# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013
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#
# Cambridge Crystallographic Data Centre
# CCDC
#
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#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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# fide research purposes only. It may contain copyright material
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data_1
_database_code_depnum_ccdc_archive 'CCDC 912951'
#TrackingRef 'ChemComm1-2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C31 H15 Fe4 O12 P S3'
_chemical_formula_sum 'C31 H15 Fe4 O12 P S3'
_chemical_formula_weight 930.01
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'
S S 0.1246 0.1234 '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/c'
_space_group_name_Hall '-P 2ybc'
_space_group_IT_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 13.1351(12)
_cell_length_b 18.8283(16)
_cell_length_c 17.9612(13)
_cell_angle_alpha 90.00
_cell_angle_beta 126.2481(13)
_cell_angle_gamma 90.00
_cell_volume 3582.3(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 296
_cell_measurement_reflns_used 6114
_cell_measurement_theta_min 1.77
_cell_measurement_theta_max 27.54
_exptl_crystal_description Block
_exptl_crystal_colour Red
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.17
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.724
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1856
_exptl_absorpt_coefficient_mu 1.867
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.706
_exptl_absorpt_correction_T_max 0.721
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296
_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 SMART APEX CCD'
_diffrn_measurement_method '\w and \f'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 52525
_diffrn_reflns_av_R_equivalents 0.0522
_diffrn_reflns_av_sigmaI/netI 0.0406
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 1.77
_diffrn_reflns_theta_max 27.54
_reflns_number_total 8223
_reflns_number_gt 6114
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'SMART (Bruker, 2002)'
_computing_cell_refinement 'SAINT-Plus (Bruker, 2003)'
_computing_data_reduction 'SAINT-Plus (Bruker, 2003)'
_computing_structure_solution 'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009);WinGX (Farrugia, 1999)'
_computing_publication_material 'publCIF (Westrip, 2010)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0324P)^2^+1.0025P] where P=(Fo^2^+2Fc^2^)/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 SHELXL
_refine_ls_extinction_coef 0.0216(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 8223
_refine_ls_number_parameters 461
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0578
_refine_ls_R_factor_gt 0.0325
_refine_ls_wR_factor_ref 0.0727
_refine_ls_wR_factor_gt 0.0645
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_restrained_S_all 1.018
_refine_ls_shift/su_max 0.002
_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 0.9916(2) 0.64627(15) 0.6041(2) 0.0577(7) Uani 1 1 d . . .
C2 C 1.1977(2) 0.72486(14) 0.72729(19) 0.0539(7) Uani 1 1 d . . .
C3 C 1.0997(3) 0.64334(14) 0.7873(2) 0.0560(7) Uani 1 1 d . . .
C4 C 1.1738(2) 0.85652(15) 0.81500(19) 0.0551(7) Uani 1 1 d . . .
C5 C 1.0686(2) 0.79189(14) 0.87937(18) 0.0487(6) Uani 1 1 d . . .
C6 C 0.9506(2) 0.90184(15) 0.76348(17) 0.0503(6) Uani 1 1 d . . .
C7 C 0.7991(2) 0.74198(14) 0.37951(16) 0.0445(6) Uani 1 1 d . . .
C8 C 0.9549(3) 0.85492(13) 0.45939(17) 0.0469(6) Uani 1 1 d . . .
C9 C 0.7507(3) 0.87662(14) 0.30700(19) 0.0527(6) Uani 1 1 d . . .
C10 C 0.9117(2) 0.96350(12) 0.56829(18) 0.0464(6) Uani 1 1 d . . .
C11 C 0.7169(2) 0.99476(13) 0.40777(17) 0.0453(6) Uani 1 1 d . . .
C12 C 0.6889(2) 0.96262(13) 0.54238(17) 0.0458(6) Uani 1 1 d . . .
C13 C 0.82324(19) 0.82357(11) 0.53579(15) 0.0320(5) Uani 1 1 d . . .
C14 C 0.61217(19) 0.79368(11) 0.56378(15) 0.0351(5) Uani 1 1 d . . .
C15 C 0.4892(2) 0.77370(15) 0.49534(18) 0.0538(7) Uani 1 1 d . . .
H15 H 0.4713 0.7467 0.4456 0.065 Uiso 1 1 calc R . .
C16 C 0.3931(2) 0.79399(17) 0.5011(2) 0.0666(8) Uani 1 1 d . . .
H16 H 0.3105 0.7807 0.4547 0.080 Uiso 1 1 calc R . .
C17 C 0.4173(3) 0.83319(16) 0.5735(2) 0.0629(8) Uani 1 1 d . . .
H17 H 0.3518 0.8460 0.5769 0.076 Uiso 1 1 calc R . .
C18 C 0.5384(3) 0.85366(16) 0.6415(2) 0.0642(8) Uani 1 1 d . . .
H18 H 0.5554 0.8807 0.6910 0.077 Uiso 1 1 calc R . .
C19 C 0.6359(2) 0.83391(14) 0.63632(18) 0.0506(6) Uani 1 1 d . . .
H19 H 0.7181 0.8481 0.6824 0.061 Uiso 1 1 calc R . .
C20 C 0.68095(19) 0.67729(11) 0.50021(15) 0.0351(5) Uani 1 1 d . . .
C21 C 0.6013(2) 0.67398(13) 0.40480(16) 0.0432(6) Uani 1 1 d . . .
H21 H 0.5900 0.7140 0.3703 0.052 Uiso 1 1 calc R . .
C22 C 0.5381(2) 0.61169(14) 0.36007(19) 0.0517(6) Uani 1 1 d . . .
H22 H 0.4847 0.6101 0.2959 0.062 Uiso 1 1 calc R . .
C23 C 0.5541(3) 0.55276(14) 0.4099(2) 0.0600(7) Uani 1 1 d . . .
H23 H 0.5109 0.5112 0.3798 0.072 Uiso 1 1 calc R . .
C24 C 0.6336(3) 0.55469(15) 0.5043(2) 0.0686(8) Uani 1 1 d . . .
H24 H 0.6452 0.5141 0.5381 0.082 Uiso 1 1 calc R . .
C25 C 0.6967(3) 0.61662(13) 0.54972(18) 0.0532(7) Uani 1 1 d . . .
H25 H 0.7501 0.6176 0.6139 0.064 Uiso 1 1 calc R . .
C26 C 0.4813(2) 0.88842(13) 0.27392(16) 0.0417(5) Uani 1 1 d . . .
C27 C 0.4502(3) 0.85787(15) 0.19315(17) 0.0562(7) Uani 1 1 d . . .
H27 H 0.5009 0.8225 0.1947 0.067 Uiso 1 1 calc R . .
C28 C 0.3428(3) 0.88038(19) 0.1097(2) 0.0756(9) Uani 1 1 d . . .
H28 H 0.3215 0.8599 0.0551 0.091 Uiso 1 1 calc R . .
C29 C 0.2679(3) 0.9321(2) 0.1067(2) 0.0815(10) Uani 1 1 d . . .
H29 H 0.1959 0.9466 0.0501 0.098 Uiso 1 1 calc R . .
C30 C 0.2985(3) 0.96286(19) 0.1867(2) 0.0772(9) Uani 1 1 d . . .
H30 H 0.2472 0.9981 0.1845 0.093 Uiso 1 1 calc R . .
C31 C 0.4058(2) 0.94130(15) 0.2707(2) 0.0576(7) Uani 1 1 d . . .
H31 H 0.4271 0.9624 0.3251 0.069 Uiso 1 1 calc R . .
Fe1 Fe 1.04365(3) 0.708556(17) 0.69733(2) 0.04006(10) Uani 1 1 d . . .
