# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shelxl
_audit_block_doi                 10.5517/cc14d871
_database_code_depnum_ccdc_archive 'CCDC 1054472'
_audit_update_record             
;
2015-03-17 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H35 Fe2 O8 P S2'
_chemical_formula_weight         922.53

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P -1'
_symmetry_cell_setting           triclinic

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

_cell_length_a                   12.1078(5)
_cell_length_b                   13.5576(6)
_cell_length_c                   14.6711(6)
_cell_angle_alpha                72.688(4)
_cell_angle_beta                 67.446(4)
_cell_angle_gamma                82.128(4)
_cell_volume                     2122.64(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6602
_cell_measurement_theta_min      2.9327
_cell_measurement_theta_max      28.9692

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19156
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8540
_reflns_number_gt                6949
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED (Oxford, 2011)'
_computing_cell_refinement       'CrysAlis RED (Oxford, 2011)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_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)+(0.0263P)²+1.8063P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8540
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0857
_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
C1 C 0.6109(3) 0.4629(2) 0.3737(2) 0.0353(7) Uani 1 1 d . . .
C2 C 0.7853(3) 0.6024(3) 0.2979(3) 0.0555(10) Uani 1 1 d . . .
C3 C 0.7557(2) 0.4883(2) 0.4760(3) 0.0378(8) Uani 1 1 d . . .
C4 C 1.0524(2) 0.5098(2) 0.2696(2) 0.0302(6) Uani 1 1 d . . .
C5 C 0.9963(2) 0.3789(2) 0.4432(2) 0.0294(6) Uani 1 1 d . . .
C6 C 0.8447(2) 0.3460(2) 0.1664(2) 0.0272(6) Uani 1 1 d . . .
C7 C 0.9246(3) 0.3269(2) 0.0726(2) 0.0370(7) Uani 1 1 d . . .
H7 H 0.9967 0.3610 0.0379 0.044 Uiso 1 1 calc R . .
C8 C 0.8961(3) 0.2592(3) 0.0332(2) 0.0473(9) Uani 1 1 d . . .
H8 H 0.9489 0.2485 -0.0289 0.057 Uiso 1 1 calc R . .
C9 C 0.7880(3) 0.2046(3) 0.0845(2) 0.0391(7) Uani 1 1 d . . .
C10 C 0.7569(3) 0.1315(3) 0.0477(3) 0.0569(10) Uani 1 1 d . . .
H10 H 0.8085 0.1182 -0.0136 0.068 Uiso 1 1 calc R . .
C11 C 0.6525(3) 0.0803(3) 0.1006(3) 0.0535(9) Uani 1 1 d . . .
H11 H 0.6344 0.0313 0.0759 0.064 Uiso 1 1 calc R . .
C12 C 0.5717(3) 0.1003(2) 0.1923(3) 0.0406(8) Uani 1 1 d . . .
H12 H 0.4999 0.0657 0.2271 0.049 Uiso 1 1 calc R . .
C13 C 0.5987(3) 0.1706(2) 0.2300(2) 0.0338(7) Uani 1 1 d . . .
H13 H 0.5452 0.1834 0.2909 0.041 Uiso 1 1 calc R . .
C14 C 0.7073(2) 0.2243(2) 0.1776(2) 0.0298(6) Uani 1 1 d . . .
C15 C 0.7380(2) 0.2972(2) 0.2159(2) 0.0283(6) Uani 1 1 d . . .
H15 H 0.6843 0.3119 0.2758 0.034 Uiso 1 1 calc R . .
C16 C 1.0852(2) 0.18222(19) 0.2257(2) 0.0207(5) Uani 1 1 d . . .
C17 C 1.1516(3) 0.1626(2) 0.1309(2) 0.0305(6) Uani 1 1 d . . .
H17 H 1.2197 0.2003 0.0876 0.037 Uiso 1 1 calc R . .
C18 C 1.1178(3) 0.0884(2) 0.1006(2) 0.0398(8) Uani 1 1 d . . .
H18 H 1.1634 0.0761 0.0375 0.048 Uiso 1 1 calc R . .
C19 C 1.0162(3) 0.0320(2) 0.1637(2) 0.0375(7) Uani 1 1 d . . .
C20 C 0.9503(3) 0.0479(2) 0.2592(2) 0.0322(7) Uani 1 1 d . . .
H20 H 0.8834 0.0089 0.3029 0.039 Uiso 1 1 calc R . .
C21 C 0.9857(2) 0.1227(2) 0.2885(2) 0.0267(6) Uani 1 1 d . . .
