data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Scheer, Manfred' 'Pushkarevsky, Nikolay' _publ_contact_author_name 'Scheer, Manfred' _publ_contact_author_email mascheer@chemie.uni-regensburg.de _publ_section_title ; Dimerization of pentanuclear clusters [Fe3Q(AsMe)(CO)9] (Q = Se, Te) as conversion pathway to novel cubane-like aggregates ; # Attachment '- Combined_CIF.cif' #=============================================================================== data_2a _database_code_depnum_ccdc_archive 'CCDC 802724' #TrackingRef '- Combined_CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 As2 Fe4 O12 Se2' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C14 H6 As2 Fe4 O12 Se2' _chemical_formula_sum 'C14 H6 As2 Fe4 O12 Se2' _chemical_formula_iupac ? _chemical_formula_weight 897.35 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 8.5776(2) _cell_length_b 29.8122(4) _cell_length_c 9.6766(2) _cell_angle_alpha 90 _cell_angle_beta 107.589(2) _cell_angle_gamma 90 _cell_volume 2358.79(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 8435 _cell_measurement_theta_min 2.8342 _cell_measurement_theta_max 31.8609 _cell_special_details ; ; _exptl_crystal_description 'flat prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.527 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 8.339 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.35434 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -80.00 -1.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -31.4530 77.0000 330.0000 0.0000 0.0000 79 #__ type_ start__ end____ width___ exp.time_ 2 omega -138.00 -84.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -31.4530 0.0000 90.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 3 omega 85.00 138.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.3905 77.0000 120.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 4 omega -20.00 33.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.3905 45.0000 180.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 5 omega 32.00 84.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.3905 -45.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 6 omega 3.00 60.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.3905 -77.0000 120.0000 0.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 7 omega -25.00 1.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.3905 -77.0000 30.0000 0.0000 0.0000 26 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 18472 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 31.99 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_max 0.925 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 7562 # number of observed reflections (> n sig(I)) _reflns_number_gt 5624 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 7562 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.025 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.135 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Se1 Se Uani 0.94177(3) 0.44619(1) 0.88885(3) 1.000 0.0123(1) . . Se2 Se Uani 0.61551(3) 0.38927(1) 0.88519(3) 1.000 0.0125(1) . . As1 As Uani 0.86046(3) 0.35443(1) 0.72923(3) 1.000 0.0125(1) . . As2 As Uani 0.96409(3) 0.35434(1) 1.04510(3) 1.000 0.0122(1) . . Fe1 Fe Uani 0.73988(5) 0.31451(1) 0.88601(5) 1.000 0.0133(1) . . Fe2 Fe Uani 0.70390(5) 0.42192(1) 0.68724(4) 1.000 0.0121(1) . . Fe3 Fe Uani 0.83626(5) 0.42148(1) 1.08579(4) 1.000 0.0123(1) . . Fe4 Fe Uani 1.11493(5) 0.37967(1) 0.88988(5) 1.000 0.0134(1) . . O1 O Uani 0.9485(3) 0.23868(7) 0.8650(3) 1.000 0.0276(8) . . O2 O Uani 0.6404(3) 0.28101(8) 1.1339(3) 1.000 0.0311(8) . . O3 O Uani 0.4389(3) 0.28903(8) 0.6565(3) 1.000 0.0298(7) . . O4 O Uani 0.4420(3) 0.37580(8) 0.4655(3) 1.000 0.0285(7) . . O5 O Uani 0.5078(3) 0.50422(7) 0.6783(3) 1.000 0.0267(7) . . O6 O Uani 0.8676(3) 0.45787(7) 0.4846(2) 1.000 0.0255(7) . . O7 O Uani 0.6978(3) 0.37522(8) 1.2886(2) 1.000 0.0259(7) . . O8 O Uani 0.6655(3) 0.50745(7) 1.0910(3) 1.000 0.0265(7) . . O9 O Uani 1.1384(3) 0.44857(7) 1.3090(2) 1.000 0.0240(7) . . O10 O Uani 1.2160(3) 0.41607(8) 0.6461(3) 1.000 0.0326(8) . . O11 O Uani 1.3784(3) 0.41648(8) 1.1355(3) 1.000 0.0279(7) . . O12 O Uani 1.2707(3) 0.29192(7) 0.9038(3) 1.000 0.0316(8) . . C1 C Uani 0.8658(4) 0.26748(10) 0.8758(3) 1.000 0.0180(8) . . C2 C Uani 0.6755(4) 0.29402(9) 1.0368(3) 1.000 0.0184(8) . . C3 C Uani 0.5568(4) 0.29793(9) 0.7435(3) 1.000 0.0176(8) . . C4 C Uani 0.5413(4) 0.39384(10) 0.5519(3) 1.000 0.0173(8) . . C5 C Uani 0.5852(3) 0.47286(10) 0.6866(3) 1.000 0.0172(8) . . C6 C Uani 0.8036(3) 0.44370(9) 0.5623(3) 1.000 0.0151(8) . . C7 C Uani 0.7510(3) 0.39373(9) 1.2100(3) 1.000 0.0161(8) . . C8 C Uani 0.7288(3) 0.47460(10) 1.0853(3) 1.000 0.0165(8) . . C9 C Uani 1.0211(3) 0.43898(10) 1.2209(3) 1.000 0.0160(8) . . C10 C Uani 1.1796(3) 0.40221(10) 0.7417(3) 1.000 0.0186(8) . . C11 C Uani 1.2774(3) 0.40288(10) 1.0390(3) 1.000 0.0176(8) . . C12 C Uani 1.2100(3) 0.32590(10) 0.8959(3) 1.000 0.0190(9) . . C13 C Uani 1.0907(4) 0.32159(10) 1.2180(3) 1.000 0.0226(9) . . C14 C Uani 0.8809(4) 0.31933(10) 0.5647(3) 1.000 0.0241(9) . . H13A H Uiso 1.17370 0.34150 1.27990 1.000 0.0270 calc R H13B H Uiso 1.14420 0.29580 1.18890 1.000 0.0270 calc R H13C H Uiso 1.01740 0.31110 1.27170 1.000 0.0270 calc R H14A H Uiso 0.77170 0.31220 0.49990 1.000 0.0290 calc R H14B H Uiso 0.94010 0.29150 0.60010 1.000 0.0290 calc R H14C H Uiso 0.94110 0.33680 0.51170 1.000 0.0290 calc R 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 Se1 0.0104(1) 0.0143(1) 0.0113(1) 0.0001(1) 0.0020(1) -0.0005(1) Se2 0.0089(1) 0.0167(1) 0.0113(1) 0.0000(1) 0.0017(1) 0.0000(1) As1 0.0109(1) 0.0145(1) 0.0111(1) 0.0000(1) 0.0019(1) 0.0012(1) As2 0.0101(1) 0.0139(1) 0.0111(1) 0.0003(1) 0.0011(1) 0.0002(1) Fe1 0.0118(2) 0.0141(2) 0.0125(2) -0.0002(2) 0.0014(2) -0.0014(2) Fe2 0.0101(2) 0.0153(2) 0.0098(2) 0.0004(2) 0.0013(2) 0.0011(2) Fe3 0.0107(2) 0.0153(2) 0.0103(2) -0.0005(2) 0.0022(2) 0.0002(2) Fe4 0.0092(2) 0.0172(2) 0.0132(2) 0.0002(2) 0.0026(2) 0.0011(2) O1 0.0280(13) 0.0219(11) 0.0339(15) 0.0009(11) 0.0107(11) 0.0038(10) O2 0.0364(14) 0.0340(13) 0.0258(14) 0.0057(11) 0.0137(11) -0.0059(11) O3 0.0245(12) 0.0358(13) 0.0237(13) -0.0059(11) -0.0009(10) -0.0086(11) O4 0.0199(12) 0.0399(13) 0.0220(13) -0.0058(11) 0.0006(9) -0.0066(10) O5 0.0259(12) 0.0240(11) 0.0287(14) 0.0009(10) 0.0058(10) 0.0077(10) O6 0.0287(12) 0.0315(12) 0.0196(12) 0.0009(10) 0.0121(10) -0.0033(10) O7 0.0273(12) 0.0344(12) 0.0182(12) 0.0051(10) 0.0102(10) -0.0009(10) O8 0.0195(12) 0.0219(11) 0.0398(15) -0.0015(11) 0.0116(10) 0.0026(9) O9 0.0196(11) 0.0297(12) 0.0181(12) -0.0038(10) -0.0012(9) -0.0025(9) O10 0.0219(12) 0.0509(15) 0.0265(14) 0.0104(12) 0.0097(10) 0.0035(11) O11 0.0159(11) 0.0391(13) 0.0244(13) -0.0056(11) -0.0003(10) -0.0012(10) O12 0.0265(13) 0.0252(11) 0.0426(16) -0.0007(12) 0.0098(11) 0.0076(10) C1 0.0195(15) 0.0187(13) 0.0138(15) 0.0003(12) 0.0020(12) -0.0051(12) C2 0.0168(15) 0.0146(13) 0.0201(16) -0.0004(12) -0.0001(12) -0.0021(11) C3 0.0199(15) 0.0154(13) 0.0177(15) -0.0012(12) 0.0060(12) -0.0010(12) C4 0.0178(15) 0.0233(14) 0.0103(14) 0.0028(12) 0.0034(11) 0.0035(12) C5 0.0141(14) 0.0213(14) 0.0139(15) 0.0035(12) 0.0010(11) 0.0003(12) C6 0.0164(14) 0.0153(12) 0.0112(14) -0.0005(11) 0.0004(11) 0.0028(11) C7 0.0139(14) 0.0210(14) 0.0115(14) -0.0021(12) 0.0009(11) 0.0033(11) C8 0.0123(14) 0.0215(14) 0.0164(15) -0.0027(12) 0.0055(11) -0.0043(11) C9 0.0168(14) 0.0179(13) 0.0134(14) 0.0006(12) 0.0049(11) 0.0021(11) C10 0.0077(13) 0.0265(15) 0.0201(16) -0.0025(13) 0.0019(11) 0.0025(11) C11 0.0124(14) 0.0222(14) 0.0203(16) 0.0034(13) 0.0083(12) 0.0034(12) C12 0.0120(14) 0.0258(15) 0.0194(16) -0.0001(13) 0.0052(12) 0.0009(12) C13 0.0209(16) 0.0228(15) 0.0188(16) 0.0045(13) -0.0018(12) 0.0006(13) C14 0.0333(18) 0.0251(16) 0.0137(15) -0.0018(13) 0.0066(13) 0.0080(14) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 Fe2 2.4672(5) . . yes Se1 Fe3 2.4568(5) . . yes Se1 Fe4 2.4760(5) . . yes Se2 Fe1 2.4699(5) . . yes Se2 Fe2 2.4636(5) . . yes Se2 Fe3 2.4605(5) . . yes As1 Fe1 2.3949(5) . . yes As1 Fe2 2.3849(5) . . yes As1 Fe4 2.3868(5) . . yes As1 C14 1.957(3) . . yes As2 Fe1 2.3852(5) . . yes As2 Fe3 2.3715(5) . . yes As2 Fe4 2.3822(5) . . yes As2 C13 1.958(3) . . yes Fe1 C1 1.791(3) . . yes Fe1 C2 1.815(3) . . yes Fe1 C3 1.818(3) . . yes Fe2 C4 1.805(3) . . yes Fe2 C5 1.827(3) . . yes Fe2 C6 1.800(3) . . yes Fe3 C7 1.788(3) . . yes Fe3 C8 1.832(3) . . yes Fe3 C9 1.801(3) . . yes Fe4 C10 1.816(3) . . yes Fe4 C11 1.813(3) . . yes Fe4 C12 1.792(3) . . yes O1 C1 1.139(4) . . yes O2 C2 1.138(4) . . yes O3 C3 1.135(4) . . yes O4 C4 1.133(4) . . yes O5 C5 1.135(4) . . yes O6 C6 1.138(4) . . yes O7 C7 1.141(4) . . yes O8 C8 1.129(4) . . yes O9 C9 1.141(4) . . yes O10 C10 1.140(4) . . yes O11 C11 1.139(4) . . yes O12 C12 1.131(4) . . yes C13 H13A 0.9800 . . no C13 H13B 0.9800 . . no C13 H13C 0.9800 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C14 H14C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 Se1 Fe3 96.60(2) . . . yes Fe2 Se1 Fe4 96.89(2) . . . yes Fe3 Se1 Fe4 96.77(2) . . . yes Fe1 Se2 Fe2 97.18(2) . . . yes Fe1 Se2 Fe3 96.95(2) . . . yes Fe2 Se2 Fe3 96.60(2) . . . yes Fe1 As1 Fe2 101.44(2) . . . yes Fe1 As1 Fe4 103.24(2) . . . yes Fe1 As1 C14 114.32(9) . . . yes Fe2 As1 Fe4 101.65(2) . . . yes Fe2 As1 C14 119.79(9) . . . yes Fe4 As1 C14 114.17(10) . . . yes Fe1 As2 Fe3 101.78(2) . . . yes Fe1 As2 Fe4 103.68(2) . . . yes Fe1 As2 C13 115.73(9) . . . yes Fe3 As2 Fe4 101.75(2) . . . yes Fe3 As2 C13 116.35(9) . . . yes Fe4 As2 C13 115.48(10) . . . yes Se2 Fe1 As1 79.54(2) . . . yes Se2 Fe1 As2 79.40(2) . . . yes Se2 Fe1 C1 166.78(11) . . . yes Se2 Fe1 C2 94.03(9) . . . yes Se2 Fe1 C3 88.26(9) . . . yes As1 Fe1 As2 75.12(2) . . . yes As1 Fe1 C1 88.34(10) . . . yes As1 Fe1 C2 166.18(9) . . . yes As1 Fe1 C3 95.40(10) . . . yes As2 Fe1 C1 92.48(10) . . . yes As2 Fe1 C2 91.75(10) . . . yes As2 Fe1 C3 165.56(9) . . . yes C1 Fe1 C2 96.65(14) . . . yes C1 Fe1 C3 98.19(14) . . . yes C2 Fe1 C3 96.63(14) . . . yes Se1 Fe2 Se2 82.90(1) . . . yes Se1 Fe2 As1 79.87(2) . . . yes Se1 Fe2 C4 169.40(10) . . . yes Se1 Fe2 C5 94.92(9) . . . yes Se1 Fe2 C6 88.75(9) . . . yes Se2 Fe2 As1 79.86(1) . . . yes Se2 Fe2 C4 91.66(10) . . . yes Se2 Fe2 C5 91.66(9) . . . yes Se2 Fe2 C6 170.11(9) . . . yes As1 Fe2 C4 90.24(10) . . . yes As1 Fe2 C5 170.49(9) . . . yes As1 Fe2 C6 93.52(9) . . . yes C4 Fe2 C5 94.33(14) . . . yes C4 Fe2 C6 95.73(13) . . . yes C5 Fe2 C6 94.32(12) . . . yes Se1 Fe3 Se2 83.17(1) . . . yes Se1 Fe3 As2 80.05(2) . . . yes Se1 Fe3 C7 169.06(9) . . . yes Se1 Fe3 C8 92.39(9) . . . yes Se1 Fe3 C9 91.51(9) . . . yes Se2 Fe3 As2 79.86(1) . . . yes Se2 Fe3 C7 88.64(9) . . . yes Se2 Fe3 C8 93.94(9) . . . yes Se2 Fe3 C9 169.97(9) . . . yes As2 Fe3 C7 91.41(9) . . . yes As2 Fe3 C8 170.69(9) . . . yes As2 Fe3 C9 90.87(9) . . . yes C7 Fe3 C8 95.40(12) . . . yes C7 Fe3 C9 95.47(13) . . . yes C8 Fe3 C9 94.78(13) . . . yes Se1 Fe4 As1 79.66(2) . . . yes Se1 Fe4 As2 79.45(2) . . . yes Se1 Fe4 C10 91.52(9) . . . yes Se1 Fe4 C11 90.77(9) . . . yes Se1 Fe4 C12 169.57(9) . . . yes As1 Fe4 As2 75.33(2) . . . yes As1 Fe4 C10 92.28(9) . . . yes As1 Fe4 C11 166.01(9) . . . yes As1 Fe4 C12 93.25(9) . . . yes As2 Fe4 C10 165.72(9) . . . yes As2 Fe4 C11 93.01(9) . . . yes As2 Fe4 C12 91.40(9) . . . yes C10 Fe4 C11 98.19(13) . . . yes C10 Fe4 C12 96.44(13) . . . yes C11 Fe4 C12 94.75(13) . . . yes Fe1 C1 O1 176.9(3) . . . yes Fe1 C2 O2 177.8(3) . . . yes Fe1 C3 O3 177.0(3) . . . yes Fe2 C4 O4 178.3(3) . . . yes Fe2 C5 O5 176.3(3) . . . yes Fe2 C6 O6 179.1(2) . . . yes Fe3 C7 O7 178.6(3) . . . yes Fe3 C8 O8 177.2(3) . . . yes Fe3 C9 O9 177.5(3) . . . yes Fe4 C10 O10 178.1(3) . . . yes Fe4 C11 O11 177.9(3) . . . yes Fe4 C12 O12 178.1(3) . . . yes As2 C13 H13A 109.00 . . . no As2 C13 H13B 109.00 . . . no As2 C13 H13C 109.00 . . . no H13A C13 H13B 110.00 . . . no H13A C13 H13C 109.00 . . . no H13B C13 H13C 109.00 . . . no As1 C14 H14A 109.00 . . . no As1 C14 H14B 109.00 . . . no As1 C14 H14C 109.00 . . . no H14A C14 H14B 110.00 . . . no H14A C14 H14C 109.00 . . . no H14B C14 H14C 109.00 . . . no 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 Fe4 Se1 Fe3 As2 -10.45(2) . . . . no Fe2 Se1 Fe3 C8 -87.20(9) . . . . no Fe4 Se1 Fe3 C8 175.02(9) . . . . no Fe2 Se1 Fe3 C9 177.95(9) . . . . no Fe4 Se1 Fe3 C9 80.17(10) . . . . no Fe3 Se1 Fe2 C5 84.58(9) . . . . no Fe4 Se1 Fe2 C5 -177.75(9) . . . . no Fe3 Se1 Fe2 C6 178.81(9) . . . . no Fe4 Se1 Fe2 C6 -83.52(9) . . . . no Fe2 Se1 Fe4 C11 179.98(10) . . . . no Fe2 Se1 Fe4 As1 -10.28(2) . . . . no Fe3 Se1 Fe4 As1 87.25(2) . . . . no Fe2 Se1 Fe4 As2 -87.10(2) . . . . no Fe3 Se1 Fe4 As2 10.42(2) . . . . no Fe2 Se1 Fe4 C10 81.77(9) . . . . no Fe3 Se1 Fe4 C10 179.29(9) . . . . no Fe2 Se1 Fe3 Se2 6.49(2) . . . . no Fe3 Se1 Fe2 Se2 -6.48(2) . . . . no Fe4 Se1 Fe2 Se2 91.19(2) . . . . no Fe3 Se1 Fe2 As1 -87.39(2) . . . . no Fe4 Se1 Fe2 As1 10.28(2) . . . . no Fe4 Se1 Fe3 Se2 -91.30(2) . . . . no Fe2 Se1 Fe3 As2 87.33(2) . . . . no Fe3 Se1 Fe4 C11 -82.49(9) . . . . no Fe1 Se2 Fe3 C7 -81.14(9) . . . . no Fe2 Se2 Fe1 C3 -85.36(10) . . . . no Fe1 Se2 Fe3 C8 -176.46(9) . . . . no Fe3 Se2 Fe1 C2 80.54(10) . . . . no Fe1 Se2 Fe2 C4 79.45(10) . . . . no Fe3 Se2 Fe2 C4 177.34(10) . . . . no Fe3 Se2 Fe1 C3 177.06(10) . . . . no Fe2 Se2 Fe3 As2 -87.55(2) . . . . no Fe2 Se2 Fe3 C7 -179.23(9) . . . . no Fe2 Se2 Fe1 As1 10.46(2) . . . . no Fe2 Se2 Fe3 C8 85.45(9) . . . . no Fe2 Se2 Fe1 As2 87.09(2) . . . . no Fe3 Se2 Fe1 As2 -10.49(2) . . . . no Fe2 Se2 Fe1 C2 178.12(10) . . . . no Fe1 Se2 Fe3 Se1 91.60(2) . . . . no Fe2 Se2 Fe3 Se1 -6.50(2) . . . . no Fe1 Se2 Fe2 Se1 -91.42(2) . . . . no Fe3 Se2 Fe2 Se1 6.47(2) . . . . no Fe1 Se2 Fe2 As1 -10.49(2) . . . . no Fe3 Se2 Fe2 As1 87.40(2) . . . . no Fe3 Se2 Fe1 As1 -87.13(2) . . . . no Fe1 Se2 Fe2 C5 173.83(9) . . . . no Fe3 Se2 Fe2 C5 -88.28(9) . . . . no Fe1 Se2 Fe3 As2 10.54(2) . . . . no C14 As1 Fe1 As2 137.00(11) . . . . no C14 As1 Fe1 C3 -54.08(14) . . . . no Fe2 As1 Fe1 C3 76.29(10) . . . . no Fe4 As1 Fe2 Se2 -95.33(2) . . . . no C14 As1 Fe2 Se2 137.83(12) . . . . no Fe1 As1 Fe2 C4 -80.69(10) . . . . no Fe4 As1 Fe2 C4 173.03(10) . . . . no Fe4 As1 Fe1 C3 -178.69(9) . . . . no C14 As1 Fe2 C4 46.18(15) . . . . no Fe1 As1 Fe2 C6 -176.44(9) . . . . no Fe4 As1 Fe2 C6 77.28(9) . . . . no C14 As1 Fe2 C6 -49.57(15) . . . . no Fe2 As1 Fe1 C1 174.35(10) . . . . no Fe4 As1 Fe1 C1 -80.62(10) . . . . no C14 As1 Fe1 C1 43.98(14) . . . . no Fe1 As1 Fe2 Se1 95.47(2) . . . . no Fe4 As1 Fe2 Se1 -10.82(2) . . . . no Fe1 As1 Fe2 Se2 10.96(2) . . . . no Fe1 As1 Fe4 Se1 -94.09(2) . . . . no Fe2 As1 Fe4 Se1 10.78(2) . . . . no C14 As1 Fe4 Se1 141.21(10) . . . . no Fe1 As1 Fe4 As2 -12.40(2) . . . . no Fe2 As1 Fe4 As2 92.47(2) . . . . no Fe2 As1 Fe1 Se2 -10.94(2) . . . . no Fe4 As1 Fe1 Se2 94.09(2) . . . . no C14 As1 Fe1 Se2 -141.31(11) . . . . no Fe2 As1 Fe1 As2 -92.64(2) . . . . no Fe4 As1 Fe1 As2 12.39(2) . . . . no C14 As1 Fe4 C12 -46.50(13) . . . . no Fe2 As1 Fe4 C12 -176.93(9) . . . . no Fe2 As1 Fe4 C10 -80.34(9) . . . . no C14 As1 Fe4 As2 -137.10(10) . . . . no C14 As1 Fe2 Se1 -137.66(12) . . . . no Fe1 As1 Fe4 C10 174.79(9) . . . . no C14 As1 Fe4 C10 50.09(13) . . . . no Fe1 As1 Fe4 C12 78.20(9) . . . . no C13 As2 Fe3 Se1 137.42(11) . . . . no Fe4 As2 Fe1 As1 -12.44(2) . . . . no Fe1 As2 Fe3 Se2 -11.07(2) . . . . no Fe4 As2 Fe3 Se1 11.03(2) . . . . no Fe3 As2 Fe1 Se2 11.05(2) . . . . no Fe4 As2 Fe1 Se2 -94.31(2) . . . . no C13 As2 Fe1 Se2 138.19(11) . . . . no Fe3 As2 Fe1 As1 92.92(2) . . . . no Fe3 As2 Fe1 C2 -82.73(10) . . . . no Fe4 As2 Fe1 C2 171.92(10) . . . . no C13 As2 Fe1 C2 44.42(14) . . . . no Fe4 As2 Fe3 Se2 95.79(2) . . . . no C13 As2 Fe3 Se2 -137.81(11) . . . . no Fe1 As2 Fe3 C7 77.29(9) . . . . no Fe4 As2 Fe3 C7 -175.85(9) . . . . no C13 As2 Fe3 C7 -49.45(14) . . . . no Fe1 As2 Fe3 C9 172.78(9) . . . . no Fe4 As2 Fe3 C9 -80.36(9) . . . . no C13 As2 Fe3 C9 46.04(14) . . . . no C13 As2 Fe1 As1 -139.94(11) . . . . no Fe3 As2 Fe1 C1 -179.47(10) . . . . no Fe4 As2 Fe1 C1 75.17(10) . . . . no C13 As2 Fe1 C1 -52.32(15) . . . . no Fe1 As2 Fe3 Se1 -95.84(2) . . . . no Fe1 As2 Fe4 Se1 94.43(2) . . . . no Fe3 As2 Fe4 Se1 -10.96(2) . . . . no C13 As2 Fe4 Se1 -137.92(10) . . . . no Fe1 As2 Fe4 As1 12.47(2) . . . . no Fe3 As2 Fe4 As1 -92.91(2) . . . . no C13 As2 Fe4 As1 140.12(10) . . . . no Fe1 As2 Fe4 C11 -175.35(9) . . . . no Fe3 As2 Fe4 C11 79.26(9) . . . . no C13 As2 Fe4 C11 -47.70(13) . . . . no Fe1 As2 Fe4 C12 -80.52(9) . . . . no Fe3 As2 Fe4 C12 174.09(9) . . . . no C13 As2 Fe4 C12 47.13(13) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se1 Se2 3.2639(4) . . no Se1 As1 3.1154(4) . . no Se1 As2 3.1058(4) . . no Se1 C5 3.194(3) . . no Se1 C6 3.022(3) . . no Se1 C8 3.125(3) . . no Se1 C9 3.084(3) . . no Se1 C10 3.109(3) . . no Se1 C11 3.088(3) . . no Se1 Se1 3.8234(4) . 3_767 no Se1 O8 3.592(3) . 3_767 no Se1 C8 3.633(3) . 3_767 no Se1 C9 3.627(3) . 3_767 no Se2 Se1 3.2639(4) . . no Se2 As1 3.1125(4) . . no Se2 As2 3.1020(4) . . no Se2 O10 3.598(3) . 1_455 no Se2 C2 3.166(3) . . no Se2 C3 3.022(3) . . no Se2 C4 3.096(3) . . no Se2 C5 3.109(3) . . no Se2 C7 3.007(3) . . no Se2 C8 3.167(3) . . no Se2 C10 3.594(3) . 1_455 no Se2 C11 3.661(3) . 1_455 no As1 Se1 3.1154(4) . . no As1 Se2 3.1125(4) . . no As1 As2 2.9139(4) . . no As1 C1 2.948(3) . . no As1 C3 3.140(3) . . no As1 C4 2.997(3) . . no As1 C6 3.075(3) . . no As1 C10 3.056(3) . . no As1 C12 3.065(3) . . no As2 Se1 3.1058(4) . . no As2 Se2 3.1020(4) . . no As2 As1 2.9139(4) . . no As2 C1 3.044(3) . . no As2 C2 3.041(3) . . no As2 C7 3.005(3) . . no As2 C9 3.000(3) . . no As2 C11 3.069(3) . . no As2 C12 3.016(3) . . no Fe4 O8 3.833(2) . 3_767 no O1 O12 3.110(4) . . no O1 C12 3.388(4) . . no O1 O2 3.206(4) . 4_554 no O1 O3 2.964(4) . 4_555 no O2 O7 3.151(3) . . no O2 O1 3.206(4) . 4_455 no O3 C1 3.095(4) . 4_454 no O3 O1 2.964(4) . 4_454 no O3 O4 3.184(4) . . no O3 O12 3.147(4) . 1_455 no O3 C2 3.316(4) . 4_454 no O4 O7 3.165(4) . 1_554 no O4 O3 3.184(4) . . no O4 O10 3.210(4) . 1_455 no O5 C6 3.348(4) . 3_666 no O5 O8 3.053(4) . 3_667 no O5 O11 2.954(3) . 3_767 no O6 C9 3.255(4) . 1_554 no O6 C7 3.180(3) . 1_554 no O6 O7 3.181(3) . 1_554 no O6 O10 3.179(4) . . no O7 O6 3.181(3) . 1_556 no O7 C4 3.266(4) . 1_556 no O7 C14 3.138(4) . 1_556 no O7 O2 3.151(3) . . no O7 O4 3.165(4) . 1_556 no O7 O11 2.960(4) . 1_455 no O7 C2 3.399(3) . . no O7 C6 3.249(3) . 1_556 no O8 Fe4 3.834(2) . 3_767 no O8 O11 3.097(4) . 3_767 no O8 Se1 3.592(3) . 3_767 no O8 C8 3.339(4) . 3_667 no O8 C10 3.216(4) . 3_767 no O8 O8 2.888(4) . 3_667 no O8 C11 3.056(4) . 3_767 no O8 O5 3.053(4) . 3_667 no O9 C5 3.324(4) . 3_767 no O9 O11 3.172(4) . . no O10 O6 3.179(4) . . no O10 C4 3.255(4) . 1_655 no O10 O4 3.210(4) . 1_655 no O10 Se2 3.598(3) . 1_655 no O11 C7 3.131(4) . 1_655 no O11 O7 2.960(4) . 1_655 no O11 O8 3.097(4) . 3_767 no O11 O9 3.172(4) . . no O11 O5 2.954(3) . 3_767 no O12 O3 3.147(4) . 1_655 no O12 O1 3.110(4) . . no O12 C3 3.280(4) . 1_655 no O12 C2 3.319(4) . 1_655 no O1 H13B 2.8400 . 4_454 no O2 H14B 2.7200 . 4_455 no O4 H13A 2.6600 . 1_454 no O7 H14A 2.7100 . 1_556 no O7 H14C 2.7600 . 1_556 no C1 As1 2.948(3) . . no C1 As2 3.044(3) . . no C1 Fe4 3.949(3) . . no C1 C2 2.693(5) . . no C1 C3 2.727(5) . . no C1 C12 3.382(4) . . no C1 C14 3.421(4) . . no C1 O3 3.095(4) . 4_555 no C1 C13 3.574(4) . 4_454 no C2 O7 3.399(3) . . no C2 C3 2.713(4) . . no C2 Se2 3.166(3) . . no C2 As2 3.041(3) . . no C2 O3 3.316(4) . 4_555 no C2 O12 3.319(4) . 1_455 no C2 C1 2.693(5) . . no C2 C7 3.378(4) . . no C2 C13 3.558(5) . . no C3 As1 3.140(3) . . no C3 C1 2.727(5) . . no C3 Se2 3.022(3) . . no C3 C13 3.590(4) . 4_454 no C3 Fe2 3.996(3) . . no C3 O12 3.280(4) . 1_455 no C3 C2 2.713(4) . . no C3 C4 3.389(4) . . no C4 C6 2.673(4) . . no C4 Fe1 3.952(3) . . no C4 C5 2.663(4) . . no C4 Se2 3.096(3) . . no C4 As1 2.997(3) . . no C4 C3 3.389(4) . . no C4 O7 3.266(4) . 1_554 no C4 O10 3.255(4) . 1_455 no C5 C6 2.660(4) . . no C5 Se2 3.109(3) . . no C5 Se1 3.194(3) . . no C5 O9 3.324(4) . 3_767 no C5 C4 2.663(4) . . no C6 Fe4 3.963(3) . . no C6 C5 2.660(4) . . no C6 As1 3.075(3) . . no C6 Se1 3.022(3) . . no C6 C4 2.673(4) . . no C6 O7 3.249(3) . 