Fe2 Fe 1.02304(3) 0.819032(17) 0.76694(2) 0.03663(10) Uani 1 1 d . . .
Fe3 Fe 0.79402(3) 0.832365(17) 0.41027(2) 0.03698(10) Uani 1 1 d . . .
Fe4 Fe 0.75896(3) 0.925405(16) 0.48971(2) 0.03425(9) Uani 1 1 d . . .
O1 O 0.9640(2) 0.60576(13) 0.54838(16) 0.0900(7) Uani 1 1 d . . .
O2 O 1.29456(19) 0.73823(12) 0.74605(17) 0.0841(7) Uani 1 1 d . . .
O3 O 1.1341(2) 0.60343(12) 0.84493(16) 0.0887(7) Uani 1 1 d . . .
O4 O 1.2707(2) 0.88114(14) 0.84727(18) 0.0963(8) Uani 1 1 d . . .
O5 O 1.09902(19) 0.77664(12) 0.95062(14) 0.0764(6) Uani 1 1 d . . .
O6 O 0.9125(2) 0.95488(11) 0.76670(16) 0.0802(6) Uani 1 1 d . . .
O7 O 0.80892(19) 0.68606(10) 0.36036(14) 0.0646(5) Uani 1 1 d . . .
O8 O 1.05379(19) 0.87124(11) 0.48468(15) 0.0701(6) Uani 1 1 d . . .
O9 O 0.7248(2) 0.90779(12) 0.24357(15) 0.0811(7) Uani 1 1 d . . .
O10 O 1.00803(18) 0.98934(10) 0.61765(15) 0.0742(6) Uani 1 1 d . . .
O11 O 0.69087(19) 1.03728(10) 0.35417(13) 0.0700(6) Uani 1 1 d . . .
O12 O 0.64516(19) 0.99088(11) 0.57284(15) 0.0729(6) Uani 1 1 d . . .
P1 P 0.74160(5) 0.76207(3) 0.56161(4) 0.03048(13) Uani 1 1 d . . .
S1 S 0.87701(5) 0.73132(3) 0.70039(4) 0.03612(14) Uani 1 1 d . . .
S2 S 0.98940(5) 0.81528(3) 0.62924(4) 0.03556(13) Uani 1 1 d . . .
S3 S 0.60583(5) 0.85286(3) 0.38299(4) 0.03764(14) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0434(15) 0.0609(17) 0.0586(18) -0.0016(15) 0.0247(14) 0.0125(13)
C2 0.0370(14) 0.0533(15) 0.0618(17) 0.0036(13) 0.0239(13) 0.0122(12)
C3 0.0527(16) 0.0444(15) 0.0597(17) 0.0051(14) 0.0271(14) 0.0048(13)
C4 0.0426(15) 0.0610(16) 0.0562(17) -0.0115(14) 0.0262(13) -0.0099(13)
C5 0.0327(13) 0.0560(15) 0.0413(15) -0.0044(12) 0.0129(12) -0.0097(11)
C6 0.0426(14) 0.0540(16) 0.0430(14) -0.0064(12) 0.0190(12) -0.0041(12)
C7 0.0426(13) 0.0525(15) 0.0428(14) -0.0029(12) 0.0276(12) -0.0022(11)
C8 0.0558(16) 0.0445(14) 0.0515(15) -0.0005(12) 0.0377(14) -0.0022(12)
C9 0.0606(17) 0.0572(16) 0.0527(16) 0.0072(13) 0.0404(15) 0.0109(13)
C10 0.0492(15) 0.0307(12) 0.0533(15) 0.0048(11) 0.0270(13) 0.0031(11)
C11 0.0447(14) 0.0387(13) 0.0452(14) 0.0002(12) 0.0225(12) 0.0009(11)
C12 0.0420(14) 0.0460(14) 0.0448(14) -0.0030(11) 0.0231(12) -0.0014(11)
C13 0.0276(10) 0.0316(11) 0.0350(12) 0.0000(9) 0.0175(10) 0.0010(9)
C14 0.0301(11) 0.0401(12) 0.0356(12) -0.0001(10) 0.0197(10) -0.0002(9)
C15 0.0302(12) 0.0750(18) 0.0481(15) -0.0180(13) 0.0188(12) -0.0041(12)
C16 0.0305(14) 0.087(2) 0.074(2) -0.0160(17) 0.0268(14) -0.0025(13)
C17 0.0478(16) 0.0732(19) 0.085(2) -0.0054(17) 0.0483(17) 0.0060(14)
C18 0.0618(18) 0.079(2) 0.0707(19) -0.0219(16) 0.0499(17) -0.0045(15)
C19 0.0380(13) 0.0658(16) 0.0501(15) -0.0158(13) 0.0272(12) -0.0071(12)
C20 0.0316(11) 0.0351(12) 0.0402(13) -0.0067(10) 0.0222(10) -0.0050(9)
C21 0.0425(13) 0.0456(14) 0.0415(14) -0.0071(11) 0.0248(12) -0.0068(11)
C22 0.0483(15) 0.0553(16) 0.0506(15) -0.0196(13) 0.0287(13) -0.0157(12)
C23 0.0618(17) 0.0428(15) 0.076(2) -0.0228(14) 0.0413(17) -0.0189(13)
C24 0.085(2) 0.0413(15) 0.071(2) -0.0031(14) 0.0412(18) -0.0140(15)
C25 0.0613(17) 0.0438(14) 0.0468(15) -0.0035(12) 0.0276(14) -0.0113(12)
C26 0.0322(12) 0.0474(13) 0.0353(13) 0.0002(11) 0.0142(10) -0.0058(10)
C27 0.0550(16) 0.0596(17) 0.0410(15) -0.0045(13) 0.0212(13) -0.0091(13)
C28 0.063(2) 0.096(2) 0.0369(16) -0.0087(16) 0.0127(15) -0.0274(19)
C29 0.0411(17) 0.110(3) 0.059(2) 0.025(2) 0.0103(15) -0.0044(18)
C30 0.0436(16) 0.093(2) 0.080(2) 0.019(2) 0.0277(17) 0.0193(16)
C31 0.0423(15) 0.0708(18) 0.0547(17) 0.0015(14) 0.0259(13) 0.0044(14)
Fe1 0.03247(18) 0.03789(19) 0.0430(2) 0.00419(15) 0.01853(16) 0.00696(14)
Fe2 0.02580(17) 0.04006(19) 0.03508(19) -0.00222(14) 0.01306(15) -0.00287(13)
Fe3 0.04078(19) 0.03778(18) 0.03724(19) 0.00039(14) 0.02574(16) 0.00167(14)
Fe4 0.03311(18) 0.03177(17) 0.03410(18) 0.00034(13) 0.01780(15) 0.00236(13)
O1 0.0791(16) 0.0944(17) 0.0792(16) -0.0328(14) 0.0372(13) 0.0100(13)
O2 0.0443(12) 0.0915(16) 0.1143(19) -0.0065(14) 0.0457(13) 0.0063(11)
O3 0.0976(17) 0.0659(14) 0.0854(16) 0.0348(13) 0.0446(14) 0.0185(13)
O4 0.0501(13) 0.120(2) 0.1107(19) -0.0370(16) 0.0430(13) -0.0405(13)
O5 0.0617(13) 0.1061(17) 0.0413(12) 0.0058(11) 0.0195(10) -0.0198(12)
O6 0.0851(16) 0.0597(13) 0.0889(16) -0.0121(12) 0.0475(13) 0.0159(12)
O7 0.0788(14) 0.0496(11) 0.0782(14) -0.0173(10) 0.0535(12) -0.0038(10)
O8 0.0597(13) 0.0806(14) 0.0869(15) 0.0010(11) 0.0526(12) -0.0158(11)
O9 0.1068(18) 0.0919(16) 0.0656(14) 0.0292(12) 0.0625(14) 0.0253(13)
O10 0.0468(11) 0.0492(11) 0.0859(15) -0.0040(10) 0.0168(11) -0.0125(9)
O11 0.0817(14) 0.0526(11) 0.0612(13) 0.0210(10) 0.0342(11) 0.0093(10)
O12 0.0783(14) 0.0787(14) 0.0832(15) -0.0113(12) 0.0595(13) 0.0120(11)
P1 0.0256(3) 0.0339(3) 0.0295(3) -0.0029(2) 0.0149(2) -0.0025(2)
S1 0.0300(3) 0.0402(3) 0.0316(3) 0.0019(2) 0.0146(2) -0.0037(2)
S2 0.0268(3) 0.0383(3) 0.0394(3) 0.0044(2) 0.0184(2) 0.0015(2)
S3 0.0366(3) 0.0393(3) 0.0336(3) 0.0006(2) 0.0190(3) -0.0004(2)
_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 1.133(3) . ?
