36(9) . . . . ?
C1B Fe2 P6 Fe1 104.55(10) . . . . ?
C3B Fe2 P6 Fe1 6.6(2) . . . . ?
P5 Fe2 P6 Fe1 -52.20(2) . . . . ?
C7 P5 C9 C11C 59.34(19) . . . . ?
Fe1 P5 C9 C11C -80.39(18) . . . . ?
Fe2 P5 C9 C11C -167.66(13) . . . . ?
P5 C9 C11C C15C 85.4(3) . . . . ?
P5 C9 C11C C12C -93.4(3) . . . . ?
P5 C9 C11C Fe3 176.12(12) . . . . ?
C19C Fe3 C11C C15C 46.6(6) . . . . ?
C18C Fe3 C11C C15C -165.8(3) . . . . ?
C12C Fe3 C11C C15C -117.9(2) . . . . ?
C16C Fe3 C11C C15C 118.9(2) . . . . ?
C13C Fe3 C11C C15C -80.69(17) . . . . ?
C17C Fe3 C11C C15C 161.8(2) . . . . ?
C20C Fe3 C11C C15C 77.8(3) . . . . ?
C14C Fe3 C11C C15C -37.52(16) . . . . ?
C19C Fe3 C11C C12C 164.5(5) . . . . ?
C18C Fe3 C11C C12C -47.9(4) . . . . ?
C16C Fe3 C11C C12C -123.2(2) . . . . ?
C13C Fe3 C11C C12C 37.20(16) . . . . ?
C17C Fe3 C11C C12C -80.3(3) . . . . ?
C20C Fe3 C11C C12C -164.3(2) . . . . ?
C15C Fe3 C11C C12C 117.9(2) . . . . ?
C14C Fe3 C11C C12C 80.38(17) . . . . ?
C19C Fe3 C11C C9 -74.3(6) . . . . ?
C18C Fe3 C11C C9 73.4(4) . . . . ?
C12C Fe3 C11C C9 121.3(3) . . . . ?
C16C Fe3 C11C C9 -1.9(3) . . . . ?
C13C Fe3 C11C C9 158.5(2) . . . . ?
C17C Fe3 C11C C9 41.0(3) . . . . ?
C20C Fe3 C11C C9 -43.0(3) . . . . ?
C15C Fe3 C11C C9 -120.8(3) . . . . ?
C14C Fe3 C11C C9 -158.3(2) . . . . ?
C15C C11C C12C C13C 0.7(3) . . . . ?
C9 C11C C12C C13C 179.7(2) . . . . ?
Fe3 C11C C12C C13C -59.14(18) . . . . ?
C15C C11C C12C Fe3 59.86(17) . . . . ?
C9 C11C C12C Fe3 -121.1(2) . . . . ?
C19C Fe3 C12C C13C -51.3(4) . . . . ?
C18C Fe3 C12C C13C -82.4(2) . . . . ?
C16C Fe3 C12C C13C -163.1(2) . . . . ?
C17C Fe3 C12C C13C -123.0(2) . . . . ?
C20C Fe3 C12C C13C 168.1(6) . . . . ?
C11C Fe3 C12C C13C 120.0(2) . . . . ?
C15C Fe3 C12C C13C 81.68(17) . . . . ?
C14C Fe3 C12C C13C 37.60(15) . . . . ?
C19C Fe3 C12C C11C -171.3(3) . . . . ?
C18C Fe3 C12C C11C 157.5(2) . . . . ?
C16C Fe3 C12C C11C 76.9(2) . . . . ?
C13C Fe3 C12C C11C -120.0(2) . . . . ?
C17C Fe3 C12C C11C 116.9(2) . . . . ?
C20C Fe3 C12C C11C 48.0(6) . . . . ?
C15C Fe3 C12C C11C -38.36(14) . . . . ?
C14C Fe3 C12C C11C -82.44(16) . . . . ?
C11C C12C C13C C14C -0.8(3) . . . . ?
Fe3 C12C C13C C14C -59.9(2) . . . . ?
C11C C12C C13C Fe3 59.08(18) . . . . ?
C19C Fe3 C13C C14C -85.2(2) . . . . ?
C18C Fe3 C13C C14C -126.9(2) . . . . ?
C12C Fe3 C13C C14C 118.8(2) . . . . ?
C16C Fe3 C13C C14C 166.8(4) . . . . ?
C17C Fe3 C13C C14C -166.3(2) . . . . ?
C20C Fe3 C13C C14C -52.7(4) . . . . ?
C11C Fe3 C13C C14C 81.24(16) . . . . ?
C15C Fe3 C13C C14C 37.42(15) . . . . ?
C19C Fe3 C13C C12C 156.0(2) . . . . ?
C18C Fe3 C13C C12C 114.3(2) . . . . ?
C16C Fe3 C13C C12C 48.0(5) . . . . ?
C17C Fe3 C13C C12C 74.9(2) . . . . ?
C20C Fe3 C13C C12C -171.5(4) . . . . ?
C11C Fe3 C13C C12C -37.54(15) . . . . ?
C15C Fe3 C13C C12C -81.36(16) . . . . ?
C14C Fe3 C13C C12C -118.8(2) . . . . ?
C12C C13C C14C C15C 0.6(3) . . . . ?
Fe3 C13C C14C C15C -58.8(2) . . . . ?
C12C C13C C14C Fe3 59.44(19) . . . . ?
C19C Fe3 C14C C13C 113.1(2) . . . . ?
C18C Fe3 C14C C13C 71.3(2) . . . . ?
C12C Fe3 C14C C13C -38.13(15) . . . . ?
C16C Fe3 C14C C13C -168.9(4) . . . . ?
C17C Fe3 C14C C13C 36.8(5) . . . . ?
C20C Fe3 C14C C13C 157.3(2) . . . . ?
C11C Fe3 C14C C13C -82.57(16) . . . . ?
C15C Fe3 C14C C13C -120.1(2) . . . . ?
C19C Fe3 C14C C15C -126.9(2) . . . . ?
C18C Fe3 C14C C15C -168.7(2) . . . . ?
C12C Fe3 C14C C15C 81.92(17) . . . . ?
C16C Fe3 C14C C15C -48.9(5) . . . . ?
C13C Fe3 C14C C15C 120.1(2) . . . . ?
C17C Fe3 C14C C15C 156.8(5) . . . . ?
C20C Fe3 C14C C15C -82.7(2) . . . . ?
C11C Fe3 C14C C15C 37.48(16) . . . . ?
C12C C11C C15C C14C -0.3(3) . . . . ?
C9 C11C C15C C14C -179.3(2) . . . . ?
Fe3 C11C C15C C14C 59.16(19) . . . . ?
C12C C11C C15C Fe3 -59.49(17) . . . . ?
C9 C11C C15C Fe3 121.5(2) . . . . ?
C13C C14C C15C C11C -0.2(3) . . . . ?
Fe3 C14C C15C C11C -59.09(18) . . . . ?
C13C C14C C15C Fe3 58.9(2) . . . . ?
C19C Fe3 C15C C11C -166.3(2) . . . . ?
C18C Fe3 C15C C11C 155.6(6) . . . . ?
C12C Fe3 C15C C11C 38.75(15) . . . . ?
C16C Fe3 C15C C11C -80.2(3) . . . . ?
C13C Fe3 C15C C11C 82.75(16) . . . . ?
C17C Fe3 C15C C11C -41.7(5) . . . . ?
C20C Fe3 C15C C11C -123.1(2) . . . . ?
C14C Fe3 C15C C11C 119.7(2) . . . . ?
C19C Fe3 C15C C14C 74.0(2) . . . . ?
C18C Fe3 C15C C14C 36.0(6) . . . . ?
C12C Fe3 C15C C14C -80.90(18) . . . . ?
C16C Fe3 C15C C14C 160.1(2) . . . . ?
C13C Fe3 C15C C14C -36.90(17) . . . . ?
C17C Fe3 C15C C14C -161.4(4) . . . . ?
C20C Fe3 C15C C14C 117.3(2) . . . . ?
C11C Fe3 C15C C14C -119.7(2) . . . . ?
C19C Fe3 C16C C20C 39.9(3) . . . . ?
C18C Fe3 C16C C20C 83.7(3) . . . . ?
C12C Fe3 C16C C20C -167.3(3) . . . . ?
C13C Fe3 C16C C20C 156.2(4) . . . . ?
C17C Fe3 C16C C20C 120.7(4) . . . . ?
C11C Fe3 C16C C20C -124.8(3) . . . . ?
C15C Fe3 C16C C20C -82.2(3) . . . . ?
C14C Fe3 C16C C20C -46.6(5) . . . . ?
C19C Fe3 C16C C17C -80.8(3) . . . . ?
C18C Fe3 C16C C17C -37.0(3) . . . . ?
C12C Fe3 C16C C17C 72.0(3) . . . . ?
C13C Fe3 C16C C17C 35.5(6) . . . . ?
C20C Fe3 C16C C17C -120.7(4) . . . . ?
C11C Fe3 C16C C17C 114.5(3) . . . . ?
C15C Fe3 C16C C17C 157.1(2) . . . . ?
C14C Fe3 C16C C17C -167.3(3) . . . . ?