1_554 no C6 O5 3.348(4) . 3_666 no C6 C10 3.400(4) . . no C7 Fe1 3.903(3) . . no C7 C2 3.378(4) . . no C7 Se2 3.007(3) . . no C7 C9 2.655(4) . . no C7 As2 3.005(3) . . no C7 O6 3.180(3) . 1_556 no C7 O11 3.131(4) . 1_455 no C7 C8 2.677(4) . . no C8 Se1 3.633(3) . 3_767 no C8 Se1 3.125(3) . . no C8 Se2 3.167(3) . . no C8 C9 2.673(4) . . no C8 C7 2.677(4) . . no C8 O8 3.339(4) . 3_667 no C9 Fe4 3.949(3) . . no C9 C8 2.673(4) . . no C9 Se1 3.627(3) . 3_767 no C9 Se1 3.084(3) . . no C9 As2 3.000(3) . . no C9 O6 3.255(4) . 1_556 no C9 C7 2.655(4) . . no C9 C11 3.381(4) . . no C9 C13 3.552(4) . . no C10 Se2 3.594(3) . 1_655 no C10 Fe2 3.997(3) . . no C10 C12 2.690(4) . . no C10 Se1 3.109(3) . . no C10 O8 3.216(4) . 3_767 no C10 As1 3.056(3) . . no C10 C6 3.400(4) . . no C10 C11 2.743(4) . . no C10 C14 3.599(4) . . no C11 As2 3.069(3) . . no C11 C10 2.743(4) . . no C11 O8 3.056(4) . 3_767 no C11 Se1 3.088(3) . . no C11 Se2 3.661(3) . 1_655 no C11 Fe3 3.983(3) . . no C11 C9 3.381(4) . . no C11 C12 2.652(4) . . no C12 C14 3.579(4) . . no C12 C1 3.382(4) . . no C12 As2 3.016(3) . . no C12 As1 3.065(3) . . no C12 C13 3.565(4) . . no C12 O1 3.388(4) . . no C12 C10 2.690(4) . . no C12 C11 2.652(4) . . no C13 C3 3.590(4) . 4_555 no C13 C1 3.574(4) . 4_555 no C14 O7 3.138(4) . 1_554 no C1 H13B 2.8900 . 4_454 no C1 H14B 3.0100 . . no C3 H13B 2.9800 . 4_454 no H13A O4 2.6600 . 1_656 no H13B O1 2.8400 . 4_555 no H13B C1 2.8900 . 4_555 no H13B C3 2.9800 . 4_555 no H14A O7 2.7100 . 1_554 no H14B C1 3.0100 . . no H14B O2 2.7200 . 4_554 no H14C O7 2.7600 . 1_554 no #===END data_2a_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 802725' #TrackingRef '- Combined_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H8 As2 Cl2 Fe4 O12 Se2' _chemical_formula_weight 982.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.2758 1.3314 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se 0.2367 1.4831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.397(2) _cell_length_b 17.966(4) _cell_length_c 15.416(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.02(3) _cell_angle_gamma 90.00 _cell_volume 2877.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.91 _exptl_crystal_description route _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 3.686 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4721 _exptl_absorpt_correction_T_max 0.6930 _exptl_absorpt_process_details 'program faceit' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24851 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.91 _reflns_number_total 10996 _reflns_number_gt 6218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHELXL-97 _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^)+(0.1000P)^2^+0.0000P] 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 0.0050(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10996 _refine_ls_number_parameters 348 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2399 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.008 _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 As2 As 0.22007(7) 0.21507(4) 0.00030(5) 0.03289(18) Uani 1 1 d . . . As1 As 0.28010(7) 0.17508(4) 0.18030(5) 0.03155(18) Uani 1 1 d . . . Se1 Se 0.41825(7) 0.08807(4) 0.03669(5) 0.03451(18) Uani 1 1 d . . . Se2 Se 0.10790(7) 0.06763(4) 0.06898(5) 0.03386(18) Uani 1 1 d . . . Fe1 Fe 0.42385(11) 0.22171(6) 0.07609(8) 0.0333(2) Uani 1 1 d . . . Fe2 Fe 0.30068(11) 0.04443(6) 0.16296(8) 0.0350(2) Uani 1 1 d . . . Fe3 Fe 0.22719(11) 0.09403(6) -0.06256(7) 0.0356(2) Uani 1 1 d . . . Fe4 Fe 0.07296(11) 0.19850(6) 0.11404(7) 0.0327(2) Uani 1 1 d . . . C1 C 0.5063(9) 0.2474(5) -0.0214(6) 0.0451(19) Uani 1 1 d . . . O1 O 0.5540(8) 0.2677(5) -0.0818(6) 0.075(2) Uani 1 1 d . . . C2 C 0.3928(9) 0.3149(5) 0.1091(7) 0.047(2) Uani 1 1 d . . . O2 O 0.3739(9) 0.3742(4) 0.1317(7) 0.082(3) Uani 1 1 d . . . C3 C 0.5658(9) 0.2095(5) 0.1487(6) 0.0439(18) Uani 1 1 d . . . O3 O 0.6516(8) 0.2059(5) 0.1940(6) 0.068(2) Uani 1 1 d . . . C4 C 0.4479(9) 0.0440(5) 0.2289(7) 0.048(2) Uani 1 1 d . . . O4 O 0.5385(9) 0.0450(5) 0.2695(6) 0.075(2) Uani 1 1 d . . . C5 C 0.1963(11) 0.0303(5) 0.2519(6) 0.050(2) Uani 1 1 d . . . O5 O 0.1324(9) 0.0274(4) 0.3087(5) 0.070(2) Uani 1 1 d . . . C6 C 0.3109(9) -0.0533(4) 0.1303(7) 0.046(2) Uani 1 1 d . . . O6 O 0.3181(8) -0.1145(4) 0.1115(6) 0.067(2) Uani 1 1 d . . . C7 C 0.2388(8) -0.0073(5) -0.0856(6) 0.0445(19) Uani 1 1 d . . . O7 O 0.2429(8) -0.0666(4) -0.1030(6) 0.069(2) Uani 1 1 d . . . C8 C 0.0781(9) 0.1092(5) -0.1229(6) 0.0448(18) Uani 1 1 d . . . O8 O -0.0131(8) 0.1205(5) -0.1628(5) 0.070(2) Uani 1 1 d . . . C9 C 0.3278(10) 0.1283(6) -0.1465(6) 0.053(2) Uani 1 1 d . . . O9 O 0.3867(9) 0.1517(6) -0.1992(6) 0.086(3) Uani 1 1 d . . . C10 C -0.0173(8) 0.1685(5) 0.2071(6) 0.0391(16) Uani 1 1 d . . . O10 O -0.0730(7) 0.1517(4) 0.2649(5) 0.0591(18) Uani 1 1 d . . . C11 C -0.0655(8) 0.2078(5) 0.0411(6) 0.0411(17) Uani 1 1 d . . . O11 O -0.1507(8) 0.2152(4) -0.0047(6) 0.0642(19) Uani 1 1 d . . . C12 C 0.0821(9) 0.2951(5) 0.1419(6) 0.0433(18) Uani 1 1 d . . . O12 O 0.0869(8) 0.3554(4) 0.1606(6) 0.072(2) Uani 1 1 d . . . C13 C 0.3102(10) 0.2111(6) 0.2995(6) 0.051(2) Uani 1 1 d . . . H13A H 0.2873 0.2639 0.3026 0.077 Uiso 1 1 calc R . . H13B H 0.4013 0.2047 0.3166 0.077 Uiso 1 1 calc R . . H13C H 0.2571 0.1825 0.3389 0.077 Uiso 1 1 calc R . . C14 C 0.1776(11) 0.2982(3) -0.0826(4) 0.059(3) Uani 1 1 d . . . H14A H 0.2454 0.3023 -0.1249 0.088 Uiso 1 1 calc R . . H14B H 0.1714 0.3450 -0.0504 0.088 Uiso 1 1 calc R . . H14C H 0.0952 0.2878 -0.1130 0.088 Uiso 1 1 calc R . . C15 C 0.1999(5) 0.0469(2) -0.4775(4) 0.32(6) Uani 0.50 1 d PRD A 1 Cl1 Cl 0.1368(5) -0.0191(2) -0.4088(4) 0.182(8) Uani 0.50 1 d PRD A 1 Cl2 Cl 0.3437(5) 0.0163(3) -0.5150(4) 0.109(3) Uani 0.50 1 d PRD A 1 C16 C 0.2802(5) 0.0481(2) -0.4227(4) 0.53(12) Uani 0.50 1 d PRD D 2 Cl3 Cl 0.2420(5) 0.1310(2) -0.4016(4) 0.115(4) Uani 0.50 1 d PRD D 2 Cl4 Cl 0.1732(5) -0.0045(2) -0.3632(4) 0.43(3) Uani 0.50 1 d PRD D 2 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 As2 0.0320(4) 0.0330(3) 0.0339(4) 0.0010(3) 0.0041(3) -0.0010(3) As1 0.0309(4) 0.0319(3) 0.0320(3) -0.0030(3) 0.0030(3) -0.0008(2) Se1 0.0313(4) 0.0329(3) 0.0396(4) -0.0044(3) 0.0055(3) 0.0008(2) Se2 0.0318(4) 0.0327(3) 0.0374(4) -0.0038(3) 0.0046(3) -0.0038(2) Fe1 0.0296(5) 0.0313(5) 0.0394(6) -0.0004(4) 0.0040(4) -0.0037(4) Fe2 0.0349(6) 0.0307(5) 0.0395(6) 0.0020(4) 0.0032(4) 0.0000(4) Fe3 0.0337(6) 0.0395(5) 0.0337(5) -0.0069(4) 0.0046(4) -0.0012(4) Fe4 0.0307(5) 0.0334(5) 0.0344(5) -0.0025(4) 0.0046(4) 0.0013(4) C1 0.049(5) 0.043(4) 0.044(4) 0.006(4) 0.009(4) -0.002(3) O1 0.060(5) 0.094(6) 0.073(5) 0.031(5) 0.030(4) -0.007(4) C2 0.042(5) 0.042(4) 0.058(5) -0.010(4) -0.002(4) -0.007(3) O2 0.079(6) 0.038(3) 0.130(8) -0.023(4) -0.002(6) -0.002(3) C3 0.046(5) 0.043(4) 0.043(4) 0.000(3) 0.005(4) 0.000(3) O3 0.053(5) 0.080(5) 0.068(5) -0.002(4) -0.020(4) 0.005(4) C4 0.043(5) 0.040(4) 0.062(6) 0.006(4) -0.001(4) 0.004(3) O4 0.062(5) 0.085(6) 0.077(6) 0.012(5) -0.023(4) 0.004(4) C5 0.063(6) 0.039(4) 0.047(5) 0.007(4) 0.004(4) 0.003(4) O5 0.076(6) 0.071(5) 0.065(5) 0.025(4) 0.033(4) 0.004(4) C6 0.043(5) 0.033(4) 0.064(6) 0.001(4) 0.014(4) 0.000(3) O6 0.077(5) 0.040(3) 0.087(6) -0.011(4) 0.020(5) -0.008(3) C7 0.033(4) 0.054(5) 0.046(5) -0.019(4) 0.000(3) 0.002(3) O7 0.061(5) 0.045(4) 0.100(6) -0.031(4) 0.002(4) 0.002(3) C8 0.051(5) 0.048(4) 0.035(4) -0.008(3) 0.000(4) -0.004(4) O8 0.072(6) 0.080(5) 0.057(5) -0.005(4) -0.020(4) 0.010(4) C9 0.052(6) 0.074(6) 0.033(4) -0.013(4) 0.007(4) 0.004(4) O9 0.078(6) 0.120(8) 0.063(5) 0.010(5) 0.028(5) -0.029(5) C10 0.031(4) 0.045(4) 0.042(4) -0.005(3) 0.004(3) 0.005(3) O10 0.059(4) 0.066(4) 0.055(4) 0.007(3) 0.025(3) 0.002(3) C11 0.039(4) 0.045(4) 0.039(4) 0.000(3) -0.004(3) 0.006(3) O11 0.048(4) 0.072(5) 0.071(5) 0.004(4) -0.011(4) 0.006(3) C12 0.044(5) 0.047(4) 0.040(4) 0.000(3) 0.013(3) 0.006(3) O12 0.074(5) 0.045(4) 0.097(6) -0.018(4) 0.022(5) 0.002(3) C13 0.051(5) 0.066(6) 0.036(4) -0.012(4) -0.003(4) 0.004(4) C14 0.063(7) 0.056(5) 0.057(6) 0.015(5) 0.004(5) -0.002(5) C15 0.19(6) 0.71(16) 0.08(3) 0.16(6) 0.03(3) 0.25(9) Cl1 0.133(10) 0.082(6) 0.34(2) 0.049(9) 0.130(13) 0.014(6) Cl2 0.069(5) 0.171(9) 0.087(6) -0.006(6) 0.026(4) 0.018(5) C16 0.41(13) 0.45(13) 0.7(2) 0.51(15) -0.40(14) -0.34(12) Cl3 0.071(5) 0.056(3) 0.216(11) -0.028(5) -0.022(6) 0.010(3) Cl4 0.146(18) 0.40(4) 0.77(8) 0.39(5) 0.14(3) 0.03(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 As2 C14 2.004(5) . ? As2 Fe3 2.3828(13) . ? As2 Fe4 2.3859(14) . ? As2 Fe1 2.3860(16) . ? As2 As1 2.9126(13) . ? As1 C13 1.963(9) . ? As1 Fe2 2.3731(13) . ? As1 Fe1 2.3845(14) . ? As1 Fe4 2.3882(15) . ? Se1 Fe2 2.4631(15) . ? Se1 Fe3 2.4665(16) . ? Se1 Fe1 2.4767(13) . ? Se2 Fe3 2.4603(15) . ? Se2 Fe2 2.4668(16) . ? Se2 Fe4 2.4821(13) . ? Fe1 C2 1.783(9) . ? Fe1 C1 1.816(9) . ? Fe1 C3 1.834(10) . ? Fe2 C5 1.796(10) . ? Fe2 C4 1.807(10) . ? Fe2 C6 1.830(8) . ? Fe3 C8 1.799(10) . ? Fe3 C9 1.801(10) . ? Fe3 C7 1.860(9) . ? Fe4 C12 1.789(9) . ? Fe4 C11 1.803(9) . ? Fe4 C10 1.823(8) . ? C1 O1 1.131(10) . ? C2 O2 1.139(10) . ? C3 O3 1.115(11) . ? C4 O4 1.114(12) . ? C5 O5 1.119(11) . ? C6 O6 1.142(10) . ? C7 O7 1.100(11) . ? C8 O8 1.132(12) . ? C9 O9 1.116(11) . ? C10 O10 1.122(10) . ? C11 O11 1.120(11) . ? C12 O12 1.122(11) . ? C15 Cl2 1.7117(12) . ? C15 Cl1 1.7338 . ? C16 Cl3 1.5782 . ? C16 Cl4 1.7448 . ? 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 C14 As2 Fe3 115.46(17) . . ? C14 As2 Fe4 115.4(3) . . ? Fe3 As2 Fe4 102.41(5) . . ? C14 As2 Fe1 116.5(3) . . ? Fe3 As2 Fe1 101.83(5) . . ? Fe4 As2 Fe1 103.15(5) . . ? C14 As2 As1 145.69(17) . . ? Fe3 As2 As1 98.84(4) . . ? Fe4 As2 As1 52.44(4) . . ? Fe1 As2 As1 52.35(4) . . ? C13 As1 Fe2 114.8(3) . . ? C13 As1 Fe1 115.6(3) . . ? Fe2 As1 Fe1 102.15(5) . . ? C13 As1 Fe4 117.0(3) . . ? Fe2 As1 Fe4 102.10(5) . . ? Fe1 As1 Fe4 103.13(5) . . ? C13 As1 As2 146.4(3) . . ? Fe2 As1 As2 98.85(4) . . ? Fe1 As1 As2 52.40(4) . . ? Fe4 As1 As2 52.37(4) . . ? Fe2 Se1 Fe3 95.32(5) . . ? Fe2 Se1 Fe1 97.05(4) . . ? Fe3 Se1 Fe1 96.97(5) . . ? Fe3 Se2 Fe2 95.38(5) . . ? Fe3 Se2 Fe4 97.53(4) . . ? Fe2 Se2 Fe4 96.87(5) . . ? C2 Fe1 C1 95.3(4) . . ? C2 Fe1 C3 95.1(4) . . ? C1 Fe1 C3 98.2(4) . . ? C2 Fe1 As1 90.8(3) . . ? C1 Fe1 As1 166.5(3) . . ? C3 Fe1 As1 93.3(3) . . ? C2 Fe1 As2 91.2(3) . . ? C1 Fe1 As2 92.5(3) . . ? C3 Fe1 As2 167.0(3) . . ? As1 Fe1 As2 75.26(4) . . ? C2 Fe1 Se1 167.8(3) . . ? C1 Fe1 Se1 92.9(3) . . ? C3 Fe1 Se1 92.6(3) . . ? As1 Fe1 Se1 79.33(4) . . ? As2 Fe1 Se1 79.55(4) . . ? C5 Fe2 C4 95.3(5) . . ? C5 Fe2 C6 96.7(4) . . ? C4 Fe2 C6 95.4(4) . . ? C5 Fe2 As1 89.7(3) . . ? C4 Fe2 As1 91.1(3) . . ? C6 Fe2 As1 170.4(3) . . ? C5 Fe2 Se1 168.0(3) . . ? C4 Fe2 Se1 90.7(3) . . ? C6 Fe2 Se1 93.0(3) . . ? As1 Fe2 Se1 79.83(4) . . ? C5 Fe2 Se2 88.4(3) . . ? C4 Fe2 Se2 170.2(3) . . ? C6 Fe2 Se2 93.1(3) . . ? As1 Fe2 Se2 79.88(4) . . ? Se1 Fe2 Se2 84.13(5) . . ? C8 Fe3 C9 95.1(4) . . ? C8 Fe3 C7 96.3(4) . . ? C9 Fe3 C7 98.9(4) . . ? C8 Fe3 As2 91.9(3) . . ? C9 Fe3 As2 90.4(3) . . ? C7 Fe3 As2 167.0(3) . . ? C8 Fe3 Se2 90.3(3) . . ? C9 Fe3 Se2 168.7(3) . . ? C7 Fe3 Se2 90.4(3) . . ? As2 Fe3 Se2 79.45(4) . . ? C8 Fe3 Se1 170.8(3) . . ? C9 Fe3 Se1 89.1(3) . . ? C7 Fe3 Se1 91.1(3) . . ? As2 Fe3 Se1 79.82(4) . . ? Se2 Fe3 Se1 84.19(5) . . ? C12 Fe4 C11 95.4(4) . . ? C12 Fe4 C10 97.0(4) . . ? C11 Fe4 C10 95.5(4) . . ? C12 Fe4 As2 91.5(3) . . ? C11 Fe4 As2 92.8(3) . . ? C10 Fe4 As2 167.5(3) . . ? C12 Fe4 As1 91.6(3) . . ? C11 Fe4 As1 166.2(3) . . ? C10 Fe4 As1 95.3(3) . . ? As2 Fe4 As1 75.19(4) . . ? C12 Fe4 Se2 168.2(3) . . ? C11 Fe4 Se2 92.0(3) . . ? C10 Fe4 Se2 91.4(3) . . ? As2 Fe4 Se2 78.96(4) . . ? As1 Fe4 Se2 79.29(4) . . ? O1 C1 Fe1 175.7(9) . . ? O2 C2 Fe1 178.7(11) . . ? O3 C3 Fe1 176.3(8) . . ? O4 C4 Fe2 178.9(9) . . ? O5 C5 Fe2 174.5(9) . . ? O6 C6 Fe2 178.7(10) . . ? O7 C7 Fe3 176.6(10) . . ? O8 C8 Fe3 177.3(9) . . ? O9 C9 Fe3 177.2(11) . . ? O10 C10 Fe4 178.5(8) . . ? O11 C11 Fe4 178.4(9) . . ? O12 C12 Fe4 178.9(8) . . ? Cl2 C15 Cl1 110.0 . . ? Cl3 C16 Cl4 103.50(7) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.787 _refine_diff_density_min -2.417 _refine_diff_density_rms 0.267 #===END #=============================================================================== data_2b_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 802726' #TrackingRef '- Combined_CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H8 As2 Cl2 Fe4 O12 Te2' _chemical_formula_structural ? _chemical_formula_sum 'C15 H8 As2 Cl2 Fe4 O12 Te2' _chemical_formula_iupac ? _chemical_formula_weight 1079.55 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 10.2566(14) _cell_length_b 17.710(3) _cell_length_c 15.4128(17) _cell_angle_alpha 90 _cell_angle_beta 92.092(14) _cell_angle_gamma 90 _cell_volume 2797.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 11602 _cell_measurement_theta_min 3.2596 _cell_measurement_theta_max 33.0107 _cell_special_details ; ; _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.465 _exptl_crystal_size_mid 0.122 _exptl_crystal_size_min 0.044 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.563 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1995 _exptl_absorpt_coefficient_mu 6.669 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.24042 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5431 # number of measured reflections (redundant set) _diffrn_reflns_number 25291 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 30.73 _diffrn_reflns_theta_full 30.73 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 8653 # number of observed reflections (> n sig(I)) _reflns_number_gt 5879 _reflns_threshold_expression >2\s(i) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0402P)^2^+3.8345P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 8653 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.316 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.222 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Te1 Te Uani 0.56458(3) 0.08991(2) 0.46047(2) 0.960 0.0136(1) . . Te2 Te Uani 0.89159(3) 0.06303(2) 0.42866(2) 0.960 0.0145(1) . . Te3 Te Uiso 0.7086(9) 0.1932(6) 0.2789(7) 0.040 0.019(2) . . Te4 Te Uiso 0.7939(8) 0.2409(5) 0.5195(6) 0.040 0.0086(16) . . As1 As Uani 0.77730(5) 0.22116(3) 0.49074(4) 0.960 0.0153(2) . . As2 As Uani 0.71669(5) 0.17658(3) 0.31282(4) 0.960 0.0146(2) . . Fe1 Fe Uani 0.76896(6) 0.10337(4) 0.56647(4) 1.000 0.0166(2) . . Fe2 Fe Uani 0.68716(6) 0.04403(4) 0.32463(5) 1.000 0.0170(2) . . Fe3 Fe Uani 0.57166(6) 0.23102(4) 0.41288(5) 1.000 0.0163(2) . . Fe4 Fe Uani 0.92854(6) 0.20157(4) 0.37819(4) 1.000 0.0160(2) . . O1 O Uani 0.6070(4) 0.1759(3) 0.6943(3) 1.000 0.0378(14) . . O2 O Uani 1.0145(4) 0.1342(3) 0.6613(3) 1.000 0.0383(14) . . O3 O Uani 0.7548(4) -0.0533(2) 0.6293(3) 1.000 0.0384(14) . . O4 O Uani 0.6735(4) -0.1173(2) 0.3704(3) 1.000 0.0345(14) . . O5 O Uani 0.4457(4) 0.0504(3) 0.2171(3) 1.000 0.0427(16) . . O6 O Uani 0.8579(4) 0.0361(2) 0.1782(3) 1.000 0.0402(16) . . O7 O Uani 0.3418(4) 0.2154(2) 0.2952(3) 1.000 0.0347(14) . . O8 O Uani 0.4389(4) 0.2851(3) 0.5657(3) 1.000 0.0425(16) . . O9 O Uani 0.6337(4) 0.3812(3) 0.3522(4) 1.000 0.0519(18) . . O10 O Uani 1.0722(4) 0.1496(2) 0.2277(2) 1.000 0.0309(11) . . O11 O Uani 0.9179(4) 0.3607(2) 0.3328(3) 1.000 0.0341(12) . . O12 O Uani 1.1622(4) 0.2163(3) 0.4931(3) 1.000 0.0392(16) . . C1 C Uani 0.6683(5) 0.1458(3) 0.6452(4) 1.000 0.0267(16) . . C2 C Uani 0.9205(5) 0.1228(3) 0.6234(3) 1.000 0.0230(14) . . C3 C Uani 0.7578(5) 0.0072(4) 0.6038(3) 1.000 0.0277(18) . . C4 C Uani 0.6782(5) -0.0556(3) 0.3540(3) 1.000 0.0234(16) . . C5 C Uani 0.5385(5) 0.0472(3) 0.2594(4) 1.000 0.0238(17) . . C6 C Uani 0.7916(5) 0.0359(3) 0.2355(3) 1.000 0.0255(17) . . C7 C Uani 0.4296(5) 0.2200(3) 0.3413(3) 1.000 0.0238(16) . . C8 C Uani 0.4886(5) 0.2631(3) 0.5068(3) 1.000 0.0246(16) . . C9 C Uani 0.6101(5) 0.3233(3) 0.3757(4) 1.000 0.0264(16) . . C10 C Uani 1.0161(5) 0.1703(3) 0.2851(3) 1.000 0.0229(14) . . C11 C Uani 0.9215(5) 0.2997(3) 0.3499(3) 1.000 0.0232(14) . . C12 C Uani 1.0714(5) 0.2104(3) 0.4491(3) 1.000 0.0230(14) . . C13 C Uani 0.8188(6) 0.3073(4) 0.5645(4) 0.960 0.0310(17) . . C14 C Uani 0.6897(5) 0.2122(3) 0.1938(3) 0.960 0.0231(17) . . Cl3 Cl Uani 0.7809(13) 0.0958(8) 0.8723(11) 0.540 0.173(6) . . Cl4 Cl Uani 0.8863(5) -0.0061(3) 0.9787(3) 0.540 0.099(2) . . C16 C Uani 0.8424(12) 0.0086(8) 0.8732(9) 0.540 0.051(5) . . Cl1 Cl Uani 0.6104(7) 0.0477(7) 1.0113(5) 0.460 0.151(5) . . Cl2 Cl Uani 0.7745(7) 0.1016(5) 0.8567(7) 0.460 0.0588(19) . . C15 C Uani 0.7386(18) 0.0327(12) 0.9598(13) 0.460 0.070(8) . . H1 H Uiso 0.75650 0.31000 0.61110 0.960 0.0470 calc . H2 H Uiso 0.81360 0.35370 0.52980 0.960 0.0470 calc . H3 H Uiso 0.90730 0.30170 0.58980 0.960 0.0470 calc . H4 H Uiso 0.59830 0.20430 0.17500 0.960 0.0340 calc . H5 H Uiso 0.71060 0.26610 0.19090 0.960 0.0340 calc . H6 H Uiso 0.74650 0.18400 0.15560 0.960 0.0340 calc . H9 H Uiso 0.91890 0.00520 0.83600 0.540 0.0610 calc . H10 H Uiso 0.77610 -0.02860 0.85280 0.540 0.0610 calc . H7 H Uiso 0.73520 -0.02000 0.93830 0.460 0.0840 calc . H8 H Uiso 0.81400 0.03630 1.00160 0.460 0.0840 calc . 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 Te1 0.0123(1) 0.0130(2) 0.0156(2) 0.0016(1) 0.0010(1) -0.0010(1) Te2 0.0137(1) 0.0148(2) 0.0150(2) 0.0021(1) 0.0010(1) 0.0029(1) As1 0.0145(2) 0.0164(3) 0.0150(3) 0.0004(2) 0.0015(2) -0.0001(2) As2 0.0144(2) 0.0151(3) 0.0144(3) 0.0020(2) 0.0002(2) -0.0001(2) Fe1 0.0149(3) 0.0195(4) 0.0153(3) 0.0022(3) 0.0008(3) 0.0002(2) Fe2 0.0189(3) 0.0152(4) 0.0169(3) -0.0006(3) 0.0013(3) -0.0004(2) Fe3 0.0146(3) 0.0153(4) 0.0189(3) 0.0002(3) 0.0006(3) 0.0019(2) Fe4 0.0144(3) 0.0182(4) 0.0155(3) 0.0020(3) 0.0010(2) -0.0007(2) O1 0.039(2) 0.044(3) 0.031(2) -0.012(2) 0.0108(19) 0.0060(19) O2 0.030(2) 0.049(3) 0.035(2) -0.005(2) -0.0105(18) -0.0088(19) O3 0.0296(19) 0.029(2) 0.056(3) 0.022(2) -0.0074(19) -0.0038(17) O4 0.040(2) 0.022(2) 0.042(3) 0.0012(18) 0.0075(19) 0.0005(17) O5 0.033(2) 0.055(3) 0.039(3) -0.006(2) -0.013(2) -0.002(2) O6 0.056(3) 0.026(2) 0.040(3) -0.0119(19) 0.022(2) -0.0105(19) O7 0.031(2) 0.036(3) 0.036(2) 0.0021(19) -0.0116(18) -0.0002(17) O8 0.033(2) 0.056(3) 0.039(3) -0.017(2) 0.0071(19) 0.003(2) O9 0.052(3) 0.018(2) 0.085(4) 0.018(2) -0.005(3) -0.003(2) O10 0.0334(19) 0.038(2) 0.0219(19) 0.0018(18) 0.0110(16) -0.0004(17) O11 0.043(2) 0.022(2) 0.038(2) 0.0050(18) 0.0102(19) -0.0045(17) O12 0.029(2) 0.050(3) 0.038(3) 0.004(2) -0.0088(19) -0.0034(19) C1 0.022(2) 0.034(3) 0.024(3) 0.005(2) 0.000(2) 0.000(2) C2 0.024(2) 0.026(3) 0.019(2) 0.001(2) -0.001(2) 0.000(2) C3 0.015(2) 0.048(4) 0.020(3) 0.007(2) -0.0006(19) 0.000(2) C4 0.021(2) 0.025(3) 0.024(3) -0.003(2) -0.002(2) -0.0020(19) C5 0.030(3) 0.013(3) 0.028(3) -0.001(2) -0.004(2) -0.0049(19) C6 0.039(3) 0.018(3) 0.020(3) -0.007(2) 0.010(2) -0.005(2) C7 0.022(2) 0.026(3) 0.023(3) 0.006(2) -0.003(2) 0.003(2) C8 0.022(2) 0.029(3) 0.023(3) -0.004(2) 0.002(2) 0.001(2) C9 0.023(2) 0.021(3) 0.035(3) 0.000(2) 0.000(2) -0.001(2) C10 0.018(2) 0.034(3) 0.016(2) 0.005(2) -0.0072(19) -0.004(2) C11 0.025(2) 0.025(3) 0.020(2) 0.004(2) 0.006(2) -0.002(2) C12 0.020(2) 0.032(3) 0.017(2) -0.003(2) 0.002(2) -0.003(2) C13 0.036(3) 0.030(3) 0.027(3) -0.008(2) 0.000(3) -0.001(2) C14 0.031(3) 0.019(3) 0.019(3) 0.005(2) -0.002(2) -0.002(2) Cl3 0.152(8) 0.134(9) 0.226(14) 0.090(8) -0.077(8) -0.073(7) Cl4 0.116(4) 0.120(5) 0.058(3) 0.025(3) -0.016(3) -0.009(3) C16 0.039(6) 0.054(9) 0.058(9) -0.017(7) -0.007(6) 0.000(6) Cl1 0.092(4) 0.295(13) 0.064(4) 0.034(6) -0.014(4) 0.003(6) Cl2 0.044(3) 0.038(3) 0.093(4) 0.027(3) -0.016(3) -0.003(2) C15 0.076(12) 0.062(13) 0.072(14) -0.018(10) -0.014(10) -0.016(10) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Fe1 2.6211(8) . . yes Te1 Fe2 2.6108(9) . . yes Te1 Fe3 2.6063(9) . . yes Te2 Fe1 2.6075(8) . . yes Te2 Fe2 2.6144(9) . . yes Te2 Fe4 2.6057(9) . . yes Te3 Fe2 2.745(11) . . yes Te3 Fe3 2.626(10) . . yes Te3 Fe4 2.683(10) . . yes Te4 Fe1 2.557(9) . . yes Te4 Fe3 2.767(9) . . yes Te4 Fe4 2.712(9) . . yes As1 Fe1 2.3935(10) . . yes As1 Fe3 2.3947(9) . . yes As1 Fe4 2.3942(9) . . yes As1 C13 1.941(7) . . yes As2 Fe2 2.3748(10) . . yes As2 Fe3 2.3850(10) . . yes As2 Fe4 2.4026(9) . . yes