C1 Fe1 1.815(3) . ?
C2 O2 1.135(3) . ?
C2 Fe1 1.787(3) . ?
C3 O3 1.135(3) . ?
C3 Fe1 1.803(3) . ?
C4 O4 1.140(3) . ?
C4 Fe2 1.773(3) . ?
C5 O5 1.129(3) . ?
C5 Fe2 1.808(3) . ?
C6 O6 1.134(3) . ?
C6 Fe2 1.808(3) . ?
C7 O7 1.139(3) . ?
C7 Fe3 1.802(3) . ?
C8 O8 1.136(3) . ?
C8 Fe3 1.794(3) . ?
C9 O9 1.140(3) . ?
C9 Fe3 1.792(3) . ?
C10 O10 1.139(3) . ?
C10 Fe4 1.784(3) . ?
C11 O11 1.138(3) . ?
C11 Fe4 1.793(3) . ?
C12 O12 1.133(3) . ?
C12 Fe4 1.806(3) . ?
C13 S2 1.809(2) . ?
C13 P1 1.815(2) . ?
C13 Fe3 2.058(2) . ?
C13 Fe4 2.061(2) . ?
C14 C19 1.374(3) . ?
C14 C15 1.384(3) . ?
C14 P1 1.823(2) . ?
C15 C16 1.380(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.360(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.368(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.384(3) . ?
C20 C25 1.386(3) . ?
C20 P1 1.833(2) . ?
C21 C22 1.386(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.362(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.369(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.383(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.379(3) . ?
C26 C31 1.383(3) . ?
C26 S3 1.781(2) . ?
C27 C28 1.384(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.362(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.372(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.383(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
Fe1 S2 2.2384(6) . ?
Fe1 S1 2.2626(7) . ?
Fe1 Fe2 2.5225(5) . ?
Fe2 S2 2.2415(7) . ?
Fe2 S1 2.2637(6) . ?
Fe3 S3 2.2510(7) . ?
Fe3 Fe4 2.4686(4) . ?
Fe4 S3 2.2419(6) . ?
P1 S1 2.1140(8) . ?
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 Fe1 177.0(3) . . ?
O2 C2 Fe1 177.1(2) . . ?
O3 C3 Fe1 178.2(3) . . ?
O4 C4 Fe2 178.7(3) . . ?
O5 C5 Fe2 178.1(2) . . ?
O6 C6 Fe2 175.5(2) . . ?
O7 C7 Fe3 175.6(2) . . ?
O8 C8 Fe3 175.2(2) . . ?
O9 C9 Fe3 176.7(3) . . ?
O10 C10 Fe4 178.4(2) . . ?
O11 C11 Fe4 177.7(2) . . ?
O12 C12 Fe4 174.7(2) . . ?
S2 C13 P1 106.19(11) . . ?
S2 C13 Fe3 111.38(10) . . ?
P1 C13 Fe3 125.15(11) . . ?
S2 C13 Fe4 115.84(10) . . ?
P1 C13 Fe4 122.17(10) . . ?
Fe3 C13 Fe4 73.65(7) . . ?
C19 C14 C15 118.9(2) . . ?
C19 C14 P1 120.57(17) . . ?
C15 C14 P1 120.40(17) . . ?
C16 C15 C14 119.8(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.8(2) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 120.7(2) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C21 C20 C25 118.3(2) . . ?
C21 C20 P1 121.72(17) . . ?
C25 C20 P1 118.99(18) . . ?
C20 C21 C22 120.7(2) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.1(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.1(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 120.4(2) . . ?
C24 C25 H25 119.8 . . ?
C20 C25 H25 119.8 . . ?
C27 C26 C31 119.9(2) . . ?
C27 C26 S3 120.5(2) . . ?
C31 C26 S3 119.09(19) . . ?
C26 C27 C28 119.3(3) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C31 119.8(3) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C26 C31 C30 120.0(3) . . ?
C26 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C2 Fe1 C3 93.29(12) . . ?
C2 Fe1 C1 97.48(12) . . ?
C3 Fe1 C1 96.79(13) . . ?
C2 Fe1 S2 87.03(9) . . ?
C3 Fe1 S2 158.44(9) . . ?
C1 Fe1 S2 104.55(9) . . ?
C2 Fe1 S1 154.15(9) . . ?
C3 Fe1 S1 89.76(9) . . ?
C1 Fe1 S1 107.65(9) . . ?
S2 Fe1 S1 80.98(2) . . ?
C2 Fe1 Fe2 98.25(9) . . ?
C3 Fe1 Fe2 102.95(9) . . ?
C1 Fe1 Fe2 153.90(8) . . ?
S2 Fe1 Fe2 55.790(19) . . ?
S1 Fe1 Fe2 56.150(17) . . ?
C4 Fe2 C5 91.82(12) . . ?
C4 Fe2 C6 94.99(12) . . ?
C5 Fe2 C6 95.86(12) . . ?
C4 Fe2 S2 89.12(9) . . ?
C5 Fe2 S2 160.50(9) . . ?
C6 Fe2 S2 103.46(8) . . ?
C4 Fe2 S1 154.34(9) . . ?
C5 Fe2 S1 90.07(8) . . ?
C6 Fe2 S1 110.28(8) . . ?
S2 Fe2 S1 80.89(2) . . ?
C4 Fe2 Fe1 98.83(9) . . ?
C5 Fe2 Fe1 105.00(8) . . ?
C6 Fe2 Fe1 154.48(8) . . ?
S2 Fe2 Fe1 55.674(17) . . ?
S1 Fe2 Fe1 56.111(18) . . ?
C9 Fe3 C8 87.68(12) . . ?
C9 Fe3 C7 99.69(11) . . ?
C8 Fe3 C7 97.36(11) . . ?
C9 Fe3 C13 155.65(10) . . ?
C8 Fe3 C13 94.46(10) . . ?
C7 Fe3 C13 104.06(9) . . ?
C9 Fe3 S3 93.41(8) . . ?
C8 Fe3 S3 152.73(8) . . ?
C7 Fe3 S3 109.26(8) . . ?
C13 Fe3 S3 73.84(6) . . ?
C9 Fe3 Fe4 102.41(8) . . ?
C8 Fe3 Fe4 96.65(8) . . ?
C7 Fe3 Fe4 154.21(8) . . ?
C13 Fe3 Fe4 53.24(6) . . ?
S3 Fe3 Fe4 56.494(17) . . ?
C10 Fe4 C11 90.75(11) . . ?
C10 Fe4 C12 96.46(11) . . ?
C11 Fe4 C12 98.17(11) . . ?