C20C C16C C17C C18C 0.8(4) . . . . ?
Fe3 C16C C17C C18C 59.8(3) . . . . ?
C20C C16C C17C Fe3 -59.0(3) . . . . ?
C19C Fe3 C17C C18C -37.2(3) . . . . ?
C12C Fe3 C17C C18C 114.9(3) . . . . ?
C16C Fe3 C17C C18C -118.9(4) . . . . ?
C13C Fe3 C17C C18C 74.0(3) . . . . ?
C20C Fe3 C17C C18C -82.2(3) . . . . ?
C11C Fe3 C17C C18C 157.4(3) . . . . ?
C15C Fe3 C17C C18C -172.7(3) . . . . ?
C14C Fe3 C17C C18C 46.4(6) . . . . ?
C19C Fe3 C17C C16C 81.7(3) . . . . ?
C18C Fe3 C17C C16C 118.9(4) . . . . ?
C12C Fe3 C17C C16C -126.2(3) . . . . ?
C13C Fe3 C17C C16C -167.1(3) . . . . ?
C20C Fe3 C17C C16C 36.7(3) . . . . ?
C11C Fe3 C17C C16C -83.7(3) . . . . ?
C15C Fe3 C17C C16C -53.8(6) . . . . ?
C14C Fe3 C17C C16C 165.3(4) . . . . ?
C16C C17C C18C C19C -0.3(4) . . . . ?
Fe3 C17C C18C C19C 59.2(3) . . . . ?
C16C C17C C18C Fe3 -59.5(3) . . . . ?
C19C Fe3 C18C C17C 120.4(4) . . . . ?
C12C Fe3 C18C C17C -80.9(3) . . . . ?
C16C Fe3 C18C C17C 38.2(3) . . . . ?
C13C Fe3 C18C C17C -123.3(3) . . . . ?
C20C Fe3 C18C C17C 81.7(3) . . . . ?
C11C Fe3 C18C C17C -47.3(5) . . . . ?
C15C Fe3 C18C C17C 168.9(5) . . . . ?
C14C Fe3 C18C C17C -162.8(3) . . . . ?
C12C Fe3 C18C C19C 158.7(2) . . . . ?
C16C Fe3 C18C C19C -82.2(3) . . . . ?
C13C Fe3 C18C C19C 116.3(3) . . . . ?
C17C Fe3 C18C C19C -120.4(4) . . . . ?
C20C Fe3 C18C C19C -38.7(3) . . . . ?
C11C Fe3 C18C C19C -167.8(3) . . . . ?
C15C Fe3 C18C C19C 48.5(7) . . . . ?
C14C Fe3 C18C C19C 76.8(3) . . . . ?
C17C C18C C19C C20C -0.3(4) . . . . ?
Fe3 C18C C19C C20C 59.5(3) . . . . ?
C17C C18C C19C Fe3 -59.7(3) . . . . ?
C12C Fe3 C19C C18C -44.9(5) . . . . ?
C16C Fe3 C19C C18C 80.2(3) . . . . ?
C13C Fe3 C19C C18C -80.6(3) . . . . ?
C17C Fe3 C19C C18C 36.2(3) . . . . ?
C20C Fe3 C19C C18C 118.8(4) . . . . ?
C11C Fe3 C19C C18C 157.9(5) . . . . ?
C15C Fe3 C19C C18C -165.1(3) . . . . ?
C14C Fe3 C19C C18C -123.5(3) . . . . ?
C18C Fe3 C19C C20C -118.8(4) . . . . ?
C12C Fe3 C19C C20C -163.7(3) . . . . ?
C16C Fe3 C19C C20C -38.6(3) . . . . ?
C13C Fe3 C19C C20C 160.6(3) . . . . ?
C17C Fe3 C19C C20C -82.6(3) . . . . ?
C11C Fe3 C19C C20C 39.1(7) . . . . ?
C15C Fe3 C19C C20C 76.1(3) . . . . ?
C14C Fe3 C19C C20C 117.8(3) . . . . ?
C17C C16C C20C C19C -1.0(4) . . . . ?
Fe3 C16C C20C C19C -59.8(2) . . . . ?
C17C C16C C20C Fe3 58.9(3) . . . . ?
C18C C19C C20C C16C 0.8(4) . . . . ?
Fe3 C19C C20C C16C 60.4(3) . . . . ?
C18C C19C C20C Fe3 -59.7(3) . . . . ?
C19C Fe3 C20C C16C -116.7(4) . . . . ?
C18C Fe3 C20C C16C -79.2(3) . . . . ?
C12C Fe3 C20C C16C 37.5(7) . . . . ?
C13C Fe3 C20C C16C -161.7(3) . . . . ?
C17C Fe3 C20C C16C -36.9(3) . . . . ?
C11C Fe3 C20C C16C 74.8(3) . . . . ?
C15C Fe3 C20C C16C 117.4(3) . . . . ?
C14C Fe3 C20C C16C 160.9(3) . . . . ?
C18C Fe3 C20C C19C 37.5(3) . . . . ?
C12C Fe3 C20C C19C 154.3(5) . . . . ?
C16C Fe3 C20C C19C 116.7(4) . . . . ?
C13C Fe3 C20C C19C -45.0(6) . . . . ?
C17C Fe3 C20C C19C 79.8(3) . . . . ?
C11C Fe3 C20C C19C -168.4(2) . . . . ?
C15C Fe3 C20C C19C -125.8(3) . . . . ?
C14C Fe3 C20C C19C -82.4(3) . . . . ?
C8 P6 C10 C11D -55.5(2) . . . . ?
Fe1 P6 C10 C11D 83.24(19) . . . . ?
Fe2 P6 C10 C11D 171.60(14) . . . . ?
P6 C10 C11D C15D -77.5(3) . . . . ?
P6 C10 C11D C12D 101.6(3) . . . . ?
P6 C10 C11D Fe4 -168.49(14) . . . . ?
C17D Fe4 C11D C15D -160.0(3) . . . . ?
C16D Fe4 C11D C15D -117.8(3) . . . . ?
C20D Fe4 C11D C15D -76.9(3) . . . . ?
C18D Fe4 C11D C15D 169.6(4) . . . . ?
C19D Fe4 C11D C15D -49.3(5) . . . . ?
C13D Fe4 C11D C15D 80.84(19) . . . . ?
C12D Fe4 C11D C15D 118.6(2) . . . . ?
C14D Fe4 C11D C15D 37.40(18) . . . . ?
C17D Fe4 C11D C12D 81.5(3) . . . . ?
C16D Fe4 C11D C12D 123.6(3) . . . . ?
C20D Fe4 C11D C12D 164.5(2) . . . . ?
C18D Fe4 C11D C12D 51.0(5) . . . . ?
C19D Fe4 C11D C12D -167.9(4) . . . . ?
C13D Fe4 C11D C12D -37.75(19) . . . . ?
C14D Fe4 C11D C12D -81.18(19) . . . . ?
C15D Fe4 C11D C12D -118.6(2) . . . . ?
C17D Fe4 C11D C10 -38.5(3) . . . . ?
C16D Fe4 C11D C10 3.6(3) . . . . ?
C20D Fe4 C11D C10 44.5(3) . . . . ?
C18D Fe4 C11D C10 -69.0(5) . . . . ?
C19D Fe4 C11D C10 72.1(5) . . . . ?
C13D Fe4 C11D C10 -157.7(3) . . . . ?
C12D Fe4 C11D C10 -120.0(3) . . . . ?
C14D Fe4 C11D C10 158.8(3) . . . . ?
C15D Fe4 C11D C10 121.4(3) . . . . ?
C15D C11D C12D C13D 0.0(3) . . . . ?
C10 C11D C12D C13D -179.3(2) . . . . ?
Fe4 C11D C12D C13D 59.4(2) . . . . ?
C15D C11D C12D Fe4 -59.38(17) . . . . ?
C10 C11D C12D Fe4 121.4(2) . . . . ?
C17D Fe4 C12D C13D 122.8(3) . . . . ?
C16D Fe4 C12D C13D 164.6(3) . . . . ?
C20D Fe4 C12D C13D -163.6(5) . . . . ?
C18D Fe4 C12D C13D 81.1(3) . . . . ?
C19D Fe4 C12D C13D 50.8(5) . . . . ?
C14D Fe4 C12D C13D -37.24(18) . . . . ?
C15D Fe4 C12D C13D -81.1(2) . . . . ?
C11D Fe4 C12D C13D -119.2(3) . . . . ?
C17D Fe4 C12D C11D -118.0(3) . . . . ?
C16D Fe4 C12D C11D -76.2(3) . . . . ?
C20D Fe4 C12D C11D -44.4(6) . . . . ?
C18D Fe4 C12D C11D -159.7(2) . . . . ?
C19D Fe4 C12D C11D 170.0(4) . . . . ?
C13D Fe4 C12D C11D 119.2(3) . . . . ?
C14D Fe4 C12D C11D 81.95(18) . . . . ?
C15D Fe4 C12D C11D 38.13(16) . . . . ?
C11D C12D C13D C14D -0.1(3) . . . . ?
Fe4 C12D C13D C14D 59.4(2) . . . . ?