As2 C14 1.950(5) . . yes Fe1 C1 1.787(6) . . yes Fe1 C2 1.790(5) . . yes Fe1 C3 1.803(7) . . yes Fe2 C4 1.825(5) . . yes Fe2 C5 1.796(6) . . yes Fe2 C6 1.778(5) . . yes Fe3 C7 1.806(5) . . yes Fe3 C8 1.798(5) . . yes Fe3 C9 1.781(5) . . yes Fe4 C10 1.807(5) . . yes Fe4 C11 1.793(5) . . yes Fe4 C12 1.803(5) . . yes Cl3 C16 1.67(2) . . yes Cl4 C16 1.692(15) . . yes Cl1 C15 1.58(2) . . yes Cl2 C15 2.05(2) . . yes O1 C1 1.134(7) . . yes O2 C2 1.127(7) . . yes O3 C3 1.142(8) . . yes O4 C4 1.123(6) . . yes O5 C5 1.135(7) . . yes O6 C6 1.134(7) . . yes O7 C7 1.130(7) . . yes O8 C8 1.127(7) . . yes O9 C9 1.117(8) . . yes O10 C10 1.134(6) . . yes O11 C11 1.112(6) . . yes O12 C12 1.137(7) . . yes C13 H3 0.9800 . . no C13 H2 0.9800 . . no C13 H1 0.9800 . . no C14 H6 0.9800 . . no C14 H5 0.9800 . . no C14 H4 0.9800 . . no C16 H10 0.9900 . . no C16 H9 0.9900 . . no C15 H7 0.9900 . . no C15 H8 0.9900 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Te1 Fe2 97.50(3) . . . yes Fe1 Te1 Fe3 93.34(3) . . . yes Fe2 Te1 Fe3 93.07(3) . . . yes Fe1 Te2 Fe2 97.76(3) . . . yes Fe1 Te2 Fe4 93.72(3) . . . yes Fe2 Te2 Fe4 93.45(3) . . . yes Fe2 Te3 Fe3 89.6(3) . . . yes Fe2 Te3 Fe4 88.9(3) . . . yes Fe3 Te3 Fe4 90.0(3) . . . yes Fe1 Te4 Fe3 91.1(3) . . . yes Fe1 Te4 Fe4 92.4(3) . . . yes Fe3 Te4 Fe4 86.5(3) . . . yes Fe1 As1 Fe3 105.16(3) . . . yes Fe1 As1 Fe4 105.23(3) . . . yes Fe1 As1 C13 114.23(19) . . . yes Fe3 As1 Fe4 103.27(4) . . . yes Fe3 As1 C13 113.99(19) . . . yes Fe4 As1 C13 113.85(19) . . . yes Fe2 As2 Fe3 105.41(3) . . . yes Fe2 As2 Fe4 105.42(3) . . . yes Fe2 As2 C14 112.20(16) . . . yes Fe3 As2 Fe4 103.31(3) . . . yes Fe3 As2 C14 114.02(15) . . . yes Fe4 As2 C14 115.47(15) . . . yes Te1 Fe1 Te2 82.29(2) . . . yes Te1 Fe1 As1 79.48(3) . . . yes Te1 Fe1 C1 89.59(18) . . . yes Te1 Fe1 C2 169.52(16) . . . yes Te1 Fe1 C3 93.12(16) . . . yes Te2 Fe1 As1 79.32(3) . . . yes Te2 Fe1 C1 167.42(19) . . . yes Te2 Fe1 C2 90.91(16) . . . yes Te2 Fe1 C3 92.25(16) . . . yes Te4 Fe1 C1 81.8(3) . . . yes Te4 Fe1 C2 82.0(3) . . . yes Te4 Fe1 C3 177.1(3) . . . yes As1 Fe1 C1 89.80(18) . . . yes As1 Fe1 C2 91.47(17) . . . yes As1 Fe1 C3 169.39(16) . . . yes C1 Fe1 C2 95.7(2) . . . yes C1 Fe1 C3 97.8(2) . . . yes C2 Fe1 C3 95.1(2) . . . yes Te1 Fe2 Te2 82.36(3) . . . yes Te1 Fe2 As2 79.65(3) . . . yes Te1 Fe2 C4 94.12(15) . . . yes Te1 Fe2 C5 90.88(19) . . . yes Te1 Fe2 C6 164.99(17) . . . yes Te2 Fe2 As2 79.52(3) . . . yes Te2 Fe2 C4 91.08(16) . . . yes Te2 Fe2 C5 169.93(18) . . . yes Te2 Fe2 C6 89.54(16) . . . yes Te3 Fe2 C4 178.2(3) . . . yes Te3 Fe2 C5 84.3(3) . . . yes Te3 Fe2 C6 79.8(3) . . . yes As2 Fe2 C4 169.29(16) . . . yes As2 Fe2 C5 91.96(17) . . . yes As2 Fe2 C6 86.49(17) . . . yes C4 Fe2 C5 96.9(2) . . . yes C4 Fe2 C6 98.7(2) . . . yes C5 Fe2 C6 95.3(2) . . . yes Te1 Fe3 As1 79.75(3) . . . yes Te1 Fe3 As2 79.56(3) . . . yes Te1 Fe3 C7 92.19(17) . . . yes Te1 Fe3 C8 93.30(17) . . . yes Te1 Fe3 C9 168.33(17) . . . yes Te3 Fe3 Te4 91.8(3) . . . yes Te3 Fe3 C7 86.3(3) . . . yes Te3 Fe3 C8 175.0(3) . . . yes Te3 Fe3 C9 81.4(3) . . . yes Te4 Fe3 C7 177.1(2) . . . yes Te4 Fe3 C8 84.6(2) . . . yes Te4 Fe3 C9 86.9(3) . . . yes As1 Fe3 As2 74.68(3) . . . yes As1 Fe3 C7 167.05(17) . . . yes As1 Fe3 C8 93.10(16) . . . yes As1 Fe3 C9 91.54(18) . . . yes As2 Fe3 C7 93.99(16) . . . yes As2 Fe3 C8 166.70(16) . . . yes As2 Fe3 C9 90.70(18) . . . yes C7 Fe3 C8 97.5(2) . . . yes C7 Fe3 C9 94.9(2) . . . yes C8 Fe3 C9 94.9(3) . . . yes Te2 Fe4 As1 79.34(3) . . . yes Te2 Fe4 As2 79.20(3) . . . yes Te2 Fe4 C10 91.74(17) . . . yes Te2 Fe4 C11 168.66(17) . . . yes Te2 Fe4 C12 91.41(17) . . . yes Te3 Fe4 Te4 91.7(3) . . . yes Te3 Fe4 C10 87.8(3) . . . yes Te3 Fe4 C11 83.6(3) . . . yes Te3 Fe4 C12 176.8(3) . . . yes Te4 Fe4 C10 177.0(3) . . . yes Te4 Fe4 C11 85.9(2) . . . yes Te4 Fe4 C12 85.3(2) . . . yes As1 Fe4 As2 74.37(3) . . . yes As1 Fe4 C10 166.79(17) . . . yes As1 Fe4 C11 90.82(16) . . . yes As1 Fe4 C12 94.70(16) . . . yes As2 Fe4 C10 94.51(16) . . . yes As2 Fe4 C11 92.80(16) . . . yes As2 Fe4 C12 166.65(16) . . . yes C10 Fe4 C11 96.9(2) . . . yes C10 Fe4 C12 95.3(2) . . . yes C11 Fe4 C12 95.1(2) . . . yes Fe1 C1 O1 176.8(5) . . . yes Fe1 C2 O2 178.1(5) . . . yes Fe1 C3 O3 177.5(4) . . . yes Fe2 C4 O4 178.6(4) . . . yes Fe2 C5 O5 178.5(5) . . . yes Fe2 C6 O6 175.2(5) . . . yes Fe3 C7 O7 177.6(5) . . . yes Fe3 C8 O8 177.9(5) . . . yes Fe3 C9 O9 179.7(6) . . . yes Fe4 C10 O10 178.6(5) . . . yes Fe4 C11 O11 179.5(3) . . . yes Fe4 C12 O12 179.3(4) . . . yes As1 C13 H1 109.00 . . . no As1 C13 H2 109.00 . . . no As1 C13 H3 109.00 . . . no H1 C13 H2 110.00 . . . no H1 C13 H3 109.00 . . . no H2 C13 H3 109.00 . . . no As2 C14 H4 109.00 . . . no As2 C14 H5 110.00 . . . no As2 C14 H6 109.00 . . . no H4 C14 H5 109.00 . . . no H4 C14 H6 109.00 . . . no H5 C14 H6 109.00 . . . no Cl3 C16 Cl4 103.8(10) . . . yes Cl3 C16 H9 111.00 . . . no Cl3 C16 H10 111.00 . . . no Cl4 C16 H9 111.00 . . . no Cl4 C16 H10 111.00 . . . no H9 C16 H10 109.00 . . . no Cl1 C15 Cl2 117.7(12) . . . yes Cl1 C15 H7 108.00 . . . no Cl1 C15 H8 108.00 . . . no Cl2 C15 H7 108.00 . . . no Cl2 C15 H8 108.00 . . . no H7 C15 H8 107.00 . . . no 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 Fe2 Te1 Fe1 Te2 2.27(3) . . . . no Fe3 Te1 Fe1 Te2 -91.28(3) . . . . no Fe2 Te1 Fe1 As1 82.76(3) . . . . no Fe3 Te1 Fe1 As1 -10.78(3) . . . . no Fe2 Te1 Fe1 C1 172.63(18) . . . . no Fe3 Te1 Fe1 C1 79.09(18) . . . . no Fe2 Te1 Fe1 C3 -89.59(16) . . . . no Fe3 Te1 Fe1 C3 176.87(16) . . . . no Fe1 Te1 Fe2 As2 -82.93(3) . . . . no Fe3 Te1 Fe2 As2 10.85(3) . . . . no Fe1 Te1 Fe3 As1 10.77(3) . . . . no Fe2 Te1 Fe3 As1 -86.94(3) . . . . no Fe1 Te1 Fe3 As2 86.90(3) . . . . no Fe1 Te1 Fe2 Te2 -2.26(3) . . . . no Fe3 Te1 Fe2 Te2 91.52(3) . . . . no Fe2 Te1 Fe3 As2 -10.81(3) . . . . no Fe1 Te1 Fe3 C7 -179.44(16) . . . . no Fe1 Te1 Fe2 C4 88.28(16) . . . . no Fe3 Te1 Fe2 C4 -177.94(16) . . . . no Fe1 Te1 Fe2 C5 -174.77(17) . . . . no Fe3 Te1 Fe2 C5 -80.98(17) . . . . no Fe2 Te1 Fe3 C7 82.85(16) . . . . no Fe1 Te1 Fe3 C8 -81.80(16) . . . . no Fe2 Te1 Fe3 C8 -179.50(16) . . . . no Fe1 Te2 Fe2 Te1 2.27(3) . . . . no Fe2 Te2 Fe1 Te1 -2.26(3) . . . . no Fe4 Te2 Fe1 Te1 91.74(3) . . . . no Fe2 Te2 Fe1 C2 -174.26(17) . . . . no Fe4 Te2 Fe1 C2 -80.26(17) . . . . no Fe4 Te2 Fe2 Te1 -91.97(3) . . . . no Fe1 Te2 Fe2 As2 83.09(3) . . . . no Fe4 Te2 Fe2 As2 -11.15(3) . . . . no Fe2 Te2 Fe1 As1 -82.94(3) . . . . no Fe4 Te2 Fe1 As1 11.07(3) . . . . no Fe2 Te2 Fe4 C12 -178.53(16) . . . . no Fe1 Te2 Fe2 C6 169.61(17) . . . . no Fe4 Te2 Fe2 C6 75.37(17) . . . . no Fe2 Te2 Fe1 C3 90.58(16) . . . . no Fe4 Te2 Fe1 C3 -175.42(16) . . . . no Fe2 Te2 Fe4 As2 11.03(3) . . . . no Fe1 Te2 Fe2 C4 -91.74(16) . . . . no Fe4 Te2 Fe2 C4 174.02(16) . . . . no Fe1 Te2 Fe4 C12 83.46(16) . . . . no Fe2 Te2 Fe4 As1 86.95(3) . . . . no Fe1 Te2 Fe4 As2 -86.99(3) . . . . no Fe2 Te2 Fe4 C10 -83.24(16) . . . . no Fe1 Te2 Fe4 As1 -11.06(3) . . . . no Fe1 Te2 Fe4 C10 178.75(16) . . . . no Fe4 As1 Fe1 C1 173.86(18) . . . . no C13 As1 Fe1 C1 48.3(3) . . . . no C13 As1 Fe1 Te2 -138.1(2) . . . . no Fe3 As1 Fe1 C1 -77.46(18) . . . . no Fe1 As1 Fe3 As2 -94.08(3) . . . . no Fe4 As1 Fe3 As2 16.01(3) . . . . no C13 As1 Fe3 As2 140.0(2) . . . . no Fe1 As1 Fe3 C8 80.58(17) . . . . no Fe4 As1 Fe1 Te2 -12.48(3) . . . . no Fe4 As1 Fe3 Te1 97.88(3) . . . . no C13 As1 Fe3 Te1 -138.1(2) . . . . no C13 As1 Fe4 C12 47.8(3) . . . . no C13 As1 Fe3 C9 49.7(3) . . . . no Fe3 As1 Fe1 Te1 12.16(3) . . . . no Fe4 As1 Fe1 Te1 -96.52(3) . . . . no C13 As1 Fe1 Te1 137.9(2) . . . . no Fe3 As1 Fe1 Te2 96.20(3) . . . . no Fe1 As1 Fe3 Te1 -12.21(3) . . . . no Fe1 As1 Fe4 Te2 12.48(3) . . . . no Fe3 As1 Fe4 Te2 -97.55(3) . . . . no C13 As1 Fe4 Te2 138.3(2) . . . . no Fe1 As1 Fe4 As2 94.13(3) . . . . no Fe3 As1 Fe4 As2 -15.91(3) . . . . no Fe4 As1 Fe3 C8 -169.33(17) . . . . no C13 As1 Fe3 C8 -45.3(3) . . . . no Fe1 As1 Fe3 C9 175.61(19) . . . . no Fe4 As1 Fe3 C9 -74.30(19) . . . . no C13 As1 Fe1 C2 -47.4(3) . . . . no Fe3 As1 Fe4 C12 171.90(17) . . . . no Fe1 As1 Fe4 C11 -173.20(16) . . . . no Fe3 As1 Fe1 C2 -173.15(16) . . . . no C13 As1 Fe4 As2 -140.0(2) . . . . no Fe1 As1 Fe4 C12 -78.07(17) . . . . no C13 As1 Fe4 C11 -47.4(3) . . . . no Fe4 As1 Fe1 C2 78.18(16) . . . . no Fe3 As1 Fe4 C11 76.77(16) . . . . no Fe4 As2 Fe2 Te2 12.54(3) . . . . no C14 As2 Fe2 C6 48.8(2) . . . . no Fe3 As2 Fe2 Te2 -96.35(3) . . . . no Fe4 As2 Fe2 C6 -77.65(16) . . . . no Fe4 As2 Fe2 C5 -172.88(19) . . . . no C14 As2 Fe2 Te2 139.00(17) . . . . no Fe3 As2 Fe2 C5 78.23(19) . . . . no C14 As2 Fe2 Te1 -136.95(17) . . . . no Fe4 As2 Fe3 Te1 -98.07(3) . . . . no C14 As2 Fe3 Te1 135.82(17) . . . . no Fe2 As2 Fe3 As1 94.45(3) . . . . no Fe4 As2 Fe3 As1 -15.95(3) . . . . no C14 As2 Fe2 C5 -46.4(3) . . . . no Fe3 As2 Fe2 C6 173.47(16) . . . . no Fe4 As2 Fe3 C7 170.44(17) . . . . no C14 As2 Fe3 C7 44.3(2) . . . . no Fe2 As2 Fe3 C9 -174.14(18) . . . . no Fe4 As2 Fe3 C9 75.45(19) . . . . no C14 As2 Fe3 C9 -50.7(3) . . . . no C14 As2 Fe3 As1 -142.06(17) . . . . no Fe2 As2 Fe3 C7 -79.16(17) . . . . no Fe4 As2 Fe2 Te1 96.59(3) . . . . no Fe2 As2 Fe3 Te1 12.33(3) . . . . no Fe3 As2 Fe2 Te1 -12.31(3) . . . . no Fe2 As2 Fe4 Te2 -12.59(3) . . . . no Fe3 As2 Fe4 Te2 97.80(3) . . . . no C14 As2 Fe4 Te2 -137.02(17) . . . . no Fe2 As2 Fe4 As1 -94.42(4) . . . . no Fe3 As2 Fe4 As1 15.98(3) . . . . no C14 As2 Fe4 As1 141.15(17) . . . . no Fe2 As2 Fe4 C10 78.32(17) . . . . no Fe3 As2 Fe4 C10 -171.28(17) . . . . no C14 As2 Fe4 C10 -46.1(2) . . . . no Fe2 As2 Fe4 C11 175.51(16) . . . . no Fe3 As2 Fe4 C11 -74.09(16) . . . . no C14 As2 Fe4 C11 51.1(2) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 Te2 3.4404(7) . . no Te1 As1 3.2104(8) . . no Te1 As2 3.1982(8) . . no Te1 C1 3.162(6) . . no Te1 C3 3.261(5) . . no Te1 C4 3.291(5) . . no Te1 C5 3.192(6) . . no Te1 C7 3.227(5) . . no Te1 C8 3.251(5) . . no Te1 Te1 3.6741(8) . 3_656 no Te1 O3 3.569(4) . 3_656 no Te1 O4 3.669(4) . 3_656 no Te1 C3 3.825(6) . 3_656 no Te1 C4 3.907(5) . 3_656 no Te2 Te1 3.4404(7) . . no Te2 As1 3.1959(8) . . no Te2 As2 3.1962(8) . . no Te2 C2 3.186(5) . . no Te2 C3 3.228(5) . . no Te2 C4 3.216(5) . . no Te2 C6 3.150(5) . . no Te2 C10 3.216(5) . . no Te2 C12 3.205(5) . . no Te2 Te2 3.7959(8) . 3_756 no Te2 O3 3.771(4) . 3_756 no Te2 C2 3.912(5) . 3_756 no Te2 C3 3.855(5) . 3_756 no Te3 Te4 3.872(14) . . no Te3 O6 3.559(11) . . no Te3 O9 3.608(12) . . no Te3 O11 3.737(11) . . no Te3 C5 3.128(12) . . no Te3 C6 2.996(12) . . no Te3 C7 3.089(11) . . no Te3 C9 2.944(12) . . no Te3 C10 3.178(11) . . no Te3 C11 3.058(11) . . no Te4 Te3 3.872(14) . . no Te4 O1 3.555(10) . . no Te4 O2 3.620(10) . . no Te4 C1 2.904(11) . . no Te4 C2 2.911(10) . . no Te4 C8 3.155(10) . . no Te4 C9 3.208(11) . . no Te4 C11 3.143(10) . . no Te4 C12 3.130(10) . . no As1 Te1 3.2104(8) . . no As1 Te2 3.1959(8) . . no As1 As2 2.8992(10) . . no As1 C1 2.982(6) . . no As1 C2 3.025(5) . . no As1 C8 3.072(5) . . no As1 C9 3.022(6) . . no As1 C11 3.011(5) . . no As1 C12 3.113(5) . . no As2 Te1 3.1982(8) . . no As2 Te2 3.1962(8) . . no As2 As1 2.8992(10) . . no As2 C5 3.026(5) . . no As2 C6 2.878(5) . . no As2 C7 3.090(5) . . no As2 C9 2.994(5) . . no As2 C10 3.118(5) . . no As2 C11 3.067(5) . . no Cl1 Cl1 2.837(13) . 3_657 no Cl2 O1 3.261(11) . . no Cl2 C1 3.488(12) . . no Cl2 O7 3.454(10) . 4_555 no Cl2 C7 3.549(10) . 4_555 no Cl3 C7 3.640(15) . 4_555 no Cl4 Cl4 2.410(7) . 3_757 no Cl4 C16 3.534(14) . 3_757 no Cl4 O9 3.295(8) . 2_646 no Cl4 O6 3.188(7) . 1_556 no O1 O10 3.155(6) . 4_455 no O1 Cl2 3.261(11) . . no O1 O4 3.184(6) . 3_656 no O1 C11 3.145(7) . 4_455 no O1 O8 3.224(7) . . no O1 O11 3.007(6) . 4_455 no O1 C10 3.216(7) . 4_455 no O2 O9 3.157(8) . 4_555 no O2 C14 3.289(7) . 4_555 no O3 Te2 3.771(4) . 3_756 no O3 O5 3.192(6) . 3_656 no O3 C10 3.366(7) . 3_756 no O3 Te1 3.569(4) . 3_656 no O4 O12 3.175(6) . 3_756 no O4 O1 3.184(6) . 3_656 no O4 Te1 3.669(4) . 3_656 no O5 O3 3.192(6) . 3_656 no O5 C16 3.385(13) . 3_656 no O6 C10 3.287(6) . . no O6 Cl4 3.188(7) . 1_554 no O6 O9 2.785(6) . 2_645 no O6 O10 3.055(5) . . no O6 C16 3.299(13) . 3_756 no O7 Cl2 3.454(10) . 4_454 no O7 O10 3.143(6) . 1_455 no O8 O10 3.032(6) . 4_455 no O8 C14 3.287(7) . 4_455 no O8 O1 3.224(7) . . no O9 O11 2.963(6) . . no O9 O2 3.157(8) . 4_454 no O9 C6 3.162(8) . 2_655 no O9 Cl4 3.295(8) . 2_656 no O9 C11 3.287(7) . . no O9 O6 2.785(6) . 2_655 no O10 C16 3.337(14) . 3_756 no O10 O1 3.155(6) . 4_554 no O10 O7 3.143(6) . 1_655 no O10 O8 3.032(6) . 4_554 no O10 O6 3.055(5) . . no O11 O1 3.007(6) . 4_554 no O11 C9 3.316(7) . . no O11 O9 2.963(6) . . no O11 C4 3.354(7) . 2_655 no O12 C14 3.345(7) . 4_555 no O12 O4 3.175(6) . 3_756 no O2 H5 2.7000 . 4_555 no O4 H5 2.5800 . 2_645 no O5 H10 2.5100 . 3_656 no O6 H8 2.7400 . 1_554 no O6 H9 2.4200 . 3_756 no O6 H6 2.8700 . . no O8 H6 2.5100 . 4_455 no O10 H9 2.9100 . 3_756 no O10 H1 2.7500 . 4_554 no C1 C2 2.652(7) . . no C1 Te1 3.162(6) . . no C1 Te4 2.904(11) . . no C1 C3 2.705(9) . . no C1 C8 3.461(8) . . no C1 C13 3.500(9) . . no C1 Cl2 3.488(12) . . no C1 As1 2.982(6) . . no C1 Fe3 3.978(6) . . no C2 Te2 3.186(5) . . no C2 Te4 2.911(10) . . no C2 As1 3.025(5) . . no C2 C12 3.510(7) . . no C2 C13 3.538(9) . . no C2 Te2 3.912(5) . 3_756 no C2 C1 2.652(7) . . no C2 C3 2.652(8) . . no C3 Te1 3.825(6) . 3_656 no C3 Te1 3.261(5) . . no C3 C1 2.705(9) . . no C3 C2 2.652(8) . . no C3 Te2 3.855(5) . 3_756 no C3 Te2 3.228(5) . . no C4 Te2 3.216(5) . . no C4 C6 2.733(7) . . no C4 O11 3.354(7) . 2_645 no C4 C5 2.709(8) . . no C4 Te1 3.907(5) . 3_656 no C4 Te1 3.291(5) . . no C5 C14 3.476(8) . . no C5 Te1 3.192(6) . . no C5 As2 3.026(5) . . no C5 Te3 3.128(12) . . no C5 C7 3.509(8) . . no C5 C6 2.643(7) . . no C5 C4 2.709(8) . . no C6 Te2 3.150(5) . . no C6 As2 2.878(5) . . no C6 C4 2.733(7) . . no C6 C5 2.643(7) . . no C6 Fe4 3.898(5) . . no C6 Te3 2.996(12) . . no C6 C14 3.347(7) . . no C6 O9 3.162(8) . 2_645 no C6 C10 3.380(7) . . no C7 C8 2.710(7) . . no C7 As2 3.090(5) . . no C7 Te3 3.089(11) . . no C7 Cl2 3.549(10) . 4_454 no C7 Te1 3.227(5) . . no C7 C5 3.509(8) . . no C7 Cl3 3.640(15) . 4_454 no C7 C14 3.570(7) . . no C7 C9 2.643(7) . . no C8 C7 2.710(7) . . no C8 Te4 3.155(10) . . no C8 As1 3.072(5) . . no C8 Te1 3.251(5) . . no C8 C9 2.638(8) . . no C8 C1 3.461(8) . . no C8 C13 3.557(8) . . no C9 As2 2.994(5) . . no C9 C8 2.638(8) . . no C9 C14 3.545(8) . . no C9 C7 2.643(7) . . no C9 Fe4 3.913(5) . . no C9 O11 3.316(7) . . no C9 Te3 2.944(12) . . no C9 C11 3.260(7) . . no C9 C13 3.560(9) . . no C9 As1 3.022(6) . . no C9 Te4 3.208(11) . . no C10 Te2 3.216(5) . . no C10 As2 3.118(5) . . no C10 O6 3.287(6) . . no C10 C12 2.667(7) . . no C10 C6 3.380(7) . . no C10 C11 2.695(7) . . no C10 O1 3.216(7) . 4_554 no C10 Te3 3.178(11) . . no C10 O3 3.366(7) . 3_756 no C11 C12 2.652(7) . . no C11 Te4 3.143(10) . . no C11 As2 3.067(5) . . no C11 Fe3 3.944(5) . . no C11 C13 3.510(8) . . no C11 C9 3.260(7) . . no C11 C10 2.695(7) . . no C11 O9 3.287(7) . . no C11 Te3 3.058(11) . . no C11 As1 3.011(5) . . no C11 O1 3.145(7) . 4_554 no C12 C11 2.652(7) . . no C12 Te2 3.205(5) . . no C12 Te4 3.130(10) . . no C12 C10 2.667(7) . . no C12 C2 3.510(7) . . no C12 As1 3.113(5) . . no C14 O2 3.289(7) . 4_454 no C14 O8 3.287(7) . 4_554 no C14 O12 3.345(7) . 4_454 no C16 O10 3.337(14) . 3_756 no C16 O5 3.385(14) . 3_656 no C16 O6 3.299(13) . 3_756 no C16 Cl4 3.534(14) . 3_757 no C1 H1 3.1000 . . no C6 H6 2.9300 . . no H1 C1 3.1000 . . no H1 O10 2.7500 . 4_455 no H3 H4 2.3200 . 4_555 no H4 H3 2.3200 . 4_454 no H5 O2 2.7000 . 4_454 no H5 O4 2.5800 . 2_655 no H6 C6 2.9300 . . no H6 O8 2.5100 . 4_554 no H6 O6 2.8700 . . no H8 O6 2.7400 . 1_556 no H9 O10 2.9100 . 3_756 no H9 O6 2.4200 . 3_756 no H10 O5 2.5100 . 3_656 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C14 H5 O4 0.9800 2.5800 3.488(6) 154.00 2_655 yes C14 H6 O8 0.9800 2.5100 3.287(7) 136.00 4_554 yes C16 H9 O6 0.9900 2.4200 3.299(13) 147.00 3_756 yes C16 H10 O5 0.9900 2.5100 3.385(14) 147.00 3_656 yes #===END data_2b_mon _database_code_depnum_ccdc_archive 'CCDC 802727' #TrackingRef '- Combined_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H6 As2 Fe4 O12 Te2' _chemical_formula_weight 994.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.2758 1.3314 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.021(3) _cell_length_b 9.977(2) _cell_length_c 19.555(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.08(3) _cell_angle_gamma 90.00 _cell_volume 2540.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 1174 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 22.42 _exptl_crystal_description route _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 3.739 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5538 _exptl_absorpt_correction_T_max 0.7829 _exptl_absorpt_process_details 'program faceit' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15121 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 22.42 _reflns_number_total 6261 _reflns_number_gt 4986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHELXL-97 _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^)+(0.0381P)^2^+1.0052P] 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 6261 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Te1 Te 0.87679(2) 1.03595(3) 0.039415(13) 0.02171(7) Uani 1 1 d . . . Te2 Te 0.62293(2) 0.94168(3) 0.033160(14) 0.02456(7) Uani 1 1 d . . . Fe1 Fe 0.88693(5) 1.01127(7) 0.17283(3) 0.02527(14) Uani 1 1 d . . . Fe2 Fe 0.60931(5) 0.90633(7) 0.16626(3) 0.02794(15) Uani 1 1 d . . . Fe4 Fe 0.79287(5) 0.79953(6) 0.02222(3) 0.02194(13) Uani 1 1 d . . . Fe3 Fe 0.70770(5) 1.17950(6) 0.04493(3) 0.02031(13) Uani 1 1 d . . . As1 As 0.78006(4) 0.82046(4) 0.14473(2) 0.02234(10) Uani 1 1 d . . . C1 C 0.8116(5) 0.6556(5) 0.1956(2) 0.0419(13) Uani 1 1 d . . . H1A H 0.7618 0.5870 0.1840 0.063 Uiso 1 1 calc R . . H1B H 0.8087 0.6736 0.2443 0.063 Uiso 1 1 calc R . . H1C H 0.8799 0.6248 0.1836 0.063 Uiso 1 1 calc R . . As2 As 0.71687(3) 1.10320(4) 0.160784(19) 0.02053(9) Uani 1 1 d . . . C2 C 0.6818(5) 1.2441(5) 0.2270(2) 0.0397(13) Uani 1 1 d . . . H2A H 0.7335 1.3141 0.2255 0.060 Uiso 1 1 calc R . . H2B H 0.6793 1.2061 0.2726 0.060 Uiso 1 1 calc R . . H2C H 0.6153 1.2818 0.2155 0.060 Uiso 1 1 calc R . . C3 C 0.8682(5) 0.9961(6) 0.2634(3) 0.0408(13) Uani 1 1 d . . . O3 O 0.8567(4) 0.9926(5) 0.32099(19) 0.0640(14) Uani 1 1 d . . . C4 C 1.0041(5) 0.9118(6) 0.1674(3) 0.0408(12) Uani 1 1 d . . . O4 O 1.0762(4) 0.8487(6) 0.1645(2) 0.0666(14) Uani 1 1 d . . . C5 C 0.9447(5) 1.1758(6) 0.1793(3) 0.0396(12) Uani 1 1 d . . . O5 O 0.9802(4) 1.2791(5) 0.1830(3) 0.0664(14) Uani 1 1 d . . . C6 C 0.5545(5) 0.7412(6) 0.1571(3) 0.0449(13) Uani 1 1 d . . . O6 O 0.5216(4) 0.6345(5) 0.1511(3) 0.0761(16) Uani 1 1 d . . . C7 C 0.4906(4) 1.0023(6) 0.1719(3) 0.0405(12) Uani 1 1 d . . . O7 O 0.4180(4) 1.0635(5) 0.1776(3) 0.0679(14) Uani 1 1 d . . . C8 C 0.6293(5) 0.8942(6) 0.2568(3) 0.0425(13) Uani 1 1 d . . . O8 O 0.6400(4) 0.8855(5) 0.3142(2) 0.0665(15) Uani 1 1 d . . . C9 C 0.7046(5) 1.2048(6) -0.0472(2) 0.0398(12) Uani 1 1 d . . . O9 O 0.7019(5) 1.2210(6) -0.1042(2) 0.0805(18) Uani 1 1 d . . . C10 C 0.5860(4) 1.2601(5) 0.0631(2) 0.0298(10) Uani 1 1 d . . . O10 O 0.5122(3) 1.3142(4) 0.0758(2) 0.0504(10) Uani 1 1 d . . . C11 C 0.7875(4) 1.3216(5) 0.0642(2) 0.0298(10) Uani 1 1 d . . . O11 O 0.8385(3) 1.4102(4) 0.0779(2) 0.0483(10) Uani 1 1 d . . . C12 C 0.7999(4) 0.8255(5) -0.0697(2) 0.0369(12) Uani 1 1 d . . . O12 O 0.8058(4) 0.8429(5) -0.12673(18) 0.0653(14) Uani 1 1 d . . . C13 C 0.7121(4) 0.6520(5) 0.0185(3) 0.0358(11) Uani 1 1 d . . . O13 O 0.6605(4) 0.5610(4) 0.0155(3) 0.0612(13) Uani 1 1 d . . . C14 C 0.9134(4) 0.7130(5) 0.0310(2) 0.0320(10) Uani 1 1 d . . . O14 O 0.9891(3) 0.6560(4) 0.0381(2) 0.0522(11) 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 Te1 0.02009(15) 0.01967(14) 0.02536(13) 0.00046(10) 0.00501(10) 0.00091(11) Te2 0.02120(16) 0.02221(14) 0.03027(14) -0.00362(11) -0.00581(10) 0.00103(11) Fe1 0.0251(4) 0.0253(3) 0.0254(3) -0.0010(2) -0.0072(2) 0.0029(3) Fe2 0.0259(4) 0.0247(3) 0.0333(3) 0.0029(3) 0.0113(3) -0.0009(3) Fe4 0.0263(4) 0.0176(3) 0.0219(3) -0.0020(2) 0.0004(2) 0.0021(2) Fe3 0.0237(3) 