C10 Fe4 C13 93.12(9) . . ?
C11 Fe4 C13 149.48(10) . . ?
C12 Fe4 C13 111.42(10) . . ?
C10 Fe4 S3 160.40(8) . . ?
C11 Fe4 S3 93.25(8) . . ?
C12 Fe4 S3 101.93(8) . . ?
C13 Fe4 S3 73.97(6) . . ?
C10 Fe4 Fe3 103.64(8) . . ?
C11 Fe4 Fe3 96.59(8) . . ?
C12 Fe4 Fe3 154.82(8) . . ?
C13 Fe4 Fe3 53.12(6) . . ?
S3 Fe4 Fe3 56.849(19) . . ?
C13 P1 C14 119.77(10) . . ?
C13 P1 C20 120.93(10) . . ?
C14 P1 C20 102.60(10) . . ?
C13 P1 S1 105.29(7) . . ?
C14 P1 S1 102.08(7) . . ?
C20 P1 S1 103.55(8) . . ?
P1 S1 Fe1 100.07(3) . . ?
P1 S1 Fe2 106.40(3) . . ?
Fe1 S1 Fe2 67.74(2) . . ?
C13 S2 Fe1 113.83(7) . . ?
C13 S2 Fe2 111.32(7) . . ?
Fe1 S2 Fe2 68.54(2) . . ?
C26 S3 Fe4 119.19(8) . . ?
C26 S3 Fe3 118.70(8) . . ?
Fe4 S3 Fe3 66.66(2) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 27.54
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.281
_refine_diff_density_min -0.353
_refine_diff_density_rms 0.070
data_2
_database_code_depnum_ccdc_archive 'CCDC 912952'
#TrackingRef 'ChemComm1-2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H15 Fe4 O14 P S3'
_chemical_formula_sum 'C28 H15 Fe4 O14 P S3'
_chemical_formula_weight 925.98
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'
S S 0.1246 0.1234 '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/c'
_space_group_name_Hall '-P 2ybc'
_space_group_IT_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.0883(9)
_cell_length_b 13.9167(13)
_cell_length_c 25.9381(14)
_cell_angle_alpha 90.00
_cell_angle_beta 102.271(3)
_cell_angle_gamma 90.00
_cell_volume 3558.4(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 296
_cell_measurement_reflns_used 6008
_cell_measurement_theta_min 1.61
_cell_measurement_theta_max 27.52
_exptl_crystal_description Prism
_exptl_crystal_colour Red
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.729
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1848
_exptl_absorpt_coefficient_mu 1.883
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.701
_exptl_absorpt_correction_T_max 0.752
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296
_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 SMART APEX CCD'
_diffrn_measurement_method '\w and \f'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 30961
_diffrn_reflns_av_R_equivalents 0.0461
_diffrn_reflns_av_sigmaI/netI 0.0435
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_theta_min 1.61
_diffrn_reflns_theta_max 27.52
_reflns_number_total 8149
_reflns_number_gt 6008
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'SMART (Bruker, 2002)'
_computing_cell_refinement 'SAINT-Plus (Bruker, 2003)'
_computing_data_reduction 'SAINT-Plus (Bruker, 2003)'
_computing_structure_solution 'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009);WinGX (Farrugia, 1999)'
_computing_publication_material 'publCIF (Westrip, 2010)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0350P)^2^+1.4860P] where P=(Fo^2^+2Fc^2^)/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 8149
_refine_ls_number_parameters 452
_refine_ls_number_restraints 7
_refine_ls_R_factor_all 0.0571
_refine_ls_R_factor_gt 0.0357
_refine_ls_wR_factor_ref 0.0889
_refine_ls_wR_factor_gt 0.0786
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0117(3) 0.8292(2) 0.95156(12) 0.0418(7) Uani 1 1 d . . .
C2 C 0.9683(3) 0.8214(3) 1.05074(13) 0.0490(8) Uani 1 1 d . . .
C3 C 1.0815(4) 0.6765(3) 1.01836(14) 0.0527(9) Uani 1 1 d . . .
C4 C 0.7274(4) 0.7131(3) 1.07229(14) 0.0581(10) Uani 1 1 d . . .
C5 C 0.8074(3) 0.5502(2) 1.04495(12) 0.0447(7) Uani 1 1 d . . .
C6 C 0.5581(3) 0.6226(2) 0.99438(12) 0.0429(7) Uani 1 1 d . . .
C7 C 0.7915(3) 0.9304(2) 0.83528(13) 0.0481(8) Uani 1 1 d . . .
C8 C 0.7470(3) 0.9911(2) 0.92946(13) 0.0451(8) Uani 1 1 d . . .
C9 C 0.5942(4) 1.0530(2) 0.84852(15) 0.0562(9) Uani 1 1 d . . .
C10 C 0.4582(3) 0.8822(3) 0.96370(15) 0.0595(10) Uani 1 1 d . . .
C11 C 0.3308(4) 0.9581(3) 0.88080(16) 0.0603(10) Uani 1 1 d . . .
C12 C 0.3283(3) 0.7660(2) 0.89388(13) 0.0427(7) Uani 1 1 d . . .
C13 C 0.6418(3) 0.80445(19) 0.90620(10) 0.0288(6) Uani 1 1 d . . .
C14 C 0.5573(3) 0.59811(19) 0.86097(10) 0.0315(6) Uani 1 1 d . . .
C15 C 0.4383(3) 0.6162(2) 0.82414(12) 0.0401(7) Uani 1 1 d . . .
H15 H 0.4195 0.6780 0.8110 0.048 Uiso 1 1 calc R . .
C16 C 0.3474(3) 0.5422(2) 0.80681(13) 0.0490(8) Uani 1 1 d . . .
H16 H 0.2681 0.5549 0.7821 0.059 Uiso 1 1 calc R . .
C17 C 0.3734(4) 0.4505(2) 0.82577(14) 0.0540(9) Uani 1 1 d . . .
H17 H 0.3119 0.4012 0.8142 0.065 Uiso 1 1 calc R . .
C18 C 0.4912(4) 0.4323(2) 0.86202(14) 0.0561(9) Uani 1 1 d . . .
H18 H 0.5092 0.3702 0.8749 0.067 Uiso 1 1 calc R . .
C19 C 0.5834(3) 0.5048(2) 0.87963(12) 0.0439(7) Uani 1 1 d . . .
H19 H 0.6631 0.4912 0.9040 0.053 Uiso 1 1 calc R . .
C20 C 0.7746(3) 0.69405(19) 0.82533(10) 0.0320(6) Uani 1 1 d . . .
C21 C 0.7001(3) 0.6907(2) 0.77359(11) 0.0389(7) Uani 1 1 d . . .
H21 H 0.6058 0.6911 0.7669 0.047 Uiso 1 1 calc R . .
C22 C 0.7663(4) 0.6867(2) 0.73212(12) 0.0496(8) Uani 1 1 d . . .
H22 H 0.7161 0.6840 0.6977 0.059 Uiso 1 1 calc R . .
C23 C 0.9055(4) 0.6867(3) 0.74124(14) 0.0609(10) Uani 1 1 d . . .
H23 H 0.9492 0.6840 0.7131 0.073 Uiso 1 1 calc R . .
C24 C 0.9805(4) 0.6907(3) 0.79250(14) 0.0636(10) Uani 1 1 d . . .
H24 H 1.0748 0.6912 0.7988 0.076 Uiso 1 1 calc R . .
C25 C 0.9156(3) 0.6940(3) 0.83455(12) 0.0471(8) Uani 1 1 d . . .
H25 H 0.9663 0.6962 0.8689 0.057 Uiso 1 1 calc R . .