C11D C12D C13D Fe4 -59.51(19) . . . . ?
C17D Fe4 C13D C14D 163.0(3) . . . . ?
C16D Fe4 C13D C14D -164.6(4) . . . . ?
C20D Fe4 C13D C14D 47.7(4) . . . . ?
C18D Fe4 C13D C14D 121.6(3) . . . . ?
C19D Fe4 C13D C14D 81.3(3) . . . . ?
C12D Fe4 C13D C14D -119.6(3) . . . . ?
C15D Fe4 C13D C14D -37.67(17) . . . . ?
C11D Fe4 C13D C14D -81.76(18) . . . . ?
C17D Fe4 C13D C12D -77.4(3) . . . . ?
C16D Fe4 C13D C12D -45.0(5) . . . . ?
C20D Fe4 C13D C12D 167.3(4) . . . . ?
C18D Fe4 C13D C12D -118.8(3) . . . . ?
C19D Fe4 C13D C12D -159.1(3) . . . . ?
C14D Fe4 C13D C12D 119.6(3) . . . . ?
C15D Fe4 C13D C12D 81.94(18) . . . . ?
C11D Fe4 C13D C12D 37.86(17) . . . . ?
C12D C13D C14D C15D 0.2(3) . . . . ?
Fe4 C13D C14D C15D 59.4(2) . . . . ?
C12D C13D C14D Fe4 -59.2(2) . . . . ?
C17D Fe4 C14D C13D -47.2(5) . . . . ?
C16D Fe4 C14D C13D 168.2(3) . . . . ?
C20D Fe4 C14D C13D -159.6(2) . . . . ?
C18D Fe4 C14D C13D -78.5(3) . . . . ?
C19D Fe4 C14D C13D -118.1(3) . . . . ?
C12D Fe4 C14D C13D 37.65(17) . . . . ?
C15D Fe4 C14D C13D 119.4(3) . . . . ?
C11D Fe4 C14D C13D 81.77(18) . . . . ?
C17D Fe4 C14D C15D -166.6(5) . . . . ?
C16D Fe4 C14D C15D 48.8(4) . . . . ?
C20D Fe4 C14D C15D 81.0(3) . . . . ?
C18D Fe4 C14D C15D 162.1(3) . . . . ?
C19D Fe4 C14D C15D 122.5(3) . . . . ?
C13D Fe4 C14D C15D -119.4(3) . . . . ?
C12D Fe4 C14D C15D -81.72(19) . . . . ?
C11D Fe4 C14D C15D -37.61(17) . . . . ?
C13D C14D C15D C11D -0.2(3) . . . . ?
Fe4 C14D C15D C11D 59.14(18) . . . . ?
C13D C14D C15D Fe4 -59.3(2) . . . . ?
C12D C11D C15D C14D 0.1(3) . . . . ?
C10 C11D C15D C14D 179.4(2) . . . . ?
Fe4 C11D C15D C14D -59.10(19) . . . . ?
C12D C11D C15D Fe4 59.24(17) . . . . ?
C10 C11D C15D Fe4 -121.5(2) . . . . ?
C17D Fe4 C15D C14D 168.7(4) . . . . ?
C16D Fe4 C15D C14D -159.3(3) . . . . ?
C20D Fe4 C15D C14D -117.6(3) . . . . ?
C18D Fe4 C15D C14D -48.8(6) . . . . ?
C19D Fe4 C15D C14D -77.8(3) . . . . ?
C13D Fe4 C15D C14D 37.41(19) . . . . ?
C12D Fe4 C15D C14D 81.5(2) . . . . ?
C11D Fe4 C15D C14D 119.6(3) . . . . ?
C17D Fe4 C15D C11D 49.1(5) . . . . ?
C16D Fe4 C15D C11D 81.0(3) . . . . ?
C20D Fe4 C15D C11D 122.7(2) . . . . ?
C18D Fe4 C15D C11D -168.4(5) . . . . ?
C19D Fe4 C15D C11D 162.6(2) . . . . ?
C13D Fe4 C15D C11D -82.23(18) . . . . ?
C12D Fe4 C15D C11D -38.18(16) . . . . ?
C14D Fe4 C15D C11D -119.6(3) . . . . ?
C17D Fe4 C16D C20D -118.0(4) . . . . ?
C18D Fe4 C16D C20D -79.8(3) . . . . ?
C19D Fe4 C16D C20D -37.8(3) . . . . ?
C13D Fe4 C16D C20D -160.4(4) . . . . ?
C12D Fe4 C16D C20D 165.1(3) . . . . ?
C14D Fe4 C16D C20D 45.1(5) . . . . ?
C15D Fe4 C16D C20D 80.2(3) . . . . ?
C11D Fe4 C16D C20D 123.1(3) . . . . ?
C20D Fe4 C16D C17D 118.0(4) . . . . ?
C18D Fe4 C16D C17D 38.2(3) . . . . ?
C19D Fe4 C16D C17D 80.2(3) . . . . ?
C13D Fe4 C16D C17D -42.4(6) . . . . ?
C12D Fe4 C16D C17D -76.9(3) . . . . ?
C14D Fe4 C16D C17D 163.1(3) . . . . ?
C15D Fe4 C16D C17D -161.7(3) . . . . ?
C11D Fe4 C16D C17D -118.9(3) . . . . ?
C20D C16D C17D C18D -0.5(4) . . . . ?
Fe4 C16D C17D C18D -61.3(3) . . . . ?
C20D C16D C17D Fe4 60.7(3) . . . . ?
C16D Fe4 C17D C18D 117.4(4) . . . . ?
C20D Fe4 C17D C18D 79.4(3) . . . . ?
C19D Fe4 C17D C18D 36.5(3) . . . . ?
C13D Fe4 C17D C18D -77.3(4) . . . . ?
C12D Fe4 C17D C18D -119.6(3) . . . . ?
C14D Fe4 C17D C18D -41.7(6) . . . . ?
C15D Fe4 C17D C18D 161.4(4) . . . . ?
C11D Fe4 C17D C18D -162.8(3) . . . . ?
C20D Fe4 C17D C16D -37.9(3) . . . . ?
C18D Fe4 C17D C16D -117.4(4) . . . . ?
C19D Fe4 C17D C16D -80.9(3) . . . . ?
C13D Fe4 C17D C16D 165.3(2) . . . . ?
C12D Fe4 C17D C16D 123.0(3) . . . . ?
C14D Fe4 C17D C16D -159.1(4) . . . . ?
C15D Fe4 C17D C16D 44.1(5) . . . . ?
C11D Fe4 C17D C16D 79.8(3) . . . . ?
C16D C17D C18D C19D 0.3(5) . . . . ?
Fe4 C17D C18D C19D -60.5(3) . . . . ?
C16D C17D C18D Fe4 60.8(3) . . . . ?
C17D Fe4 C18D C19D 119.0(5) . . . . ?
C16D Fe4 C18D C19D 80.3(3) . . . . ?
C20D Fe4 C18D C19D 36.5(3) . . . . ?
C13D Fe4 C18D C19D -118.4(3) . . . . ?
C12D Fe4 C18D C19D -161.6(3) . . . . ?
C14D Fe4 C18D C19D -76.2(4) . . . . ?
C15D Fe4 C18D C19D -39.6(7) . . . . ?
C11D Fe4 C18D C19D 161.0(4) . . . . ?
C16D Fe4 C18D C17D -38.7(3) . . . . ?
C20D Fe4 C18D C17D -82.5(3) . . . . ?
C19D Fe4 C18D C17D -119.0(5) . . . . ?
C13D Fe4 C18D C17D 122.5(3) . . . . ?
C12D Fe4 C18D C17D 79.4(4) . . . . ?
C14D Fe4 C18D C17D 164.7(3) . . . . ?
C15D Fe4 C18D C17D -158.7(5) . . . . ?
C11D Fe4 C18D C17D 42.0(6) . . . . ?
C17D C18D C19D C20D 0.0(5) . . . . ?
Fe4 C18D C19D C20D -59.6(3) . . . . ?
C17D C18D C19D Fe4 59.6(3) . . . . ?
C17D Fe4 C19D C18D -37.9(3) . . . . ?
C16D Fe4 C19D C18D -82.3(3) . . . . ?
C20D Fe4 C19D C18D -120.7(4) . . . . ?
C13D Fe4 C19D C18D 79.9(3) . . . . ?
C12D Fe4 C19D C18D 43.0(6) . . . . ?
C14D Fe4 C19D C18D 122.5(3) . . . . ?
C15D Fe4 C19D C18D 164.8(3) . . . . ?
C11D Fe4 C19D C18D -157.8(4) . . . . ?
C17D Fe4 C19D C20D 82.8(3) . . . . ?
C16D Fe4 C19D C20D 38.5(3) . . . . ?
C18D Fe4 C19D C20D 120.7(4) . . . . ?
C13D Fe4 C19D C20D -159.4(3) . . . . ?
C12D Fe4 C19D C20D 163.7(4) . . . . ?
C14D Fe4 C19D C20D -116.8(3) . . . . ?
C15D Fe4 C19D C20D -74.5(3) . . . . ?
C11D Fe4 C19D C20D -37.0(6) . . . . ?