H21 H 0.9413 0.1333 0.3525 0.032 Uiso 1 1 calc R . .
C22 C 0.8837(5) -0.0961(3) 0.1890(3) 0.0856(16) Uani 1 1 d . . .
H22A H 0.8731 -0.1421 0.1545 0.128 Uiso 1 1 calc R . .
H22B H 0.8152 -0.0501 0.2029 0.128 Uiso 1 1 calc R . .
H22C H 0.8922 -0.1355 0.2523 0.128 Uiso 1 1 calc R . .
C23 C 1.2458(2) 0.34638(19) 0.1488(2) 0.0214(5) Uani 1 1 d . . .
C24 C 1.3649(2) 0.3126(2) 0.1284(2) 0.0247(6) Uani 1 1 d . . .
H24 H 1.3851 0.2634 0.1794 0.030 Uiso 1 1 calc R . .
C25 C 1.4541(2) 0.3506(2) 0.0339(2) 0.0265(6) Uani 1 1 d . . .
H25 H 1.5331 0.3280 0.0227 0.032 Uiso 1 1 calc R . .
C26 C 1.4248(2) 0.4220(2) -0.0433(2) 0.0258(6) Uani 1 1 d . . .
C27 C 1.3067(2) 0.4590(2) -0.0233(2) 0.0307(6) Uani 1 1 d . . .
H27 H 1.2870 0.5089 -0.0742 0.037 Uiso 1 1 calc R . .
C28 C 1.2193(2) 0.4221(2) 0.0710(2) 0.0271(6) Uani 1 1 d . . .
H28 H 1.1412 0.4481 0.0832 0.033 Uiso 1 1 calc R . .
C29 C 1.6236(2) 0.4248(2) -0.1652(2) 0.0387(7) Uani 1 1 d . . .
H29A H 1.6687 0.4580 -0.2354 0.058 Uiso 1 1 calc R . .
H29B H 1.6269 0.3514 -0.1556 0.058 Uiso 1 1 calc R . .
H29C H 1.6569 0.4405 -0.1215 0.058 Uiso 1 1 calc R . .
C30 C 1.2001(2) 0.21625(19) 0.35240(19) 0.0213(5) Uani 1 1 d . . .
C31 C 1.2577(2) 0.2733(2) 0.3852(2) 0.0268(6) Uani 1 1 d . . .
H31 H 1.2569 0.3450 0.3613 0.032 Uiso 1 1 calc R . .
C32 C 1.3161(2) 0.2260(2) 0.4524(2) 0.0290(6) Uani 1 1 d . . .
H32 H 1.3544 0.2656 0.4730 0.035 Uiso 1 1 calc R . .
C33 C 1.3170(3) 0.1193(2) 0.4888(2) 0.0335(7) Uani 1 1 d . . .
C34 C 1.2598(3) 0.0612(2) 0.4573(2) 0.0365(7) Uani 1 1 d . . .
H34 H 1.2597 -0.0104 0.4821 0.044 Uiso 1 1 calc R . .
C35 C 1.2029(2) 0.1093(2) 0.3892(2) 0.0288(6) Uani 1 1 d . . .
H35 H 1.1661 0.0695 0.3677 0.035 Uiso 1 1 calc R . .
C36 C 1.4460(4) 0.1201(3) 0.5773(3) 0.0621(11) Uani 1 1 d . . .
H36A H 1.4784 0.0736 0.6249 0.093 Uiso 1 1 calc R . .
H36B H 1.3998 0.1741 0.6064 0.093 Uiso 1 1 calc R . .
H36C H 1.5101 0.1498 0.5150 0.093 Uiso 1 1 calc R . .
C37 C 0.7572(2) 0.24804(19) 0.5427(2) 0.0234(6) Uani 1 1 d . . .
C38 C 0.6422(2) 0.2709(2) 0.6011(2) 0.0269(6) Uani 1 1 d . . .
H38 H 0.5951 0.3173 0.5697 0.032 Uiso 1 1 calc R . .
C39 C 0.8287(2) 0.1770(2) 0.5895(2) 0.0293(6) Uani 1 1 d . . .
H39 H 0.9064 0.1614 0.5502 0.035 Uiso 1 1 calc R . .
C40 C 0.7844(3) 0.1310(2) 0.6925(2) 0.0337(7) Uani 1 1 d . . .
H40 H 0.8322 0.0839 0.7225 0.040 Uiso 1 1 calc R . .
C41 C 0.6661(3) 0.1541(2) 0.7544(2) 0.0290(6) Uani 1 1 d . . .