C26 C 0.3828(3) 0.9356(2) 0.76584(12) 0.0466(8) Uani 1 1 d . . .
H26A H 0.3571 0.9915 0.7838 0.056 Uiso 1 1 calc R . .
H26B H 0.4324 0.9577 0.7399 0.056 Uiso 1 1 calc R . .
C27 C 0.2579(4) 0.8835(3) 0.73857(14) 0.0552(9) Uani 1 1 d . . .
C28 C 0.0498(5) 0.9054(4) 0.6792(2) 0.1154(12) Uani 1 1 d U . .
H28A H 0.0664 0.8551 0.6561 0.173 Uiso 1 1 calc R . .
H28B H -0.0019 0.9556 0.6589 0.173 Uiso 1 1 calc R . .
H28C H -0.0001 0.8800 0.7038 0.173 Uiso 1 1 calc R . .
Fe1 Fe 0.93465(4) 0.74971(3) 0.992250(15) 0.03317(11) Uani 1 1 d . . .
Fe2 Fe 0.73451(4) 0.65836(3) 1.011479(15) 0.03329(11) Uani 1 1 d . . .
Fe3 Fe 0.65452(4) 0.93593(3) 0.870598(16) 0.03452(11) Uani 1 1 d . . .
Fe4 Fe 0.44942(4) 0.86124(3) 0.895248(17) 0.03495(11) Uani 1 1 d . . .
O1 O 1.0603(2) 0.87986(19) 0.92681(10) 0.0619(7) Uani 1 1 d . . .
O2 O 0.9904(3) 0.8650(2) 1.08916(10) 0.0824(9) Uani 1 1 d . . .
O3 O 1.1751(3) 0.6334(2) 1.03696(12) 0.0912(10) Uani 1 1 d . . .
O4 O 0.7224(4) 0.7492(2) 1.11140(11) 0.1100(13) Uani 1 1 d . . .
O5 O 0.8557(3) 0.48441(19) 1.06721(10) 0.0716(8) Uani 1 1 d . . .
O6 O 0.4460(2) 0.6032(2) 0.98553(11) 0.0683(7) Uani 1 1 d . . .
O7 O 0.8742(3) 0.9334(2) 0.81168(11) 0.0780(8) Uani 1 1 d . . .
O8 O 0.8077(3) 1.03090(18) 0.96551(10) 0.0680(7) Uani 1 1 d . . .
O9 O 0.5563(3) 1.12832(19) 0.83546(14) 0.0969(11) Uani 1 1 d . . .
O10 O 0.4523(3) 0.8932(3) 1.00704(12) 0.1064(12) Uani 1 1 d . . .
O11 O 0.2562(3) 1.0204(2) 0.87197(15) 0.1080(12) Uani 1 1 d . . .
O12 O 0.2461(2) 0.70998(19) 0.89516(11) 0.0691(7) Uani 1 1 d . . .
O13 O 0.2326(3) 0.8010(2) 0.74397(13) 0.0967(11) Uani 1 1 d . . .
O14 O 0.1771(3) 0.9435(2) 0.70758(14) 0.1113(11) Uani 1 1 d U . .
P1 P 0.68829(7) 0.69135(5) 0.88036(3) 0.02722(15) Uani 1 1 d . . .
S1 S 0.83126(7) 0.62658(5) 0.94189(3) 0.03189(16) Uani 1 1 d . . .
S2 S 0.72220(7) 0.80511(5) 0.97588(3) 0.03154(15) Uani 1 1 d . . .
S3 S 0.49190(7) 0.85831(5) 0.81351(3) 0.03647(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0369(17) 0.0450(18) 0.0434(18) -0.0048(14) 0.0080(14) -0.0012(14)
C2 0.0391(18) 0.063(2) 0.0431(19) -0.0051(16) 0.0044(15) -0.0131(16)
C3 0.045(2) 0.053(2) 0.053(2) -0.0003(16) -0.0038(16) -0.0005(16)
C4 0.083(3) 0.053(2) 0.044(2) -0.0004(16) 0.0252(19) -0.0225(19)
C5 0.0455(19) 0.0479(19) 0.0379(17) 0.0029(15) 0.0021(14) -0.0098(15)
C6 0.0458(19) 0.0405(17) 0.0426(18) 0.0046(14) 0.0101(15) -0.0023(14)
C7 0.0411(18) 0.051(2) 0.052(2) 0.0098(16) 0.0096(16) -0.0027(15)
C8 0.0437(18) 0.0365(17) 0.057(2) 0.0011(15) 0.0147(16) -0.0097(14)
C9 0.048(2) 0.041(2) 0.073(2) 0.0021(17) -0.0020(18) -0.0067(16)
C10 0.0392(19) 0.079(3) 0.063(2) -0.012(2) 0.0180(17) 0.0086(18)
C11 0.057(2) 0.048(2) 0.086(3) 0.0157(19) 0.037(2) 0.0125(18)
C12 0.0323(16) 0.0442(18) 0.0514(19) 0.0017(15) 0.0084(14) 0.0070(14)
C13 0.0265(13) 0.0293(14) 0.0303(14) 0.0010(11) 0.0057(11) -0.0013(11)
C14 0.0321(15) 0.0317(14) 0.0315(14) -0.0048(11) 0.0088(12) -0.0062(12)
C15 0.0344(16) 0.0362(16) 0.0475(18) -0.0037(13) 0.0038(14) -0.0040(13)
C16 0.0352(17) 0.054(2) 0.054(2) -0.0096(16) 0.0004(15) -0.0088(15)
C17 0.052(2) 0.047(2) 0.062(2) -0.0103(17) 0.0106(18) -0.0217(16)
C18 0.066(2) 0.0377(18) 0.063(2) 0.0031(16) 0.0094(19) -0.0114(16)
C19 0.0453(18) 0.0405(17) 0.0429(18) 0.0018(14) 0.0026(14) -0.0048(14)
C20 0.0369(15) 0.0313(14) 0.0291(14) -0.0015(11) 0.0101(12) -0.0038(12)
C21 0.0442(17) 0.0415(17) 0.0307(15) 0.0032(13) 0.0072(13) -0.0043(14)
C22 0.066(2) 0.055(2) 0.0283(16) -0.0007(14) 0.0110(15) -0.0056(17)
C23 0.071(3) 0.078(3) 0.042(2) -0.0064(18) 0.0331(19) -0.008(2)
C24 0.045(2) 0.097(3) 0.056(2) -0.010(2) 0.0256(18) -0.007(2)
C25 0.0376(17) 0.071(2) 0.0346(17) -0.0087(15) 0.0114(14) -0.0058(16)
C26 0.0440(18) 0.0451(18) 0.0466(19) 0.0128(15) 0.0003(15) -0.0008(15)
C27 0.045(2) 0.062(2) 0.052(2) 0.0115(18) -0.0040(16) -0.0053(17)
C28 0.0784(19) 0.104(2) 0.129(2) 0.0418(19) -0.0557(17) -0.0146(17)
Fe1 0.0296(2) 0.0377(2) 0.0302(2) -0.00153(17) 0.00175(17) -0.00427(17)
Fe2 0.0370(2) 0.0363(2) 0.0265(2) 0.00016(17) 0.00654(17) -0.00629(17)
Fe3 0.0297(2) 0.0311(2) 0.0423(2) 0.00371(18) 0.00681(18) -0.00233(17)
Fe4 0.0272(2) 0.0331(2) 0.0459(3) 0.00039(18) 0.01086(18) 0.00176(17)
O1 0.0572(15) 0.0697(17) 0.0626(16) 0.0085(13) 0.0216(13) -0.0160(13)
O2 0.085(2) 0.106(2) 0.0552(17) -0.0394(16) 0.0130(15) -0.0325(18)
O3 0.0690(19) 0.095(2) 0.093(2) 0.0049(18) -0.0209(17) 0.0323(17)
O4 0.199(4) 0.094(2) 0.0545(17) -0.0342(17) 0.068(2) -0.055(2)
O5 0.0737(18) 0.0627(17) 0.0686(17) 0.0241(14) -0.0067(14) 0.0020(14)
O6 0.0398(14) 0.0762(18) 0.087(2) 0.0145(15) 0.0093(13) -0.0087(13)
O7 0.0660(17) 0.095(2) 0.087(2) 0.0149(16) 0.0469(16) 0.0004(15)
O8 0.0729(18) 0.0606(16) 0.0657(17) -0.0151(14) 0.0038(14) -0.0281(14)
O9 0.091(2) 0.0405(16) 0.144(3) 0.0247(17) -0.011(2) 0.0061(15)
O10 0.081(2) 0.184(4) 0.0604(19) -0.028(2) 0.0291(17) 0.029(2)
O11 0.103(2) 0.081(2) 0.160(3) 0.052(2) 0.073(2) 0.0585(19)
O12 0.0429(14) 0.0635(16) 0.104(2) 0.0035(15) 0.0239(14) -0.0156(13)
O13 0.075(2) 0.070(2) 0.121(3) 0.0249(19) -0.0328(18) -0.0219(16)
O14 0.0750(18) 0.100(2) 0.125(2) 0.0437(18) -0.0550(16) -0.0146(15)
P1 0.0258(3) 0.0301(4) 0.0253(3) -0.0014(3) 0.0045(3) -0.0017(3)
S1 0.0324(4) 0.0334(4) 0.0279(3) -0.0020(3) 0.0020(3) 0.0030(3)
S2 0.0333(4) 0.0319(4) 0.0295(4) -0.0042(3) 0.0071(3) -0.0015(3)
S3 0.0330(4) 0.0345(4) 0.0401(4) 0.0038(3) 0.0037(3) 0.0013(3)
_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 1.133(4) . ?