C18D C19D C20D C16D -0.4(5) . . . . ?
Fe4 C19D C20D C16D -60.2(3) . . . . ?
C18D C19D C20D Fe4 59.8(3) . . . . ?
C17D C16D C20D C19D 0.6(4) . . . . ?
Fe4 C16D C20D C19D 60.8(3) . . . . ?
C17D C16D C20D Fe4 -60.2(3) . . . . ?
C17D Fe4 C20D C19D -79.3(3) . . . . ?
C16D Fe4 C20D C19D -117.7(4) . . . . ?
C18D Fe4 C20D C19D -35.7(3) . . . . ?
C13D Fe4 C20D C19D 47.5(5) . . . . ?
C12D Fe4 C20D C19D -159.7(4) . . . . ?
C14D Fe4 C20D C19D 81.7(3) . . . . ?
C15D Fe4 C20D C19D 124.3(3) . . . . ?
C11D Fe4 C20D C19D 166.3(3) . . . . ?
C17D Fe4 C20D C16D 38.4(3) . . . . ?
C18D Fe4 C20D C16D 81.9(3) . . . . ?
C19D Fe4 C20D C16D 117.7(4) . . . . ?
C13D Fe4 C20D C16D 165.2(4) . . . . ?
C12D Fe4 C20D C16D -42.1(6) . . . . ?
C14D Fe4 C20D C16D -160.7(3) . . . . ?
C15D Fe4 C20D C16D -118.1(3) . . . . ?
C11D Fe4 C20D C16D -76.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.054


####################################################################### 
# 
# 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_twin_p21
_database_code_depnum_ccdc_archive 'CCDC 1473787'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;
_audit_creation_date             2016-02-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H32 Fe2 O8 P2'
_chemical_formula_sum            'C48 H32 Fe2 O8 P2'
_chemical_formula_weight         910.37
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.944(8)
_cell_length_b                   26.47(2)
_cell_length_c                   11.313(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.73(4)
_cell_angle_gamma                90
_cell_volume                     2374(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    408
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      18.684
_cell_measurement_theta_min      3.326
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1052 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.5761.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'yellowish orange'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.1735
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15590
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.371
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4543
_reflns_number_total             7339
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7339
_refine_ls_number_restraints     389
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.1106
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1894P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2733
_refine_ls_wR_factor_ref         0.2961
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.83(6) 0.17(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O3B-C3B \\sim O3A-C3A \\sim O1B-C1B \\sim O1A-C1A \\sim O2B-C2B \\sim O2A-C2A
 with sigma of 0.02
 Fe1B-C1B \\sim Fe1A-C1A \\sim Fe1A-C3A \\sim Fe1B-C2B \\sim Fe1A-C2A \\sim
Fe1B-C3B
 with sigma of 0.02
 C17B-C18B \\sim C16B-C15B
 with sigma of 0.02
 C28A-C27A \\sim C29A-C28A \\sim C30A-C29A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A)
Uanis(Fe1A) = Uanis(C3A) = Uanis(O3A)
5. Rigid body (RIGU) restrains
 C11B, C12B, H12B, C13B, C14B, C15B, C16B, H16B, C17B, H17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11B, C21B, C22B, C23B, H23B, C24B, H24B, C25B, H25B, C26B, H26B, C27B, C28B,
 H28B, C29B, H29B, C30B, C32B, H32A, H32B, H32C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C12A, C13A, H13A, C14A, C15A, H15A, C16A, H16A, C17A, C18A, H18A, C19A,
 C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11A, H18A, C21A, C22A, C23A, H23A, C24A, H24A, C25A, H25A, C26A, H26A, C27A,
 C28A, H28A, C29A, H29A, C30A, C31A, H31A, H31B, H31C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Fe1A, O2A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 P1A(H1A), P1B(H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C12A(H12A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C28A(H28A), C29A(H29A),
 C12B(H12B), C13B(H13B), C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B),
 C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C28B(H28B), C29B(H29B)
6.c Fitted hexagon refined as free rotating group:
 C13A(C12A,C11A,C20A,C19A,C14A), C22A(C23A,C24A,C25A,C26A,C27A)
6.d Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C32B(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.5772(3) 0.97869(9) 0.5285(2) 0.0407(7) Uani 1 1 d D U . . .
P1A P 0.8110(7) 0.94809(18) 0.4655(4) 0.0434(12) Uani 1 1 d . . . . .
H1A H 0.8101 0.9517 0.3775 0.052 Uiso 1 1 calc R . . . .
O1A O 0.372(2) 1.0408(7) 0.6763(12) 0.075(5) Uani 1 1 d D U . . .
O2A O 0.323(2) 0.9380(6) 0.3579(14) 0.081(5) Uani 1 1 d D U . . .
O3A O 0.5790(15) 0.8996(4) 0.7140(9) 0.0407(7) Uani 1 1 d D U . . .
O11A O 0.5446(18) 0.8224(7) 0.4133(12) 0.071(4) Uani 1 1 d . U . . .
C1A C 0.455(3) 1.0184(9) 0.6135(14) 0.065(6) Uani 1 1 d D U . . .
C2A C 0.408(3) 0.9538(10) 0.440(2) 0.077(7) Uani 1 1 d D U . . .
C3A C 0.582(2) 0.9278(6) 0.6314(14) 0.0407(7) Uani 1 1 d D U . . .
C13A C 1.064(2) 0.8345(5) 0.6430(9) 0.066(3) Uani 1 1 d . U . . .
H13A H 1.1284 0.8302 0.7160 0.079 Uiso 1 1 calc R U . . .
C12A C 0.988(2) 0.8808(4) 0.6155(10) 0.066(3) Uani 1 1 d G U . . .
H12A H 1.0018 0.9082 0.6696 0.079 Uiso 1 1 calc R . . . .
C11A C 0.8937(19) 0.8871(4) 0.5089(11) 0.066(3) Uani 1 1 d G U . . .
C20A C 0.8742(15) 0.8470(4) 0.4297(8) 0.029(3) Uani 1 1 d G U . . .
C19A C 0.9494(17) 0.8007(4) 0.4572(9) 0.041(4) Uani 1 1 d G U . . .
C14A C 1.0441(19) 0.7944(4) 0.5639(11) 0.066(3) Uani 1 1 d G U . . .
C15A C 1.098(2) 0.7404(8) 0.5936(17) 0.049(4) Uani 1 1 d . U . . .
H15A H 1.1475 0.7337 0.6706 0.059 Uiso 1 1 calc R U . . .
C16A C 1.080(3) 0.7037(8) 0.5213(15) 0.050(4) Uani 1 1 d . U . . .
H16A H 1.1366 0.6727 0.5383 0.060 Uiso 1 1 calc R U . . .
C17A C 0.978(3) 0.7087(8) 0.4180(17) 0.055(5) Uani 1 1 d . U . . .
H17A H 0.9453 0.6799 0.3719 0.066 Uiso 1 1 calc R . . . .
C18A C 0.922(2) 0.7584(7) 0.3820(16) 0.043(4) Uani 1 1 d . U . . .
H18A H 0.8650 0.7629 0.3061 0.051 Uiso 1 1 calc R U . . .
C21A C 0.770(2) 0.8527(6) 0.3108(14) 0.034(3) Uani 1 1 d . U . . .
C22A C 0.8455(13) 0.8699(4) 0.2078(7) 0.030(3) Uani 1 1 d . U . . .
C23A C 1.0157(12) 0.8819(5) 0.2067(8) 0.040(4) Uani 1 1 d G U . . .
H23A H 1.0855 0.8810 0.2782 0.048 Uiso 1 1 calc R U . . .
C24A C 1.0839(11) 0.8953(5) 0.1011(10) 0.059(5) Uani 1 1 d G U . . .
H24A H 1.2003 0.9036 0.1003 0.070 Uiso 1 1 calc R U . . .
C25A C 0.9819(16) 0.8967(5) -0.0035(8) 0.054(4) Uani 1 1 d G U . . .
H25A H 1.0285 0.9059 -0.0757 0.065 Uiso 1 1 calc R U . . .
C26A C 0.8117(15) 0.8847(5) -0.0024(8) 0.064(5) Uani 1 1 d G U . . .
H26A H 0.7420 0.8856 -0.0738 0.076 Uiso 1 1 calc R U . . .
C27A C 0.7435(11) 0.8713(5) 0.1033(9) 0.043(4) Uani 1 1 d DG U . . .
C28A C 0.571(2) 0.8552(8) 0.0950(17) 0.057(5) Uani 1 1 d D U . . .
H28A H 0.5086 0.8553 0.0204 0.068 Uiso 1 1 calc R U . . .
C29A C 0.491(3) 0.8388(9) 0.2009(14) 0.060(5) Uani 1 1 d D U . . .
H29A H 0.3755 0.8293 0.2006 0.072 Uiso 1 1 calc R U . . .
C30A C 0.602(2) 0.8382(8) 0.3050(15) 0.045(4) Uani 1 1 d D U . . .
C31A C 0.369(4) 0.8079(16) 0.420(3) 0.114(12) Uani 1 1 d . U . . .
H31A H 0.3542 0.7726 0.3947 0.171 Uiso 1 1 calc GR U . . .