C42 C 0.5943(2) 0.2251(2) 0.7076(2) 0.0275(6) Uani 1 1 d . . .
C43 C 0.4766(3) 0.2493(2) 0.7691(2) 0.0367(7) Uani 1 1 d . . .
H43 H 0.4288 0.2961 0.7388 0.044 Uiso 1 1 calc R . .
C44 C 0.4331(3) 0.2051(2) 0.8717(2) 0.0401(8) Uani 1 1 d . . .
H44 H 0.3557 0.2216 0.9109 0.048 Uiso 1 1 calc R . .
C45 C 0.5035(3) 0.1351(2) 0.9187(2) 0.0418(8) Uani 1 1 d . . .
H45 H 0.4732 0.1058 0.9892 0.050 Uiso 1 1 calc R . .
C46 C 0.6169(3) 0.1094(2) 0.8617(2) 0.0394(7) Uani 1 1 d . . .
H46 H 0.6626 0.0618 0.8938 0.047 Uiso 1 1 calc R . .
O1 O 0.51126(18) 0.45824(19) 0.3887(2) 0.0551(7) Uani 1 1 d . . .
O2 O 0.7968(3) 0.68880(19) 0.2591(3) 0.1056(13) Uani 1 1 d . . .
O3 O 0.75320(19) 0.50261(18) 0.5500(2) 0.0507(6) Uani 1 1 d . . .
O4 O 1.09699(19) 0.58842(16) 0.23574(19) 0.0475(6) Uani 1 1 d . . .
O5 O 1.00849(18) 0.37235(17) 0.51820(17) 0.0414(5) Uani 1 1 d . . .
O6 O 0.9887(2) -0.03732(18) 0.12538(19) 0.0604(7) Uani 1 1 d . . .
O7 O 1.50199(17) 0.46116(15) -0.14023(15) 0.0358(5) Uani 1 1 d . . .
O8 O 1.3707(2) 0.06462(17) 0.55545(18) 0.0523(6) Uani 1 1 d . . .
P1 P 1.12461(6) 0.28490(5) 0.26446(5) 0.01954(15) Uani 1 1 d . . .
S1 S 0.80667(6) 0.29733(5) 0.40704(5) 0.02232(15) Uani 1 1 d . . .
S2 S 0.88855(6) 0.44403(5) 0.20371(6) 0.02865(16) Uani 1 1 d . . .
Fe1 Fe 0.97354(3) 0.39197(3) 0.32737(3) 0.02261(10) Uani 1 1 d . . .
Fe2 Fe 0.76532(3) 0.46875(3) 0.35750(3) 0.02915(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.147(3) . ?
C1 Fe2 1.802(3) . ?
C2 O2 1.142(4) . ?
C2 Fe2 1.766(3) . ?
C3 O3 1.147(4) . ?
C3 Fe2 1.794(4) . ?
C4 O4 1.145(3) . ?
C4 Fe1 1.781(3) . ?
C5 O5 1.142(3) . ?
C5 Fe1 1.778(3) . ?
C6 C15 1.365(4) . ?
C6 C7 1.420(4) . ?
C6 S2 1.789(3) . ?
C7 C8 1.361(4) . ?
C8 C9 1.416(4) . ?
C9 C10 1.412(4) . ?
C9 C14 1.419(4) . ?
C10 C11 1.360(5) . ?
C11 C12 1.405(5) . ?
C12 C13 1.364(4) . ?
C13 C14 1.415(4) . ?
C14 C15 1.421(4) . ?
C16 C21 1.387(4) . ?
C16 C17 1.399(4) . ?
C16 P1 1.831(2) . ?
C17 C18 1.377(4) . ?
C18 C19 1.385(4) . ?
C19 O6 1.362(3) . ?
C19 C20 1.386(4) . ?
C20 C21 1.384(4) . ?
C22 O6 1.431(5) . ?
C23 C24 1.395(3) . ?
C23 C28 1.397(4) . ?
C23 P1 1.820(3) . ?
C24 C25 1.390(4) . ?
C25 C26 1.381(4) . ?
C26 O7 1.359(3) . ?
C26 C27 1.397(4) . ?
C27 C28 1.377(4) . ?
C29 O7 1.428(3) . ?
C30 C35 1.389(3) . ?
C30 C31 1.394(4) . ?
C30 P1 1.823(3) . ?
C31 C32 1.385(4) . ?
C32 C33 1.385(4) . ?
C33 O8 1.361(3) . ?
C33 C34 1.388(4) . ?
C34 C35 1.384(4) . ?
C36 O8 1.433(4) . ?