C1 Fe1 1.814(3) . ?
C2 O2 1.147(4) . ?
C2 Fe1 1.787(3) . ?
C3 O3 1.136(4) . ?
C3 Fe1 1.807(4) . ?
C4 O4 1.143(4) . ?
C4 Fe2 1.767(4) . ?
C5 O5 1.136(4) . ?
C5 Fe2 1.814(3) . ?
C6 O6 1.137(4) . ?
C6 Fe2 1.810(3) . ?
C7 O7 1.135(4) . ?
C7 Fe3 1.814(3) . ?
C8 O8 1.146(4) . ?
C8 Fe3 1.785(3) . ?
C9 O9 1.143(4) . ?
C9 Fe3 1.790(4) . ?
C10 O10 1.149(4) . ?
C10 Fe4 1.783(4) . ?
C11 O11 1.140(4) . ?
C11 Fe4 1.788(4) . ?
C12 O12 1.144(4) . ?
C12 Fe4 1.798(3) . ?
C13 P1 1.811(3) . ?
C13 S2 1.817(3) . ?
C13 Fe4 2.058(3) . ?
C13 Fe3 2.066(3) . ?
C14 C15 1.389(4) . ?
C14 C19 1.392(4) . ?
C14 P1 1.844(3) . ?
C15 C16 1.389(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.373(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.383(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C25 1.391(4) . ?
C20 C21 1.393(4) . ?
C20 P1 1.824(3) . ?
C21 C22 1.383(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.373(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.384(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.495(4) . ?
C26 S3 1.822(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 O13 1.190(4) . ?
C27 O14 1.316(4) . ?
C28 O14 1.439(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Fe1 S2 2.2319(8) . ?
Fe1 S1 2.2696(8) . ?
Fe1 Fe2 2.5238(6) . ?
Fe2 S2 2.2339(8) . ?
Fe2 S1 2.2705(8) . ?
Fe3 S3 2.2402(8) . ?
Fe3 Fe4 2.5166(6) . ?
Fe4 S3 2.2509(9) . ?
P1 S1 2.1122(10) . ?
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 Fe1 178.9(3) . . ?
O2 C2 Fe1 178.0(3) . . ?
O3 C3 Fe1 176.5(3) . . ?
O4 C4 Fe2 179.4(4) . . ?
O5 C5 Fe2 177.6(3) . . ?
O6 C6 Fe2 176.5(3) . . ?
O7 C7 Fe3 175.0(3) . . ?
O8 C8 Fe3 176.1(3) . . ?
O9 C9 Fe3 178.6(4) . . ?
O10 C10 Fe4 174.1(3) . . ?
O11 C11 Fe4 179.2(5) . . ?
O12 C12 Fe4 174.7(3) . . ?
P1 C13 S2 106.04(13) . . ?
P1 C13 Fe4 126.41(14) . . ?
S2 C13 Fe4 110.12(13) . . ?
P1 C13 Fe3 123.96(13) . . ?
S2 C13 Fe3 112.52(13) . . ?
Fe4 C13 Fe3 75.21(9) . . ?
C15 C14 C19 118.7(3) . . ?
C15 C14 P1 121.6(2) . . ?
C19 C14 P1 119.3(2) . . ?
C14 C15 C16 120.2(3) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.7(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 119.2(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 121.0(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C14 120.1(3) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
C25 C20 C21 119.3(3) . . ?
C25 C20 P1 120.4(2) . . ?
C21 C20 P1 120.2(2) . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 120.8(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 119.7(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 120.1(3) . . ?
C24 C25 H25 120.0 . . ?
C20 C25 H25 120.0 . . ?
C27 C26 S3 111.2(2) . . ?
C27 C26 H26A 109.4 . . ?
S3 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
S3 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
O13 C27 O14 124.3(3) . . ?
O13 C27 C26 126.3(3) . . ?
O14 C27 C26 109.4(3) . . ?
O14 C28 H28A 109.5 . . ?
O14 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O14 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 Fe1 C3 90.21(16) . . ?
C2 Fe1 C1 97.22(15) . . ?
C3 Fe1 C1 98.23(15) . . ?
C2 Fe1 S2 88.30(11) . . ?
C3 Fe1 S2 160.71(12) . . ?
C1 Fe1 S2 101.04(10) . . ?
C2 Fe1 S1 153.04(11) . . ?
C3 Fe1 S1 91.73(11) . . ?
C1 Fe1 S1 109.08(10) . . ?
S2 Fe1 S1 81.14(3) . . ?
C2 Fe1 Fe2 97.43(10) . . ?
C3 Fe1 Fe2 105.59(12) . . ?
C1 Fe1 Fe2 151.87(10) . . ?
S2 Fe1 Fe2 55.63(2) . . ?
S1 Fe1 Fe2 56.24(2) . . ?
C4 Fe2 C6 96.49(16) . . ?
C4 Fe2 C5 91.13(16) . . ?
C6 Fe2 C5 99.59(14) . . ?
C4 Fe2 S2 88.04(12) . . ?
C6 Fe2 S2 100.66(10) . . ?
C5 Fe2 S2 159.70(10) . . ?
C4 Fe2 S1 154.12(12) . . ?
C6 Fe2 S1 108.54(10) . . ?
C5 Fe2 S1 91.13(10) . . ?
S2 Fe2 S1 81.08(3) . . ?
C4 Fe2 Fe1 98.36(11) . . ?
C6 Fe2 Fe1 151.21(10) . . ?
C5 Fe2 Fe1 104.62(10) . . ?
S2 Fe2 Fe1 55.55(2) . . ?
S1 Fe2 Fe1 56.21(2) . . ?