0.0184(3) 0.0189(3) 0.0011(2) -0.0002(2) 0.0027(2) As1 0.0258(2) 0.0206(2) 0.02062(18) 0.00192(15) 0.00210(15) 0.00190(17) C1 0.065(4) 0.030(3) 0.031(2) 0.008(2) -0.001(2) 0.010(3) As2 0.0233(2) 0.0208(2) 0.01754(17) -0.00093(14) 0.00137(14) 0.00168(16) C2 0.053(4) 0.036(3) 0.030(2) -0.013(2) 0.009(2) 0.007(2) C3 0.048(4) 0.038(3) 0.037(3) -0.003(2) -0.013(2) 0.011(2) O3 0.085(4) 0.083(4) 0.0244(18) 0.0015(19) -0.0077(19) 0.025(3) C4 0.035(3) 0.041(3) 0.046(3) 0.001(2) -0.004(2) 0.004(2) O4 0.038(3) 0.082(4) 0.079(3) 0.006(3) -0.004(2) 0.033(3) C5 0.038(3) 0.039(3) 0.042(3) -0.009(2) -0.014(2) 0.000(2) O5 0.069(4) 0.046(3) 0.085(3) -0.010(2) -0.028(3) -0.024(2) C6 0.036(3) 0.039(3) 0.059(3) 0.000(3) 0.015(2) -0.002(2) O6 0.074(4) 0.044(3) 0.110(4) -0.009(3) 0.030(3) -0.025(3) C7 0.034(3) 0.037(3) 0.051(3) -0.002(2) 0.015(2) 0.003(2) O7 0.039(3) 0.066(3) 0.099(4) 0.000(3) 0.018(2) 0.020(2) C8 0.040(3) 0.035(3) 0.053(3) 0.007(2) 0.024(2) 0.000(2) O8 0.086(4) 0.080(4) 0.034(2) 0.017(2) 0.026(2) 0.007(3) C9 0.045(3) 0.046(3) 0.028(2) 0.004(2) -0.001(2) 0.008(3) O9 0.102(5) 0.115(5) 0.0245(19) 0.019(2) -0.001(2) 0.021(4) C10 0.033(3) 0.027(2) 0.030(2) 0.0014(18) -0.0024(18) 0.003(2) O10 0.033(2) 0.049(3) 0.069(3) -0.009(2) 0.0036(18) 0.0160(19) C11 0.034(3) 0.022(2) 0.033(2) 0.0022(18) 0.0004(18) 0.0057(19) O11 0.050(3) 0.0252(19) 0.070(3) -0.0036(18) -0.004(2) -0.0082(18) C12 0.043(3) 0.037(3) 0.031(2) -0.004(2) 0.000(2) 0.005(2) O12 0.092(4) 0.080(4) 0.0235(18) -0.0010(19) 0.0051(19) 0.006(3) C13 0.038(3) 0.023(2) 0.046(3) 0.003(2) -0.008(2) 0.005(2) O13 0.048(3) 0.026(2) 0.109(4) 0.003(2) -0.024(2) -0.0078(19) C14 0.035(3) 0.025(2) 0.037(2) 0.0012(19) 0.0032(19) 0.003(2) O14 0.035(3) 0.039(2) 0.083(3) 0.004(2) 0.008(2) 0.0127(19) _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 Te1 Fe4 2.6210(8) . ? Te1 Fe1 2.6237(8) . ? Te1 Fe3 2.6290(8) . ? Te2 Fe3 2.6269(8) . ? Te2 Fe2 2.6328(9) . ? Te2 Fe4 2.6372(8) . ? Fe1 C3 1.794(5) . ? Fe1 C5 1.810(6) . ? Fe1 C4 1.823(6) . ? Fe1 As2 2.4081(9) . ? Fe1 As1 2.4208(9) . ? Fe2 C8 1.794(6) . ? Fe2 C6 1.804(6) . ? Fe2 C7 1.822(6) . ? Fe2 As2 2.4148(9) . ? Fe2 As1 2.4201(9) . ? Fe4 C14 1.799(5) . ? Fe4 C13 1.811(6) . ? Fe4 C12 1.819(5) . ? Fe4 As1 2.4108(8) . ? Fe3 C11 1.797(5) . ? Fe3 C10 1.812(5) . ? Fe3 C9 1.819(5) . ? Fe3 As2 2.3928(8) . ? As1 C1 1.965(5) . ? As2 C2 1.965(4) . ? C3 O3 1.138(6) . ? C4 O4 1.133(7) . ? C5 O5 1.132(7) . ? C6 O6 1.154(7) . ? C7 O7 1.131(7) . ? C8 O8 1.134(7) . ? C9 O9 1.128(6) . ? C10 O10 1.130(6) . ? C11 O11 1.138(6) . ? C12 O12 1.131(6) . ? C13 O13 1.131(7) . ? C14 O14 1.146(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe4 Te1 Fe1 93.64(2) . . ? Fe4 Te1 Fe3 98.42(3) . . ? Fe1 Te1 Fe3 92.94(3) . . ? Fe3 Te2 Fe2 93.63(2) . . ? Fe3 Te2 Fe4 98.07(3) . . ? Fe2 Te2 Fe4 93.78(3) . . ? C3 Fe1 C5 93.7(3) . . ? C3 Fe1 C4 97.3(3) . . ? C5 Fe1 C4 98.6(3) . . ? C3 Fe1 As2 90.12(19) . . ? C5 Fe1 As2 92.48(19) . . ? C4 Fe1 As2 166.17(19) . . ? C3 Fe1 As1 94.5(2) . . ? C5 Fe1 As1 165.40(17) . . ? C4 Fe1 As1 92.26(19) . . ? As2 Fe1 As1 75.47(3) . . ? C3 Fe1 Te1 169.28(19) . . ? C5 Fe1 Te1 90.27(17) . . ? C4 Fe1 Te1 91.94(17) . . ? As2 Fe1 Te1 79.75(3) . . ? As1 Fe1 Te1 79.63(3) . . ? C8 Fe2 C6 95.3(3) . . ? C8 Fe2 C7 95.6(3) . . ? C6 Fe2 C7 98.7(3) . . ? C8 Fe2 As2 90.89(19) . . ? C6 Fe2 As2 165.39(18) . . ? C7 Fe2 As2 93.87(18) . . ? C8 Fe2 As1 90.92(19) . . ? C6 Fe2 As1 91.30(19) . . ? C7 Fe2 As1 167.53(18) . . ? As2 Fe2 As1 75.36(3) . . ? C8 Fe2 Te2 167.24(19) . . ? C6 Fe2 Te2 92.97(19) . . ? C7 Fe2 Te2 92.75(18) . . ? As2 Fe2 Te2 78.89(3) . . ? As1 Fe2 Te2 79.18(3) . . ? C14 Fe4 C13 96.9(2) . . ? C14 Fe4 C12 96.7(2) . . ? C13 Fe4 C12 96.1(2) . . ? C14 Fe4 As1 90.46(15) . . ? C13 Fe4 As1 93.97(17) . . ? C12 Fe4 As1 166.81(17) . . ? C14 Fe4 Te1 93.23(16) . . ? C13 Fe4 Te1 168.20(17) . . ? C12 Fe4 Te1 88.69(18) . . ? As1 Fe4 Te1 79.86(2) . . ? C14 Fe4 Te2 169.16(15) . . ? C13 Fe4 Te2 87.31(17) . . ? C12 Fe4 Te2 92.72(18) . . ? As1 Fe4 Te2 79.26(3) . . ? Te1 Fe4 Te2 81.69(2) . . ? C11 Fe3 C10 96.5(2) . . ? C11 Fe3 C9 96.3(2) . . ? C10 Fe3 C9 96.6(2) . . ? C11 Fe3 As2 91.42(15) . . ? C10 Fe3 As2 89.89(14) . . ? C9 Fe3 As2 169.29(18) . . ? C11 Fe3 Te2 166.81(15) . . ? C10 Fe3 Te2 92.92(16) . . ? C9 Fe3 Te2 91.70(19) . . ? As2 Fe3 Te2 79.40(3) . . ? C11 Fe3 Te1 87.39(16) . . ? C10 Fe3 Te1 169.18(14) . . ? C9 Fe3 Te1 93.01(18) . . ? As2 Fe3 Te1 79.91(3) . . ? Te2 Fe3 Te1 81.73(2) . . ? C1 As1 Fe4 114.57(15) . . ? C1 As1 Fe2 113.55(19) . . ? Fe4 As1 Fe2 105.57(4) . . ? C1 As1 Fe1 115.07(19) . . ? Fe4 As1 Fe1 104.66(3) . . ? Fe2 As1 Fe1 102.13(3) . . ? C2 As2 Fe3 112.61(16) . . ? C2 As2 Fe1 114.99(19) . . ? Fe3 As2 Fe1 104.98(4) . . ? C2 As2 Fe2 114.68(18) . . ? Fe3 As2 Fe2 105.82(3) . . ? Fe1 As2 Fe2 102.66(3) . . ? O3 C3 Fe1 176.9(6) . . ? O4 C4 Fe1 179.1(6) . . ? O5 C5 Fe1 179.4(6) . . ? O6 C6 Fe2 178.5(6) . . ? O7 C7 Fe2 177.5(6) . . ? O8 C8 Fe2 178.7(6) . . ? O9 C9 Fe3 179.5(6) . . ? O10 C10 Fe3 177.3(5) . . ? O11 C11 Fe3 178.3(4) . . ? O12 C12 Fe4 178.8(6) . . ? O13 C13 Fe4 178.8(5) . . ? O14 C14 Fe4 178.2(5) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 22.42 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.859 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.149 _vrf_PLAT029_nas1f ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94 RESPONSE: A cusp of data is missing due to datacollection by rotation around the spindle axis only. ; #===END data_2b_ort _database_code_depnum_ccdc_archive 'CCDC 802728' #TrackingRef '- Combined_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H6 As2 Fe4 O12 Te2' _chemical_formula_weight 994.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.2758 1.3314 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.9710 1.0960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ima2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' '-x+1, y+1/2, z+1/2' _cell_length_a 26.694(3) _cell_length_b 16.950(2) _cell_length_c 11.046(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4997.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 1316 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 22.42 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 3.801 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5429 _exptl_absorpt_correction_T_max 0.7962 _exptl_absorpt_process_details 'program faceit' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17892 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 22.42 _reflns_number_total 6323 _reflns_number_gt 5670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHELXL-97 _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^)+(0.0428P)^2^+15.9401P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 6323 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Te1 Te 0.314412(14) 0.02546(2) 0.22127(4) 0.02169(8) Uani 1 1 d . . . As1 As 0.2500 0.06389(5) 0.46168(8) 0.02120(17) Uani 1 2 d S . . C1 C 0.2500 0.1237(6) 0.6131(10) 0.034(2) Uani 1 2 d S . . H1A H 0.2244 0.1642 0.6096 0.051 Uiso 0.50 1 calc PR . . H1B H 0.2825 0.1482 0.6245 0.051 Uiso 0.50 1 calc PR . . H1C H 0.2431 0.0884 0.6802 0.051 Uiso 0.50 1 calc PR . . As2 As 0.2500 -0.10087(5) 0.37548(8) 0.02124(16) Uani 1 2 d S . . C2 C 0.2500 -0.2116(5) 0.4268(10) 0.039(2) Uani 1 2 d S . . H2A H 0.2757 -0.2402 0.3829 0.058 Uiso 0.50 1 calc PR . . H2B H 0.2175 -0.2348 0.4100 0.058 Uiso 0.50 1 calc PR . . H2C H 0.2568 -0.2145 0.5130 0.058 Uiso 0.50 1 calc PR . . Fe1 Fe 0.2500 0.13727(7) 0.27381(12) 0.0205(2) Uani 1 2 d S . . Fe2 Fe 0.2500 -0.08526(7) 0.15955(11) 0.0232(2) Uani 1 2 d S . . Fe3 Fe 0.32059(3) -0.02479(5) 0.44588(8) 0.02313(18) Uani 1 1 d . . . C3 C 0.2500 0.1664(5) 0.1146(9) 0.0297(18) Uani 1 2 d S . . O3 O 0.2500 0.1807(5) 0.0147(8) 0.049(2) Uani 1 2 d S . . C4 C 0.3013(3) 0.2011(4) 0.3213(7) 0.0323(14) Uani 1 1 d . . . O4 O 0.3337(2) 0.2396(4) 0.3494(6) 0.0510(15) Uani 1 1 d . . . C6 C 0.3010(3) -0.1559(4) 0.1486(7) 0.0370(15) Uani 1 1 d . . . O6 O 0.3323(2) -0.2006(4) 0.1441(7) 0.0556(16) Uani 1 1 d . . . C7 C 0.2500 -0.0536(7) -0.0003(11) 0.040(2) Uani 1 2 d S . . O7 O 0.2500 -0.0338(6) -0.0970(9) 0.064(3) Uani 1 2 d S . . C9 C 0.3120(3) -0.0656(4) 0.5938(6) 0.0318(14) Uani 1 1 d . . . O9 O 0.3081(2) -0.0928(4) 0.6870(5) 0.0547(16) Uani 1 1 d . . . C10 C 0.3690(2) -0.0972(4) 0.4037(7) 0.0310(14) Uani 1 1 d . . . O10 O 0.3983(2) -0.1408(3) 0.3789(6) 0.0458(13) Uani 1 1 d . . . C11 C 0.3613(3) 0.0556(4) 0.4924(8) 0.0380(16) Uani 1 1 d . . . O11 O 0.3845(2) 0.1073(4) 0.5263(8) 0.0602(18) Uani 1 1 d . . . Te2 Te 0.437647(14) -0.02676(2) 1.10865(4) 0.02463(9) Uani 1 1 d . . . As3 As 0.48485(2) 0.08345(3) 0.90165(6) 0.02449(13) Uani 1 1 d . . . C12 C 0.4676(3) 0.1714(4) 0.7979(7) 0.0419(19) Uani 1 1 d . . . H12A H 0.4324 0.1841 0.8078 0.063 Uiso 1 1 calc R . . H12B H 0.4740 0.1573 0.7142 0.063 Uiso 1 1 calc R . . H12C H 0.4878 0.2168 0.8197 0.063 Uiso 1 1 calc R . . Fe4 Fe 0.43208(3) -0.03010(5) 0.87116(9) 0.02626(19) Uani 1 1 d . . . Fe5 Fe 0.48010(3) 0.11296(5) 1.11417(9) 0.02367(17) Uani 1 1 d . . . C13 C 0.3769(3) 0.0330(4) 0.8650(8) 0.0367(16) Uani 1 1 d . . . O13 O 0.3436(2) 0.0730(3) 0.8574(7) 0.0589(18) Uani 1 1 d . . . C14 C 0.3986(3) -0.1242(4) 0.8759(8) 0.0425(18) Uani 1 1 d . . . O14 O 0.3779(3) -0.1822(3) 0.8783(7) 0.065(2) Uani 1 1 d . . . C15 C 0.4426(3) -0.0348(4) 0.7095(8) 0.0381(16) Uani 1 1 d . . . O15 O 0.4489(3) -0.0398(4) 0.6101(6) 0.0589(17) Uani 1 1 d . . . C16 C 0.4809(3) 0.1131(4) 1.2803(7) 0.0328(14) Uani 1 1 d . . . O16 O 0.4813(3) 0.1121(4) 1.3811(6) 0.0576(16) Uani 1 1 d . . . C17 C 0.5192(3) 0.1991(4) 1.0935(7) 0.0348(15) Uani 1 1 d . . . O17 O 0.5440(2) 0.2522(3) 1.0776(7) 0.0588(18) Uani 1 1 d . . . C18 C 0.4209(3) 0.1648(4) 1.0964(6) 0.0314(13) Uani 1 1 d . . . O18 O 0.3845(2) 0.1980(3) 1.0849(6) 0.0484(15) 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 Te1 0.01908(16) 0.02158(18) 0.02442(19) 0.00043(16) 0.00282(15) 0.00099(13) As1 0.0215(4) 0.0202(4) 0.0218(4) -0.0008(3) 0.000 0.000 C1 0.043(5) 0.031(4) 0.029(5) -0.012(4) 0.000 0.000 As2 0.0215(4) 0.0190(4) 0.0232(4) 0.0014(3) 0.000 0.000 C2 0.049(6) 0.020(4) 0.048(7) 0.015(4) 0.000 0.000 Fe1 0.0214(5) 0.0154(5) 0.0248(6) 0.0008(4) 0.000 0.000 Fe2 0.0260(6) 0.0218(6) 0.0218(6) -0.0045(5) 0.000 0.000 Fe3 0.0209(4) 0.0238(4) 0.0247(4) 0.0012(3) -0.0038(3) 0.0010(3) C3 0.036(4) 0.024(4) 0.030(5) -0.005(4) 0.000 0.000 O3 0.061(5) 0.047(5) 0.038(4) 0.017(4) 0.000 0.000 C4 0.031(3) 0.033(3) 0.034(3) -0.007(3) 0.004(3) -0.001(3) O4 0.047(3) 0.044(3) 0.062(4) -0.014(3) -0.005(3) -0.020(3) C6 0.041(4) 0.037(4) 0.033(4) -0.003(3) -0.002(3) -0.003(3) O6 0.052(3) 0.048(3) 0.067(4) -0.019(3) -0.003(3) 0.020(3) C7 0.043(6) 0.044(6) 0.032(6) -0.004(5) 0.000 0.000 O7 0.066(6) 0.093(8) 0.032(5) -0.009(5) 0.000 0.000 C9 0.031(3) 0.038(4) 0.026(3) 0.000(3) 0.000(3) -0.004(3) O9 0.054(4) 0.078(5) 0.031(3) 0.014(3) -0.007(3) 0.009(3) C10 0.033(3) 0.028(3) 0.032(3) 0.003(3) -0.004(3) 0.001(2) O10 0.041(3) 0.046(3) 0.050(3) 0.003(3) 0.005(3) 0.019(2) C11 0.034(3) 0.034(3) 0.046(4) -0.002(3) -0.008(3) 0.002(3) O11 0.045(3) 0.041(3) 0.094(5) -0.018(3) -0.021(3) -0.010(3) Te2 0.01998(17) 0.02192(18) 0.0320(2) 0.00389(17) 0.00244(16) 0.00170(13) As3 0.0245(3) 0.0203(3) 0.0287(3) 0.0005(2) 0.0036(3) 0.0028(2) C12 0.053(4) 0.023(3) 0.050(5) 0.020(3) 0.006(4) 0.007(3) Fe4 0.0254(4) 0.0217(4) 0.0316(5) 0.0018(3) -0.0065(4) 0.0017(3) Fe5 0.0243(4) 0.0191(4) 0.0276(4) -0.0015(4) 0.0046(4) 0.0033(3) C13 0.030(3) 0.026(3) 0.053(5) 0.004(3) -0.011(3) -0.002(2) O13 0.036(3) 0.044(3) 0.097(5) 0.001(3) -0.015(3) 0.016(3) C14 0.044(4) 0.034(4) 0.049(5) -0.001(3) -0.021(4) -0.002(3) O14 0.078(4) 0.034(3) 0.084(5) 0.009(3) -0.030(4) -0.021(3) C15 0.040(4) 0.033(4) 0.041(4) 0.001(3) -0.012(3) 0.001(3) O15 0.066(4) 0.077(4) 0.034(3) -0.002(3) -0.021(3) 0.009(3) C16 0.030(3) 0.034(3) 0.034(4) 0.003(3) 0.005(3) 0.002(3) O16 0.060(4) 0.075(4) 0.038(4) 0.002(3) 0.001(3) 0.000(3) C17 0.033(3) 0.033(3) 0.039(4) -0.001(3) 0.013(3) 0.004(3) O17 0.058(4) 0.028(3) 0.091(5) -0.009(3) 0.025(4) -0.013(3) C18 0.036(3) 0.032(3) 0.026(3) 0.003(3) 0.004(3) 0.000(3) O18 0.041(3) 0.039(3) 0.065(4) 0.010(3) 0.000(3) 0.019(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 Te1 Fe1 2.6240(10) . ? Te1 Fe3 2.6283(11) . ? Te1 Fe2 2.6350(11) . ? As1 C1 1.956(9) . ? As1 Fe3 2.4166(11) 4 ? As1 Fe3 2.4166(11) . ? As1 Fe1 2.4195(15) . ? As2 C2 1.960(9) . ? As2 Fe2 2.3998(15) . ? As2 Fe3 2.4120(11) . ? As2 Fe3 2.4120(11) 4 ? Fe1 C4 1.821(7) . ? Fe1 C4 1.821(7) 4 ? Fe1 C3 1.827(11) . ? Fe1 Te1 2.6240(10) 4 ? Fe2 C6 1.817(8) 4 ? Fe2 C6 1.817(8) . ? Fe2 C7 1.845(12) . ? Fe2 Te1 2.6350(11) 4 ? Fe3 C9 1.789(7) . ? Fe3 C11 1.816(7) . ? Fe3 C10 1.842(7) . ? C3 O3 1.129(13) . ? C4 O4 1.128(9) . ? C6 O6 1.130(9) . ? C7 O7 1.120(15) . ? C9 O9 1.133(9) . ? C10 O10 1.111(8) . ? C11 O11 1.138(9) . ? Te2 Fe5 2.6261(10) . ? Te2 Fe4 2.6281(12) . ? Te2 Fe5 2.6380(10) 2_655 ? As3 C12 1.936(6) . ? As3 Fe5 2.4036(13) . ? As3 Fe4 2.4085(11) . ? As3 Fe4 2.4184(11) 2_655 ? Fe4 C15 1.810(9) . ? Fe4 C13 1.821(7) . ? Fe4 C14 1.829(8) . ? Fe4 As3 2.4184(11) 2_655 ? Fe5 C17 1.810(7) . ? Fe5 C18 1.818(7) . ? Fe5 C16 1.835(8) . ? Fe5 Te2 2.6380(10) 2_655 ? C13 O13 1.122(8) . ? C14 O14 1.129(9) . ? C15 O15 1.115(11) . ? C16 O16 1.114(9) . ? C17 O17 1.131(9) . ? C18 O18 1.130(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 Fe1 Te1 Fe3 93.81(4) . . ? Fe1 Te1 Fe2 98.28(3) . . ? Fe3 Te1 Fe2 93.12(4) . . ? C1 As1 Fe3 112.60(17) . 4 ? C1 As1 Fe3 112.60(17) . . ? Fe3 As1 Fe3 102.46(5) 4 . ? C1 As1 Fe1 117.8(3) . . ? Fe3 As1 Fe1 104.94(4) 4 . ? Fe3 As1 Fe1 104.94(4) . . ? C2 As2 Fe2 113.1(3) . . ? C2 As2 Fe3 114.74(18) . . ? Fe2 As2 Fe3 105.16(4) . . ? C2 As2 Fe3 114.74(18) . 4 ? Fe2 As2 Fe3 105.16(4) . 4 ? Fe3 As2 Fe3 102.74(5) . 4 ? C4 Fe1 C4 97.4(4) . 4 ? C4 Fe1 C3 96.7(3) . . ? C4 Fe1 C3 96.7(3) 4 . ? C4 Fe1 As1 93.3(2) . . ? C4 Fe1 As1 93.3(2) 4 . ? C3 Fe1 As1 164.8(3) . . ? C4 Fe1 Te1 170.0(2) . 4 ? C4 Fe1 Te1 90.0(2) 4 4 ? C3 Fe1 Te1 89.0(2) . 4 ? As1 Fe1 Te1 79.54(4) . 4 ? C4 Fe1 Te1 90.0(2) . . ? C4 Fe1 Te1 170.0(2) 4 . ? C3 Fe1 Te1 89.0(2) . . ? As1 Fe1 Te1 79.54(4) . . ? Te1 Fe1 Te1 81.88(4) 4 . ? C6 Fe2 C6 97.1(5) 4 . ? C6 Fe2 C7 97.3(3) 4 . ? C6 Fe2 C7 97.3(3) . . ? C6 Fe2 As2 89.6(2) 4 . ? C6 Fe2 As2 89.6(2) . . ? C7 Fe2 As2 169.4(4) . . ? C6 Fe2 Te1 167.3(2) 4 . ? C6 Fe2 Te1 89.9(2) . . ? C7 Fe2 Te1 92.3(3) . . ? As2 Fe2 Te1 79.71(4) . . ? C6 Fe2 Te1 89.9(2) 4 4 ? C6 Fe2 Te1 167.3(2) . 4 ? C7 Fe2 Te1 92.3(3) . 4 ? As2 Fe2 Te1 79.71(4) . 4 ? Te1 Fe2 Te1 81.47(4) . 4 ? C9 Fe3 C11 96.2(4) . . ? C9 Fe3 C10 93.7(3) . . ? C11 Fe3 C10 98.7(3) . . ? C9 Fe3 As2 89.3(2) . . ? C11 Fe3 As2 163.6(2) . . ? C10 Fe3 As2 96.3(2) . . ? C9 Fe3 As1 94.3(2) . . ? C11 Fe3 As1 88.8(2) . . ? C10 Fe3 As1 168.4(2) . . ? As2 Fe3 As1 75.33(4) . . ? C9 Fe3 Te1 168.4(2) . . ? C11 Fe3 Te1 93.5(3) . . ? C10 Fe3 Te1 91.2(2) . . ? As2 Fe3 Te1 79.63(4) . . ? As1 Fe3 Te1 79.50(3) . . ? O3 C3 Fe1 176.7(8) . . ? O4 C4 Fe1 178.6(7) . . ? O6 C6 Fe2 178.4(8) . . ? O7 C7 Fe2 179.5(11) . . ? O9 C9 Fe3 177.6(7) . . ? O10 C10 Fe3 179.5(7) . . ? O11 C11 Fe3 175.8(8) . . ? Fe5 Te2 Fe4 93.84(3) . . ? Fe5 Te2 Fe5 98.04(3) . 2_655 ? Fe4 Te2 Fe5 93.33(3) . 2_655 ? C12 As3 Fe5 113.9(3) . . ? C12 As3 Fe4 113.2(3) . . ? Fe5 As3 Fe4 105.79(4) . . ? C12 As3 Fe4 115.0(3) . 2_655 ? Fe5 As3 Fe4 105.20(4) . 2_655 ? Fe4 As3 Fe4 102.59(4) . 2_655 ? C15 Fe4 C13 96.6(4) . . ? C15 Fe4 C14 93.8(4) . . ? C13 Fe4 C14 96.8(3) . . ? C15 Fe4 As3 94.7(2) . . ? C13 Fe4 As3 90.5(2) . . ? C14 Fe4 As3 168.1(2) . . ? C15 Fe4 As3 88.8(2) . 2_655 ? C13 Fe4 As3 165.0(2) . 2_655 ? C14 Fe4 As3 96.8(2) . 2_655 ? As3 Fe4 As3 75.12(4) . 2_655 ? C15 Fe4 Te2 167.7(2) . . ? C13 Fe4 Te2 94.0(3) . . ? C14 Fe4 Te2 91.0(3) . . ? As3 Fe4 Te2 79.06(3) . . ? As3 Fe4 Te2 79.47(3) 2_655 . ? C17 Fe5 C18 95.6(3) . . ? C17 Fe5 C16 96.8(3) . . ? C18 Fe5 C16 96.7(3) . . ? C17 Fe5 As3 90.8(2) . . ? C18 Fe5 As3 92.4(2) . . ? C16 Fe5 As3 167.5(2) . . ? C17 Fe5 Te2 166.8(2) . . ? C18 Fe5 Te2 93.3(2) . . ? C16 Fe5 Te2 91.7(2) . . ? As3 Fe5 Te2 79.19(3) . . ? C17 Fe5 Te2 87.9(2) . 2_655 ? C18 Fe5 Te2 171.2(2) . 2_655 ? C16 Fe5 Te2 90.8(2) . 2_655 ? As3 Fe5 Te2 79.53(3) . 2_655 ? Te2 Fe5 Te2 81.90(3) . 2_655 ? O13 C13 Fe4 177.6(8) . . ? O14 C14 Fe4 179.8(8) . . ? O15 C15 Fe4 178.1(7) . . ? O16 C16 Fe5 179.0(8) . . ? O17 C17 Fe5 178.2(7) . . ? O18 C18 Fe5 178.9(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.42 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.560 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.148 #===END # CIF-file generated for np253F3 Nikolay/Scheer #=============================================================================== data_3b_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 802729' #TrackingRef '- Combined_CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H6 As2 Fe6 O15 Te2), C H2 Cl2' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C17 H6 As2 Fe6 O15 Te2, 0.5(C H2 Cl2)' _chemical_formula_sum 'C35 H14 As4 Cl2 Fe12 O30 Te4' _chemical_formula_iupac ? _chemical_formula_weight 2465.61 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 17.7104(4) _cell_length_b 11.0072(2) _cell_length_c 31.0735(6) _cell_angle_alpha 90 _cell_angle_beta 92.1845(18) _cell_angle_gamma 90 _cell_volume 6053.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 11207 _cell_measurement_theta_min 2.8901 _cell_measurement_theta_max 31.8888 _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.180 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.706 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 4600 _exptl_absorpt_coefficient_mu 7.014 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.71455 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 22321 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 32.07 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_max 0.920 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 9746 # number of observed reflections (> n sig(I)) _reflns_number_gt 7446 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 9746 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.987 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.152 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Te1 Te Uani 0.24428(1) 0.17694(2) 0.07976(1) 1.000 0.0159(1) . . Te2 Te Uani 0.18138(1) -0.11405(2) 0.16076(1) 1.000 0.0193(1) . . As1 As Uani 0.36062(2) 0.12088(3) 0.16125(1) 1.000 0.0158(1) . . As2 As Uani 0.35113(2) -0.11700(3) 0.08681(1) 1.000 0.0152(1) . . Fe1 Fe Uani 0.29768(3) 0.30027(4) 0.14163(1) 1.000 0.0164(1) . . Fe2 Fe Uani 0.22174(3) 0.09679(4) 0.15805(1) 1.000 0.0168(1) . . Fe3 Fe Uani 0.22223(3) -0.06530(4) 0.08799(1) 1.000 0.0161(1) . . Fe4 Fe Uani 0.31950(3) -0.09943(4) 0.15944(1) 1.000 0.0162(1) . . Fe5 Fe Uani 0.44472(3) 0.00624(4) 0.11662(1) 1.000 0.0171(1) . . Fe6 Fe Uani 0.34331(3) 0.04586(4) 0.04014(1) 1.000 0.0148(1) . . O1 O Uani 0.41656(17) 0.4396(2) 0.10171(9) 1.000 0.0316(9) . . O2 O Uani 0.17535(17) 0.4774(3) 0.12736(10) 1.000 0.0406(10) . . O3 O Uani 0.32395(17) 0.4040(2) 0.22742(8) 1.000 0.0294(8) . . O4 O Uani 0.07140(17) 0.1998(3) 0.14498(10) 1.000 0.0410(10) . . O5 O Uani 0.22577(18) 0.1570(2) 0.24903(8) 1.000 0.0340(9) . . O6 O Uani 0.19556(18) -0.3041(3) 0.05128(12) 1.000 0.0491(11) . . O7 O Uani 0.07641(17) -0.0043(3) 0.04623(11) 1.000 0.0479(11) . . O8 O Uani 0.34496(16) -0.0961(2) 0.25289(8) 1.000 0.0302(8) . . O9 O Uani 0.3501(2) -0.3586(2) 0.16468(9) 1.000 0.0418(12) . . O10 O Uani 0.52173(19) -0.0843(3) 0.19455(9) 1.000 0.0475(11) . . O11 O Uani 0.55062(15) -0.1352(2) 0.06692(8) 1.000 0.0280(8) . . O12 O Uani 0.52828(17) 0.2344(3) 0.10640(11) 1.000 0.0398(10) . . O13 O Uani 0.44170(15) -0.0961(2) -0.01370(8) 1.000 0.0243(7) . . O14 O Uani 0.41991(16) 0.2770(2) 0.02203(9) 1.000 0.0312(9) . . O15 O Uani 0.22610(15) 0.0363(2) -0.02896(8) 1.000 0.0260(8) . . C1 C Uani 0.3707(2) 0.3830(3) 0.11638(10) 1.000 0.0220(10) . . C2 C Uani 0.2217(2) 0.4064(3) 0.13225(11) 1.000 0.0244(11) . . C3 C Uani 0.3136(2) 0.3609(3) 0.19424(11) 1.000 0.0205(10) . . C4 C Uani 0.1311(2) 0.1615(3) 0.15013(11) 1.000 0.0258(11) . . C5 C Uani 0.2237(2) 0.1332(3) 0.21341(11) 1.000 0.0223(10) . . C6 C Uani 0.2073(2) -0.2105(4) 0.06574(12) 1.000 0.0267(11) . . C7 C Uani 0.1334(2) -0.0237(4) 0.06230(12) 1.000 0.0262(11) . . C8 C Uani 0.3367(2) -0.0950(3) 0.21646(11) 1.000 0.0224(10) . . C9 C Uani 0.3388(2) -0.2570(3) 0.16196(11) 1.000 0.0255(10) . . C10 C Uani 0.4904(2) -0.0495(4) 0.16453(12) 1.000 0.0295(11) . . C11 C Uani 0.5083(2) -0.0808(3) 0.08552(11) 1.000 0.0220(10) . . C12 C Uani 0.4945(2) 0.1471(4) 0.11027(13) 1.000 0.0286(11) . . C13 C Uani 0.4036(2) -0.0413(3) 0.00770(10) 1.000 0.0187(9) . . C14 C Uani 0.3907(2) 0.1891(3) 0.03012(10) 1.000 0.0213(10) . . C15 C Uani 0.2709(2) 0.0397(3) -0.00176(10) 1.000 0.0188(9) . . C16 C Uani 0.4130(2) 0.1493(4) 0.21745(11) 1.000 0.0263(11) . . C17 C Uani 0.3788(2) -0.2768(3) 0.06585(12) 1.000 0.0266(11) . . Cl1 Cl Uani 0.00345(12) -0.0359(2) 0.20617(8) 0.702(3) 0.0737(9) . . Cl2 Cl Uani 0.00000 0.1887(3) 0.25000 0.596(12) 0.0568(13) . . C18 C Uani 0.00000 0.0436(9) 0.25000 1.000 0.122(6) . . H16A H Uiso 0.44730 0.21870 0.21520 1.000 0.0400 calc R H16B H Uiso 0.44210 0.07680 0.22590 1.000 0.0400 calc R H16C H Uiso 0.37570 0.16650 0.23910 1.000 0.0400 calc R H17A H Uiso 0.34020 -0.33600 0.07350 1.000 0.0400 calc R H17B H Uiso 0.42770 -0.30080 0.07910 1.000 0.0400 calc R H17C H Uiso 0.38250 -0.27410 0.03450 1.000 0.0400 calc R H18A H Uiso -0.04610 0.01780 0.26450 0.500 0.1460 calc . H18B H Uiso 0.04350 0.01780 0.26880 0.500 0.1460 calc . 