C37 C38 1.376(4) . ?
C37 C39 1.408(4) . ?
C37 S1 1.781(3) . ?
C38 C42 1.411(4) . ?
C39 C40 1.366(4) . ?
C40 C41 1.422(4) . ?
C41 C42 1.410(4) . ?
C41 C46 1.419(4) . ?
C42 C43 1.419(4) . ?
C43 C44 1.357(4) . ?
C44 C45 1.394(4) . ?
C45 C46 1.367(4) . ?
P1 Fe1 2.2538(7) . ?
S1 Fe1 2.2584(7) . ?
S1 Fe2 2.2661(7) . ?
S2 Fe2 2.2715(8) . ?
S2 Fe1 2.3063(8) . ?
Fe1 Fe2 2.5169(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Fe2 176.9(3) . . ?
O2 C2 Fe2 179.1(3) . . ?
O3 C3 Fe2 177.6(3) . . ?
O4 C4 Fe1 175.9(3) . . ?
O5 C5 Fe1 178.2(3) . . ?
C15 C6 C7 119.5(3) . . ?
C15 C6 S2 124.8(2) . . ?
C7 C6 S2 115.4(2) . . ?
C8 C7 C6 120.4(3) . . ?
C7 C8 C9 121.5(3) . . ?
C10 C9 C8 123.2(3) . . ?
C10 C9 C14 118.5(3) . . ?
C8 C9 C14 118.3(3) . . ?
C11 C10 C9 120.8(3) . . ?
C10 C11 C12 120.9(3) . . ?
C13 C12 C11 119.9(3) . . ?
C12 C13 C14 120.8(3) . . ?
C13 C14 C9 119.1(3) . . ?
C13 C14 C15 121.8(3) . . ?
C9 C14 C15 119.1(3) . . ?
C6 C15 C14 121.2(3) . . ?
C21 C16 C17 117.4(2) . . ?
C21 C16 P1 120.98(19) . . ?
C17 C16 P1 121.6(2) . . ?
C18 C17 C16 121.1(3) . . ?
C17 C18 C19 120.3(3) . . ?
O6 C19 C18 115.7(3) . . ?
O6 C19 C20 124.4(3) . . ?
C18 C19 C20 119.9(3) . . ?
C21 C20 C19 119.0(3) . . ?
C20 C21 C16 122.3(3) . . ?
C24 C23 C28 117.5(2) . . ?
C24 C23 P1 122.5(2) . . ?
C28 C23 P1 119.57(19) . . ?
C25 C24 C23 121.9(2) . . ?
C26 C25 C24 119.6(2) . . ?
O7 C26 C25 125.5(2) . . ?
O7 C26 C27 115.2(2) . . ?
C25 C26 C27 119.3(2) . . ?
C28 C27 C26 120.6(3) . . ?
C27 C28 C23 121.1(2) . . ?
C35 C30 C31 117.9(2) . . ?
C35 C30 P1 123.3(2) . . ?
C31 C30 P1 118.79(19) . . ?
C32 C31 C30 121.7(2) . . ?
C31 C32 C33 119.4(3) . . ?
O8 C33 C32 124.6(3) . . ?
O8 C33 C34 115.7(3) . . ?
C32 C33 C34 119.7(3) . . ?
C35 C34 C33 120.3(3) . . ?
C34 C35 C30 120.9(3) . . ?
C38 C37 C39 119.7(2) . . ?
C38 C37 S1 119.0(2) . . ?
C39 C37 S1 120.9(2) . . ?
C37 C38 C42 121.3(3) . . ?
C40 C39 C37 120.3(3) . . ?
C39 C40 C41 121.0(3) . . ?
C42 C41 C46 118.2(3) . . ?
C42 C41 C40 118.8(3) . . ?
C46 C41 C40 123.0(3) . . ?
C41 C42 C38 119.0(2) . . ?
C41 C42 C43 119.1(3) . . ?
C38 C42 C43 121.9(3) . . ?
C44 C43 C42 120.8(3) . . ?
C43 C44 C45 120.5(3) . . ?
C46 C45 C44 120.3(3) . . ?
C45 C46 C41 121.1(3) . . ?
C19 O6 C22 116.7(3) . . ?
C26 O7 C29 117.5(2) . . ?
C33 O8 C36 117.2(2) . . ?
C23 P1 C30 103.69(11) . . ?
C23 P1 C16 101.74(12) . . ?
C30 P1 C16 103.89(11) . . ?
C23 P1 Fe1 115.29(8) . . ?
C30 P1 Fe1 114.40(8) . . ?