H31B H 0.2973 0.8297 0.3677 0.171 Uiso 1 1 calc GR U . . .
H31C H 0.3365 0.8115 0.5016 0.171 Uiso 1 1 calc GR U . . .
Fe1B Fe 0.8744(3) 1.02231(9) 0.55181(18) 0.0361(6) Uani 1 1 d D . . . .
P1B P 0.6687(6) 1.04028(15) 0.4178(3) 0.0321(10) Uani 1 1 d . . . . .
H1B H 0.6979 1.0256 0.3403 0.039 Uiso 1 1 calc R . . . .
O1B O 0.7964(19) 1.1094(6) 0.6959(14) 0.070(4) Uani 1 1 d D U . . .
O2B O 1.1445(17) 1.0570(6) 0.4057(12) 0.066(4) Uani 1 1 d D U . . .
O3B O 1.049(2) 0.9860(6) 0.7669(10) 0.067(4) Uani 1 1 d D U . . .
O11B O 0.9078(17) 1.1434(6) 0.2259(13) 0.062(4) Uani 1 1 d . U . . .
C1B C 0.828(3) 1.0752(7) 0.6368(16) 0.058(5) Uani 1 1 d D U . . .
C2B C 1.038(2) 1.0430(7) 0.4666(15) 0.050(5) Uani 1 1 d D U . . .
C3B C 0.981(3) 0.9955(10) 0.6770(17) 0.080(8) Uani 1 1 d D U . . .
C11B C 0.582(2) 1.1023(6) 0.3912(13) 0.030(3) Uani 1 1 d . U . . .
C12B C 0.516(2) 1.1294(7) 0.4871(15) 0.041(4) Uani 1 1 d . U . . .
H12B H 0.5139 1.1150 0.5639 0.049 Uiso 1 1 calc R U . . .
C13B C 0.455(2) 1.1785(7) 0.4625(15) 0.044(4) Uani 1 1 d . U . . .
H13B H 0.4115 1.1973 0.5251 0.053 Uiso 1 1 calc R . . . .
C14B C 0.456(3) 1.2010(7) 0.3498(15) 0.047(5) Uani 1 1 d . U . . .
C15B C 0.387(2) 1.2514(7) 0.3305(16) 0.042(4) Uani 1 1 d D U . . .
H15B H 0.3459 1.2689 0.3961 0.050 Uiso 1 1 calc R . . . .
C16B C 0.379(3) 1.2736(7) 0.2287(16) 0.052(4) Uani 1 1 d D U . . .
H16B H 0.3256 1.3054 0.2143 0.062 Uiso 1 1 calc R U . . .
C17B C 0.465(2) 1.2434(6) 0.1331(17) 0.045(4) Uani 1 1 d D U . . .
H17B H 0.4753 1.2589 0.0582 0.053 Uiso 1 1 calc R U . . .
C18B C 0.524(2) 1.1975(6) 0.1490(15) 0.045(4) Uani 1 1 d D U . . .
H18B H 0.5681 1.1799 0.0846 0.054 Uiso 1 1 calc R . . . .
C19B C 0.523(3) 1.1754(7) 0.2538(15) 0.047(4) Uani 1 1 d . U . . .
C20B C 0.592(2) 1.1259(6) 0.2686(13) 0.035(4) Uani 1 1 d . U . . .
C21B C 0.666(2) 1.0955(6) 0.1787(11) 0.030(3) Uani 1 1 d . U . . .
C22B C 0.570(3) 1.0609(7) 0.1102(14) 0.042(4) Uani 1 1 d . U . . .
C23B C 0.408(3) 1.0483(8) 0.1264(15) 0.050(4) Uani 1 1 d . U . . .
H23B H 0.3512 1.0654 0.1858 0.060 Uiso 1 1 calc R U . . .
C24B C 0.321(3) 1.0108(9) 0.0585(18) 0.071(6) Uani 1 1 d . U . . .
H24B H 0.2146 0.9977 0.0773 0.085 Uiso 1 1 calc R U . . .
C25B C 0.412(3) 0.9934(8) -0.0465(16) 0.055(5) Uani 1 1 d . U . . .
H25B H 0.3539 0.9743 -0.1071 0.067 Uiso 1 1 calc R U . . .
C26B C 0.557(3) 1.0036(7) -0.0543(16) 0.050(4) Uani 1 1 d . U . . .
H26B H 0.6082 0.9880 -0.1187 0.060 Uiso 1 1 calc R U . . .
C27B C 0.662(3) 1.0338(9) 0.0141(16) 0.063(5) Uani 1 1 d . U . . .
C28B C 0.824(3) 1.0453(9) -0.004(2) 0.074(7) Uani 1 1 d . U . . .
H28B H 0.8762 1.0286 -0.0664 0.088 Uiso 1 1 calc R U . . .
C29B C 0.922(3) 1.0811(8) 0.0658(17) 0.055(5) Uani 1 1 d . U . . .
H29B H 1.0375 1.0874 0.0560 0.066 Uiso 1 1 calc R U . . .
C30B C 0.822(3) 1.1078(6) 0.1565(15) 0.043(4) Uani 1 1 d . U . . .
C32B C 1.085(3) 1.1537(8) 0.207(2) 0.071(7) Uani 1 1 d . U . . .
H32A H 1.1496 1.1222 0.2135 0.107 Uiso 1 1 calc GR U . . .
H32B H 1.1304 1.1779 0.2662 0.107 Uiso 1 1 calc GR U . . .
H32C H 1.0937 1.1680 0.1274 0.107 Uiso 1 1 calc GR U . . .


_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
Fe1A P1A 2.188(6) . ?
Fe1A C1A 1.757(17) . ?
Fe1A C2A 1.752(16) . ?
Fe1A C3A 1.780(13) . ?
Fe1A Fe1B 2.626(4) . ?
Fe1A P1B 2.207(5) . ?
P1A H1A 1.0000 . ?
P1A C11A 1.800(9) . ?
P1A Fe1B 2.236(5) . ?
O1A C1A 1.163(17) . ?
O2A C2A 1.188(17) . ?
O3A C3A 1.197(14) . ?
O11A C30A 1.40(2) . ?
O11A C31A 1.46(3) . ?
C13A H13A 0.9500 . ?
C13A C12A 1.3900 . ?
C13A C14A 1.3900 . ?
C12A H12A 0.9500 . ?
C12A C11A 1.3900 . ?
C11A C20A 1.3900 . ?
C20A C19A 1.3900 . ?
C20A C21A 1.540(19) . ?
C19A C14A 1.3900 . ?
C19A C18A 1.41(2) . ?
C14A C15A 1.52(2) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.27(3) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.39(3) . ?
C17A H17A 0.9500 . ?
C17A C18A 1.44(3) . ?
C18A H18A 0.9500 . ?
C21A C22A 1.420(18) . ?
C21A C30A 1.38(3) . ?
C22A C23A 1.3900 . ?
C22A C27A 1.3900 . ?
C23A H23A 0.9500 . ?
C23A C24A 1.3900 . ?
C24A H24A 0.9500 . ?
C24A C25A 1.3900 . ?
C25A H25A 0.9500 . ?
C25A C26A 1.3900 . ?
C26A H26A 0.9500 . ?
C26A C27A 1.3900 . ?
C27A C28A 1.432(17) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.459(19) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.426(19) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
Fe1B P1B 2.207(5) . ?
Fe1B C1B 1.752(15) . ?
Fe1B C2B 1.754(13) . ?
Fe1B C3B 1.753(15) . ?
P1B H1B 1.0000 . ?
P1B C11B 1.798(17) . ?
O1B C1B 1.161(16) . ?
O2B C2B 1.185(16) . ?
O3B C3B 1.149(16) . ?
O11B C30B 1.38(2) . ?
O11B C32B 1.46(3) . ?
C11B C12B 1.43(2) . ?
C11B C20B 1.53(2) . ?
C12B H12B 0.9500 . ?
C12B C13B 1.41(3) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.41(2) . ?
C14B C15B 1.45(2) . ?
C14B C19B 1.41(2) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.29(2) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.54(3) . ?
C17B H17B 0.9500 . ?
C17B C18B 1.31(2) . ?
C18B H18B 0.9500 . ?
C18B C19B 1.32(2) . ?
C19B C20B 1.43(2) . ?
C20B C21B 1.45(2) . ?
C21B C22B 1.39(2) . ?
C21B C30B 1.32(3) . ?
C22B C23B 1.35(3) . ?
C22B C27B 1.52(3) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.41(3) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.50(3) . ?
C25B H25B 0.9500 . ?
C25B C26B 1.19(3) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.36(3) . ?
C27B C28B 1.35(3) . ?
C28B H28B 0.9500 . ?
C28B C29B 1.43(3) . ?
C29B H29B 0.9500 . ?
C29B C30B 1.51(3) . ?
C32B H32A 0.9800 . ?
C32B H32B 0.9800 . ?
C32B H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1A Fe1A Fe1B 54.44(16) . . ?
P1A Fe1A P1B 76.76(19) . . ?
C1A Fe1A P1A 155.4(7) . . ?
C1A Fe1A C3A 94.9(10) . . ?