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 Te1 0.0182(1) 0.0147(1) 0.0150(1) -0.0004(1) 0.0019(1) -0.0003(1) Te2 0.0232(1) 0.0163(1) 0.0186(1) 0.0003(1) 0.0052(1) -0.0041(1) As1 0.0195(2) 0.0123(2) 0.0155(1) -0.0021(1) -0.0013(1) 0.0001(1) As2 0.0178(2) 0.0123(2) 0.0156(1) -0.0022(1) 0.0015(1) -0.0006(1) Fe1 0.0208(2) 0.0123(2) 0.0161(2) -0.0017(2) 0.0015(2) 0.0000(2) Fe2 0.0213(2) 0.0140(2) 0.0153(2) -0.0004(2) 0.0052(2) 0.0002(2) Fe3 0.0173(2) 0.0151(2) 0.0158(2) -0.0022(2) 0.0010(2) -0.0029(2) Fe4 0.0223(2) 0.0117(2) 0.0147(2) -0.0002(2) 0.0007(2) 0.0003(2) Fe5 0.0153(2) 0.0160(2) 0.0198(2) -0.0031(2) -0.0012(2) 0.0010(2) Fe6 0.0161(2) 0.0145(2) 0.0138(2) -0.0019(2) 0.0023(2) -0.0015(2) O1 0.0384(17) 0.0214(13) 0.0358(15) 0.0018(11) 0.0134(13) -0.0049(12) O2 0.0348(17) 0.0295(15) 0.057(2) -0.0026(14) -0.0028(15) 0.0139(14) O3 0.0414(17) 0.0252(14) 0.0216(12) -0.0049(10) 0.0014(11) 0.0027(12) O4 0.0336(17) 0.0416(18) 0.0489(18) 0.0139(14) 0.0165(14) 0.0191(15) O5 0.057(2) 0.0266(14) 0.0194(12) -0.0057(10) 0.0136(13) -0.0015(14) O6 0.0391(19) 0.0324(17) 0.075(2) -0.0289(16) -0.0090(17) -0.0055(14) O7 0.0287(16) 0.0477(19) 0.066(2) 0.0172(16) -0.0165(15) -0.0074(15) O8 0.0351(16) 0.0346(15) 0.0203(12) 0.0010(11) -0.0059(11) -0.0030(13) O9 0.081(3) 0.0176(13) 0.0278(14) 0.0040(11) 0.0168(15) 0.0092(15) O10 0.047(2) 0.064(2) 0.0301(15) -0.0082(14) -0.0160(14) 0.0285(17) O11 0.0260(14) 0.0302(14) 0.0280(13) -0.0015(11) 0.0050(11) 0.0079(12) O12 0.0277(16) 0.0276(15) 0.064(2) -0.0062(14) 0.0004(14) -0.0096(13) O13 0.0221(13) 0.0257(13) 0.0256(12) -0.0060(10) 0.0073(10) -0.0008(11) O14 0.0340(16) 0.0224(14) 0.0380(15) -0.0034(11) 0.0131(12) -0.0064(12) O15 0.0290(14) 0.0292(14) 0.0195(12) -0.0015(10) -0.0047(10) -0.0001(12) C1 0.032(2) 0.0165(16) 0.0175(15) -0.0034(12) -0.0006(14) 0.0025(15) C2 0.028(2) 0.0219(18) 0.0233(17) -0.0034(13) 0.0001(15) -0.0012(15) C3 0.0246(18) 0.0164(16) 0.0207(16) -0.0005(12) 0.0025(14) 0.0006(13) C4 0.031(2) 0.0228(18) 0.0242(17) 0.0027(14) 0.0105(15) 0.0033(16) C5 0.031(2) 0.0138(16) 0.0229(16) -0.0009(12) 0.0099(15) -0.0032(14) C6 0.0189(18) 0.0275(19) 0.0336(19) -0.0092(15) 0.0017(15) -0.0029(15) C7 0.0216(19) 0.0271(19) 0.0298(19) 0.0060(15) 0.0008(15) -0.0035(16) C8 0.0243(19) 0.0180(16) 0.0248(17) 0.0010(13) 0.0006(14) -0.0001(14) C9 0.039(2) 0.0207(18) 0.0173(15) 0.0017(13) 0.0063(15) 0.0031(16) C10 0.027(2) 0.031(2) 0.0302(19) -0.0092(16) -0.0038(16) 0.0087(16) C11 0.0190(18) 0.0230(17) 0.0238(17) 0.0010(13) -0.0034(14) -0.0007(14) C12 0.0208(19) 0.027(2) 0.038(2) -0.0079(15) 0.0017(16) 0.0002(15) C13 0.0196(17) 0.0164(16) 0.0200(15) -0.0005(12) 0.0010(13) -0.0046(13) C14 0.0221(18) 0.0240(18) 0.0182(15) -0.0058(13) 0.0050(13) 0.0008(15) C15 0.0246(18) 0.0149(15) 0.0172(14) -0.0014(11) 0.0059(13) 0.0003(13) C16 0.029(2) 0.0259(19) 0.0233(17) -0.0040(14) -0.0089(15) 0.0002(16) C17 0.033(2) 0.0166(17) 0.0305(18) -0.0070(14) 0.0053(16) 0.0033(15) Cl1 0.0414(11) 0.0803(16) 0.1016(18) -0.0202(13) 0.0308(11) -0.0148(11) Cl2 0.081(3) 0.0379(17) 0.0509(18) 0.0000 -0.0068(16) 0.0000 C18 0.112(10) 0.046(6) 0.204(15) 0.0000 -0.036(10) 0.0000 _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Fe1 2.5090(5) . . yes Te1 Fe2 2.6325(5) . . yes Te1 Fe3 2.7083(5) . . yes Te1 Fe6 2.6149(5) . . yes Te2 Fe2 2.4308(5) . . yes Te2 Fe3 2.4596(5) . . yes Te2 Fe4 2.4534(6) . . yes As1 Fe1 2.3370(6) . . yes As1 Fe2 2.4721(6) . . yes As1 Fe4 2.5320(6) . . yes As1 Fe5 2.4273(6) . . yes As1 C16 1.971(3) . . yes As2 Fe3 2.3544(6) . . yes As2 Fe4 2.3540(5) . . yes As2 Fe5 2.3083(6) . . yes As2 Fe6 2.3066(5) . . yes As2 C17 1.945(3) . . yes Fe1 Fe2 2.6717(7) . . yes Fe1 C1 1.787(3) . . yes Fe1 C2 1.797(3) . . yes Fe1 C3 1.778(3) . . yes Fe2 Fe3 2.8150(6) . . yes Fe2 Fe4 2.7674(7) . . yes Fe2 C4 1.765(4) . . yes Fe2 C5 1.765(3) . . yes Fe3 Fe4 2.7833(7) . . yes Fe3 Fe6 2.9239(7) . . yes Fe3 C6 1.757(4) . . yes Fe3 C7 1.796(4) . . yes Fe4 Fe5 2.8752(7) . . yes Fe4 C8 1.787(3) . . yes Fe4 C9 1.769(3) . . yes Fe5 Fe6 2.9559(7) . . yes Fe5 C10 1.776(4) . . yes Fe5 C11 1.790(3) . . yes Fe5 C12 1.798(4) . . yes Fe6 C13 1.777(3) . . yes Fe6 C14 1.819(3) . . yes Fe6 C15 1.794(3) . . yes Cl1 C18 1.622(6) . . yes Cl2 C18 1.597(10) . . yes O1 C1 1.133(4) . . yes O2 C2 1.139(5) . . yes O3 C3 1.143(4) . . yes O4 C4 1.144(5) . . yes O5 C5 1.137(4) . . yes O6 C6 1.140(5) . . yes O7 C7 1.129(5) . . yes O8 C8 1.136(4) . . yes O9 C9 1.139(4) . . yes O10 C10 1.134(5) . . yes O11 C11 1.135(4) . . yes O12 C12 1.141(5) . . yes O13 C13 1.138(4) . . yes O14 C14 1.130(4) . . yes O15 C15 1.138(4) . . yes C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C16 H16A 0.9800 . . no C17 H17C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C18 H18A 0.9900 . . no C18 H18B 0.9900 . . no C18 H18A 0.9900 . 2_555 no C18 H18B 0.9900 . 2_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Te1 Fe2 62.56(2) . . . yes Fe1 Te1 Fe3 120.79(2) . . . yes Fe1 Te1 Fe6 114.79(2) . . . yes Fe2 Te1 Fe3 63.60(1) . . . yes Fe2 Te1 Fe6 112.22(2) . . . yes Fe3 Te1 Fe6 66.61(2) . . . yes Fe2 Te2 Fe3 70.28(2) . . . yes Fe2 Te2 Fe4 69.03(2) . . . yes Fe3 Te2 Fe4 69.02(2) . . . yes Fe1 As1 Fe2 67.43(2) . . . yes Fe1 As1 Fe4 132.03(2) . . . yes Fe1 As1 Fe5 125.95(2) . . . yes Fe1 As1 C16 107.51(13) . . . yes Fe2 As1 Fe4 67.14(2) . . . yes Fe2 As1 Fe5 123.54(2) . . . yes Fe2 As1 C16 119.12(10) . . . yes Fe4 As1 Fe5 70.83(2) . . . yes Fe4 As1 C16 107.28(13) . . . yes Fe5 As1 C16 108.09(11) . . . yes Fe3 As2 Fe4 72.48(2) . . . yes Fe3 As2 Fe5 122.25(2) . . . yes Fe3 As2 Fe6 77.70(2) . . . yes Fe3 As2 C17 118.73(11) . . . yes Fe4 As2 Fe5 76.14(2) . . . yes Fe4 As2 Fe6 121.88(2) . . . yes Fe4 As2 C17 117.88(11) . . . yes Fe5 As2 Fe6 79.66(2) . . . yes Fe5 As2 C17 118.66(11) . . . yes Fe6 As2 C17 120.14(11) . . . yes Te1 Fe1 As1 84.54(2) . . . yes Te1 Fe1 Fe2 60.98(1) . . . yes Te1 Fe1 C1 101.38(10) . . . yes Te1 Fe1 C2 88.25(11) . . . yes Te1 Fe1 C3 161.70(11) . . . yes As1 Fe1 Fe2 58.70(2) . . . yes As1 Fe1 C1 101.49(11) . . . yes As1 Fe1 C2 159.75(11) . . . yes As1 Fe1 C3 91.14(11) . . . yes Fe2 Fe1 C1 152.73(11) . . . yes Fe2 Fe1 C2 101.34(11) . . . yes Fe2 Fe1 C3 101.67(11) . . . yes C1 Fe1 C2 98.48(16) . . . yes C1 Fe1 C3 96.91(15) . . . yes C2 Fe1 C3 89.81(16) . . . yes Te1 Fe2 Te2 114.02(2) . . . yes Te1 Fe2 As1 79.37(2) . . . yes Te1 Fe2 Fe1 56.45(1) . . . yes Te1 Fe2 Fe3 59.51(1) . . . yes Te1 Fe2 Fe4 99.16(2) . . . yes Te1 Fe2 C4 84.55(11) . . . yes Te1 Fe2 C5 145.73(11) . . . yes Te2 Fe2 As1 113.23(2) . . . yes Te2 Fe2 Fe1 163.30(2) . . . yes Te2 Fe2 Fe3 55.34(1) . . . yes Te2 Fe2 Fe4 55.87(2) . . . yes Te2 Fe2 C4 97.07(11) . . . yes Te2 Fe2 C5 100.25(11) . . . yes As1 Fe2 Fe1 53.87(2) . . . yes As1 Fe2 Fe3 93.83(2) . . . yes As1 Fe2 Fe4 57.46(2) . . . yes As1 Fe2 C4 149.39(11) . . . yes As1 Fe2 C5 87.36(12) . . . yes Fe1 Fe2 Fe3 111.54(2) . . . yes Fe1 Fe2 Fe4 109.76(2) . . . yes Fe1 Fe2 C4 95.56(11) . . . yes Fe1 Fe2 C5 90.26(11) . . . yes Fe3 Fe2 Fe4 59.81(2) . . . yes Fe3 Fe2 C4 100.23(11) . . . yes Fe3 Fe2 C5 153.76(11) . . . yes Fe4 Fe2 C4 151.93(11) . . . yes Fe4 Fe2 C5 99.96(11) . . . yes C4 Fe2 C5 91.62(16) . . . yes Te1 Fe3 Te2 110.50(2) . . . yes Te1 Fe3 As2 95.34(2) . . . yes Te1 Fe3 Fe2 56.89(1) . . . yes Te1 Fe3 Fe4 96.96(2) . . . yes Te1 Fe3 Fe6 55.17(1) . . . yes Te1 Fe3 C6 151.43(13) . . . yes Te1 Fe3 C7 80.45(14) . . . yes Te2 Fe3 As2 106.32(2) . . . yes Te2 Fe3 Fe2 54.38(1) . . . yes Te2 Fe3 Fe4 55.39(1) . . . yes Te2 Fe3 Fe6 143.70(2) . . . yes Te2 Fe3 C6 96.79(13) . . . yes Te2 Fe3 C7 100.42(12) . . . yes As2 Fe3 Fe2 101.35(2) . . . yes As2 Fe3 Fe4 53.76(2) . . . yes As2 Fe3 Fe6 50.42(2) . . . yes As2 Fe3 C6 84.58(12) . . . yes As2 Fe3 C7 152.63(12) . . . yes Fe2 Fe3 Fe4 59.25(2) . . . yes Fe2 Fe3 Fe6 98.74(2) . . . yes Fe2 Fe3 C6 151.14(13) . . . yes Fe2 Fe3 C7 98.84(13) . . . yes Fe4 Fe3 Fe6 91.06(2) . . . yes Fe4 Fe3 C6 105.69(13) . . . yes Fe4 Fe3 C7 153.37(12) . . . yes Fe6 Fe3 C6 106.43(12) . . . yes Fe6 Fe3 C7 108.32(13) . . . yes C6 Fe3 C7 86.61(18) . . . yes Te2 Fe4 As1 110.40(2) . . . yes Te2 Fe4 As2 106.53(2) . . . yes Te2 Fe4 Fe2 55.10(2) . . . yes Te2 Fe4 Fe3 55.60(2) . . . yes Te2 Fe4 Fe5 145.23(2) . . . yes Te2 Fe4 C8 96.76(12) . . . yes Te2 Fe4 C9 97.24(12) . . . yes As1 Fe4 As2 91.22(2) . . . yes As1 Fe4 Fe2 55.40(2) . . . yes As1 Fe4 Fe3 93.28(2) . . . yes As1 Fe4 Fe5 52.88(2) . . . yes As1 Fe4 C8 85.06(11) . . . yes As1 Fe4 C9 152.02(12) . . . yes As2 Fe4 Fe2 102.75(2) . . . yes As2 Fe4 Fe3 53.77(2) . . . yes As2 Fe4 Fe5 51.21(2) . . . yes As2 Fe4 C8 156.21(12) . . . yes As2 Fe4 C9 84.79(11) . . . yes Fe2 Fe4 Fe3 60.95(2) . . . yes Fe2 Fe4 Fe5 99.80(2) . . . yes Fe2 Fe4 C8 94.42(11) . . . yes Fe2 Fe4 C9 152.33(12) . . . yes Fe3 Fe4 Fe5 92.35(2) . . . yes Fe3 Fe4 C8 149.79(12) . . . yes Fe3 Fe4 C9 106.28(11) . . . yes Fe5 Fe4 C8 110.03(11) . . . yes Fe5 Fe4 C9 105.42(12) . . . yes C8 Fe4 C9 87.57(15) . . . yes As1 Fe5 As2 95.04(2) . . . yes As1 Fe5 Fe4 56.28(2) . . . yes As1 Fe5 Fe6 90.88(2) . . . yes As1 Fe5 C10 88.31(13) . . . yes As1 Fe5 C11 177.83(11) . . . yes As1 Fe5 C12 85.90(13) . . . yes As2 Fe5 Fe4 52.64(2) . . . yes As2 Fe5 Fe6 50.15(2) . . . yes As2 Fe5 C10 115.49(14) . . . yes As2 Fe5 C11 85.74(11) . . . yes As2 Fe5 C12 144.12(13) . . . yes Fe4 Fe5 Fe6 88.63(2) . . . yes Fe4 Fe5 C10 78.88(12) . . . yes Fe4 Fe5 C11 123.07(11) . . . yes Fe4 Fe5 C12 142.15(13) . . . yes Fe6 Fe5 C10 165.48(13) . . . yes Fe6 Fe5 C11 91.17(11) . . . yes Fe6 Fe5 C12 94.02(13) . . . yes C10 Fe5 C11 89.53(17) . . . yes C10 Fe5 C12 100.38(18) . . . yes C11 Fe5 C12 94.66(17) . . . yes Te1 Fe6 As2 99.10(2) . . . yes Te1 Fe6 Fe3 58.23(1) . . . yes Te1 Fe6 Fe5 95.79(2) . . . yes Te1 Fe6 C13 173.26(11) . . . yes Te1 Fe6 C14 85.67(11) . . . yes Te1 Fe6 C15 83.61(11) . . . yes As2 Fe6 Fe3 51.88(2) . . . yes As2 Fe6 Fe5 50.20(2) . . . yes As2 Fe6 C13 85.07(11) . . . yes As2 Fe6 C14 139.86(11) . . . yes As2 Fe6 C15 116.82(11) . . . yes Fe3 Fe6 Fe5 87.96(2) . . . yes Fe3 Fe6 C13 122.05(11) . . . yes Fe3 Fe6 C14 143.33(11) . . . yes Fe3 Fe6 C15 80.53(11) . . . yes Fe5 Fe6 C13 90.95(11) . . . yes Fe5 Fe6 C14 89.73(10) . . . yes Fe5 Fe6 C15 166.83(11) . . . yes C13 Fe6 C14 94.57(15) . . . yes C13 Fe6 C15 89.78(15) . . . yes C14 Fe6 C15 103.31(15) . . . yes Fe1 C1 O1 176.8(3) . . . yes Fe1 C2 O2 176.9(3) . . . yes Fe1 C3 O3 177.5(3) . . . yes Fe2 C4 O4 177.8(3) . . . yes Fe2 C5 O5 179.3(3) . . . yes Fe3 C6 O6 178.1(3) . . . yes Fe3 C7 O7 176.1(4) . . . yes Fe4 C8 O8 176.8(3) . . . yes Fe4 C9 O9 178.0(3) . . . yes Fe5 C10 O10 177.8(3) . . . yes Fe5 C11 O11 177.5(3) . . . yes Fe5 C12 O12 177.7(3) . . . yes Fe6 C13 O13 178.8(3) . . . yes Fe6 C14 O14 177.0(3) . . . yes Fe6 C15 O15 178.6(3) . . . yes As1 C16 H16A 109.00 . . . no As1 C16 H16B 109.00 . . . no As1 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 110.00 . . . no H16B C16 H16C 110.00 . . . no As2 C17 H17A 109.00 . . . no As2 C17 H17B 109.00 . . . no As2 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H17A C17 H17C 110.00 . . . no H17B C17 H17C 110.00 . . . no Cl1 C18 Cl1 114.7(6) . . 2_555 yes H18A C18 H18B 107.00 . . . no H18A C18 H18A 147.00 . . 2_555 no H18A C18 H18B 63.00 . . 2_555 no H18A C18 H18B 63.00 2_555 . . no H18B C18 H18B 147.00 . . 2_555 no H18A C18 H18B 107.00 2_555 . 2_555 no 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 Fe2 Te1 Fe1 As1 57.05(2) . . . . no Fe3 Te1 Fe1 As1 30.25(2) . . . . no Fe6 Te1 Fe1 As1 -46.22(2) . . . . no Fe3 Te1 Fe1 Fe2 -26.80(2) . . . . no Fe6 Te1 Fe1 Fe2 -103.28(2) . . . . no Fe2 Te1 Fe1 C1 157.70(11) . . . . no Fe3 Te1 Fe1 C1 130.90(11) . . . . no Fe6 Te1 Fe1 C1 54.43(11) . . . . no Fe2 Te1 Fe1 C2 -104.00(11) . . . . no Fe3 Te1 Fe1 C2 -130.80(11) . . . . no Fe6 Te1 Fe1 C2 152.73(11) . . . . no Fe1 Te1 Fe6 Fe5 30.51(2) . . . . no Fe2 Te1 Fe6 Fe5 -38.42(2) . . . . no Fe3 Te1 Fe6 Fe5 -83.98(2) . . . . no Fe1 Te1 Fe6 C14 -58.78(10) . . . . no Fe2 Te1 Fe6 C14 -127.71(10) . . . . no Fe3 Te1 Fe6 C14 -173.27(10) . . . . no Fe1 Te1 Fe6 C15 -162.72(11) . . . . no Fe2 Te1 Fe6 C15 128.36(11) . . . . no Fe3 Te1 Fe6 C15 82.79(11) . . . . no Fe6 Te1 Fe3 As2 32.36(2) . . . . no Fe1 Te1 Fe3 Fe2 26.54(2) . . . . no Fe6 Te1 Fe3 Fe2 132.44(2) . . . . no Fe1 Te1 Fe3 Fe4 -19.47(3) . . . . no Fe2 Te1 Fe3 Fe4 -46.01(2) . . . . no Fe6 Te1 Fe3 Fe4 86.43(2) . . . . no Fe1 Te1 Fe3 Fe6 -105.90(2) . . . . no Fe2 Te1 Fe3 Fe6 -132.44(2) . . . . no Fe1 Te1 Fe3 C6 -162.0(2) . . . . no Fe2 Te1 Fe3 C6 171.5(3) . . . . no Fe6 Te1 Fe3 C6 -56.1(2) . . . . no Fe1 Te1 Fe3 C7 133.75(12) . . . . no Fe2 Te1 Fe3 C7 107.21(12) . . . . no Fe6 Te1 Fe3 C7 -120.35(12) . . . . no Fe6 Te1 Fe2 Fe1 107.35(2) . . . . no Fe1 Te1 Fe2 Fe3 -154.37(2) . . . . no Fe6 Te1 Fe2 Fe3 -47.03(2) . . . . no Fe1 Te1 Fe2 Fe4 -107.70(2) . . . . no Fe3 Te1 Fe2 Fe4 46.68(2) . . . . no Fe6 Te1 Fe2 Fe4 -0.35(2) . . . . no Fe1 Te1 Fe2 C4 100.37(11) . . . . no Fe3 Te1 Fe2 C4 -105.26(11) . . . . no Fe6 Te1 Fe2 C4 -152.28(11) . . . . no Fe1 Te1 Fe2 C5 15.5(2) . . . . no Fe3 Te1 Fe2 C5 169.9(2) . . . . no Fe6 Te1 Fe2 C5 122.9(2) . . . . no Fe2 Te1 Fe6 Fe3 45.57(2) . . . . no Fe1 Te1 Fe3 Te2 36.11(3) . . . . no Fe2 Te1 Fe3 Te2 9.57(2) . . . . no Fe6 Te1 Fe3 Te2 142.01(2) . . . . no Fe1 Te1 Fe3 As2 -73.54(2) . . . . no Fe2 Te1 Fe3 As2 -100.08(2) . . . . no Fe3 Te1 Fe2 Te2 -9.93(2) . . . . no Fe6 Te1 Fe2 Te2 -56.96(3) . . . . no Fe1 Te1 Fe2 As1 -53.47(2) . . . . no Fe3 Te1 Fe2 As1 100.91(2) . . . . no Fe6 Te1 Fe2 As1 53.88(2) . . . . no Fe3 Te1 Fe2 Fe1 154.37(2) . . . . no Fe1 Te1 Fe2 Te2 -164.31(3) . . . . no Fe1 Te1 Fe6 As2 81.06(2) . . . . no Fe2 Te1 Fe6 As2 12.13(2) . . . . no Fe3 Te1 Fe6 As2 -33.43(2) . . . . no Fe1 Te1 Fe6 Fe3 114.49(2) . . . . no Fe4 Te2 Fe2 C5 -95.15(12) . . . . no Fe3 Te2 Fe4 C9 -104.80(11) . . . . no Fe3 Te2 Fe4 Fe2 76.12(2) . . . . no Fe3 Te2 Fe2 Fe4 -74.34(2) . . . . no Fe3 Te2 Fe2 C4 97.57(11) . . . . no Fe4 Te2 Fe2 C4 171.91(11) . . . . no Fe3 Te2 Fe2 C5 -169.48(12) . . . . no Fe3 Te2 Fe4 C8 166.81(11) . . . . no Fe2 Te2 Fe4 C9 179.09(11) . . . . no Fe4 Te2 Fe3 Fe2 -74.35(2) . . . . no Fe2 Te2 Fe4 Fe3 -76.12(2) . . . . no Fe2 Te2 Fe4 Fe5 -50.14(4) . . . . no Fe3 Te2 Fe4 Fe5 25.97(3) . . . . no Fe2 Te2 Fe4 C8 90.69(11) . . . . no Fe3 Te2 Fe2 Te1 10.41(2) . . . . no Fe2 Te2 Fe3 As2 92.44(2) . . . . no Fe2 Te2 Fe4 As1 3.47(2) . . . . no Fe4 Te2 Fe2 Te1 84.75(2) . . . . no Fe3 Te2 Fe2 As1 -77.96(2) . . . . no Fe4 Te2 Fe2 As1 -3.63(2) . . . . no Fe4 Te2 Fe2 Fe3 74.34(2) . . . . no Fe4 Te2 Fe3 Te1 -84.21(2) . . . . no Fe4 Te2 Fe3 C7 -167.82(14) . . . . no Fe4 Te2 Fe3 As2 18.09(2) . . . . no Fe4 Te2 Fe3 C6 104.40(12) . . . . no Fe2 Te2 Fe3 Fe4 74.35(2) . . . . no Fe2 Te2 Fe3 C6 178.75(12) . . . . no Fe2 Te2 Fe4 As2 -94.23(2) . . . . no Fe2 Te2 Fe3 C7 -93.47(14) . . . . no Fe4 Te2 Fe3 Fe6 -25.62(3) . . . . no Fe2 Te2 Fe3 Fe6 48.73(4) . . . . no Fe3 Te2 Fe4 As2 -18.11(2) . . . . no Fe3 Te2 Fe4 As1 79.59(2) . . . . no Fe2 Te2 Fe3 Te1 -9.86(2) . . . . no Fe1 As1 Fe4 Fe5 121.57(3) . . . . no Fe5 As1 Fe2 C5 148.59(11) . . . . no Fe4 As1 Fe2 Te2 3.56(2) . . . . no Fe2 As1 Fe4 Fe3 50.91(2) . . . . no Fe5 As1 Fe4 Fe3 -90.47(2) . . . . no Fe4 As1 Fe2 C5 103.58(11) . . . . no C16 As1 Fe1 C2 -104.5(3) . . . . no Fe2 As1 Fe1 C3 102.99(11) . . . . no C16 As1 Fe4 Fe3 165.87(11) . . . . no Fe1 As1 Fe4 Fe3 31.10(3) . . . . no C16 As1 Fe1 C3 -11.94(16) . . . . no Fe1 As1 Fe2 C5 -92.25(11) . . . . no C16 As1 Fe2 C4 94.6(3) . . . . no C16 As1 Fe4 Te2 111.50(11) . . . . no C16 As1 Fe2 C5 5.88(18) . . . . no Fe1 As1 Fe4 Fe2 -19.82(3) . . . . no Fe5 As1 Fe4 Fe2 -141.39(2) . . . . no C16 As1 Fe4 Fe2 114.96(11) . . . . no Fe5 As1 Fe1 C1 -43.77(11) . . . . no C16 As1 Fe1 C1 85.35(15) . . . . no Fe2 As1 Fe1 C2 10.5(3) . . . . no Fe4 As1 Fe1 C2 30.2(3) . . . . no Fe5 As1 Fe1 C2 126.4(3) . . . . no Fe4 As1 Fe1 C3 122.76(12) . . . . no Fe5 As1 Fe1 C3 -141.06(12) . . . . no C16 As1 Fe4 Fe5 -103.66(11) . . . . no Fe1 As1 Fe4 C8 -118.66(12) . . . . no Fe2 As1 Fe4 C8 -98.84(12) . . . . no Fe5 As1 Fe4 C8 119.77(12) . . . . no C16 As1 Fe4 C8 16.12(16) . . . . no Fe1 As1 Fe4 C9 166.0(2) . . . . no Fe2 As1 Fe4 C9 -174.2(2) . . . . no Fe5 As1 Fe4 C9 44.5(2) . . . . no C16 As1 Fe4 C9 -59.2(3) . . . . no Fe5 As1 Fe2 Fe1 -119.16(3) . . . . no C16 As1 Fe2 Fe1 98.13(15) . . . . no Fe1 As1 Fe2 Fe3 114.01(2) . . . . no Fe1 As1 Fe5 As2 -90.87(3) . . . . no Fe1 As1 Fe2 Te1 56.01(1) . . . . no Fe2 As1 Fe4 Fe5 141.39(2) . . . . no Fe1 As1 Fe2 C4 -3.5(2) . . . . no Fe4 As1 Fe2 C4 -167.7(2) . . . . no Fe5 As1 Fe2 C4 -122.7(2) . . . . no Fe2 As1 Fe1 Te1 -59.19(2) . . . . no Fe4 As1 Fe1 Te1 -39.42(3) . . . . no Fe1 As1 Fe4 As2 84.87(3) . . . . no Fe2 As1 Fe4 As2 104.69(2) . . . . no Fe5 As1 Fe4 As2 -36.69(2) . . . . no C16 As1 Fe4 As2 -140.35(11) . . . . no Fe5 As1 Fe1 Fe2 115.96(3) . . . . no C16 As1 Fe1 Fe2 -114.93(11) . . . . no Fe2 As1 Fe1 C1 -159.72(11) . . . . no Fe4 As1 Fe1 C1 -139.95(11) . . . . no Fe4 As1 Fe5 C10 -77.74(13) . . . . no C16 As1 Fe5 C10 24.80(18) . . . . no Fe4 As1 Fe2 Te1 -108.17(2) . . . . no Fe5 As1 Fe2 Te1 -63.16(2) . . . . no C16 As1 Fe2 Te1 154.13(15) . . . . no Fe1 As1 Fe2 Te2 167.74(2) . . . . no Fe1 As1 Fe4 Te2 -23.28(3) . . . . no Fe2 As1 Fe4 Te2 -3.46(2) . . . . no Fe5 As1 Fe4 Te2 -144.84(2) . . . . no Fe5 As1 Fe2 Te2 48.57(3) . . . . no C16 As1 Fe2 Te2 -94.14(15) . . . . no Fe4 As1 Fe2 Fe1 -164.17(2) . . . . no Fe2 As1 Fe5 Fe6 44.14(3) . . . . no Fe4 As1 Fe5 Fe6 87.76(2) . . . . no C16 As1 Fe5 Fe6 -169.70(13) . . . . no Fe4 As1 Fe2 Fe3 -50.17(2) . . . . no Fe5 As1 Fe2 Fe3 -5.16(3) . . . . no C16 As1 Fe2 Fe3 -147.87(15) . . . . no Fe1 As1 Fe2 Fe4 164.17(2) . . . . no Fe5 As1 Fe2 Fe4 45.01(2) . . . . no C16 As1 Fe2 Fe4 -97.70(15) . . . . no C16 As1 Fe5 C12 -75.73(18) . . . . no Fe2 As1 Fe5 Fe4 -43.62(2) . . . . no C16 As1 Fe5 Fe4 102.55(13) . . . . no Fe5 As1 Fe1 Te1 56.76(3) . . . . no C16 As1 Fe1 Te1 -174.12(11) . . . . no Fe4 As1 Fe1 Fe2 19.78(3) . . . . no Fe2 As1 Fe5 C12 138.10(13) . . . . no Fe4 As1 Fe5 C12 -178.28(13) . . . . no Fe1 As1 Fe5 Fe4 -128.57(3) . . . . no Fe1 As1 Fe5 C10 153.69(13) . . . . no Fe2 As1 Fe5 C10 -121.37(13) . . . . no Fe1 As1 Fe5 Fe6 -40.81(3) . . . . no Fe1 As1 Fe5 C12 53.15(13) . . . . no Fe2 As1 Fe5 As2 -5.92(3) . . . . no Fe4 As1 Fe5 As2 37.71(2) . . . . no C16 As1 Fe5 As2 140.25(13) . . . . no Fe4 As2 Fe6 C13 161.78(11) . . . . no Fe5 As2 Fe6 C13 95.37(11) . . . . no Fe6 As2 Fe3 Fe2 -92.02(2) . . . . no C17 As2 Fe3 Fe6 -117.81(13) . . . . no Fe3 As2 Fe4 Te2 18.54(2) . . . . no Fe5 As2 Fe4 Te2 149.40(2) . . . . no Fe6 As2 Fe4 Te2 81.18(3) . . . . no C17 As2 Fe3 C6 -1.26(18) . . . . no Fe4 As2 Fe3 C7 174.2(3) . . . . no Fe5 As2 Fe3 C7 114.0(3) . . . . no C17 As2 Fe4 Te2 -95.24(12) . . . . no Fe4 As2 Fe3 C6 -113.97(13) . . . . no Fe5 As2 Fe3 C6 -174.23(13) . . . . no Fe6 As2 Fe3 C6 116.55(13) . . . . no Fe3 As2 Fe6 C13 -138.13(11) . . . . no C17 As2 Fe3 Fe4 112.72(13) . . . . no Fe4 As2 Fe3 Fe6 129.47(2) . . . . no Fe5 As2 Fe3 Fe6 69.22(2) . . . . no