C16 P1 Fe1 116.11(8) . . ?
C37 S1 Fe1 117.89(9) . . ?
C37 S1 Fe2 112.41(9) . . ?
Fe1 S1 Fe2 67.60(2) . . ?
C6 S2 Fe2 115.29(9) . . ?
C6 S2 Fe1 117.83(9) . . ?
Fe2 S2 Fe1 66.70(2) . . ?
C5 Fe1 C4 90.72(13) . . ?
C5 Fe1 P1 97.13(9) . . ?
C4 Fe1 P1 98.39(9) . . ?
C5 Fe1 S1 93.50(9) . . ?
C4 Fe1 S1 153.96(9) . . ?
P1 Fe1 S1 106.54(3) . . ?
C5 Fe1 S2 159.83(9) . . ?
C4 Fe1 S2 87.47(9) . . ?
P1 Fe1 S2 103.01(3) . . ?
S1 Fe1 S2 79.82(3) . . ?
C5 Fe1 Fe2 104.49(9) . . ?
C4 Fe1 Fe2 97.74(9) . . ?
P1 Fe1 Fe2 152.74(3) . . ?
S1 Fe1 Fe2 56.35(2) . . ?
S2 Fe1 Fe2 55.99(2) . . ?
C2 Fe2 C3 90.35(17) . . ?
C2 Fe2 C1 98.54(14) . . ?
C3 Fe2 C1 103.15(13) . . ?
C2 Fe2 S1 160.86(11) . . ?
C3 Fe2 S1 92.83(10) . . ?
C1 Fe2 S1 99.10(9) . . ?
C2 Fe2 S2 86.47(13) . . ?
C3 Fe2 S2 146.11(9) . . ?
C1 Fe2 S2 110.70(10) . . ?
S1 Fe2 S2 80.40(3) . . ?
C2 Fe2 Fe1 105.03(11) . . ?
C3 Fe2 Fe1 91.32(9) . . ?
C1 Fe2 Fe1 152.23(9) . . ?
S1 Fe2 Fe1 56.05(2) . . ?
S2 Fe2 Fe1 57.31(2) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.061
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane, hexane'
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc14d882
_database_code_depnum_ccdc_archive 'CCDC 1054473'
_audit_update_record             
;
2015-03-17 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H14 Fe2 O6 S2'
_chemical_formula_sum            'C26 H14 Fe2 O6 S2'
_chemical_formula_weight         598.19

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-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                   25.545(4)
_cell_length_b                   26.670(4)
_cell_length_c                   7.3447(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5003.9(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    803
_cell_measurement_theta_min      2.8243
_cell_measurement_theta_max      29.0394

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.366
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_reflns_number            11221
_diffrn_reflns_av_unetI/netI     0.1902
_diffrn_reflns_av_R_equivalents  0.1320
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.985
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             4228
_reflns_number_gt                2058
_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       'X-calibur S oxford'
_computing_cell_refinement       'X-calibur S SAINT'
_computing_data_reduction        'X-calibur S SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Oxford SHELXTL'
_computing_publication_material  'Oxford SHELXTL'

_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)+(0.0574P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       .
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4228
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.0923
_refine_ls_wR_factor_ref         0.2031
_refine_ls_wR_factor_gt          0.1526
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.970
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.020

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 0.03175(6) 0.08910(5) 0.03554(19) 0.0430(5) Uani 1 1 d . . . . .
Fe2 Fe 0.06639(6) 0.16152(6) -0.14153(19) 0.0460(5) Uani 1 1 d . . . . .
S1 S 0.00444(10) 0.16933(10) 0.0797(3) 0.0440(7) Uani 1 1 d . . . . .
S2 S 0.10414(10) 0.13222(10) 0.1182(3) 0.0483(8) Uani 1 1 d . . . . .
C1 C -0.0610(4) 0.1832(4) 0.0053(12) 0.040(3) Uani 1 1 d . . . . .
C6 C -0.1016(4) 0.1537(4) 0.0487(12) 0.046(3) Uani 1 1 d . . . . .
H6 H -0.0955 0.1229 0.1044 0.055 Uiso 1 1 calc R U . . .
O3 O 0.0899(3) 0.0085(3) -0.1368(12) 0.084(3) Uani 1 1 d . . . . .
C3 C -0.1188(5) 0.2451(4) -0.1166(13) 0.054(3) Uani 1 1 d . . . . .
H3 H -0.1243 0.2763 -0.1702 0.065 Uiso 1 1 calc R U . . .