C8 Fe3 C9 87.84(15) . . ?
C8 Fe3 C7 97.73(15) . . ?
C9 Fe3 C7 96.93(16) . . ?
C8 Fe3 C13 94.01(12) . . ?
C9 Fe3 C13 154.12(14) . . ?
C7 Fe3 C13 108.35(13) . . ?
C8 Fe3 S3 161.65(10) . . ?
C9 Fe3 S3 94.34(11) . . ?
C7 Fe3 S3 100.09(11) . . ?
C13 Fe3 S3 76.23(8) . . ?
C8 Fe3 Fe4 105.60(10) . . ?
C9 Fe3 Fe4 102.42(12) . . ?
C7 Fe3 Fe4 150.03(11) . . ?
C13 Fe3 Fe4 52.26(7) . . ?
S3 Fe3 Fe4 56.12(2) . . ?
C10 Fe4 C11 88.54(17) . . ?
C10 Fe4 C12 91.72(16) . . ?
C11 Fe4 C12 97.46(15) . . ?
C10 Fe4 C13 94.57(13) . . ?
C11 Fe4 C13 152.56(14) . . ?
C12 Fe4 C13 109.66(12) . . ?
C10 Fe4 S3 164.13(12) . . ?
C11 Fe4 S3 93.97(12) . . ?
C12 Fe4 S3 103.46(10) . . ?
C13 Fe4 S3 76.14(7) . . ?
C10 Fe4 Fe3 108.42(12) . . ?
C11 Fe4 Fe3 100.67(11) . . ?
C12 Fe4 Fe3 153.06(10) . . ?
C13 Fe4 Fe3 52.53(7) . . ?
S3 Fe4 Fe3 55.72(2) . . ?
C27 O14 C28 116.6(3) . . ?
C13 P1 C20 118.44(12) . . ?
C13 P1 C14 119.03(12) . . ?
C20 P1 C14 103.59(12) . . ?
C13 P1 S1 106.28(9) . . ?
C20 P1 S1 103.72(9) . . ?
C14 P1 S1 103.91(9) . . ?
P1 S1 Fe1 105.61(4) . . ?
P1 S1 Fe2 100.24(3) . . ?
Fe1 S1 Fe2 67.54(2) . . ?
C13 S2 Fe1 113.29(9) . . ?
C13 S2 Fe2 112.36(9) . . ?
Fe1 S2 Fe2 68.82(3) . . ?
C26 S3 Fe3 114.57(11) . . ?
C26 S3 Fe4 114.84(11) . . ?
Fe3 S3 Fe4 68.16(3) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 27.52
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.532
_refine_diff_density_min -0.891
_refine_diff_density_rms 0.074
data_3
_database_code_depnum_ccdc_archive 'CCDC 917815'
#TrackingRef 'ChemComm3.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C11 H8 Fe2 O8 S3'
_chemical_formula_sum 'C11 H8 Fe2 O8 S3'
_chemical_formula_weight 476.08
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_space_group_name_Hall '-P 1'
_space_group_IT_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.9461(11)
_cell_length_b 8.1411(12)
_cell_length_c 14.798(2)
_cell_angle_alpha 98.041(2)
_cell_angle_beta 101.942(2)
_cell_angle_gamma 104.491(3)
_cell_volume 888.0(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 296
_cell_measurement_reflns_used 3509
_cell_measurement_theta_min 2.64
_cell_measurement_theta_max 27.35
_exptl_crystal_description Block
_exptl_crystal_colour Red
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.781
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 476
_exptl_absorpt_coefficient_mu 2.020
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.746
_exptl_absorpt_correction_T_max 0.811
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296
_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 SMART APEX CCD'
_diffrn_measurement_method '\w and \f'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 7707
_diffrn_reflns_av_R_equivalents 0.0282
_diffrn_reflns_av_sigmaI/netI 0.0369
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.64
_diffrn_reflns_theta_max 27.35
_reflns_number_total 3932
_reflns_number_gt 3509
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'SMART (Bruker, 2002)'
_computing_cell_refinement 'SAINT-Plus (Bruker, 2003)'
_computing_data_reduction 'SAINT-Plus (Bruker, 2003)'
_computing_structure_solution 'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009);WinGX (Farrugia, 1999)'
_computing_publication_material 'publCIF (Westrip, 2010)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0386P)^2^+0.3992P] where P=(Fo^2^+2Fc^2^)/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 3932
_refine_ls_number_parameters 219
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0331
_refine_ls_R_factor_gt 0.0287
_refine_ls_wR_factor_ref 0.0823
_refine_ls_wR_factor_gt 0.0787
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_restrained_S_all 1.025
_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 0.7622(5) 0.7802(3) 0.35962(19) 0.0575(7) Uani 1 1 d . . .
C2 C 0.4720(4) 0.5059(4) 0.2407(2) 0.0526(6) Uani 1 1 d . . .
C3 C 0.6782(4) 0.7376(3) 0.17696(18) 0.0475(5) Uani 1 1 d . . .
C4 C 0.5361(4) 0.2002(4) 0.10985(19) 0.0523(6) Uani 1 1 d . . .
C5 C 0.7336(4) 0.4450(3) 0.04989(18) 0.0512(6) Uani 1 1 d . . .
C6 C 0.8905(4) 0.2104(3) 0.10643(18) 0.0499(6) Uani 1 1 d . . .
C7 C 0.7367(3) 0.4311(3) 0.34396(15) 0.0351(4) Uani 1 1 d . . .
C8 C 0.7329(5) 0.2711(4) 0.5003(2) 0.0689(8) Uani 1 1 d . . .
H8A H 0.6457 0.1710 0.4589 0.103 Uiso 1 1 calc R . .
H8B H 0.7122 0.2802 0.5623 0.103 Uiso 1 1 calc R . .
H8C H 0.8514 0.2602 0.5034 0.103 Uiso 1 1 calc R . .
C9 C 1.0835(3) 0.7339(3) 0.17871(18) 0.0498(6) Uani 1 1 d . . .
H9A H 1.1502 0.6828 0.1405 0.060 Uiso 1 1 calc R . .
H9B H 0.9934 0.7697 0.1377 0.060 Uiso 1 1 calc R . .
C10 C 1.2084(4) 0.8867(3) 0.2522(2) 0.0529(6) Uani 1 1 d . . .
C11 C 1.2231(6) 1.1418(5) 0.3544(3) 0.0915(12) Uani 1 1 d . . .
H11A H 1.2421 1.1012 0.4125 0.137 Uiso 1 1 calc R . .
H11B H 1.1571 1.2253 0.3586 0.137 Uiso 1 1 calc R . .
H11C H 1.3370 1.1946 0.3430 0.137 Uiso 1 1 calc R . .
Fe1 Fe 0.70982(4) 0.59957(4) 0.26254(2) 0.03406(10) Uani 1 1 d . . .
Fe2 Fe 0.76157(4) 0.34682(4) 0.15064(2) 0.03644(10) Uani 1 1 d . . .
O1 O 0.7970(5) 0.8957(3) 0.41948(17) 0.1002(10) Uani 1 1 d . . .
O2 O 0.3216(3) 0.4428(4) 0.2266(2) 0.0837(7) Uani 1 1 d . . .
O3 O 0.6540(3) 0.8261(3) 0.12612(16) 0.0734(6) Uani 1 1 d . . .
O4 O 0.3963(3) 0.1068(3) 0.08579(18) 0.0843(7) Uani 1 1 d . . .
O5 O 0.7185(4) 0.5066(3) -0.01466(15) 0.0793(7) Uani 1 1 d . . .
O6 O 0.9721(3) 0.1299(3) 0.07799(18) 0.0817(7) Uani 1 1 d . . .