Fe4 As2 Fe3 Te1 94.72(2) . . . . no Fe5 As2 Fe3 Te1 34.46(3) . . . . no Fe6 As2 Fe3 Te1 -34.75(2) . . . . no Fe5 As2 Fe3 Te2 -78.73(3) . . . . no Fe6 As2 Fe3 Te2 -147.95(2) . . . . no C17 As2 Fe3 Te2 94.24(13) . . . . no Fe4 As2 Fe3 Fe2 37.46(2) . . . . no Fe5 As2 Fe3 Fe2 -22.80(3) . . . . no Fe3 As2 Fe4 C8 -173.7(3) . . . . no Fe5 As2 Fe4 C8 -42.8(3) . . . . no C17 As2 Fe3 Fe2 150.17(12) . . . . no Fe5 As2 Fe3 Fe4 -60.26(2) . . . . no Fe6 As2 Fe3 Fe4 -129.47(2) . . . . no Fe6 As2 Fe4 C9 177.21(12) . . . . no C17 As2 Fe4 C9 0.79(17) . . . . no Fe4 As2 Fe6 Fe5 66.41(3) . . . . no C17 As2 Fe6 Fe5 -117.25(12) . . . . no C17 As2 Fe6 C13 -21.88(17) . . . . no Fe3 As2 Fe6 C14 130.62(17) . . . . no Fe4 As2 Fe6 C14 70.53(17) . . . . no Fe5 As2 Fe6 C14 4.11(17) . . . . no C17 As2 Fe6 C14 -113.1(2) . . . . no Fe3 As2 Fe6 C15 -50.87(12) . . . . no Fe4 As2 Fe6 C15 -110.97(12) . . . . no Fe5 As2 Fe6 C15 -177.38(12) . . . . no C17 As2 Fe6 C15 65.38(17) . . . . no Fe6 As2 Fe5 C10 177.46(14) . . . . no C17 As2 Fe5 C10 -63.73(19) . . . . no Fe3 As2 Fe5 C11 -163.31(11) . . . . no Fe4 As2 Fe5 C11 138.18(11) . . . . no Fe6 As2 Fe5 C11 -95.10(11) . . . . no C17 As2 Fe5 C11 23.72(17) . . . . no Fe3 As2 Fe5 C12 -71.3(2) . . . . no Fe4 As2 Fe5 C12 -129.8(2) . . . . no C17 As2 Fe3 Te1 -152.57(12) . . . . no Fe4 As2 Fe3 Te2 -18.47(2) . . . . no Fe6 As2 Fe4 Fe3 62.64(3) . . . . no C17 As2 Fe4 Fe3 -113.78(12) . . . . no Fe3 As2 Fe4 Fe5 -130.86(2) . . . . no Fe6 As2 Fe4 Fe5 -68.22(3) . . . . no C17 As2 Fe4 Fe5 115.37(12) . . . . no Fe6 As2 Fe4 C8 -111.0(3) . . . . no C17 As2 Fe4 C8 72.6(3) . . . . no Fe3 As2 Fe4 C9 114.57(12) . . . . no Fe5 As2 Fe4 C9 -114.58(12) . . . . no Fe5 As2 Fe6 Fe3 -126.51(2) . . . . no C17 As2 Fe6 Fe3 116.25(12) . . . . no Fe3 As2 Fe6 Fe5 126.51(2) . . . . no C17 As2 Fe5 As1 -154.25(12) . . . . no C17 As2 Fe4 Fe2 -152.23(12) . . . . no Fe3 As2 Fe5 Fe4 58.52(2) . . . . no Fe6 As2 Fe5 Fe4 126.72(2) . . . . no C17 As2 Fe5 Fe4 -114.46(12) . . . . no Fe3 As2 Fe5 Fe6 -68.21(2) . . . . no Fe4 As2 Fe5 Fe6 -126.72(2) . . . . no Fe6 As2 Fe3 C7 44.8(3) . . . . no C17 As2 Fe3 C7 -73.1(3) . . . . no Fe3 As2 Fe4 As1 -93.17(2) . . . . no Fe5 As2 Fe4 As1 37.68(2) . . . . no Fe6 As2 Fe4 As1 -30.53(3) . . . . no C17 As2 Fe4 As1 153.05(12) . . . . no Fe3 As2 Fe4 Fe2 -38.45(2) . . . . no Fe5 As2 Fe4 Fe2 92.40(2) . . . . no Fe6 As2 Fe4 Fe2 24.19(3) . . . . no Fe6 As2 Fe5 As1 86.93(2) . . . . no Fe6 As2 Fe5 C12 -3.0(2) . . . . no C17 As2 Fe5 C12 115.8(2) . . . . no Fe5 As2 Fe4 Fe3 130.86(2) . . . . no C17 As2 Fe6 Te1 152.78(12) . . . . no Fe4 As2 Fe6 Fe3 -60.10(2) . . . . no Fe3 As2 Fe5 As1 18.72(3) . . . . no C17 As2 Fe5 Fe6 118.82(13) . . . . no Fe3 As2 Fe6 Te1 36.54(2) . . . . no Fe4 As2 Fe6 Te1 -23.56(3) . . . . no Fe5 As2 Fe6 Te1 -89.97(2) . . . . no Fe4 As2 Fe5 As1 -39.79(2) . . . . no Fe3 As2 Fe5 C10 109.25(14) . . . . no Fe4 As2 Fe5 C10 50.74(14) . . . . no C3 Fe1 Fe2 Fe4 -98.29(12) . . . . no Te1 Fe1 Fe2 As1 102.12(2) . . . . no C3 Fe1 Fe2 C4 94.04(16) . . . . no C3 Fe1 Fe2 Fe3 -162.65(12) . . . . no C3 Fe1 Fe2 As1 -84.15(12) . . . . no Te1 Fe1 Fe2 Fe4 87.98(2) . . . . no Te1 Fe1 Fe2 C4 -79.69(11) . . . . no Te1 Fe1 Fe2 C5 -171.34(12) . . . . no C3 Fe1 Fe2 C5 2.39(16) . . . . no C2 Fe1 Fe2 Fe3 105.17(11) . . . . no C2 Fe1 Fe2 Fe4 169.53(11) . . . . no C1 Fe1 Fe2 Fe3 -30.7(2) . . . . no C1 Fe1 Fe2 Fe4 33.7(2) . . . . no C1 Fe1 Fe2 C4 -134.0(3) . . . . no C1 Fe1 Fe2 C5 134.4(3) . . . . no C2 Fe1 Fe2 Te1 81.55(11) . . . . no C2 Fe1 Fe2 As1 -176.33(11) . . . . no As1 Fe1 Fe2 Te1 -102.12(2) . . . . no As1 Fe1 Fe2 Fe3 -78.50(2) . . . . no Te1 Fe1 Fe2 Fe3 23.62(2) . . . . no C3 Fe1 Fe2 Te1 173.73(12) . . . . no C2 Fe1 Fe2 C5 -89.79(16) . . . . no C1 Fe1 Fe2 Te1 -54.3(2) . . . . no C1 Fe1 Fe2 As1 47.8(2) . . . . no As1 Fe1 Fe2 C4 178.19(11) . . . . no As1 Fe1 Fe2 C5 86.54(11) . . . . no As1 Fe1 Fe2 Fe4 -14.14(2) . . . . no C2 Fe1 Fe2 C4 1.87(16) . . . . no C4 Fe2 Fe4 Te2 -17.3(2) . . . . no C4 Fe2 Fe4 As1 166.7(2) . . . . no Fe1 Fe2 Fe4 Fe3 -104.03(2) . . . . no Fe3 Fe2 Fe4 C8 -161.55(11) . . . . no Fe1 Fe2 Fe4 As2 -69.01(3) . . . . no Te2 Fe2 Fe3 C7 96.53(13) . . . . no As1 Fe2 Fe3 Te1 -75.29(2) . . . . no Fe3 Fe2 Fe4 C9 -68.3(2) . . . . no Fe1 Fe2 Fe4 As1 13.54(2) . . . . no C4 Fe2 Fe4 Fe5 136.4(2) . . . . no C4 Fe2 Fe4 C8 -112.4(3) . . . . no Fe1 Fe2 Fe4 Fe5 -16.80(2) . . . . no Fe1 Fe2 Fe4 C8 94.43(11) . . . . no Fe1 Fe2 Fe4 C9 -172.4(2) . . . . no Fe3 Fe2 Fe4 Te2 -66.39(2) . . . . no Fe3 Fe2 Fe4 As1 117.57(2) . . . . no Fe3 Fe2 Fe4 As2 35.02(2) . . . . no Fe3 Fe2 Fe4 Fe5 87.23(2) . . . . no C5 Fe2 Fe4 Fe3 162.08(12) . . . . no C5 Fe2 Fe4 Fe5 -110.69(12) . . . . no C5 Fe2 Fe4 C8 0.54(16) . . . . no C5 Fe2 Fe4 C9 93.7(3) . . . . no C4 Fe2 Fe4 As2 84.1(2) . . . . no C4 Fe2 Fe4 Fe3 49.1(2) . . . . no Fe1 Fe2 Fe4 Te2 -170.42(2) . . . . no Te1 Fe2 Fe3 Te2 -168.96(2) . . . . no Te1 Fe2 Fe3 As2 89.00(2) . . . . no Te1 Fe2 Fe3 Fe4 123.80(2) . . . . no Te1 Fe2 Fe3 Fe6 37.80(2) . . . . no Te1 Fe2 Fe3 C6 -171.5(3) . . . . no Te1 Fe2 Fe3 C7 -72.43(13) . . . . no Te2 Fe2 Fe3 Te1 168.96(2) . . . . no Te2 Fe2 Fe3 As2 -102.04(2) . . . . no Te2 Fe2 Fe3 Fe4 -67.24(2) . . . . no Te2 Fe2 Fe3 Fe6 -153.25(2) . . . . no Te2 Fe2 Fe3 C6 -2.6(3) . . . . no C5 Fe2 Fe3 C6 21.4(4) . . . . no C5 Fe2 Fe3 C7 120.5(3) . . . . no As1 Fe2 Fe3 Te2 115.75(2) . . . . no As1 Fe2 Fe3 As2 13.70(2) . . . . no As1 Fe2 Fe3 Fe4 48.51(2) . . . . no As1 Fe2 Fe3 Fe6 -37.50(2) . . . . no As1 Fe2 Fe3 C6 113.2(3) . . . . no As1 Fe2 Fe3 C7 -147.72(13) . . . . no Fe1 Fe2 Fe3 Te1 -22.80(2) . . . . no C4 Fe2 Fe4 C9 -19.2(3) . . . . no C5 Fe2 Fe4 Te2 95.69(12) . . . . no C5 Fe2 Fe4 As1 -80.35(12) . . . . no C5 Fe2 Fe4 As2 -162.90(12) . . . . no Te2 Fe2 Fe4 C9 -2.0(2) . . . . no As1 Fe2 Fe4 Te2 176.05(2) . . . . no As1 Fe2 Fe4 As2 -82.55(2) . . . . no As1 Fe2 Fe4 Fe3 -117.57(2) . . . . no As1 Fe2 Fe4 Fe5 -30.33(2) . . . . no As1 Fe2 Fe4 C8 80.89(11) . . . . no As1 Fe2 Fe4 C9 174.1(2) . . . . no Fe4 Fe2 Fe3 C6 64.7(3) . . . . no Fe4 Fe2 Fe3 C7 163.78(13) . . . . no C4 Fe2 Fe3 Te1 77.39(11) . . . . no C4 Fe2 Fe3 Te2 -91.56(11) . . . . no C4 Fe2 Fe3 As2 166.39(11) . . . . no C4 Fe2 Fe3 Fe4 -158.81(11) . . . . no C4 Fe2 Fe3 Fe6 115.19(11) . . . . no C4 Fe2 Fe3 C6 -94.1(3) . . . . no C4 Fe2 Fe3 C7 4.97(17) . . . . no C5 Fe2 Fe3 Te1 -167.1(3) . . . . no C5 Fe2 Fe3 Te2 24.0(3) . . . . no C5 Fe2 Fe3 As2 -78.1(3) . . . . no C5 Fe2 Fe3 Fe4 -43.3(3) . . . . no C5 Fe2 Fe3 Fe6 -129.3(3) . . . . no Te1 Fe2 Fe4 Te2 -112.89(2) . . . . no Te1 Fe2 Fe4 As1 71.07(2) . . . . no Te1 Fe2 Fe4 As2 -11.48(2) . . . . no Te1 Fe2 Fe4 Fe3 -46.50(2) . . . . no Te1 Fe2 Fe4 Fe5 40.74(2) . . . . no Te1 Fe2 Fe4 C8 151.96(11) . . . . no Te1 Fe2 Fe4 C9 -114.8(2) . . . . no Fe1 Fe2 Fe3 Te2 168.24(3) . . . . no Fe1 Fe2 Fe3 As2 66.20(3) . . . . no Fe1 Fe2 Fe3 Fe4 101.00(3) . . . . no Fe1 Fe2 Fe3 Fe6 15.00(3) . . . . no Fe1 Fe2 Fe3 C6 165.7(2) . . . . no Fe1 Fe2 Fe3 C7 -95.23(13) . . . . no Fe4 Fe2 Fe3 Te1 -123.80(2) . . . . no Fe4 Fe2 Fe3 Te2 67.24(2) . . . . no Fe4 Fe2 Fe3 As2 -34.80(2) . . . . no Fe4 Fe2 Fe3 Fe6 -86.00(2) . . . . no Te2 Fe2 Fe4 As2 101.41(2) . . . . no Te2 Fe2 Fe4 Fe3 66.39(2) . . . . no Te2 Fe2 Fe4 Fe5 153.62(2) . . . . no Te2 Fe2 Fe4 C8 -95.16(11) . . . . no Te2 Fe2 Fe4 As1 -176.05(2) . . . . no Te1 Fe3 Fe6 As2 136.25(2) . . . . no Te1 Fe3 Fe6 Fe5 98.09(2) . . . . no C7 Fe3 Fe4 Fe2 -38.0(3) . . . . no C7 Fe3 Fe4 Fe5 -137.9(3) . . . . no C7 Fe3 Fe4 C8 0.8(4) . . . . no C7 Fe3 Fe4 C9 115.3(3) . . . . no Te2 Fe3 Fe6 Fe5 21.20(4) . . . . no Te2 Fe3 Fe6 C13 111.05(13) . . . . no Te2 Fe3 Fe6 C14 -65.61(18) . . . . no Te2 Fe3 Fe6 C15 -165.22(11) . . . . no As2 Fe3 Fe6 Te1 -136.25(2) . . . . no As2 Fe3 Fe6 Fe5 -38.16(2) . . . . no As2 Fe3 Fe6 C13 51.68(13) . . . . no As2 Fe3 Fe6 C14 -124.97(18) . . . . no As2 Fe3 Fe6 C15 135.42(11) . . . . no Fe2 Fe3 Fe6 Te1 -38.71(2) . . . . no Te1 Fe3 Fe6 C13 -172.06(13) . . . . no Te1 Fe3 Fe6 C14 11.28(18) . . . . no Te1 Fe3 Fe6 C15 -88.32(11) . . . . no Te2 Fe3 Fe6 Te1 -76.89(3) . . . . no Te2 Fe3 Fe6 As2 59.36(4) . . . . no C6 Fe3 Fe4 Fe5 107.04(12) . . . . no C6 Fe3 Fe4 C8 -114.2(2) . . . . no C6 Fe3 Fe4 C9 0.22(17) . . . . no C7 Fe3 Fe4 Te2 27.6(3) . . . . no C7 Fe3 Fe4 As1 -85.0(3) . . . . no C7 Fe3 Fe4 As2 -174.1(3) . . . . no Fe4 Fe3 Fe6 C14 -86.46(18) . . . . no Fe4 Fe3 Fe6 C15 173.93(11) . . . . no C6 Fe3 Fe6 Te1 155.56(13) . . . . no C6 Fe3 Fe6 As2 -68.19(13) . . . . no C6 Fe3 Fe6 Fe5 -106.35(13) . . . . no C6 Fe3 Fe6 C13 -16.51(18) . . . . no C6 Fe3 Fe6 C14 166.8(2) . . . . no C6 Fe3 Fe6 C15 67.23(17) . . . . no C7 Fe3 Fe6 Te1 63.68(14) . . . . no C7 Fe3 Fe6 As2 -160.06(14) . . . . no C7 Fe3 Fe6 Fe5 161.78(14) . . . . no C7 Fe3 Fe6 C13 -108.38(19) . . . . no C7 Fe3 Fe6 C14 75.0(2) . . . . no C7 Fe3 Fe6 C15 -24.64(18) . . . . no Fe2 Fe3 Fe4 Fe5 -99.91(2) . . . . no Fe2 Fe3 Fe4 C8 38.9(2) . . . . no Fe2 Fe3 Fe4 C9 153.28(12) . . . . no Fe6 Fe3 Fe4 Te2 165.17(2) . . . . no Fe6 Fe3 Fe4 As1 52.59(2) . . . . no Fe6 Fe3 Fe4 As2 -36.52(2) . . . . no Fe6 Fe3 Fe4 Fe2 99.55(2) . . . . no Fe6 Fe3 Fe4 Fe5 -0.36(2) . . . . no Fe2 Fe3 Fe6 As2 97.54(2) . . . . no Fe2 Fe3 Fe6 Fe5 59.38(2) . . . . no Fe2 Fe3 Fe6 C13 149.23(13) . . . . no Fe2 Fe3 Fe6 C14 -27.43(18) . . . . no Fe2 Fe3 Fe6 C15 -127.04(11) . . . . no Fe4 Fe3 Fe6 Te1 -97.74(2) . . . . no Fe4 Fe3 Fe6 As2 38.51(2) . . . . no Fe4 Fe3 Fe6 Fe5 0.35(2) . . . . no Fe4 Fe3 Fe6 C13 90.19(13) . . . . no Te1 Fe3 Fe4 C9 -162.20(12) . . . . no Te2 Fe3 Fe4 As1 -112.58(2) . . . . no Te2 Fe3 Fe4 As2 158.32(2) . . . . no Te2 Fe3 Fe4 Fe2 -65.62(2) . . . . no Te2 Fe3 Fe4 Fe5 -165.52(2) . . . . no Te2 Fe3 Fe4 C8 -26.8(2) . . . . no Te2 Fe3 Fe4 C9 87.66(12) . . . . no As2 Fe3 Fe4 Te2 -158.32(2) . . . . no As2 Fe3 Fe4 As1 89.11(2) . . . . no As2 Fe3 Fe4 Fe2 136.06(2) . . . . no As2 Fe3 Fe4 Fe5 36.16(2) . . . . no As2 Fe3 Fe4 C8 174.9(2) . . . . no As2 Fe3 Fe4 C9 -70.66(12) . . . . no Fe2 Fe3 Fe4 Te2 65.62(2) . . . . no Fe2 Fe3 Fe4 As1 -46.96(2) . . . . no Fe2 Fe3 Fe4 As2 -136.06(2) . . . . no Fe6 Fe3 Fe4 C9 -107.17(12) . . . . no C6 Fe3 Fe4 Te2 -87.44(12) . . . . no C6 Fe3 Fe4 As1 159.98(12) . . . . no C6 Fe3 Fe4 As2 70.88(12) . . . . no C6 Fe3 Fe4 Fe2 -153.06(13) . . . . no Te1 Fe3 Fe4 Fe2 44.53(2) . . . . no Fe6 Fe3 Fe4 C8 138.4(2) . . . . no Te1 Fe3 Fe4 C8 83.4(2) . . . . no Te1 Fe3 Fe4 Te2 110.14(2) . . . . no Te1 Fe3 Fe4 As1 -2.44(2) . . . . no Te1 Fe3 Fe4 Fe5 -55.38(2) . . . . no Te1 Fe3 Fe4 As2 -91.54(2) . . . . no C9 Fe4 Fe5 Fe6 107.95(12) . . . . no C9 Fe4 Fe5 C10 -64.62(18) . . . . no C9 Fe4 Fe5 As2 69.97(12) . . . . no Fe2 Fe4 Fe5 Fe6 -60.56(2) . . . . no Fe2 Fe4 Fe5 C10 126.87(14) . . . . no C9 Fe4 Fe5 As1 -160.07(12) . . . . no C9 Fe4 Fe5 C11 17.45(18) . . . . no C9 Fe4 Fe5 C12 -157.3(2) . . . . no Fe2 Fe4 Fe5 C11 -151.06(13) . . . . no Fe3 Fe4 Fe5 Fe6 0.35(2) . . . . no Fe3 Fe4 Fe5 C10 -172.22(14) . . . . no Fe3 Fe4 Fe5 C11 -90.15(14) . . . . no Fe3 Fe4 Fe5 C12 95.1(2) . . . . no Fe2 Fe4 Fe5 C12 34.2(2) . . . . no Fe3 Fe4 Fe5 As1 92.33(2) . . . . no Fe3 Fe4 Fe5 As2 -37.63(2) . . . . no C8 Fe4 Fe5 C10 28.46(18) . . . . no C8 Fe4 Fe5 C11 110.53(18) . . . . no C8 Fe4 Fe5 C12 -64.2(2) . . . . no Te2 Fe4 Fe5 As1 71.13(4) . . . . no Te2 Fe4 Fe5 As2 -58.84(4) . . . . no Te2 Fe4 Fe5 Fe6 -20.85(4) . . . . no Te2 Fe4 Fe5 C10 166.58(14) . . . . no Te2 Fe4 Fe5 C11 -111.35(14) . . . . no Te2 Fe4 Fe5 C12 73.9(2) . . . . no As1 Fe4 Fe5 As2 -129.97(2) . . . . no As1 Fe4 Fe5 Fe6 -91.98(2) . . . . no As1 Fe4 Fe5 C10 95.45(14) . . . . no C8 Fe4 Fe5 As1 -66.99(12) . . . . no C8 Fe4 Fe5 As2 163.05(12) . . . . no C8 Fe4 Fe5 Fe6 -158.97(12) . . . . no As2 Fe4 Fe5 C11 -52.52(13) . . . . no As2 Fe4 Fe5 C12 132.8(2) . . . . no Fe2 Fe4 Fe5 As1 31.42(2) . . . . no Fe2 Fe4 Fe5 As2 -98.55(2) . . . . no As1 Fe4 Fe5 C12 2.8(2) . . . . no As2 Fe4 Fe5 As1 129.97(2) . . . . no As1 Fe4 Fe5 C11 177.52(14) . . . . no As2 Fe4 Fe5 C10 -134.58(14) . . . . no As2 Fe4 Fe5 Fe6 37.99(2) . . . . no As1 Fe5 Fe6 As2 -95.83(2) . . . . no As1 Fe5 Fe6 Te1 1.20(2) . . . . no As2 Fe5 Fe6 C13 -82.78(11) . . . . no As2 Fe5 Fe6 C14 -177.35(11) . . . . no As1 Fe5 Fe6 Fe3 -56.58(2) . . . . no As1 Fe5 Fe6 C13 -178.62(11) . . . . no As1 Fe5 Fe6 C14 86.82(11) . . . . no As2 Fe5 Fe6 Te1 97.03(2) . . . . no As2 Fe5 Fe6 Fe3 39.25(2) . . . . no C11 Fe5 Fe6 Te1 -179.51(11) . . . . no C11 Fe5 Fe6 As2 83.46(11) . . . . no C11 Fe5 Fe6 Fe3 122.72(11) . . . . no C11 Fe5 Fe6 C13 0.68(15) . . . . no C11 Fe5 Fe6 C14 -93.89(15) . . . . no C12 Fe5 Fe6 Te1 -84.76(13) . . . . no C12 Fe5 Fe6 As2 178.21(13) . . . . no C12 Fe5 Fe6 Fe3 -142.53(13) . . . . no C12 Fe5 Fe6 C13 95.43(17) . . . . no C12 Fe5 Fe6 C14 0.86(16) . . . . no Fe4 Fe5 Fe6 Te1 57.44(2) . . . . no Fe4 Fe5 Fe6 As2 -39.59(2) . . . . no Fe4 Fe5 Fe6 Fe3 -0.34(2) . . . . no Fe4 Fe5 Fe6 C13 -122.37(11) . . . . no Fe4 Fe5 Fe6 C14 143.06(11) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 As1 3.2621(4) . . no Te1 As2 3.7504(4) . . no Te1 O4 3.744(3) . . no Te1 O7 3.697(3) . . no Te1 O15 3.719(2) . . no Te1 C1 3.355(3) . . no Te1 C2 3.041(3) . . no Te1 C4 3.027(3) . . no Te1 C7 2.991(4) . . no Te1 C14 3.070(3) . . no Te1 C15 3.002(3) . . no Te1 O15 3.577(2) . 7_555 no Te1 C15 3.953(3) . 7_555 no Te2 As2 3.8531(4) . . no Te2 Cl1 3.606(2) . . no Te2 C4 3.175(3) . . no Te2 C5 3.248(3) . . no Te2 C6 3.187(4) . . no Te2 C7 3.298(4) . . no Te2 C8 3.201(4) . . no Te2 C9 3.200(3) . . no Te2 O12 3.555(3) . 5_445 no Te2 O3 3.485(2) . 6_545 no As1 Te1 3.2621(4) . . no As1 As2 3.4936(5) . . no As1 Fe3 3.8683(6) . . no As1 Fe6 3.8536(5) . . no As1 C1 3.212(3) . . no As1 C3 2.965(3) . . no As1 C5 2.971(4) . . no As1 C8 2.971(3) . . no As1 C10 2.965(4) . . no As1 C12 2.916(4) . . no As2 Te1 3.7504(4) . . no As2 Te2 3.8531(4) . . no As2 As1 3.4936(5) . . no As2 C6 2.802(4) . . no As2 C9 2.813(3) . . no As2 C10 3.466(4) . . no As2 C11 2.814(4) . . no As2 C13 2.788(3) . . no As2 C15 3.503(3) . . no Fe3 O15 3.805(3) . . no Fe4 O10 3.708(3) . . no Cl1 C3 3.555(4) . 5_445 no Cl1 O4 3.460(4) . . no Cl1 C4 3.628(4) . . no Cl1 Te2 3.606(2) . . no Cl1 O3 3.338(4) . 5_445 no Cl2 O10 3.068(4) . 6_555 no Cl2 O10 3.068(4) . 5_455 no Cl1 H16A 2.9000 . 5_445 no O1 O12 3.003(4) . . no O1 O14 3.058(4) . . no O1 O9 3.213(4) . 1_565 no O1 C17 3.373(4) . 1_565 no O2 O11 3.103(4) . 5_455 no O2 C11 3.250(5) . 5_455 no O3 C8 3.393(5) . 6_555 no O3 O5 3.019(3) . 6_555 no O3 Cl1 3.338(4) . 5_555 no O3 C5 3.252(4) . 6_555 no O3 C16 3.237(5) . . no O3 O8 3.076(4) . 6_555 no O3 Te2 3.485(2) . 6_555 no O4 O10 2.983(5) . 5_455 no O4 O11 3.041(4) . 5_455 no O4 Cl1 3.460(4) . . no O4 C11 3.215(5) . 5_455 no O4 C10 3.179(5) . 5_455 no O5 C8 3.149(4) . 6_555 no O5 C9 3.177(4) . 6_555 no O5 O8 2.992(3) . 6_555 no O5 O3 3.019(3) . 6_545 no O5 C3 3.249(4) . . no O5 O9 3.050(4) . 6_555 no O6 O13 2.875(4) . 7_545 no O6 C17 3.273(5) . . no O6 C15 3.085(5) . 7_545 no O6 C13 3.016(5) . 7_545 no O6 O15 3.002(4) . 7_545 no O8 O5 2.992(3) . 6_545 no O8 C16 3.172(5) . . no O8 C5 3.399(4) . 6_545 no O8 O10 2.822(4) . 2_655 no O8 C3 3.341(4) . 6_545 no O8 O3 3.076(4) . 6_545 no O9 O5 3.050(4) . 6_545 no O9 O1 3.213(4) . 1_545 no O9 C3 3.292(4) . 1_545 no O9 C17 3.259(5) . . no O9 C1 3.243(4) . 1_545 no O10 O4 2.983(5) . 5_545 no O10 O8 2.822(4) . 2_655 no O10 Cl2 3.068(4) . 6_545 no O10 C16 3.306(5) . . no O10 Cl2 3.068(4) . 5_545 no O10 C8 3.374(5) . . no O11 C14 3.281(4) . 3_655 no O11 C17 3.418(4) . . no O11 O4 3.041(4) . 5_545 no O11 C13 3.297(4) . . no O11 O14 3.234(4) . 3_655 no O11 C13 3.155(4) . 3_655 no O11 O13 3.042(3) . 3_655 no O11 O13 3.133(4) . . no O11 O2 3.103(4) . 5_545 no O12 Te2 3.555(3) . 5_555 no O12 C1 3.260(5) . . no O12 O14 3.224(4) . . no O12 O1 3.003(4) . . no O12 C14 3.371(5) . . no O13 C13 3.129(4) . 3_655 no O13 O11 3.042(3) . 3_655 no O13 C17 3.394(4) . . no O13 O6 2.875(4) . 7_545 no O13 C14 3.199(4) . 3_655 no O13 C11 3.263(4) . . no O13 C11 3.116(4) . 3_655 no O13 O14 3.176(4) . 3_655 no O13 O13 3.055(3) . 3_655 no O13 C12 3.295(5) . 3_655 no O13 O11 3.133(4) . . no O14 O1 3.058(4) . . no O14 O11 3.234(4) . 3_655 no O14 C1 3.303(4) . . no O14 O13 3.176(4) . 3_655 no O14 C12 3.321(5) . . no O14 O12 3.224(4) . . no O15 C7 3.395(4) . . no O15 Te1 3.577(2) . 7_555 no O15 C1 3.279(4) . 7_555 no O15 O6 3.002(4) . 7_545 no O3 H18B 2.6600 . 6_555 no O3 H18A 2.8300 . 5_555 no O3 H16C 2.7900 . . no O5 H16C 2.6900 . . no O6 H17A 2.6500 . . no O8 H16B 2.7200 . . no O9 H17A 2.8400 . . no O10 H16B 2.4900 . . no O11 H17B 2.8800 . . no O13 H17C 2.7000 . . no O15 H17A 2.8300 . 7_545 no C1 As1 3.212(3) . . no C1 O9 3.243(4) . 1_565 no C1 O12 3.260(5) . . no C1 O14 3.303(4) . . no C1 C2 2.715(5) . . no C1 C3 2.669(5) . . no C1 C12 3.408(5) . . no C1 Te1 3.355(3) . . no C1 C14 3.455(5) . . no C1 O15 3.279(4) . 7_555 no C2 Te1 3.041(3) . . no C2 Fe2 3.501(3) . . no C2 O3 3.408(4) . . no C2 C1 2.715(5) . . no C2 C3 2.524(5) . . no C2 C4 3.197(5) . . no C3 Fe2 3.496(3) . . no C3 O2 3.402(5) . . no C3 O5 3.249(4) . . no C3 O9 3.292(4) . 1_565 no C3 C1 2.669(5) . . no C3 C2 2.524(5) . . no C3 As1 2.965(3) . . no C3 O8 3.341(4) . 6_555 no C3 C5 3.040(5) . . no C3 C16 2.991(5) . . no C3 Cl1 3.555(4) . 5_555 no C4 Fe1 3.342(4) . . no C4 C5 2.531(5) . . no C4 C2 3.197(5) . . no C4 Te1 3.027(3) . . no C4 Fe3 3.578(3) . . no C4 Cl1 3.628(4) . . no C4 C7 3.408(5) . . no C4 Te2 3.175(3) . . no C5 C3 3.040(5) . . no C5 C4 2.531(5) . . no C5 Te2 3.248(3) . . no C5 As1 2.971(4) . . no C5 O8 3.399(4) . 6_555 no C5 Fe4 3.531(3) . . no C5 C16 3.355(5) . . no C5 C8 3.211(5) . . no C5 O3 3.252(4) . 6_545 no C5 Fe1 3.209(3) . . no C6 Fe4 3.672(4) . . no C6 C7 2.438(6) . . no C6 As2 2.802(4) . . no C6 C17 3.124(5) . . no C6 Te2 3.187(4) . . no C6 O7 3.284(5) . . no C6 Fe6 3.814(4) . . no C7 C15 3.279(5) . . no C7 Te2 3.298(4) . . no C7 C4 3.408(5) . . no C7 C6 2.438(6) . . no C7 O6 3.299(5) . . no C7 O15 3.395(4) . . no C7 Fe2 3.564(4) . . no C7 Te1 2.991(4) . . no C7 Fe6 3.883(4) . . no C8 Fe5 3.870(3) . . no C8 As1 2.971(3) . . no C8 C9 2.461(5) . . no C8 Te2 3.201(4) . . no C8 C10 3.256(5) . . no C8 Fe2 3.408(3) . . no C8 C16 3.009(5) . . no C8 O9 3.331(4) . . no C8 O10 3.374(5) . . no C8 C5 3.211(5) . . no C8 O5 3.149(4) . 6_545 no C8 O3 3.393(5) . 6_545 no C9 As2 2.813(3) . . no C9 Fe3 3.693(3) . . no C9 O8 3.333(4) . . no C9 C8 2.461(5) . . no C9 Fe5 3.755(3) . . no C9 O5 3.177(4) . 6_545 no C9 Te2 3.200(3) . . no C9 C10 3.524(5) . . no C9 C17 3.103(5) . . no C10 C11 2.511(5) . . no C10 As2 3.466(4) . . no C10 C12 2.746(6) . . no C10 C16 3.089(6) . . no C10 As1 2.965(4) . . no C10 C8 3.256(5) . . no C10 C9 3.524(5) . . no C10 Fe4 3.074(4) . . no C10 O11 3.387(5) . . no C10 O4 3.179(5) . 5_545 no C11 C13 3.022(5) . . no C11 C12 2.638(5) . . no C11 O13 3.263(4) . . no C11 C17 3.191(5) . . no C11 C10 2.511(5) . . no C11 Fe6 3.487(4) . . no C11 O10 3.387(4) . . no C11 As2 2.814(4) . . no C11 O4 3.215(5) . 5_545 no C11 O2 3.250(5) . 5_545 no C11 O13 3.116(4) . 3_655 no C12 As1 2.916(4) . . no C12 C1 3.408(5) . . no C12 Fe6 3.566(4) . . no C12 O14 3.321(5) . . no C12 C11 2.638(5) . . no C12 C14 3.074(5) . . no C12 C10 2.746(6) . . no C12 O13 3.295(5) . 3_655 no C13 O15 3.411(4) . . no C13 C17 3.200(5) . . no C13 C15 2.520(5) . . no C13 As2 2.788(3) . . no C13 C11 3.022(5) . . no C13 O6 3.016(5) . 7_545 no C13 C14 2.642(5) . . no C13 O11 3.155(4) . 3_655 no C13 O13 3.129(4) . 3_655 no C13 C13 3.583(5) . 3_655 no C13 O11 3.297(4) . . no C13 Fe5 3.474(3) . . no C14 C12 3.074(5) . . no C14 O12 3.371(5) . . no C14 Fe5 3.463(3) . . no C14 O11 3.281(4) . 3_655 no C14 C13 2.642(5) . . no C14 C1 3.455(5) . . no C14 Te1 3.070(3) . . no C14 O13 3.199(4) . 3_655 no C14 C15 2.833(5) . . no C15 Te1 3.953(3) . 7_555 no C15 Fe3 3.169(3) . . no C15 As2 3.503(3) . . no C15 C7 3.279(5) . . no C15 Te1 3.002(3) . . no C15 O13 3.407(4) . . no C15 C14 2.833(5) . . no C15 O6 3.085(5) . 7_545 no C15 C13 2.520(5) . . no C16 O10 3.306(5) . . no C16 O3 3.237(5) . . no C16 O8 3.172(5) . . no C17 O13 3.394(4) . . no C17 O11 3.418(4) . . no C17 O9 3.259(5) . . no C17 O6 3.273(5) . . no C17 O1 3.373(4) . 1_545 no C3 H16A 2.8900 . . no C3 H16C 2.7600 . . no C5 H16C 2.8000 . . no C6 H17A 2.7300 . . no C8 H16C 3.0400 . . no C8 H16B 2.6700 . . no C9 H17A 2.8800 . . no C10 H16B 2.5300 . . no C11 H17B 2.8100 . . no C13 H17C 2.7200 . . no H16A Cl1 2.9000 . 