O1 O 0.0044(4) 0.0463(3) 0.3898(11) 0.097(3) Uani 1 1 d . . . . .
C5 C -0.1533(4) 0.1688(5) 0.0108(12) 0.051(3) Uani 1 1 d . . . . .
C15 C 0.2558(5) 0.0998(4) 0.0137(14) 0.051(3) Uani 1 1 d . . . . .
O2 O -0.0548(3) 0.0597(3) -0.1963(11) 0.079(3) Uani 1 1 d . . . . .
C26 C 0.0199(4) 0.1653(4) -0.3200(14) 0.054(3) Uani 1 1 d . . . . .
C2 C -0.0694(4) 0.2296(4) -0.0823(12) 0.049(3) Uani 1 1 d . . . . .
H2 H -0.0411 0.2495 -0.1163 0.059 Uiso 1 1 calc R U . . .
O4 O 0.1351(3) 0.1072(4) -0.3885(11) 0.086(3) Uani 1 1 d . . . . .
C23 C 0.0682(4) 0.0399(5) -0.0638(16) 0.059(3) Uani 1 1 d . . . . .
C22 C -0.0225(5) 0.0722(4) -0.0995(16) 0.061(3) Uani 1 1 d . . . . .
C11 C 0.1649(4) 0.0988(4) 0.0905(13) 0.044(3) Uani 1 1 d . . . . .
C19 C 0.3535(5) 0.0537(7) 0.0304(17) 0.088(5) Uani 1 1 d . . . . .
H19 H 0.3865 0.0390 0.0372 0.105 Uiso 1 1 calc R U . . .
C16 C 0.2056(4) 0.1235(4) 0.0124(13) 0.052(3) Uani 1 1 d . . . . .
H16 H 0.2010 0.1549 -0.0404 0.062 Uiso 1 1 calc R U . . .
O6 O -0.0105(3) 0.1668(4) -0.4347(10) 0.086(3) Uani 1 1 d . . . . .
C25 C 0.0952(5) 0.2228(5) -0.1437(16) 0.068(4) Uani 1 1 d . . . . .
C12 C 0.1702(5) 0.0522(4) 0.1699(15) 0.067(4) Uani 1 1 d . . . . .
H12 H 0.1416 0.0370 0.2256 0.080 Uiso 1 1 calc R U . . .
C14 C 0.2620(5) 0.0522(5) 0.0927(14) 0.056(3) Uani 1 1 d . . . . .
C4 C -0.1617(4) 0.2150(4) -0.0726(12) 0.044(3) Uani 1 1 d . . . . .
C20 C 0.3123(6) 0.0298(5) 0.0957(14) 0.068(4) Uani 1 1 d . . . . .
H20 H 0.3163 -0.0021 0.1444 0.082 Uiso 1 1 calc R U . . .
C21 C 0.0143(4) 0.0617(4) 0.2503(16) 0.054(3) Uani 1 1 d . . . . .
C10 C -0.1973(5) 0.1390(5) 0.0555(14) 0.063(3) Uani 1 1 d . . . . .
H10 H -0.1927 0.1075 0.1073 0.075 Uiso 1 1 calc R U . . .
C17 C 0.3002(5) 0.1250(5) -0.0582(14) 0.066(4) Uani 1 1 d . . . . .
H17 H 0.2969 0.1567 -0.1095 0.079 Uiso 1 1 calc R U . . .
C24 C 0.1092(4) 0.1284(5) -0.2894(15) 0.058(3) Uani 1 1 d . . . . .
C7 C -0.2135(5) 0.2316(5) -0.1048(13) 0.065(4) Uani 1 1 d . . . . .
H7 H -0.2191 0.2628 -0.1584 0.078 Uiso 1 1 calc R U . . .
C9 C -0.2462(5) 0.1566(7) 0.0226(16) 0.084(5) Uani 1 1 d . . . . .
H9 H -0.2748 0.1371 0.0558 0.101 Uiso 1 1 calc R U . . .
O5 O 0.1153(4) 0.2608(4) -0.1451(14) 0.119(4) Uani 1 1 d . . . . .
C18 C 0.3476(5) 0.1021(6) -0.0509(17) 0.082(4) Uani 1 1 d . . . . .
H18 H 0.3768 0.1181 -0.0995 0.098 Uiso 1 1 calc R U . . .
C8 C -0.2551(6) 0.2027(6) -0.0586(16) 0.078(5) Uani 1 1 d . . . . .
H8 H -0.2890 0.2136 -0.0811 0.094 Uiso 1 1 calc R U . . .
C13 C 0.2185(5) 0.0280(5) 0.1663(15) 0.073(4) Uani 1 1 d . . . . .