C1A Fe1A Fe1B 101.8(8) . . ?
C1A Fe1A P1B 94.7(8) . . ?
C2A Fe1A P1A 108.2(10) . . ?
C2A Fe1A C1A 96.2(12) . . ?
C2A Fe1A C3A 94.2(10) . . ?
C2A Fe1A Fe1B 151.0(9) . . ?
C2A Fe1A P1B 102.9(9) . . ?
C3A Fe1A P1A 87.1(7) . . ?
C3A Fe1A Fe1B 106.5(6) . . ?
C3A Fe1A P1B 159.4(6) . . ?
P1B Fe1A Fe1B 53.50(14) . . ?
Fe1A P1A H1A 109.7 . . ?
Fe1A P1A Fe1B 72.83(17) . . ?
C11A P1A Fe1A 123.1(6) . . ?
C11A P1A H1A 109.7 . . ?
C11A P1A Fe1B 127.0(4) . . ?
Fe1B P1A H1A 109.7 . . ?
C30A O11A C31A 119.6(19) . . ?
O1A C1A Fe1A 174(2) . . ?
O2A C2A Fe1A 163(2) . . ?
O3A C3A Fe1A 169.1(15) . . ?
C12A C13A H13A 120.0 . . ?
C12A C13A C14A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C13A C12A H12A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
C12A C11A P1A 120.7(6) . . ?
C12A C11A C20A 120.0 . . ?
C20A C11A P1A 119.1(6) . . ?
C11A C20A C21A 121.3(9) . . ?
C19A C20A C11A 120.0 . . ?
C19A C20A C21A 118.7(9) . . ?
C20A C19A C18A 121.0(10) . . ?
C14A C19A C20A 120.0 . . ?
C14A C19A C18A 118.8(10) . . ?
C13A C14A C15A 123.8(11) . . ?
C19A C14A C13A 120.0 . . ?
C19A C14A C15A 115.5(11) . . ?
C14A C15A H15A 118.1 . . ?
C16A C15A C14A 123.9(17) . . ?
C16A C15A H15A 118.1 . . ?
C15A C16A H16A 119.9 . . ?
C15A C16A C17A 120.3(18) . . ?
C17A C16A H16A 119.9 . . ?
C16A C17A H17A 120.6 . . ?
C16A C17A C18A 118.7(18) . . ?
C18A C17A H17A 120.6 . . ?
C19A C18A C17A 121.3(16) . . ?
C19A C18A H18A 119.3 . . ?
C17A C18A H18A 119.3 . . ?
C22A C21A C20A 121.1(14) . . ?
C30A C21A C20A 118.4(14) . . ?
C30A C21A C22A 120.4(15) . . ?
C23A C22A C21A 122.9(10) . . ?
C23A C22A C27A 120.0 . . ?
C27A C22A C21A 116.9(10) . . ?
C22A C23A H23A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C24A C25A C26A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C27A C26A C25A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C22A C27A C28A 123.4(10) . . ?
C26A C27A C22A 120.0 . . ?
C26A C27A C28A 116.4(10) . . ?
C27A C28A H28A 120.0 . . ?
C27A C28A C29A 120.0(15) . . ?
C29A C28A H28A 120.0 . . ?
C28A C29A H29A 123.2 . . ?
C30A C29A C28A 113.7(17) . . ?
C30A C29A H29A 123.2 . . ?
O11A C30A C29A 120.3(17) . . ?
C21A C30A O11A 114.2(15) . . ?
C21A C30A C29A 125.4(17) . . ?
O11A C31A H31A 109.5 . . ?
O11A C31A H31B 109.5 . . ?
O11A C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
P1A Fe1B Fe1A 52.73(16) . . ?
P1B Fe1B Fe1A 53.48(15) . . ?
P1B Fe1B P1A 75.75(17) . . ?
C1B Fe1B Fe1A 100.7(8) . . ?
C1B Fe1B P1A 153.1(8) . . ?
C1B Fe1B P1B 91.8(8) . . ?
C1B Fe1B C2B 104.0(9) . . ?
C2B Fe1B Fe1A 140.8(6) . . ?
C2B Fe1B P1A 100.9(6) . . ?
C2B Fe1B P1B 95.6(7) . . ?
C3B Fe1B Fe1A 106.7(9) . . ?
C3B Fe1B P1A 94.6(9) . . ?
C3B Fe1B P1B 160.0(9) . . ?
C3B Fe1B C1B 89.3(12) . . ?
C3B Fe1B C2B 103.5(12) . . ?
Fe1A P1B Fe1B 73.02(15) . . ?
Fe1A P1B H1B 108.4 . . ?
Fe1B P1B H1B 108.4 . . ?
C11B P1B Fe1A 129.3(5) . . ?
C11B P1B Fe1B 124.7(6) . . ?
C11B P1B H1B 108.4 . . ?
C30B O11B C32B 119.0(14) . . ?
O1B C1B Fe1B 178.0(18) . . ?
O2B C2B Fe1B 177.7(19) . . ?
O3B C3B Fe1B 169(2) . . ?
C12B C11B P1B 119.1(12) . . ?
C12B C11B C20B 121.7(15) . . ?
C20B C11B P1B 119.0(10) . . ?
C11B C12B H12B 121.5 . . ?
C13B C12B C11B 116.9(15) . . ?
C13B C12B H12B 121.5 . . ?
C12B C13B H13B 118.4 . . ?
C12B C13B C14B 123.2(16) . . ?
C14B C13B H13B 118.4 . . ?
C13B C14B C15B 120.1(16) . . ?
C13B C14B C19B 121.1(17) . . ?
C19B C14B C15B 118.8(16) . . ?
C14B C15B H15B 118.4 . . ?
C16B C15B C14B 123.3(18) . . ?
C16B C15B H15B 118.4 . . ?
C15B C16B H16B 123.5 . . ?
C15B C16B C17B 113.1(17) . . ?
C17B C16B H16B 123.5 . . ?
C16B C17B H17B 118.1 . . ?
C18B C17B C16B 123.8(18) . . ?
C18B C17B H17B 118.1 . . ?
C17B C18B H18B 119.7 . . ?
C17B C18B C19B 120.6(18) . . ?
C19B C18B H18B 119.7 . . ?
C14B C19B C20B 120.8(15) . . ?
C18B C19B C14B 120.2(17) . . ?
C18B C19B C20B 119.0(16) . . ?
C19B C20B C11B 116.2(13) . . ?
C19B C20B C21B 126.8(14) . . ?
C21B C20B C11B 117.1(13) . . ?
C22B C21B C20B 121.5(17) . . ?
C30B C21B C20B 115.2(15) . . ?
C30B C21B C22B 122.7(15) . . ?
C21B C22B C27B 116.0(18) . . ?
C23B C22B C21B 125.2(16) . . ?
C23B C22B C27B 118.7(16) . . ?
C22B C23B H23B 118.7 . . ?
C22B C23B C24B 122.6(19) . . ?
C24B C23B H23B 118.7 . . ?
C23B C24B H24B 123.2 . . ?
C23B C24B C25B 114(2) . . ?
C25B C24B H24B 123.2 . . ?
C24B C25B H25B 119.7 . . ?
C26B C25B C24B 120.5(19) . . ?
C26B C25B H25B 119.7 . . ?
C25B C26B H26B 114.8 . . ?
C25B C26B C27B 130(2) . . ?
C27B C26B H26B 114.8 . . ?
C26B C27B C22B 112(2) . . ?
C28B C27B C22B 120.3(17) . . ?
C28B C27B C26B 126.8(19) . . ?
C27B C28B H28B 118.2 . . ?
C27B C28B C29B 123.5(19) . . ?
C29B C28B H28B 118.2 . . ?
C28B C29B H29B 123.2 . . ?
C28B C29B C30B 114(2) . . ?
C30B C29B H29B 123.2 . . ?
O11B C30B C29B 116.7(17) . . ?
C21B C30B O11B 119.6(15) . . ?
C21B C30B C29B 123.4(16) . . ?
O11B C32B H32A 109.5 . . ?
O11B C32B H32B 109.5 . . ?
O11B C32B H32C 109.5 . . ?
H32A C32B H32B 109.5 . . ?
H32A C32B H32C 109.5 . . ?
H32B C32B H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1A P1A C11A C12A -82.5(9) . . . . ?
Fe1A P1A C11A C20A 103.0(8) . . . . ?
Fe1A Fe1B C3B O3B -115(12) . . . . ?
Fe1A P1B C11B C12B 40.0(17) . . . . ?
Fe1A P1B C11B C20B -144.0(10) . . . . ?
P1A Fe1A C2A O2A -35(8) . . . . ?
P1A Fe1A C3A O3A 136(8) . . . . ?
P1A C11A C20A C19A 174.5(12) . . . . ?
P1A C11A C20A C21A -5.5(14) . . . . ?
P1A Fe1B C3B O3B -167(12) . . . . ?
C1A Fe1A C2A O2A 142(8) . . . . ?
C1A Fe1A C3A O3A -19(8) . . . . ?
C2A Fe1A C3A O3A -116(8) . . . . ?
C3A Fe1A C2A O2A -123(8) . . . . ?