5_555 no H16A C3 2.8900 . . no H16B O8 2.7200 . . no H16B C8 2.6700 . . no H16B C10 2.5300 . . no H16B O10 2.4900 . . no H16B H16B 2.4900 . 2_655 no H16C O3 2.7900 . . no H16C O5 2.6900 . . no H16C C3 2.7600 . . no H16C C5 2.8000 . . no H16C C8 3.0400 . . no H17A O6 2.6500 . . no H17A C6 2.7300 . . no H17A C9 2.8800 . . no H17A O15 2.8300 . 7_545 no H17A O9 2.8400 . . no H17B O11 2.8800 . . no H17B C11 2.8100 . . no H17C O13 2.7000 . . no H17C C13 2.7200 . . no H18A O3 2.8300 . 5_445 no H18B O3 2.6600 . 6_545 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C16 H16B O10 0.9800 2.4900 3.306(5) 141.00 . yes #===END #=============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 802730' #TrackingRef '- Combined_CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 As2 Fe4 O12 Se' _chemical_formula_structural ? _chemical_formula_sum 'C14 H6 As2 Fe4 O12 Se' _chemical_formula_iupac ? _chemical_formula_weight 818.39 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.9663(4) _cell_length_b 10.5051(4) _cell_length_c 10.6381(5) _cell_angle_alpha 85.208(4) _cell_angle_beta 85.591(4) _cell_angle_gamma 79.623(4) _cell_volume 1089.56(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 4804 _cell_measurement_theta_min 4.17 _cell_measurement_theta_max 62.10 _cell_special_details ; ; _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.495 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 26.798 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34732 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5431 # number of measured reflections (redundant set) _diffrn_reflns_number 9282 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 62.19 _diffrn_reflns_theta_full 62.19 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3373 # number of observed reflections (> n sig(I)) _reflns_number_gt 2704 _reflns_threshold_expression >2\s(i) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0416P)^2^] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3373 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.949 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.123 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Se1 Se Uani 0.43612(5) 0.07502(4) 0.13491(5) 1.000 0.0181(2) . . As1 As Uani 0.14665(5) 0.16655(4) 0.28616(5) 1.000 0.0179(2) . . As2 As Uani 0.41808(5) 0.24596(4) 0.27536(5) 1.000 0.0170(2) . . Fe1 Fe Uani 0.21950(7) 0.37991(6) 0.21428(7) 1.000 0.0180(2) . . Fe2 Fe Uani 0.25616(7) 0.25297(7) 0.44095(7) 1.000 0.0184(2) . . Fe3 Fe Uani 0.21670(7) 0.16916(7) 0.05780(7) 1.000 0.0183(2) . . Fe4 Fe Uani 0.25933(7) -0.04198(6) 0.20977(7) 1.000 0.0182(2) . . O1 O Uani 0.2946(4) 0.5988(3) 0.3280(4) 1.000 0.0308(11) . . O2 O Uani -0.0704(4) 0.5041(4) 0.2182(4) 1.000 0.0399(14) . . O3 O Uani 0.3252(4) 0.4797(3) -0.0321(4) 1.000 0.0356(14) . . O4 O Uani -0.0160(4) 0.3656(4) 0.5453(4) 1.000 0.0385(12) . . O5 O Uani 0.3965(4) 0.4215(4) 0.5731(4) 1.000 0.0381(14) . . O6 O Uani 0.3156(4) 0.0340(3) 0.6291(4) 1.000 0.0369(14) . . O7 O Uani -0.0559(4) 0.3060(3) -0.0007(4) 1.000 0.0335(11) . . O8 O Uani 0.3368(4) 0.2474(3) -0.1908(4) 1.000 0.0337(12) . . O9 O Uani 0.1522(4) -0.0469(3) -0.0649(4) 1.000 0.0327(11) . . O10 O Uani 0.3860(4) -0.2703(3) 0.0724(4) 1.000 0.0319(11) . . O11 O Uani 0.0035(4) -0.1438(4) 0.2597(4) 1.000 0.0362(12) . . O12 O Uani 0.3766(4) -0.1569(4) 0.4458(4) 1.000 0.0390(14) . . C1 C Uani 0.2647(5) 0.5111(5) 0.2863(5) 1.000 0.0221(17) . . C2 C Uani 0.0410(6) 0.4535(5) 0.2162(5) 1.000 0.0269(16) . . C3 C Uani 0.2812(5) 0.4347(4) 0.0595(5) 1.000 0.0237(16) . . C4 C Uani 0.0903(6) 0.3218(5) 0.5049(5) 1.000 0.0271(16) . . C5 C Uani 0.3433(5) 0.3571(5) 0.5198(5) 1.000 0.0245(17) . . C6 C Uani 0.2943(5) 0.1158(5) 0.5526(5) 1.000 0.0261(17) . . C7 C Uani 0.0488(6) 0.2531(5) 0.0240(5) 1.000 0.0252(16) . . C8 C Uani 0.2910(5) 0.2207(4) -0.0920(5) 1.000 0.0242(16) . . C9 C Uani 0.1849(5) 0.0222(5) 0.0025(5) 1.000 0.0248(17) . . C10 C Uani 0.3390(5) -0.1804(5) 0.1216(5) 1.000 0.0231(17) . . C11 C Uani 0.1016(6) -0.1027(5) 0.2402(5) 1.000 0.0251(16) . . C12 C Uani 0.3301(6) -0.1080(5) 0.3570(6) 1.000 0.0269(16) . . C13 C Uani -0.0500(5) 0.1720(5) 0.3231(5) 1.000 0.0280(17) . . C14 C Uani 0.5971(5) 0.2936(5) 0.2621(5) 1.000 0.0236(16) . . H1 H Uiso -0.09390 0.26050 0.34040 1.000 0.0420 calc R H2 H Uiso -0.06470 0.11290 0.39720 1.000 0.0420 calc R H3 H Uiso -0.08960 0.14510 0.25030 1.000 0.0420 calc R H4 H Uiso 0.66250 0.22300 0.30090 1.000 0.0350 calc R H5 H Uiso 0.59390 0.37260 0.30590 1.000 0.0350 calc R H6 H Uiso 0.62580 0.30930 0.17280 1.000 0.0350 calc R 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 Se1 0.0193(3) 0.0167(2) 0.0184(3) -0.0028(2) 0.0008(2) -0.0038(2) As1 0.0174(3) 0.0174(3) 0.0194(3) -0.0027(2) 0.0003(2) -0.0046(2) As2 0.0180(3) 0.0153(2) 0.0180(3) -0.0015(2) -0.0003(2) -0.0040(2) Fe1 0.0195(4) 0.0143(3) 0.0198(4) -0.0012(3) -0.0016(3) -0.0020(3) Fe2 0.0216(4) 0.0168(4) 0.0173(4) -0.0026(3) 0.0002(3) -0.0046(3) Fe3 0.0211(4) 0.0169(4) 0.0171(4) -0.0004(3) -0.0026(3) -0.0038(3) Fe4 0.0205(4) 0.0150(4) 0.0196(4) -0.0010(3) -0.0003(3) -0.0048(3) O1 0.041(2) 0.0206(18) 0.033(2) -0.0045(17) -0.0015(18) -0.0102(16) O2 0.027(2) 0.036(2) 0.054(3) -0.0056(19) -0.0100(19) 0.0057(18) O3 0.054(3) 0.0240(19) 0.030(2) -0.0003(17) 0.005(2) -0.0137(17) O4 0.034(2) 0.038(2) 0.040(2) -0.0086(19) 0.011(2) -0.0003(18) O5 0.057(3) 0.035(2) 0.030(2) -0.0081(19) -0.009(2) -0.023(2) O6 0.061(3) 0.0256(19) 0.024(2) 0.0037(18) -0.0109(19) -0.0067(17) O7 0.028(2) 0.0295(18) 0.041(2) 0.0015(17) -0.0113(18) 0.0024(17) O8 0.047(2) 0.033(2) 0.021(2) 0.0003(17) 0.0017(18) -0.0096(17) O9 0.044(2) 0.0258(18) 0.032(2) -0.0042(17) -0.0128(18) -0.0106(17) O10 0.042(2) 0.0204(18) 0.033(2) -0.0088(17) 0.0064(18) -0.0052(16) O11 0.031(2) 0.037(2) 0.043(2) 0.0059(18) 0.0004(18) -0.0179(18) O12 0.054(3) 0.032(2) 0.029(2) 0.0012(19) -0.014(2) 0.0008(18) C1 0.025(3) 0.021(3) 0.017(3) -0.001(2) 0.003(2) 0.003(2) C2 0.030(3) 0.019(2) 0.032(3) -0.002(2) -0.002(3) -0.005(2) C3 0.030(3) 0.014(2) 0.027(3) -0.008(2) -0.003(2) 0.000(2) C4 0.038(3) 0.022(2) 0.022(3) 0.004(2) -0.005(3) -0.008(2) C5 0.033(3) 0.023(3) 0.017(3) 0.005(2) 0.002(2) -0.008(2) C6 0.031(3) 0.024(3) 0.026(3) -0.006(3) 0.001(2) -0.011(2) C7 0.034(3) 0.019(2) 0.025(3) -0.002(2) -0.001(3) -0.011(2) C8 0.029(3) 0.019(2) 0.025(3) -0.006(2) -0.005(2) -0.002(2) C9 0.025(3) 0.024(3) 0.024(3) 0.004(2) -0.005(2) -0.002(2) C10 0.026(3) 0.021(3) 0.024(3) 0.003(2) -0.001(2) -0.011(2) C11 0.036(3) 0.020(2) 0.018(3) 0.001(2) 0.000(2) -0.003(2) C12 0.032(3) 0.016(2) 0.032(3) -0.002(2) 0.000(3) -0.003(2) C13 0.022(3) 0.029(3) 0.034(3) -0.005(2) 0.003(2) -0.008(2) C14 0.021(3) 0.026(2) 0.027(3) 0.000(2) -0.003(2) -0.013(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 As2 2.4042(7) . . yes Se1 Fe3 2.4071(9) . . yes Se1 Fe4 2.3770(9) . . yes As1 Fe1 2.5199(8) . . yes As1 Fe2 2.3685(9) . . yes As1 Fe3 2.4748(9) . . yes As1 Fe4 2.4477(8) . . yes As1 C13 1.961(5) . . yes As2 Fe1 2.3154(8) . . yes As2 Fe2 2.2923(9) . . yes As2 C14 1.930(5) . . yes Fe1 Fe2 2.6738(10) . . yes Fe1 Fe3 2.8842(10) . . yes Fe1 C1 1.773(5) . . yes Fe1 C2 1.807(6) . . yes Fe1 C3 1.798(5) . . yes Fe2 C4 1.788(6) . . yes Fe2 C5 1.806(5) . . yes Fe2 C6 1.794(5) . . yes Fe3 Fe4 2.6231(10) . . yes Fe3 C7 1.793(6) . . yes Fe3 C8 1.789(5) . . yes Fe3 C9 1.785(5) . . yes Fe4 C9 2.385(5) . . yes Fe4 C10 1.823(5) . . yes Fe4 C11 1.798(6) . . yes Fe4 C12 1.801(6) . . yes O1 C1 1.150(6) . . yes O2 C2 1.141(7) . . yes O3 C3 1.139(7) . . yes O4 C4 1.143(7) . . yes O5 C5 1.140(7) . . yes O6 C6 1.136(6) . . yes O7 C7 1.129(7) . . yes O8 C8 1.147(7) . . yes O9 C9 1.164(6) . . yes O10 C10 1.127(6) . . yes O11 C11 1.136(7) . . yes O12 C12 1.128(7) . . yes C13 H1 0.9800 . . no C13 H2 0.9800 . . no C13 H3 0.9800 . . no C14 H4 0.9800 . . no C14 H5 0.9800 . . no C14 H6 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As2 Se1 Fe3 90.35(3) . . . yes As2 Se1 Fe4 104.99(3) . . . yes Fe3 Se1 Fe4 66.50(3) . . . yes Fe1 As1 Fe2 66.23(3) . . . yes Fe1 As1 Fe3 70.54(3) . . . yes Fe1 As1 Fe4 123.79(3) . . . yes Fe1 As1 C13 116.08(15) . . . yes Fe2 As1 Fe3 125.33(3) . . . yes Fe2 As1 Fe4 117.06(3) . . . yes Fe2 As1 C13 114.51(16) . . . yes Fe3 As1 Fe4 64.40(3) . . . yes Fe3 As1 C13 113.66(16) . . . yes Fe4 As1 C13 111.78(15) . . . yes Se1 As2 Fe1 101.25(3) . . . yes Se1 As2 Fe2 118.08(3) . . . yes Se1 As2 C14 104.69(16) . . . yes Fe1 As2 Fe2 70.94(3) . . . yes Fe1 As2 C14 125.15(16) . . . yes Fe2 As2 C14 130.63(16) . . . yes As1 Fe1 As2 75.43(2) . . . yes As1 Fe1 Fe2 54.17(2) . . . yes As1 Fe1 Fe3 54.00(2) . . . yes As1 Fe1 C1 136.94(17) . . . yes As1 Fe1 C2 88.35(17) . . . yes As1 Fe1 C3 128.90(14) . . . yes As2 Fe1 Fe2 54.13(3) . . . yes As2 Fe1 Fe3 81.24(3) . . . yes As2 Fe1 C1 90.68(17) . . . yes As2 Fe1 C2 159.37(17) . . . yes As2 Fe1 C3 98.40(16) . . . yes Fe2 Fe1 Fe3 101.39(3) . . . yes Fe2 Fe1 C1 84.50(17) . . . yes Fe2 Fe1 C2 105.97(17) . . . yes Fe2 Fe1 C3 152.27(16) . . . yes Fe3 Fe1 C1 164.15(17) . . . yes Fe3 Fe1 C2 99.66(17) . . . yes Fe3 Fe1 C3 74.91(14) . . . yes C1 Fe1 C2 92.7(2) . . . yes C1 Fe1 C3 93.0(2) . . . yes C2 Fe1 C3 101.7(2) . . . yes As1 Fe2 As2 78.91(3) . . . yes As1 Fe2 Fe1 59.60(3) . . . yes As1 Fe2 C4 87.88(18) . . . yes As1 Fe2 C5 162.23(17) . . . yes As1 Fe2 C6 101.97(17) . . . yes As2 Fe2 Fe1 54.93(3) . . . yes As2 Fe2 C4 148.36(17) . . . yes As2 Fe2 C5 90.41(17) . . . yes As2 Fe2 C6 111.34(17) . . . yes Fe1 Fe2 C4 93.59(17) . . . yes Fe1 Fe2 C5 102.63(17) . . . yes Fe1 Fe2 C6 157.14(17) . . . yes C4 Fe2 C5 94.2(2) . . . yes C4 Fe2 C6 99.4(2) . . . yes C5 Fe2 C6 95.1(2) . . . yes Se1 Fe3 As1 82.59(3) . . . yes Se1 Fe3 Fe1 86.70(3) . . . yes Se1 Fe3 Fe4 56.20(3) . . . yes Se1 Fe3 C7 170.49(17) . . . yes Se1 Fe3 C8 92.59(16) . . . yes Se1 Fe3 C9 95.03(17) . . . yes As1 Fe3 Fe1 55.46(2) . . . yes As1 Fe3 Fe4 57.30(2) . . . yes As1 Fe3 C7 89.30(17) . . . yes As1 Fe3 C8 159.17(15) . . . yes As1 Fe3 C9 107.24(17) . . . yes Fe1 Fe3 Fe4 105.34(3) . . . yes Fe1 Fe3 C7 84.62(17) . . . yes Fe1 Fe3 C8 104.18(15) . . . yes Fe1 Fe3 C9 162.33(17) . . . yes Fe4 Fe3 C7 122.78(18) . . . yes Fe4 Fe3 C8 134.84(15) . . . yes Fe4 Fe3 C9 62.13(17) . . . yes C7 Fe3 C8 93.3(2) . . . yes C7 Fe3 C9 92.1(2) . . . yes C8 Fe3 C9 93.3(2) . . . yes Se1 Fe4 As1 83.79(3) . . . yes Se1 Fe4 Fe3 57.30(2) . . . yes Se1 Fe4 C9 81.86(13) . . . yes Se1 Fe4 C10 91.35(16) . . . yes Se1 Fe4 C11 166.02(18) . . . yes Se1 Fe4 C12 97.32(19) . . . yes As1 Fe4 Fe3 58.30(2) . . . yes As1 Fe4 C9 91.22(13) . . . yes As1 Fe4 C10 168.49(17) . . . yes As1 Fe4 C11 89.61(17) . . . yes As1 Fe4 C12 96.14(18) . . . yes Fe3 Fe4 C9 41.42(13) . . . yes Fe3 Fe4 C10 110.36(17) . . . yes Fe3 Fe4 C11 108.79(17) . . . yes Fe3 Fe4 C12 143.35(18) . . . yes C9 Fe4 C10 77.7(2) . . . yes C9 Fe4 C11 86.0(2) . . . yes C9 Fe4 C12 172.5(2) . . . yes C10 Fe4 C11 92.8(2) . . . yes C10 Fe4 C12 94.8(2) . . . yes C11 Fe4 C12 95.6(3) . . . yes Fe1 C1 O1 177.1(5) . . . yes Fe1 C2 O2 177.5(5) . . . yes Fe1 C3 O3 172.5(4) . . . yes Fe2 C4 O4 179.7(6) . . . yes Fe2 C5 O5 177.9(5) . . . yes Fe2 C6 O6 175.7(5) . . . yes Fe3 C7 O7 178.1(5) . . . yes Fe3 C8 O8 176.0(4) . . . yes Fe3 C9 Fe4 76.45(19) . . . yes Fe3 C9 O9 158.9(5) . . . yes Fe4 C9 O9 124.7(4) . . . yes Fe4 C10 O10 176.2(5) . . . yes Fe4 C11 O11 178.5(5) . . . yes Fe4 C12 O12 175.5(5) . . . yes As1 C13 H1 109.00 . . . no As1 C13 H2 109.00 . . . no As1 C13 H3 109.00 . . . no H1 C13 H2 109.00 . . . no H1 C13 H3 110.00 . . . no H2 C13 H3 109.00 . . . no As2 C14 H4 109.00 . . . no As2 C14 H5 109.00 . . . no As2 C14 H6 109.00 . . . no H4 C14 H5 109.00 . . . no H4 C14 H6 110.00 . . . no H5 C14 H6 109.00 . . . no 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 Fe3 Se1 As2 Fe1 -5.99(3) . . . . no Fe4 Se1 As2 Fe1 -71.71(3) . . . . no Fe3 Se1 As2 Fe2 68.27(4) . . . . no Fe4 Se1 As2 Fe2 2.55(4) . . . . no Fe3 Se1 As2 C14 -137.21(16) . . . . no Fe4 Se1 As2 C14 157.07(16) . . . . no As2 Se1 Fe3 C9 -157.64(17) . . . . no Fe4 Se1 Fe3 C9 -51.42(17) . . . . no Fe3 Se1 Fe4 C12 -151.49(18) . . . . no As2 Se1 Fe4 C12 -67.78(18) . . . . no Fe4 Se1 Fe3 C8 -145.00(14) . . . . no Fe3 Se1 Fe4 As1 -56.07(3) . . . . no As2 Se1 Fe4 Fe3 83.71(3) . . . . no As2 Se1 Fe4 C9 119.78(13) . . . . no Fe3 Se1 Fe4 C9 36.07(13) . . . . no As2 Se1 Fe4 C10 -162.81(17) . . . . no Fe3 Se1 Fe4 C10 113.48(17) . . . . no As2 Se1 Fe4 As1 27.64(3) . . . . no Fe4 Se1 Fe3 As1 55.35(3) . . . . no As2 Se1 Fe3 Fe1 4.72(3) . . . . no As2 Se1 Fe3 As1 -50.87(2) . . . . no As2 Se1 Fe3 C8 108.78(14) . . . . no As2 Se1 Fe3 Fe4 -106.22(3) . . . . no Fe4 Se1 Fe3 Fe1 110.94(3) . . . . no Fe4 As1 Fe1 Fe2 -107.66(4) . . . . no C13 As1 Fe1 Fe2 106.81(17) . . . . no Fe4 As1 Fe1 C3 37.4(2) . . . . no Fe2 As1 Fe1 Fe3 145.67(3) . . . . no Fe3 As1 Fe1 Fe2 -145.67(3) . . . . no C13 As1 Fe1 Fe3 -107.52(17) . . . . no Fe2 As1 Fe1 C1 -18.9(2) . . . . no Fe4 As1 Fe1 Fe3 38.01(4) . . . . no Fe3 As1 Fe1 C1 -164.6(2) . . . . no Fe4 As1 Fe1 C1 -126.6(2) . . . . no C13 As1 Fe1 C3 -108.1(3) . . . . no Fe4 As1 Fe3 C9 38.66(18) . . . . no C13 As1 Fe3 C9 -65.2(2) . . . . no Fe1 As1 Fe2 C6 -165.40(17) . . . . no Fe3 As1 Fe2 C6 -124.73(17) . . . . no C13 As1 Fe1 As2 162.81(17) . . . . no Fe3 As1 Fe1 C3 -0.6(2) . . . . no Fe1 As1 Fe2 C4 95.42(17) . . . . no Fe3 As1 Fe2 C4 136.09(17) . . . . no Fe4 As1 Fe2 C4 -147.37(17) . . . . no C13 As1 Fe2 C4 -13.7(2) . . . . no Fe2 As1 Fe3 C9 144.84(18) . . . . no Fe1 As1 Fe4 Fe3 -40.08(4) . . . . no Fe4 As1 Fe2 C6 -48.19(17) . . . . no C13 As1 Fe2 C6 85.5(2) . . . . no C13 As1 Fe1 C1 87.9(3) . . . . no Fe2 As1 Fe1 C2 -111.12(17) . . . . no Fe3 As1 Fe1 C2 103.20(17) . . . . no Fe4 As1 Fe1 C2 141.21(17) . . . . no C13 As1 Fe1 C2 -4.3(2) . . . . no Fe2 As1 Fe1 C3 145.1(2) . . . . no C13 As1 Fe2 Fe1 -109.09(17) . . . . no Fe1 As1 Fe4 C12 111.80(19) . . . . no Fe2 As1 Fe4 C12 33.5(2) . . . . no Fe3 As1 Fe4 C12 151.87(19) . . . . no C13 As1 Fe4 C12 -101.4(3) . . . . no C13 As1 Fe4 Se1 161.88(17) . . . . no Fe1 As1 Fe3 C9 -175.92(18) . . . . no Fe2 As1 Fe4 Fe3 -118.38(4) . . . . no C13 As1 Fe4 Fe3 106.73(17) . . . . no Fe2 As1 Fe4 C9 -144.91(13) . . . . no Fe3 As1 Fe4 C9 -26.53(13) . . . . no C13 As1 Fe4 C9 80.2(2) . . . . no Fe1 As1 Fe4 C11 -152.58(17) . . . . no Fe2 As1 Fe4 C11 129.12(17) . . . . no Fe3 As1 Fe4 C11 -112.50(17) . . . . no C13 As1 Fe4 C11 -5.8(2) . . . . no Fe4 As1 Fe1 As2 -51.66(4) . . . . no Fe1 As1 Fe4 Se1 15.07(4) . . . . no Fe2 As1 Fe4 Se1 -63.23(4) . . . . no Fe3 As1 Fe4 Se1 55.15(3) . . . . no C13 As1 Fe3 C8 124.2(5) . . . . no Fe4 As1 Fe3 Se1 -54.33(3) . . . . no C13 As1 Fe3 Se1 -158.17(17) . . . . no Fe2 As1 Fe3 Fe1 -39.24(4) . . . . no Fe1 As1 Fe4 C9 -66.60(13) . . . . no Fe1 As1 Fe3 Fe4 145.42(3) . . . . no Fe2 As1 Fe3 Fe4 106.18(4) . . . . no C13 As1 Fe3 Fe4 -103.84(17) . . . . no Fe1 As1 Fe3 C7 -83.95(17) . . . . no Fe2 As1 Fe3 C7 -123.19(18) . . . . no Fe4 As1 Fe3 C7 130.63(18) . . . . no C13 As1 Fe3 C7 26.8(2) . . . . no Fe1 As1 Fe3 C8 13.4(4) . . . . no Fe2 As1 Fe3 C8 -25.8(4) . . . . no Fe4 As1 Fe3 C8 -132.0(4) . . . . no Fe2 As1 Fe3 Se1 51.85(4) . . . . no Fe4 As1 Fe2 As2 61.54(4) . . . . no C13 As1 Fe2 As2 -164.77(17) . . . . no Fe3 As1 Fe2 Fe1 40.67(4) . . . . no Fe4 As1 Fe3 Fe1 -145.42(3) . . . . no C13 As1 Fe3 Fe1 110.74(17) . . . . no Fe1 As1 Fe2 As2 -55.68(3) . . . . no Fe3 As1 Fe2 As2 -15.01(4) . . . . no Fe4 As1 Fe2 Fe1 117.22(4) . . . . no Fe2 As1 Fe1 As2 56.00(3) . . . . no Fe3 As1 Fe1 As2 -89.67(3) . . . . no Fe1 As1 Fe3 Se1 91.09(3) . . . . no C14 As2 Fe2 C6 -80.4(3) . . . . no C14 As2 Fe1 Fe2 -126.8(2) . . . . no Se1 As2 Fe1 Fe2 116.04(3) . . . . no C14 As2 Fe1 As1 177.14(19) . . . . no Fe1 As2 Fe2 C6 159.15(18) . . . . no Se1 As2 Fe1 As1 60.00(3) . . . . no Fe2 As2 Fe1 As1 -56.04(3) . . . . no Se1 As2 Fe2 C4 -99.4(3) . . . . no Se1 As2 Fe1 Fe3 5.06(3) . . . . no Se1 As2 Fe2 As1 -32.34(3) . . . . no Fe1 As2 Fe2 As1 60.50(3) . . . . no C14 As2 Fe2 As1 -179.1(2) . . . . no Se1 As2 Fe2 Fe1 -92.85(3) . . . . no C14 As2 Fe2 Fe1 120.4(2) . . . . no C14 As2 Fe1 C3 49.0(2) . . . . no Fe1 As2 Fe2 C4 -6.5(3) . . . . no C14 As2 Fe2 C4 113.9(4) . . . . no Se1 As2 Fe2 C5 161.96(17) . . . . no Fe1 As2 Fe2 C5 -105.20(17) . . . . no C14 As2 Fe2 C5 15.2(3) . . . . no Se1 As2 Fe2 C6 66.30(18) . . . . no Se1 As2 Fe1 C1 -161.25(17) . . . . no Fe2 As2 Fe1 C1 82.71(17) . . . . no C14 As2 Fe1 C1 -44.1(3) . . . . no Se1 As2 Fe1 C2 99.2(5) . . . . no Fe2 As2 Fe1 C2 -16.8(5) . . . . no Fe2 As2 Fe1 Fe3 -110.98(3) . . . . no C14 As2 Fe1 Fe3 122.20(19) . . . . no Fe2 As2 Fe1 C3 175.82(15) . . . . no C14 As2 Fe1 C2 -143.7(5) . . . . no Se1 As2 Fe1 C3 -68.14(15) . . . . no C1 Fe1 Fe2 C5 -13.4(2) . . . . no C3 Fe1 Fe3 C8 4.4(2) . . . . no C1 Fe1 Fe2 C6 -153.5(5) . . . . no C3 Fe1 Fe3 C7 -87.6(2) . . . . no C3 Fe1 Fe3 Fe4 149.86(17) . . . . no C1 Fe1 Fe2 C4 81.7(2) . . . . no As1 Fe1 Fe2 As2 98.01(3) . . . . no As1 Fe1 Fe2 C4 -85.42(18) . . . . no As1 Fe1 Fe2 C5 179.49(17) . . . . no As1 Fe1 Fe2 C6 39.4(4) . . . . no As2 Fe1 Fe2 As1 -98.01(3) . . . . no As2 Fe1 Fe2 C4 176.57(18) . . . . no As2 Fe1 Fe2 C5 81.47(17) . . . . no As2 Fe1 Fe2 C6 -58.6(4) . . . . no Fe3 Fe1 Fe2 As1 -27.74(3) . . . . no Fe3 Fe1 Fe2 As2 70.28(3) . . . . no Fe3 Fe1 Fe2 C4 -113.16(18) . . . . no Fe3 Fe1 Fe2 C5 151.75(17) . . . . no Fe3 Fe1 Fe2 C6 11.7(4) . . . . no C1 Fe1 Fe2 As1 167.15(17) . . . . no C1 Fe1 Fe2 As2 -94.84(17) . . . . no C2 Fe1 Fe3 C8 104.1(2) . . . . no C3 Fe1 Fe3 Se1 96.27(17) . . . . no C3 Fe1 Fe3 As1 179.54(17) . . . . no As1 Fe1 Fe3 C8 -175.11(17) . . . . no As2 Fe1 Fe3 Se1 -4.96(3) . . . . no C2 Fe1 Fe2 As1 75.89(18) . . . . no C2 Fe1 Fe2 As2 173.91(18) . . . . no C2 Fe1 Fe2 C4 -9.5(3) . . . . no C2 Fe1 Fe2 C5 -104.6(2) . . . . no C2 Fe1 Fe2 C6 115.3(5) . . . . no C3 Fe1 Fe2 As1 -106.9(3) . . . . no C3 Fe1 Fe2 As2 -8.9(3) . . . . no C3 Fe1 Fe2 C4 167.7(4) . . . . no C3 Fe1 Fe2 C5 72.6(4) . . . . no C3 Fe1 Fe2 C6 -67.5(5) . . . . no As1 Fe1 Fe3 Se1 -83.27(3) . . . . no As1 Fe1 Fe3 Fe4 -29.69(3) . . . . no As1 Fe1 Fe3 C7 92.86(18) . . . . no Fe2 Fe1 Fe3 As1 27.80(3) . . . . no Fe2 Fe1 Fe3 Fe4 -1.89(4) . . . . no As2 Fe1 Fe3 As1 78.31(3) . . . . no As2 Fe1 Fe3 Fe4 48.63(3) . . . . no As2 Fe1 Fe3 C7 171.17(18) . . . . no As2 Fe1 Fe3 C8 -96.80(17) . . . . no Fe2 Fe1 Fe3 Se1 -55.47(3) . . . . no C2 Fe1 Fe3 C7 12.1(2) . . . . no C2 Fe1 Fe3 Se1 -164.08(17) . . . . no Fe2 Fe1 Fe3 C7 120.66(18) . . . . no Fe2 Fe1 Fe3 C8 -147.31(17) . . . . no C2 Fe1 Fe3 As1 -80.80(17) . . . . no C2 Fe1 Fe3 Fe4 -110.49(17) . . . . no Se1 Fe3 Fe4 C9 -118.25(19) . . . . no Se1 Fe3 Fe4 As1 104.20(3) . . . . no C9 Fe3 Fe4 C10 40.3(3) . . . . no C9 Fe3 Fe4 C11 -60.2(3) . . . . no C9 Fe3 Fe4 C12 170.7(4) . . . . no Se1 Fe3 Fe4 C10 -77.98(17) . . . . no Se1 Fe3 Fe4 C11 -178.42(18) . . . . no Se1 Fe3 Fe4 C12 52.5(3) . . . . no As1 Fe3 Fe4 Se1 -104.20(3) . . . . no As1 Fe3 Fe4 C9 137.56(19) . . . . no As1 Fe3 Fe4 C10 177.83(18) . . . . no As1 Fe3 Fe4 C11 77.38(18) . . . . no As1 Fe3 Fe4 C12 -51.7(3) . . . . no Fe1 Fe3 Fe4 Se1 -75.20(3) . . . . no Fe1 Fe3 Fe4 As1 29.00(3) . . . . no Fe1 Fe3 Fe4 C9 166.55(19) . . . . no Fe1 Fe3 Fe4 C10 -153.18(17) . . . . no Fe1 Fe3 Fe4 C11 106.38(18) . . . . no Fe1 Fe3 Fe4 C12 -22.7(3) . . . . no C7 Fe3 Fe4 Se1 -168.7(2) . . . . no C7 Fe3 Fe4 As1 -64.5(2) . . . . no C7 Fe3 Fe4 C9 73.1(3) . . . . no C7 Fe3 Fe4 C10 113.3(3) . . . . no C7 Fe3 Fe4 C11 12.9(3) . . . . no C7 Fe3 Fe4 C12 -116.2(4) . . . . no C8 Fe3 Fe4 Se1 53.9(2) . . . . no C8 Fe3 Fe4 As1 158.1(2) . . . . no C8 Fe3 Fe4 C9 -64.3(3) . . . . no C8 Fe3 Fe4 C10 -24.1(3) . . . . no C8 Fe3 Fe4 C11 -124.5(3) . . . . no C8 Fe3 Fe4 C12 106.4(4) . . . . no C9 Fe3 Fe4 Se1 118.25(19) . . . . no C9 Fe3 Fe4 As1 -137.56(19) . . . . no Se1 Fe3 C9 Fe4 47.30(10) . . . . no As1 Fe3 C9 Fe4 -36.49(13) . . . . no C7 Fe3 C9 Fe4 -126.40(19) . . . . no C8 Fe3 C9 Fe4 140.19(18) . . . . no Se1 Fe3 C9 O9 -135.1(12) . . . . no As1 Fe3 C9 O9 141.1(12) . . . . no Fe4 Fe3 C9 O9 177.6(13) . . . . no C7 Fe3 C9 O9 51.2(13) . . . . no C8 Fe3 C9 O9 -42.2(13) . . . . no Se1 Fe4 C9 Fe3 -48.49(13) . . . . no As1 Fe4 C9 Fe3 35.05(15) . . . . no C10 Fe4 C9 Fe3 -141.7(2) . . . . no C11 Fe4 C9 Fe3 124.6(2) . . . . no Se1 Fe4 C9 O9 132.6(5) . . . . no As1 Fe4 C9 O9 -143.9(5) . . . . no Fe3 Fe4 C9 O9 -179.0(6) . . . . no C10 Fe4 C9 O9 39.4(5) . . . . no C11 Fe4 C9 O9 -54.4(5) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se1 C8 3.063(5) . . no Se1 C9 3.120(5) . . no Se1 C10 3.029(5) . . no Se1 C12 3.160(6) . . no Se1 Se1 3.4374(7) . 