H13 H 0.2217 -0.0043 0.2129 0.087 Uiso 1 1 calc R 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
Fe1 C22 1.763(12) . ?
Fe1 C23 1.768(13) . ?
Fe1 C21 1.795(12) . ?
Fe1 S2 2.261(3) . ?
Fe1 S1 2.274(3) . ?
Fe1 Fe2 2.491(2) . ?
Fe2 C26 1.771(12) . ?
Fe2 C24 1.777(12) . ?
Fe2 C25 1.793(13) . ?
Fe2 S2 2.276(3) . ?
Fe2 S1 2.278(3) . ?
S1 C1 1.797(10) . ?
S2 C11 1.801(10) . ?
C1 C6 1.341(12) . ?
C1 C2 1.411(13) . ?
C6 C5 1.410(13) . ?
O3 C23 1.137(12) . ?
C3 C2 1.351(12) . ?
C3 C4 1.396(13) . ?
O1 C21 1.133(11) . ?
C5 C4 1.394(14) . ?
C5 C10 1.414(14) . ?
C15 C14 1.404(14) . ?
C15 C17 1.420(14) . ?
C15 C16 1.429(13) . ?
O2 C22 1.138(11) . ?
C26 O6 1.146(11) . ?
O4 C24 1.135(12) . ?
C11 C16 1.358(12) . ?
C11 C12 1.381(13) . ?
C19 C20 1.321(15) . ?
C19 C18 1.429(17) . ?
C25 O5 1.135(13) . ?
C12 C13 1.392(14) . ?
C14 C13 1.395(14) . ?
C14 C20 1.417(14) . ?
C4 C7 1.415(13) . ?
C10 C9 1.355(14) . ?
C17 C18 1.359(14) . ?
C7 C8 1.355(15) . ?
C9 C8 1.385(18) . ?

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
C22 Fe1 C23 89.5(5) . . ?
C22 Fe1 C21 101.3(5) . . ?
C23 Fe1 C21 101.0(5) . . ?
C22 Fe1 S2 157.6(4) . . ?
C23 Fe1 S2 93.3(4) . . ?
C21 Fe1 S2 100.0(3) . . ?
C22 Fe1 S1 94.6(4) . . ?
C23 Fe1 S1 156.9(4) . . ?
C21 Fe1 S1 100.5(4) . . ?
S2 Fe1 S1 74.57(10) . . ?
C22 Fe1 Fe2 100.6(4) . . ?
C23 Fe1 Fe2 100.0(3) . . ?
C21 Fe1 Fe2 149.6(3) . . ?
S2 Fe1 Fe2 56.98(8) . . ?
S1 Fe1 Fe2 56.90(8) . . ?
C26 Fe2 C24 89.4(5) . . ?
C26 Fe2 C25 102.5(5) . . ?
C24 Fe2 C25 101.2(5) . . ?
C26 Fe2 S2 157.5(4) . . ?
C24 Fe2 S2 94.6(4) . . ?
C25 Fe2 S2 98.4(4) . . ?
C26 Fe2 S1 93.3(3) . . ?
C24 Fe2 S1 155.4(4) . . ?
C25 Fe2 S1 102.0(4) . . ?
S2 Fe2 S1 74.21(10) . . ?
C26 Fe2 Fe1 101.1(4) . . ?
C24 Fe2 Fe1 98.8(4) . . ?
C25 Fe2 Fe1 149.0(4) . . ?
S2 Fe2 Fe1 56.41(8) . . ?
S1 Fe2 Fe1 56.74(8) . . ?
C1 S1 Fe1 115.9(3) . . ?
C1 S1 Fe2 116.6(3) . . ?
Fe1 S1 Fe2 66.35(8) . . ?
C11 S2 Fe1 115.0(4) . . ?
C11 S2 Fe2 116.1(3) . . ?
Fe1 S2 Fe2 66.61(9) . . ?
C6 C1 C2 120.4(10) . . ?
C6 C1 S1 121.7(8) . . ?
C2 C1 S1 117.5(8) . . ?
C1 C6 C5 120.6(10) . . ?
C2 C3 C4 120.9(11) . . ?
C4 C5 C6 119.0(11) . . ?
C4 C5 C10 118.4(10) . . ?
C6 C5 C10 122.7(11) . . ?
C14 C15 C17 119.4(11) . . ?
C14 C15 C16 120.2(11) . . ?
C17 C15 C16 120.3(11) . . ?
O6 C26 Fe2 178.6(12) . . ?