C13A C12A C11A P1A -174.4(13) . . . . ?
C13A C12A C11A C20A 0.0 . . . . ?
C13A C14A C15A C16A 179.9(17) . . . . ?
C12A C13A C14A C19A 0.0 . . . . ?
C12A C13A C14A C15A -170.1(17) . . . . ?
C12A C11A C20A C19A 0.0 . . . . ?
C12A C11A C20A C21A 180.0(13) . . . . ?
C11A C20A C19A C14A 0.0 . . . . ?
C11A C20A C19A C18A 175.5(15) . . . . ?
C11A C20A C21A C22A 88.5(15) . . . . ?
C11A C20A C21A C30A -94.8(16) . . . . ?
C20A C19A C14A C13A 0.0 . . . . ?
C20A C19A C14A C15A 170.9(15) . . . . ?
C20A C19A C18A C17A -170.5(15) . . . . ?
C20A C21A C22A C23A 0.8(18) . . . . ?
C20A C21A C22A C27A 176.7(10) . . . . ?
C20A C21A C30A O11A 4(2) . . . . ?
C20A C21A C30A C29A -176.9(17) . . . . ?
C19A C20A C21A C22A -91.5(15) . . . . ?
C19A C20A C21A C30A 85.2(17) . . . . ?
C19A C14A C15A C16A 9(3) . . . . ?
C14A C13A C12A C11A 0.0 . . . . ?
C14A C19A C18A C17A 5(2) . . . . ?
C14A C15A C16A C17A -14(3) . . . . ?
C15A C16A C17A C18A 13(3) . . . . ?
C16A C17A C18A C19A -9(3) . . . . ?
C18A C19A C14A C13A -175.6(15) . . . . ?
C18A C19A C14A C15A -4.7(16) . . . . ?
C21A C20A C19A C14A -180.0(13) . . . . ?
C21A C20A C19A C18A -4.4(17) . . . . ?
C21A C22A C23A C24A 175.8(12) . . . . ?
C21A C22A C27A C26A -176.0(12) . . . . ?
C21A C22A C27A C28A -1.6(16) . . . . ?
C22A C21A C30A O11A -179.6(15) . . . . ?
C22A C21A C30A C29A 0(3) . . . . ?
C22A C23A C24A C25A 0.0 . . . . ?
C22A C27A C28A C29A 3(3) . . . . ?
C23A C22A C27A C26A 0.0 . . . . ?
C23A C22A C27A C28A 174.4(15) . . . . ?
C23A C24A C25A C26A 0.0 . . . . ?
C24A C25A C26A C27A 0.0 . . . . ?
C25A C26A C27A C22A 0.0 . . . . ?
C25A C26A C27A C28A -174.8(14) . . . . ?
C26A C27A C28A C29A 177.9(16) . . . . ?
C27A C22A C23A C24A 0.0 . . . . ?
C27A C28A C29A C30A -3(3) . . . . ?
C28A C29A C30A O11A -178.9(19) . . . . ?
C28A C29A C30A C21A 2(3) . . . . ?
C30A C21A C22A C23A -175.9(13) . . . . ?
C30A C21A C22A C27A 0.0(19) . . . . ?
C31A O11A C30A C21A 178(2) . . . . ?
C31A O11A C30A C29A -2(3) . . . . ?
Fe1B Fe1A C2A O2A 13(9) . . . . ?
Fe1B Fe1A C3A O3A 84(8) . . . . ?
Fe1B P1A C11A C12A 10.4(11) . . . . ?
Fe1B P1A C11A C20A -164.1(6) . . . . ?
Fe1B P1B C11B C12B -56.2(16) . . . . ?
Fe1B P1B C11B C20B 119.8(12) . . . . ?
P1B Fe1A C2A O2A 45(8) . . . . ?
P1B Fe1A C3A O3A 98(8) . . . . ?
P1B Fe1B C3B O3B -107(11) . . . . ?
P1B C11B C12B C13B 177.9(14) . . . . ?
P1B C11B C20B C19B -179.3(14) . . . . ?
P1B C11B C20B C21B 2(2) . . . . ?
C1B Fe1B C3B O3B -14(12) . . . . ?
C2B Fe1B C3B O3B 90(12) . . . . ?
C11B C12B C13B C14B 0(3) . . . . ?
C11B C20B C21B C22B 85.5(19) . . . . ?
C11B C20B C21B C30B -103.1(18) . . . . ?
C12B C11B C20B C19B -3(2) . . . . ?
C12B C11B C20B C21B 178.0(16) . . . . ?
C12B C13B C14B C15B 178.5(18) . . . . ?
C12B C13B C14B C19B -1(3) . . . . ?
C13B C14B C15B C16B -178(2) . . . . ?
C13B C14B C19B C18B -179(2) . . . . ?
C13B C14B C19B C20B 0(3) . . . . ?
C14B C15B C16B C17B -5(3) . . . . ?
C14B C19B C20B C11B 2(3) . . . . ?
C14B C19B C20B C21B -179.2(19) . . . . ?
C15B C14B C19B C18B 1(3) . . . . ?
C15B C14B C19B C20B 179.9(18) . . . . ?
C15B C16B C17B C18B 7(3) . . . . ?
C16B C17B C18B C19B -5(3) . . . . ?
C17B C18B C19B C14B 1(3) . . . . ?
C17B C18B C19B C20B -178.5(18) . . . . ?
C18B C19B C20B C11B -178.6(18) . . . . ?
C18B C19B C20B C21B 0(3) . . . . ?
C19B C14B C15B C16B 2(3) . . . . ?
C19B C20B C21B C22B -93(2) . . . . ?
C19B C20B C21B C30B 79(2) . . . . ?
C20B C11B C12B C13B 2(3) . . . . ?
C20B C21B C22B C23B -7(3) . . . . ?
C20B C21B C22B C27B 176.4(16) . . . . ?
C20B C21B C30B O11B 7(2) . . . . ?
C20B C21B C30B C29B -179.6(16) . . . . ?
C21B C22B C23B C24B -176.2(19) . . . . ?
C21B C22B C27B C26B -175.5(18) . . . . ?
C21B C22B C27B C28B -2(3) . . . . ?
C22B C21B C30B O11B 178.1(16) . . . . ?
C22B C21B C30B C29B -8(3) . . . . ?
C22B C23B C24B C25B -11(3) . . . . ?
C22B C27B C28B C29B 2(4) . . . . ?
C23B C22B C27B C26B 7(3) . . . . ?
C23B C22B C27B C28B -180(2) . . . . ?
C23B C24B C25B C26B 14(3) . . . . ?
C24B C25B C26B C27B -7(4) . . . . ?
C25B C26B C27B C22B -4(4) . . . . ?
C25B C26B C27B C28B -177(3) . . . . ?
C26B C27B C28B C29B 174(2) . . . . ?
C27B C22B C23B C24B 1(3) . . . . ?
C27B C28B C29B C30B -4(4) . . . . ?
C28B C29B C30B O11B -179.1(19) . . . . ?
C28B C29B C30B C21B 7(3) . . . . ?
C30B C21B C22B C23B -177.6(18) . . . . ?
C30B C21B C22B C27B 6(3) . . . . ?
C32B O11B C30B C21B 175.1(19) . . . . ?
C32B O11B C30B C29B 1(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.019 -0.007 0.227 9.7 0.0 ?
2 0.648 0.214 0.915 224.9 65.9 ?
3 0.019 0.493 0.773 9.7 0.0 ?
4 -0.573 0.714 0.085 224.9 65.7 ?
5 0.400 0.458 0.783 7.3 0.0 ?
6 0.600 0.958 0.217 7.3 0.0 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.83(6)
2 0.17(6)
# start Validation Reply Form
_vrf_PLAT341_twin_p21            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02339 Ang.
RESPONSE: Of total reflections, only ~ 60% reflections were observed.
In addition, reciprocal lattice showed presence of another domain which
was not possible to index and include as a twinned fraction. As a result,
the least-squares refinement had to be carried out with restraints on the 
geometry (using command SADI) and ADPs (using command RIGU) that yielded
low bond precision. 

;
# end Validation Reply Form
####################################################################### 
# 
# 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_ar95a
_database_code_depnum_ccdc_archive 'CCDC 1473790'
_audit_update_record             
;
2016-04-13 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Fe2 O6 P2'
_chemical_formula_sum            'C18 H12 Fe2 O6 P2'
_chemical_formula_weight         497.92

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9932(4)
_cell_length_b                   10.0403(4)
_cell_length_c                   12.2463(5)
_cell_angle_alpha                96.863(3)
_cell_angle_beta                 98.726(3)
_cell_angle_gamma                111.771(4)
_cell_volume                     996.23(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    10235
_cell_measurement_theta_min      2.4900
_cell_measurement_theta_max      30.6890?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.225
_exptl_absorpt_coefficient_mu    1.648
_shelx_estimated_absorpt_T_min   0.576
_shelx_estimated_absorpt_T_max   0.708
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   micro-source
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_reflns_number            15414
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.225
_diffrn_reflns_theta_max         28.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4923
_reflns_number_gt                4493
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    
'CrystaMaker (CrystalMaker Software ltd., 2012)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0292P)²+0.2442P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4923
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0592
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.20624(2) 0.43536(2) 0.81403(2) 0.01952(6) Uani 1 1 d . . . . .