O7 O 1.3636(3) 0.9030(3) 0.2858(2) 0.0975(9) Uani 1 1 d . . .
O8 O 1.1220(3) 0.9971(3) 0.27760(16) 0.0652(5) Uani 1 1 d . . .
S1 S 0.77509(9) 0.25345(7) 0.29205(4) 0.04266(14) Uani 1 1 d . . .
S2 S 0.71289(10) 0.46301(8) 0.45595(4) 0.05125(17) Uani 1 1 d . . .
S3 S 0.97697(7) 0.57715(7) 0.24279(4) 0.03642(13) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.092(2) 0.0459(14) 0.0453(14) 0.0126(11) 0.0216(14) 0.0335(14)
C2 0.0479(14) 0.0658(16) 0.0622(16) 0.0302(13) 0.0228(12) 0.0319(13)
C3 0.0525(14) 0.0468(13) 0.0466(13) 0.0113(11) 0.0129(11) 0.0192(11)
C4 0.0520(15) 0.0587(15) 0.0415(13) 0.0053(11) 0.0069(11) 0.0140(12)
C5 0.0573(15) 0.0547(14) 0.0343(12) 0.0008(11) 0.0070(11) 0.0112(12)
C6 0.0528(14) 0.0478(13) 0.0447(13) -0.0031(11) 0.0120(11) 0.0136(11)
C7 0.0345(10) 0.0376(10) 0.0328(10) 0.0063(8) 0.0068(8) 0.0117(8)
C8 0.100(2) 0.0657(18) 0.0449(15) 0.0281(14) 0.0158(16) 0.0244(17)
C9 0.0476(13) 0.0576(15) 0.0476(14) 0.0149(11) 0.0226(11) 0.0101(11)
C10 0.0428(13) 0.0518(14) 0.0633(17) 0.0232(12) 0.0169(12) 0.0029(11)
C11 0.097(3) 0.064(2) 0.082(3) -0.0087(18) 0.002(2) -0.0045(19)
Fe1 0.03914(18) 0.03438(17) 0.03379(17) 0.00882(12) 0.01163(13) 0.01666(13)
Fe2 0.04036(18) 0.03732(17) 0.03019(17) 0.00153(12) 0.00728(13) 0.01284(13)
O1 0.188(3) 0.0552(13) 0.0583(14) -0.0031(11) 0.0287(17) 0.0474(16)
O2 0.0412(11) 0.1120(19) 0.114(2) 0.0535(17) 0.0246(12) 0.0296(12)
O3 0.0983(17) 0.0671(13) 0.0675(14) 0.0395(11) 0.0170(12) 0.0355(12)
O4 0.0523(13) 0.0944(18) 0.0787(16) 0.0082(13) 0.0006(11) -0.0097(12)
O5 0.1095(19) 0.0851(16) 0.0391(11) 0.0207(11) 0.0099(11) 0.0234(14)
O6 0.0800(16) 0.0817(16) 0.0886(16) -0.0120(13) 0.0321(13) 0.0395(13)
O7 0.0434(12) 0.0817(17) 0.146(3) 0.0152(17) 0.0003(14) 0.0044(11)
O8 0.0552(11) 0.0573(11) 0.0676(13) -0.0029(10) 0.0048(10) 0.0059(9)
S1 0.0564(3) 0.0364(3) 0.0399(3) 0.0092(2) 0.0124(3) 0.0206(2)
S2 0.0750(4) 0.0472(3) 0.0364(3) 0.0100(2) 0.0221(3) 0.0189(3)
S3 0.0345(3) 0.0398(3) 0.0335(3) 0.0047(2) 0.0081(2) 0.0100(2)
_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 1.132(3) . ?
C1 Fe1 1.804(3) . ?
C2 O2 1.139(3) . ?
C2 Fe1 1.792(3) . ?
C3 O3 1.133(3) . ?
C3 Fe1 1.827(3) . ?
C4 O4 1.130(3) . ?
C4 Fe2 1.811(3) . ?
C5 O5 1.138(3) . ?
C5 Fe2 1.788(3) . ?
C6 O6 1.129(3) . ?
C6 Fe2 1.832(2) . ?
C7 S1 1.668(2) . ?
C7 S2 1.698(2) . ?
C7 Fe1 1.970(2) . ?
C8 S2 1.807(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.507(4) . ?
C9 S3 1.837(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O7 1.197(3) . ?
C10 O8 1.319(3) . ?
C11 O8 1.448(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Fe1 S3 2.2497(7) . ?
Fe1 Fe2 2.6262(5) . ?
Fe2 S3 2.2400(6) . ?
Fe2 S1 2.3155(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Fe1 178.5(3) . . ?
O2 C2 Fe1 178.5(3) . . ?
O3 C3 Fe1 176.9(2) . . ?
O4 C4 Fe2 178.6(3) . . ?
O5 C5 Fe2 178.7(3) . . ?
O6 C6 Fe2 178.1(3) . . ?
S1 C7 S2 123.58(13) . . ?
S1 C7 Fe1 114.44(12) . . ?
S2 C7 Fe1 121.92(11) . . ?
S2 C8 H8A 109.5 . . ?
S2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
S2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 S3 106.60(17) . . ?
C10 C9 H9A 110.4 . . ?
S3 C9 H9A 110.4 . . ?
C10 C9 H9B 110.4 . . ?
S3 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
O7 C10 O8 124.3(3) . . ?
O7 C10 C9 124.7(3) . . ?
O8 C10 C9 111.0(2) . . ?
O8 C11 H11A 109.5 . . ?
O8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2 Fe1 C1 104.11(14) . . ?
C2 Fe1 C3 91.48(12) . . ?
C1 Fe1 C3 91.35(12) . . ?
C2 Fe1 C7 86.81(10) . . ?
C1 Fe1 C7 94.41(10) . . ?
C3 Fe1 C7 174.24(10) . . ?
C2 Fe1 S3 149.37(9) . . ?
C1 Fe1 S3 105.38(11) . . ?
C3 Fe1 S3 95.90(8) . . ?
C7 Fe1 S3 82.89(6) . . ?
C2 Fe1 Fe2 95.56(9) . . ?
C1 Fe1 Fe2 158.11(10) . . ?
C3 Fe1 Fe2 97.74(8) . . ?
C7 Fe1 Fe2 76.97(6) . . ?
S3 Fe1 Fe2 54.030(16) . . ?
C5 Fe2 C4 92.23(12) . . ?
C5 Fe2 C6 94.89(12) . . ?
C4 Fe2 C6 100.85(12) . . ?
C5 Fe2 S3 94.64(9) . . ?
C4 Fe2 S3 154.81(9) . . ?
C6 Fe2 S3 102.66(8) . . ?
C5 Fe2 S1 170.14(9) . . ?
C4 Fe2 S1 87.03(9) . . ?
C6 Fe2 S1 94.91(9) . . ?
S3 Fe2 S1 82.11(2) . . ?
C5 Fe2 Fe1 94.20(8) . . ?
C4 Fe2 Fe1 100.99(9) . . ?
C6 Fe2 Fe1 155.95(8) . . ?
S3 Fe2 Fe1 54.372(18) . . ?
S1 Fe2 Fe1 76.32(2) . . ?
C10 O8 C11 116.4(3) . . ?
C7 S1 Fe2 92.25(8) . . ?
C7 S2 C8 106.61(13) . . ?
C9 S3 Fe2 114.52(9) . . ?
C9 S3 Fe1 114.27(9) . . ?
Fe2 S3 Fe1 71.60(2) . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full 27.35
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max 0.404
_refine_diff_density_min -0.299
_refine_diff_density_rms 0.068