C3 C2 C1 119.8(11) . . ?
O3 C23 Fe1 175.9(12) . . ?
O2 C22 Fe1 174.6(11) . . ?
C16 C11 C12 122.7(10) . . ?
C16 C11 S2 117.9(8) . . ?
C12 C11 S2 118.8(9) . . ?
C20 C19 C18 120.2(13) . . ?
C11 C16 C15 118.0(10) . . ?
O5 C25 Fe2 177.5(13) . . ?
C11 C12 C13 119.7(11) . . ?
C13 C14 C15 119.2(11) . . ?
C13 C14 C20 121.4(12) . . ?
C15 C14 C20 119.3(12) . . ?
C5 C4 C3 119.3(10) . . ?
C5 C4 C7 119.6(11) . . ?
C3 C4 C7 121.0(11) . . ?
C19 C20 C14 120.9(14) . . ?
O1 C21 Fe1 176.8(11) . . ?
C9 C10 C5 119.8(12) . . ?
C18 C17 C15 119.0(12) . . ?
O4 C24 Fe2 177.4(10) . . ?
C8 C7 C4 120.8(12) . . ?
C10 C9 C8 122.3(14) . . ?
C17 C18 C19 121.1(13) . . ?
C7 C8 C9 119.0(13) . . ?
C12 C13 C14 120.0(11) . . ?

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
Fe1 S1 C1 C6 48.1(9) . . . . ?
Fe2 S1 C1 C6 123.3(7) . . . . ?
Fe1 S1 C1 C2 -139.4(6) . . . . ?
Fe2 S1 C1 C2 -64.2(8) . . . . ?
C2 C1 C6 C5 -1.2(14) . . . . ?
S1 C1 C6 C5 171.2(7) . . . . ?
C1 C6 C5 C4 -0.1(14) . . . . ?
C1 C6 C5 C10 -179.4(9) . . . . ?
C4 C3 C2 C1 -2.4(15) . . . . ?
C6 C1 C2 C3 2.4(14) . . . . ?
S1 C1 C2 C3 -170.2(7) . . . . ?
Fe1 S2 C11 C16 134.5(7) . . . . ?
Fe2 S2 C11 C16 59.5(9) . . . . ?
Fe1 S2 C11 C12 -53.8(9) . . . . ?
Fe2 S2 C11 C12 -128.8(8) . . . . ?
C12 C11 C16 C15 -0.1(15) . . . . ?
S2 C11 C16 C15 171.2(7) . . . . ?
C14 C15 C16 C11 0.5(14) . . . . ?
C17 C15 C16 C11 -176.9(9) . . . . ?
C16 C11 C12 C13 -2.1(17) . . . . ?
S2 C11 C12 C13 -173.4(8) . . . . ?
C17 C15 C14 C13 178.8(10) . . . . ?
C16 C15 C14 C13 1.3(15) . . . . ?
C17 C15 C14 C20 -1.3(15) . . . . ?
C16 C15 C14 C20 -178.8(9) . . . . ?
C6 C5 C4 C3 0.1(14) . . . . ?
C10 C5 C4 C3 179.5(9) . . . . ?
C6 C5 C4 C7 -177.4(9) . . . . ?
C10 C5 C4 C7 2.0(14) . . . . ?
C2 C3 C4 C5 1.1(15) . . . . ?
C2 C3 C4 C7 178.6(9) . . . . ?
C18 C19 C20 C14 -2.3(19) . . . . ?
C13 C14 C20 C19 -178.1(11) . . . . ?
C15 C14 C20 C19 2.1(16) . . . . ?
C4 C5 C10 C9 -2.2(16) . . . . ?
C6 C5 C10 C9 177.1(10) . . . . ?
C14 C15 C17 C18 0.9(16) . . . . ?
C16 C15 C17 C18 178.3(10) . . . . ?
C5 C4 C7 C8 -1.2(16) . . . . ?
C3 C4 C7 C8 -178.7(10) . . . . ?
C5 C10 C9 C8 1.7(18) . . . . ?
C15 C17 C18 C19 -1.1(19) . . . . ?
C20 C19 C18 C17 2(2) . . . . ?
C4 C7 C8 C9 0.6(18) . . . . ?
C10 C9 C8 C7 -0.9(19) . . . . ?
C11 C12 C13 C14 4.0(17) . . . . ?
C15 C14 C13 C12 -3.6(17) . . . . ?
C20 C14 C13 C12 176.5(10) . . . . ?

_refine_diff_density_max         0.428
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.088

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane, hexane'
_chemical_properties_physical    Air-sensitive