Fe2 Fe 0.33121(2) 0.30566(2) 0.67330(2) 0.01994(6) Uani 1 1 d . . . . .
P1 P 0.13063(4) 0.19750(4) 0.75772(3) 0.01998(8) Uani 1 1 d . . . . .
P2 P 0.16192(4) 0.41416(4) 0.62901(3) 0.02015(8) Uani 1 1 d . . . . .
O1 O -0.08593(15) 0.47011(15) 0.86459(11) 0.0412(3) Uani 1 1 d . . . . .
O2 O 0.34114(14) 0.42436(13) 1.04448(9) 0.0308(2) Uani 1 1 d . . . . .
O3 O 0.44593(17) 0.73593(14) 0.83804(12) 0.0475(4) Uani 1 1 d . . . . .
O4 O 0.22902(17) 0.10170(15) 0.45927(11) 0.0451(3) Uani 1 1 d . . . . .
O5 O 0.56402(15) 0.20583(16) 0.79605(12) 0.0455(3) Uani 1 1 d . . . . .
O6 O 0.60248(16) 0.56034(17) 0.63840(14) 0.0544(4) Uani 1 1 d . . . . .
C1 C 0.02803(19) 0.45683(17) 0.84410(13) 0.0270(3) Uani 1 1 d . . . . .
C2 C 0.28973(17) 0.42633(16) 0.95400(13) 0.0233(3) Uani 1 1 d . . . . .
C3 C 0.3516(2) 0.61980(18) 0.82795(13) 0.0294(3) Uani 1 1 d . . . . .
C4 C 0.27059(19) 0.18022(18) 0.54353(14) 0.0282(3) Uani 1 1 d . . . . .
C5 C 0.47189(19) 0.24514(18) 0.75176(14) 0.0286(3) Uani 1 1 d . . . . .
C6 C 0.4974(2) 0.46148(19) 0.65146(15) 0.0318(4) Uani 1 1 d . . . . .
C7 C 0.12855(18) 0.06390(16) 0.84496(12) 0.0229(3) Uani 1 1 d . . . . .
C8 C -0.0130(2) -0.06415(17) 0.82616(14) 0.0296(3) Uani 1 1 d . . . . .
H8 H -0.1073 -0.0764 0.7723 0.036 Uiso 1 1 calc R U . . .
C9 C -0.0156(2) -0.17307(19) 0.88626(17) 0.0391(4) Uani 1 1 d . . . . .
H9 H -0.1115 -0.2605 0.8727 0.047 Uiso 1 1 calc R U . . .
C10 C 0.1197(3) -0.1558(2) 0.96541(16) 0.0398(4) Uani 1 1 d . . . . .
H10 H 0.1169 -0.2314 1.0058 0.048 Uiso 1 1 calc R U . . .
C11 C 0.2594(2) -0.0287(2) 0.98622(14) 0.0352(4) Uani 1 1 d . . . . .
H11 H 0.3522 -0.0166 1.0414 0.042 Uiso 1 1 calc R U . . .
C12 C 0.2640(2) 0.08157(17) 0.92632(13) 0.0285(3) Uani 1 1 d . . . . .
H12 H 0.3599 0.1692 0.9410 0.034 Uiso 1 1 calc R U . . .
C13 C -0.03801(17) 0.31207(15) 0.53586(12) 0.0211(3) Uani 1 1 d . . . . .
C14 C -0.04809(19) 0.27036(18) 0.42149(13) 0.0268(3) Uani 1 1 d . . . . .
H14 H 0.0490 0.2967 0.3926 0.032 Uiso 1 1 calc R U . . .
C15 C -0.1989(2) 0.19061(19) 0.34953(13) 0.0301(3) Uani 1 1 d . . . . .
H15 H -0.2049 0.1635 0.2715 0.036 Uiso 1 1 calc R U . . .
C16 C -0.34114(19) 0.15025(18) 0.39106(14) 0.0302(3) Uani 1 1 d . . . . .
H16 H -0.4444 0.0951 0.3417 0.036 Uiso 1 1 calc R U . . .
C17 C -0.33226(19) 0.19033(19) 0.50427(14) 0.0317(4) Uani 1 1 d . . . . .
H17 H -0.4296 0.1623 0.5329 0.038 Uiso 1 1 calc R U . . .
C18 C -0.18176(19) 0.27147(18) 0.57668(13) 0.0277(3) Uani 1 1 d . . . . .
H18 H -0.1768 0.2995 0.6545 0.033 Uiso 1 1 calc R U . . .
H1 H -0.016(2) 0.124(2) 0.6920(15) 0.030(5) Uiso 1 1 d . . . . .
H2 H 0.220(2) 0.527(2) 0.5843(15) 0.034(5) 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 1.7796(16) . yes
Fe1 C2 1.7909(16) . yes
Fe1 C3 1.7969(17) . yes
Fe1 P2 2.2104(4) . yes
Fe1 P1 2.2138(4) . yes
Fe1 Fe2 2.6582(3) . yes
Fe2 C4 1.7771(17) . yes
Fe2 C5 1.7983(16) . yes
Fe2 C6 1.7998(17) . yes
Fe2 P1 2.2097(4) . yes
Fe2 P2 2.2180(4) . yes
P1 C7 1.8086(15) . ?
P1 H1 1.323(18) . ?
P2 C13 1.8210(15) . ?
P2 H2 1.288(19) . ?
O1 C1 1.1413(19) . ?
O2 C2 1.1394(18) . ?
O3 C3 1.138(2) . ?
O4 C4 1.138(2) . ?
O5 C5 1.137(2) . ?
O6 C6 1.137(2) . ?
C7 C12 1.392(2) . ?
C7 C8 1.398(2) . ?
C8 C9 1.385(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.392(2) . ?
C13 C18 1.393(2) . ?
C14 C15 1.386(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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 96.69(7) . . ?
C1 Fe1 C3 103.65(8) . . ?
C2 Fe1 C3 91.83(7) . . ?
C1 Fe1 P2 101.69(5) . . ?
C2 Fe1 P2 160.75(5) . . ?
C3 Fe1 P2 89.41(5) . . ?
C1 Fe1 P1 105.48(5) . . ?
C2 Fe1 P1 91.40(5) . . ?
C3 Fe1 P1 150.10(6) . . ?
P2 Fe1 P1 78.260(16) . . ?
C1 Fe1 Fe2 146.85(5) . . ?
C2 Fe1 Fe2 107.60(5) . . ?
C3 Fe1 Fe2 97.89(6) . . ?
P2 Fe1 Fe2 53.242(12) . . ?
P1 Fe1 Fe2 52.994(12) . . ?
C4 Fe2 C5 100.27(7) . . ?
C4 Fe2 C6 103.57(8) . . ?
C5 Fe2 C6 91.41(7) . . ?
C4 Fe2 P1 101.07(5) . . ?
C5 Fe2 P1 93.78(5) . . ?
C6 Fe2 P1 153.46(6) . . ?
C4 Fe2 P2 96.67(5) . . ?
C5 Fe2 P2 162.39(6) . . ?
C6 Fe2 P2 89.26(5) . . ?
P1 Fe2 P2 78.186(15) . . ?
C4 Fe2 Fe1 140.58(5) . . ?
C5 Fe2 Fe1 109.72(5) . . ?
C6 Fe2 Fe1 100.72(6) . . ?
P1 Fe2 Fe1 53.134(12) . . ?
P2 Fe2 Fe1 52.980(12) . . ?
C7 P1 Fe2 124.96(5) . . ?
C7 P1 Fe1 127.31(5) . . ?
Fe2 P1 Fe1 73.873(14) . . ?
C7 P1 H1 98.0(8) . . ?
Fe2 P1 H1 116.4(7) . . ?
Fe1 P1 H1 117.3(8) . . ?
C13 P2 Fe1 123.69(5) . . ?
C13 P2 Fe2 120.63(5) . . ?
Fe1 P2 Fe2 73.778(14) . . ?
C13 P2 H2 102.1(8) . . ?
Fe1 P2 H2 120.4(8) . . ?
Fe2 P2 H2 115.6(8) . . ?
O1 C1 Fe1 179.18(15) . . ?
O2 C2 Fe1 177.57(14) . . ?
O3 C3 Fe1 178.64(15) . . ?
O4 C4 Fe2 178.10(14) . . ?
O5 C5 Fe2 176.17(15) . . ?
O6 C6 Fe2 179.54(18) . . ?
C12 C7 C8 119.26(14) . . ?
C12 C7 P1 122.52(12) . . ?
C8 C7 P1 118.16(12) . . ?
C9 C8 C7 119.82(16) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 120.59(17) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.17(16) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 119.93(17) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C7 120.20(16) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 118.91(14) . . ?
C14 C13 P2 119.53(11) . . ?
C18 C13 P2 121.54(11) . . ?
C15 C14 C13 120.39(14) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.24(15) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 119.76(15) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.33(15) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 120.36(15) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?

_refine_diff_density_max         0.307
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.062

_shelxl_version_number           2013-4