2_655 no Se1 O10 3.488(4) . 2_655 no Se1 C8 3.776(5) . 2_655 no Se1 C10 3.625(5) . 2_655 no As1 Se1 3.2221(7) . . no As1 As2 2.9625(7) . . no As1 C2 3.058(5) . . no As1 C4 2.914(5) . . no As1 C6 3.254(5) . . no As1 C7 3.038(5) . . no As1 C9 3.454(5) . . no As1 C11 3.027(5) . . no As1 C12 3.190(5) . . no As2 C1 2.933(5) . . no As2 C3 3.132(5) . . no As2 C5 2.929(5) . . no As2 C6 3.386(5) . . no Fe2 O1 3.807(3) . . no Fe3 O3 3.649(3) . . no Fe3 O9 2.901(4) . . no Fe4 O1 3.840(3) . 1_545 no Fe4 O9 3.195(4) . . no O1 Fe4 3.840(3) . 1_565 no O1 O5 3.196(6) . . no O1 O10 3.092(6) . 1_565 no O1 O12 3.206(5) . 1_565 no O1 C5 3.113(6) . . no O1 C10 3.125(6) . 1_565 no O1 C12 3.206(6) . 1_565 no O1 O4 2.967(6) . 2_566 no O2 O7 3.229(6) . . no O2 O4 3.206(6) . 2_566 no O3 O10 3.109(5) . 1_565 no O3 O8 3.062(5) . . no O3 C14 3.414(6) . 2_665 no O3 C8 2.930(5) . . no O3 O7 3.194(5) . 2_565 no O4 C2 3.263(7) . 2_566 no O4 C1 3.095(7) . 2_566 no O4 C13 3.319(7) . . no O4 C4 3.242(7) . 2_566 no O4 O1 2.967(6) . 2_566 no O4 O2 3.206(6) . 2_566 no O4 O4 2.971(6) . 2_566 no O4 O11 2.979(6) . 2_556 no O5 O1 3.196(6) . . no O5 O8 3.066(6) . 1_556 no O5 C1 3.408(7) . . no O5 O5 3.114(6) . 2_666 no O6 C12 3.347(7) . . no O6 O8 3.113(5) . 1_556 no O6 O12 2.868(6) . . no O7 C3 3.253(6) . 2_565 no O7 O3 3.194(5) . 2_565 no O7 O9 3.056(5) . 2_555 no O7 C2 3.184(7) . . no O7 O2 3.229(6) . . no O7 C2 3.283(6) . 2_565 no O8 O3 3.062(5) . . no O8 C5 3.196(7) . 1_554 no O8 O10 3.178(6) . 2_655 no O8 C10 3.307(6) . 2_655 no O8 O6 3.113(5) . 1_554 no O8 C3 3.395(6) . . no O8 O5 3.066(6) . 1_554 no O8 C6 3.250(7) . 1_554 no O9 O7 3.056(5) . 2_555 no O9 C9 3.342(7) . 2_555 no O9 O11 3.065(6) . 2_555 no O9 C7 3.188(7) . 2_555 no O9 C11 3.339(7) . 2_555 no O10 O1 3.092(6) . 1_545 no O10 O3 3.109(5) . 1_545 no O10 C1 3.408(6) . 1_545 no O10 C8 3.377(6) . 2_655 no O10 O8 3.178(6) . 2_655 no O10 Se1 3.488(4) . 2_655 no O11 C4 3.183(7) . 2_556 no O11 C13 3.380(7) . . no O11 O4 2.979(6) . 2_556 no O11 O9 3.065(6) . 2_555 no O12 C14 3.321(7) . 2_656 no O12 C5 3.204(7) . 2_656 no O12 C6 3.118(7) . . no O12 O6 2.868(6) . . no O12 C6 3.386(7) . 2_656 no O12 O1 3.206(5) . 1_545 no O2 H1 2.8100 . . no O3 H6 2.6700 . 2_665 no O4 H1 2.7500 . . no O5 H5 2.6300 . 2_666 no O6 H4 2.7100 . 2_656 no O9 H3 2.4700 . 2_555 no O10 H6 2.6900 . 2_655 no O12 H4 2.7400 . 2_656 no C1 As2 2.933(5) . . no C1 Fe2 3.063(5) . . no C1 O5 3.408(7) . . no C1 O10 3.408(6) . 1_565 no C1 C2 2.590(8) . . no C1 C3 2.590(7) . . no C1 C4 3.498(8) . . no C1 C5 2.928(7) . . no C1 O4 3.095(7) . 2_566 no C2 As1 3.058(5) . . no C2 Fe2 3.616(6) . . no C2 Fe3 3.651(5) . . no C2 O7 3.184(7) . . no C2 C1 2.590(8) . . no C2 C3 2.796(8) . . no C2 C4 3.296(7) . . no C2 C7 3.042(7) . . no C2 C13 3.333(7) . . no C2 O4 3.263(7) . 2_566 no C2 O7 3.283(6) . 2_565 no C3 C2 2.796(8) . . no C3 As2 3.132(5) . . no C3 Fe3 2.975(4) . . no C3 O8 3.395(6) . . no C3 C1 2.590(7) . . no C3 O7 3.253(6) . 2_565 no C3 C7 3.316(8) . . no C3 C8 2.857(6) . . no C4 C5 2.632(8) . . no C4 As1 2.914(5) . . no C4 Fe1 3.308(5) . . no C4 C1 3.498(8) . . no C4 C2 3.296(7) . . no C4 C6 2.732(8) . . no C4 C13 3.145(8) . . no C4 O4 3.242(7) . 2_566 no C4 O11 3.183(7) . 2_556 no C5 Fe1 3.539(5) . . no C5 C1 2.928(7) . . no C5 As2 2.929(5) . . no C5 O12 3.204(7) . 2_656 no C5 O1 3.113(6) . . no C5 O8 3.196(7) . 1_556 no C5 C4 2.632(8) . . no C5 C6 2.657(7) . . no C6 O8 3.250(7) . 1_556 no C6 C4 2.732(8) . . no C6 As1 3.254(5) . . no C6 As2 3.386(5) . . no C6 C5 2.657(7) . . no C6 O12 3.118(7) . . no C6 O12 3.386(7) . 2_656 no C6 C12 3.223(8) . . no C7 Fe1 3.250(6) . . no C7 O9 3.327(6) . . no C7 As1 3.038(5) . . no C7 C13 3.345(8) . . no C7 Fe4 3.897(5) . . no C7 O9 3.188(7) . 2_555 no C7 C2 3.042(7) . . no C7 C3 3.316(8) . . no C7 C8 2.604(8) . . no C7 C9 2.576(7) . . no C8 C3 2.857(6) . . no C8 C7 2.604(8) . . no C8 Fe1 3.748(5) . . no C8 Se1 3.063(5) . . no C8 O10 3.377(6) . 2_655 no C8 O3 2.930(5) . . no C8 O9 3.332(6) . . no C8 Se1 3.776(5) . 2_655 no C8 C9 2.600(7) . . no C9 C8 2.600(7) . . no C9 C11 2.885(8) . . no C9 O9 3.342(7) . 2_555 no C9 Se1 3.120(5) . . no C9 As1 3.454(5) . . no C9 O10 3.412(6) . . no C9 C7 2.576(7) . . no C9 C10 2.677(7) . . no C10 O9 2.921(7) . . no C10 C11 2.622(8) . . no C10 C12 2.668(8) . . no C10 Se1 3.029(5) . . no C10 Fe3 3.678(5) . . no C10 O1 3.125(6) . 1_545 no C10 C9 2.677(7) . . no C10 O8 3.307(6) . 2_655 no C10 Se1 3.625(5) . 2_655 no C11 C9 2.885(8) . . no C11 C13 3.168(7) . . no C11 C10 2.622(8) . . no C11 As1 3.027(5) . . no C11 Fe3 3.626(5) . . no C11 O9 3.266(7) . . no C11 O9 3.339(7) . 2_555 no C11 C12 2.667(9) . . no C12 As1 3.190(5) . . no C12 Se1 3.160(6) . . no C12 O6 3.347(7) . . no C12 C6 3.223(8) . . no C12 O1 3.206(6) . 1_545 no C12 C11 2.667(9) . . no C12 Fe2 3.896(5) . . no C12 C10 2.668(8) . . no C13 O11 3.380(7) . . no C13 O4 3.319(7) . . no C14 O3 3.414(6) . 2_665 no C14 O12 3.321(7) . 2_656 no C2 H1 2.8200 . . no C4 H1 2.8200 . . no C7 H3 2.9300 . . no C11 H3 2.9400 . . no C11 H2 3.0900 . . no C13 H4 2.8400 . 1_455 no H1 O2 2.8100 . . no H1 O4 2.7500 . . no H1 C2 2.8200 . . no H1 C4 2.8200 . . no H1 H4 2.6000 . 1_455 no H2 C11 3.0900 . . no H3 C7 2.9300 . . no H3 C11 2.9400 . . no H3 H4 2.4900 . 1_455 no H3 O9 2.4700 . 2_555 no H4 C13 2.8400 . 1_655 no H4 H1 2.6000 . 1_655 no H4 H3 2.4900 . 1_655 no H4 O6 2.7100 . 2_656 no H4 O12 2.7400 . 2_656 no H5 O5 2.6300 . 2_666 no H6 O3 2.6700 . 2_665 no H6 O10 2.6900 . 2_655 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C13 H3 O9 0.9800 2.4700 3.439(7) 170.00 2_555 yes #===END #=============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 802731' #TrackingRef '- Combined_CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H6 As2 Fe3 O9' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C11 H6 As2 Fe3 O9' _chemical_formula_sum 'C11 H6 As2 Fe3 O9' _chemical_formula_iupac ? _chemical_formula_weight 599.55 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_space_group_name_H-M 'C m c 21' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 -x,y,z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2-y,1/2+z 7 1/2-x,1/2+y,z 8 1/2+x,1/2-y,1/2+z _cell_length_a 10.6982(4) _cell_length_b 12.3724(4) _cell_length_c 13.0665(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1729.51(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 4388 _cell_measurement_theta_min 3.0981 _cell_measurement_theta_max 32.2030 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour 'ruby red' _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.160 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.303 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 6.322 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.69973 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -60.00 59.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -24.5856 45.0000 180.0000 0.0000 0.0000 119 #__ type_ start__ end____ width___ exp.time_ 2 omega -10.00 52.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 25.5231 45.0000 300.0000 0.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 3 omega -58.00 -12.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 25.5231 -45.0000 150.0000 0.0000 0.0000 46 #__ type_ start__ end____ width___ exp.time_ 4 omega -58.00 2.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 25.5231 -45.0000 210.0000 0.0000 0.0000 60 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 6230 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 32.41 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 2526 # number of observed reflections (> n sig(I)) _reflns_number_gt 2307 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0318P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(12) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ? _refine_ls_number_reflns 2526 _refine_ls_number_parameters 128 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0521 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.757 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.105 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags As1 As Uani 0.36923(2) 0.20325(2) 0.96105(2) 1.000 0.0126(1) . . Fe1 Fe Uani 0.50000 0.06605(5) 0.90522(4) 1.000 0.0138(2) . . Fe2 Fe Uani 0.50000 0.27434(5) 0.83522(4) 1.000 0.0126(2) . . Fe3 Fe Uani 0.50000 0.32734(5) 1.03883(4) 1.000 0.0129(1) . . O1 O Uani 0.50000 -0.0716(3) 1.0864(3) 1.000 0.0352(11) . . O2 O Uani 0.2969(2) -0.0315(2) 0.7864(2) 1.000 0.0325(8) . . O3 O Uani 0.2918(2) 0.2362(2) 0.69547(18) 1.000 0.0292(7) . . O4 O Uani 0.50000 0.5098(3) 0.8220(3) 1.000 0.0288(10) . . O5 O Uani 0.7045(2) 0.4829(2) 1.06746(19) 1.000 0.0324(8) . . O6 O Uani 0.50000 0.2282(3) 1.2411(3) 1.000 0.0272(10) . . C1 C Uani 0.50000 -0.0183(4) 1.0158(3) 1.000 0.0212(11) . . C2 C Uani 0.3765(3) 0.0060(2) 0.8321(2) 1.000 0.0202(8) . . C3 C Uani 0.3726(3) 0.2522(3) 0.7502(2) 1.000 0.0179(8) . . C4 C Uani 0.50000 0.4173(4) 0.8323(3) 1.000 0.0193(11) . . C5 C Uani 0.6244(3) 0.4228(3) 1.0553(2) 1.000 0.0200(8) . . C6 C Uani 0.50000 0.2679(3) 1.1629(3) 1.000 0.0158(11) . . C7 C Uani 0.1884(2) 0.2121(3) 0.9495(3) 1.000 0.0198(8) . . H7A H Uiso 0.15030 0.19420 1.01560 1.000 0.0240 calc R H7B H Uiso 0.15930 0.16100 0.89740 1.000 0.0240 calc R H7C H Uiso 0.16440 0.28560 0.92980 1.000 0.0240 calc R 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 As1 0.0089(1) 0.0160(1) 0.0130(1) -0.0003(1) 0.0002(1) -0.0002(1) Fe1 0.0115(2) 0.0142(3) 0.0157(3) 0.0001(2) 0.0000 0.0000 Fe2 0.0102(2) 0.0157(3) 0.0119(3) 0.0006(2) 0.0000 0.0000 Fe3 0.0106(2) 0.0158(3) 0.0124(2) -0.0013(2) 0.0000 0.0000 O1 0.034(2) 0.040(2) 0.0315(19) 0.0218(17) 0.0000 0.0000 O2 0.0292(13) 0.0318(13) 0.0366(13) -0.0065(11) -0.0111(11) -0.0083(10) O3 0.0215(12) 0.0455(15) 0.0205(11) -0.0012(10) -0.0078(9) 0.0006(10) O4 0.0349(19) 0.0187(16) 0.0327(19) 0.0025(14) 0.0000 0.0000 O5 0.0273(13) 0.0313(13) 0.0385(15) 0.0020(11) -0.0062(10) -0.0140(10) O6 0.0260(17) 0.0371(19) 0.0185(16) 0.0052(14) 0.0000 0.0000 C1 0.0115(18) 0.022(2) 0.030(2) -0.0015(17) 0.0000 0.0000 C2 0.0194(14) 0.0172(13) 0.0240(14) -0.0020(12) 0.0010(12) 0.0019(10) C3 0.0175(14) 0.0204(14) 0.0159(13) 0.0003(11) 0.0017(10) -0.0005(11) C4 0.0180(19) 0.023(2) 0.0169(18) 0.0028(17) 0.0000 0.0000 C5 0.0158(14) 0.0228(14) 0.0213(15) 0.0006(12) 0.0000(10) 0.0025(11) C6 0.0120(19) 0.0208(19) 0.0146(18) -0.0020(15) 0.0000 0.0000 C7 0.0087(11) 0.0291(14) 0.0215(15) -0.0011(13) 0.0023(11) -0.0003(10) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 Fe1 2.3175(5) . . yes As1 Fe2 2.3311(5) . . yes As1 Fe3 2.3124(5) . . yes As1 C7 1.944(2) . . yes As1 As1 2.7980(3) . 3_655 yes Fe1 Fe2 2.7346(9) . . yes Fe1 C1 1.782(4) . . yes Fe1 C2 1.792(3) . . yes Fe1 C2 1.792(3) . 3_655 yes Fe2 Fe3 2.7401(8) . . yes Fe2 C3 1.780(3) . . yes Fe2 C4 1.769(5) . . yes Fe2 C3 1.780(3) . 3_655 yes Fe3 C5 1.792(3) . . yes Fe3 C6 1.780(4) . . yes Fe3 C5 1.792(3) . 3_655 yes O1 C1 1.134(6) . . yes O2 C2 1.139(4) . . yes O3 C3 1.139(4) . . yes O4 C4 1.152(6) . . yes O5 C5 1.146(4) . . yes O6 C6 1.134(5) . . yes C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 As1 Fe2 72.07(2) . . . yes Fe1 As1 Fe3 105.04(2) . . . yes Fe1 As1 C7 128.15(11) . . . yes As1 As1 Fe1 52.87(1) 3_655 . . yes Fe2 As1 Fe3 72.33(2) . . . yes Fe2 As1 C7 121.42(11) . . . yes As1 As1 Fe2 53.12(1) 3_655 . . yes Fe3 As1 C7 126.79(11) . . . yes As1 As1 Fe3 52.77(1) 3_655 . . yes As1 As1 C7 174.50(11) 3_655 . . yes As1 Fe1 Fe2 54.20(2) . . . yes As1 Fe1 C1 100.00(12) . . . yes As1 Fe1 C2 91.52(9) . . . yes As1 Fe1 As1 74.27(2) . . 3_655 yes As1 Fe1 C2 156.45(9) . . 3_655 yes Fe2 Fe1 C1 145.38(15) . . . yes Fe2 Fe1 C2 102.26(8) . . . yes As1 Fe1 Fe2 54.20(2) 3_655 . . yes Fe2 Fe1 C2 102.26(8) . . 3_655 yes C1 Fe1 C2 100.92(13) . . . yes As1 Fe1 C1 100.00(12) 3_655 . . yes C1 Fe1 C2 100.92(13) . . 3_655 yes As1 Fe1 C2 156.45(9) 3_655 . . yes C2 Fe1 C2 95.02(13) . . 3_655 yes As1 Fe1 C2 91.52(9) 3_655 . 3_655 yes As1 Fe2 Fe1 53.74(2) . . . yes As1 Fe2 Fe3 53.52(1) . . . yes As1 Fe2 C3 85.56(10) . . . yes As1 Fe2 C4 113.11(10) . . . yes As1 Fe2 As1 73.76(2) . . 3_655 yes As1 Fe2 C3 147.34(12) . . 3_655 yes Fe1 Fe2 Fe3 84.31(2) . . . yes Fe1 Fe2 C3 93.66(12) . . . yes Fe1 Fe2 C4 161.70(13) . . . yes As1 Fe2 Fe1 53.74(2) 3_655 . . yes Fe1 Fe2 C3 93.66(12) . . 3_655 yes Fe3 Fe2 C3 130.01(9) . . . yes Fe3 Fe2 C4 77.39(13) . . . yes As1 Fe2 Fe3 53.52(1) 3_655 . . yes Fe3 Fe2 C3 130.01(9) . . 3_655 yes C3 Fe2 C4 98.07(15) . . . yes As1 Fe2 C3 147.34(12) 3_655 . . yes C3 Fe2 C3 99.97(14) . . 3_655 yes As1 Fe2 C4 113.11(10) 3_655 . . yes C3 Fe2 C4 98.07(15) 3_655 . . yes As1 Fe2 C3 85.56(10) 3_655 . 3_655 yes As1 Fe3 Fe2 54.15(2) . . . yes As1 Fe3 C5 159.97(9) . . . yes As1 Fe3 C6 97.24(10) . . . yes As1 Fe3 As1 74.46(2) . . 3_655 yes As1 Fe3 C5 92.35(11) . . 3_655 yes Fe2 Fe3 C5 105.92(9) . . . yes Fe2 Fe3 C6 141.75(13) . . . yes As1 Fe3 Fe2 54.15(2) 3_655 . . yes Fe2 Fe3 C5 105.92(9) . . 3_655 yes C5 Fe3 C6 99.37(12) . . . yes As1 Fe3 C5 92.35(11) 3_655 . . yes C5 Fe3 C5 95.90(16) . . 3_655 yes As1 Fe3 C6 97.24(10) 3_655 . . yes C5 Fe3 C6 99.37(12) 3_655 . . yes As1 Fe3 C5 159.97(9) 3_655 . 3_655 yes Fe1 C1 O1 179.7(4) . . . yes Fe1 C2 O2 179.1(3) . . . yes Fe2 C3 O3 178.8(3) . . . yes Fe2 C4 O4 174.5(4) . . . yes Fe3 C5 O5 178.8(3) . . . yes Fe3 C6 O6 178.7(4) . . . yes As1 C7 H7A 109.00 . . . no As1 C7 H7B 110.00 . . . no As1 C7 H7C 109.00 . . . no H7A C7 H7B 110.00 . . . no H7A C7 H7C 109.00 . . . no H7B C7 H7C 109.00 . . . no 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 As1 As1 Fe2 94.89(3) . . 3_655 . no Fe1 As1 As1 Fe3 -169.75(3) . . 3_655 . no Fe2 As1 As1 Fe1 -94.89(3) . . 3_655 . no Fe2 As1 As1 Fe3 95.36(3) . . 3_655 . no Fe3 As1 As1 Fe1 169.75(3) . . 3_655 . no Fe3 As1 As1 Fe2 -95.36(3) . . 3_655 . no Fe3 As1 Fe1 Fe2 -65.33(2) . . . . no C7 As1 Fe1 Fe2 116.27(15) . . . . no As1 As1 Fe1 Fe2 -56.90(2) 3_655 . . . no Fe2 As1 Fe1 C1 154.57(9) . . . . no Fe3 As1 Fe1 C1 89.24(9) . . . . no C7 As1 Fe1 C1 -89.16(17) . . . . no As1 As1 Fe1 C1 97.68(9) 3_655 . . . no Fe2 As1 Fe1 C2 -104.06(9) . . . . no Fe3 As1 Fe1 C2 -169.39(9) . . . . no C7 As1 Fe1 C2 12.21(17) . . . . no As1 As1 Fe1 C2 -160.96(9) 3_655 . . . no Fe2 As1 Fe1 As1 56.90(2) . . . 3_655 no Fe3 As1 Fe1 As1 -8.43(2) . . . 3_655 no C7 As1 Fe1 As1 173.17(15) . . . 3_655 no Fe2 As1 Fe1 C2 2.2(2) . . . 3_655 no Fe3 As1 Fe1 C2 -63.2(2) . . . 3_655 no C7 As1 Fe1 C2 118.5(3) . . . 3_655 no Fe3 As1 Fe2 As1 -56.31(2) . 3_655 . . no As1 As1 Fe2 Fe1 -56.61(2) . 3_655 . . no As1 As1 Fe2 Fe3 56.31(2) . 3_655 . . no As1 As1 Fe2 C3 -52.86(18) . 3_655 . . no Fe1 As1 Fe2 C3 3.75(18) . 3_655 . . no Fe3 As1 Fe2 C3 -109.16(18) . 3_655 . . no As1 As1 Fe2 C4 108.67(9) . 3_655 . . no Fe1 As1 Fe3 Fe2 65.15(2) . . . . no C7 As1 Fe3 Fe2 -116.42(14) . . . . no As1 As1 Fe3 Fe2 56.71(2) 3_655 . . . no Fe1 As1 Fe3 C5 58.8(3) . . . . no Fe2 As1 Fe3 C5 -6.4(3) . . . . no C7 As1 Fe3 C5 -122.8(4) . . . . no As1 As1 Fe3 C5 50.3(3) 3_655 . . . no Fe1 As1 Fe3 C6 -87.09(8) . . . . no Fe2 As1 Fe3 C6 -152.24(8) . . . . no Fe2 As1 Fe1 As1 -56.90(2) . 3_655 . . no Fe3 As1 Fe1 As1 8.43(2) . 3_655 . . no As1 As1 Fe1 Fe2 56.90(2) . 3_655 . . no As1 As1 Fe1 C1 -97.68(9) . 3_655 . . no As1 As1 Fe1 C2 54.7(2) . 3_655 . . no Fe2 As1 Fe1 C2 -2.2(2) . 3_655 . . no Fe3 As1 Fe1 C2 63.2(2) . 3_655 . . no Fe3 As1 Fe2 Fe1 112.91(2) . . . . no C7 As1 Fe2 Fe1 -124.27(13) . . . . no As1 As1 Fe2 Fe1 56.61(2) 3_655 . . . no Fe1 As1 Fe2 Fe3 -112.91(2) . . . . no C7 As1 Fe2 Fe3 122.82(13) . . . . no As1 As1 Fe2 Fe3 -56.31(2) 3_655 . . . no Fe1 As1 Fe2 C3 97.83(12) . . . . no Fe3 As1 Fe2 C3 -149.26(12) . . . . no C7 As1 Fe2 C3 -26.44(18) . . . . no As1 As1 Fe2 C3 154.44(12) 3_655 . . . no Fe1 As1 Fe2 C4 -165.28(9) . . . . no Fe3 As1 Fe2 C4 -52.36(9) . . . . no C7 As1 Fe2 C4 70.45(16) . . . . no As1 As1 Fe2 C4 -108.67(9) 3_655 . . . no Fe1 As1 Fe2 As1 -56.61(2) . . . 3_655 no Fe3 As1 Fe2 As1 56.31(2) . . . 3_655 no C7 As1 Fe2 As1 179.12(13) . . . 3_655 no Fe1 As1 Fe2 C3 -3.75(18) . . . 3_655 no Fe3 As1 Fe2 C3 109.16(18) . . . 3_655 no C7 As1 Fe2 C3 -128.0(2) . . . 3_655 no As1 As1 Fe3 Fe2 -56.71(2) . 3_655 . . no As1 As1 Fe3 C5 -164.70(10) . 3_655 . . no Fe1 As1 Fe3 C5 -173.15(9) . 3_655 . . no Fe2 As1 Fe3 C5 -108.00(9) . 3_655 . . no Fe1 As1 Fe2 As1 56.61(2) . 3_655 . . no C7 As1 Fe3 C6 91.34(16) . . . . no As1 As1 Fe3 C6 -95.54(8) 3_655 . . . no Fe1 As1 Fe3 As1 8.45(2) . . . 3_655 no Fe2 As1 Fe3 As1 -56.71(2) . . . 3_655 no C7 As1 Fe3 As1 -173.13(14) . . . 3_655 no Fe1 As1 Fe3 C5 173.15(9) . . . 3_655 no Fe2 As1 Fe3 C5 108.00(9) . . . 3_655 no C7 As1 Fe3 C5 -8.42(17) . . . 3_655 no Fe1 As1 Fe3 As1 -8.45(2) . 3_655 . . no Fe2 As1 Fe3 As1 56.71(2) . 3_655 . . no As1 As1 Fe3 C6 95.54(8) . 3_655 . . no C2 Fe1 Fe2 C3 -99.12(14) . . . 3_655 no As1 Fe1 Fe2 As1 -96.20(2) 3_655 . . . no C2 Fe1 Fe2 As1 -179.11(10) 3_655 . . . no C2 Fe1 Fe2 C3 99.12(14) 3_655 . . . no As1 Fe1 Fe2 C3 -177.97(10) 3_655 . . . no As1 Fe1 Fe2 C3 -81.77(10) . . . . no As1 Fe1 Fe2 As1 96.20(2) . . . 3_655 no As1 Fe1 Fe2 C3 177.97(10) . . . 3_655 no C1 Fe1 Fe2 As1 -48.10(1) . . . . no C1 Fe1 Fe2 Fe3 0.00 . . . . no C1 Fe1 Fe2 C3 -129.87(10) . . . . no C2 Fe1 Fe2 As1 82.91(10) . . . . no C2 Fe1 Fe2 Fe3 131.01(10) . . . . no C2 Fe1 Fe2 C3 1.14(14) . . . . no C2 Fe1 Fe2 As1 179.11(10) . . . 3_655 no As1 Fe1 Fe2 Fe3 48.10(1) . . . . no As1 Fe2 Fe3 C5 177.73(12) . . . . no As1 Fe2 Fe3 As1 96.56(2) . . . 3_655 no As1 Fe2 Fe3 C5 -81.18(12) . . . 3_655 no As1 Fe2 Fe3 C6 48.28(1) . . . . no Fe1 Fe2 Fe3 C5 129.45(12) . . . . no Fe1 Fe2 Fe3 C6 0.00 . . . . no C3 Fe2 Fe3 As1 41.72(16) . . . . no C3 Fe2 Fe3 C5 -140.6(2) . . . . no C3 Fe2 Fe3 C6 90.00(16) . . . . no C3 Fe2 Fe3 As1 138.27(16) . . . 3_655 no C3 Fe2 Fe3 C5 -39.5(2) . . . 3_655 no C4 Fe2 Fe3 As1 131.72(1) . . . . no C4 Fe2 Fe3 C5 -50.55(12) . . . . no C4 Fe2 Fe3 C6 180.00 . . . . no As1 Fe2 Fe3 As1 -96.56(2) 3_655 . . . no As1 Fe2 Fe3 C5 81.18(12) 3_655 . . . no C3 Fe2 Fe3 As1 -138.27(16) 3_655 . . . no C3 Fe2 Fe3 C5 39.5(2) 3_655 . . . no Fe1 Fe2 Fe3 As1 -48.28(1) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag As1 C1 3.160(4) . . no As1 C2 2.967(3) . . no As1 C3 2.821(3) . . no As1 C4 3.435(4) . . no As1 C6 3.091(3) . . no As1 C5 2.983(4) . 3_655 no As1 O5 3.532(2) . 5_445 no Fe3 O4 3.623(4) . . no Fe3 O3 3.815(2) . 6_555 no Fe3 O3 3.815(2) . 8_555 no O1 C3 3.381(5) . 2_655 no O1 C3 3.381(5) . 4_555 no O2 C4 3.294(2) . 5_445 no O2 C3 3.267(4) . 7_545 no O2 C4 3.294(2) . 7_545 no O2 O5 3.086(4) . 8_454 no O3 Fe3 3.815(2) . 6_554 no O3 O6 3.209(2) . 6_554 no O3 C6 3.151(2) . 6_554 no O3 C7 3.284(5) . 6_554 no O3 C5 3.230(4) . 8_454 no O3 Fe3 3.815(2) . 8_454 no O3 O6 3.209(2) . 8_454 no O3 C6 3.151(2) . 8_454 no O5 As1 3.532(2) . 5_555 no O5 O2 3.086(4) . 8_555 no O5 C7 3.232(4) . 5_555 no O5 C1 3.233(2) . 5_555 no O5 C1 3.233(2) . 7_655 no O6 O3 3.209(2) . 6_555 no O6 C2 3.399(4) . 2_655 no O6 O3 3.209(2) . 8_555 no O6 C2 3.399(4) . 4_555 no O3 H7A 2.5800 . 6_554 no O4 H7B 2.7200 . 7_555 no O4 H7B 2.7200 . 5_555 no O5 H7A 2.7600 . 5_555 no C1 As1 3.160(4) . . no C1 C2 2.756(4) . . no C1 As1 3.160(4) . 3_655 no C1 C2 2.756(4) . 3_655 no C1 O5 3.233(2) . 5_445 no C1 O5 3.233(2) . 7_645 no C2 As1 2.967(3) . . no C2 Fe2 3.574(3) . . no C2 C1 2.756(4) . . no C2 C3 3.229(4) . . no C2 C7 3.592(4) . . no C2 O6 3.399(4) . 2_654 no C2 C2 2.643(5) . 3_655 no C2 O6 3.399(4) . 4_554 no C3 C3 2.726(5) . 3_655 no C3 As1 2.821(3) . . no C3 Fe1 3.356(3) . . no C3 C2 3.229(4) . . no C3 C4 2.680(5) . . no C3 C7 3.303(4) . . no C3 O1 3.381(5) . 2_654 no C3 O1 3.381(5) . 4_554 no C3 O2 3.267(4) . 7_555 no C4 C3 2.680(5) . 3_655 no C4 As1 3.435(4) . . no C4 Fe3 2.919(4) . . no C4 C3 2.680(5) . . no C4 C5 3.204(4) . . no C4 As1 3.435(4) . 3_655 no C4 O2 3.294(2) . 7_555 no C4 C5 3.204(4) . 3_655 no C4 O2 3.294(2) . 5_555 no C5 As1 2.983(4) . 3_655 no C5 Fe2 3.663(3) . . no C5 C4 3.204(4) . . no C5 C6 2.724(5) . . no C5 O3 3.230(4) . 8_555 no C5 C5 2.662(5) . 3_655 no C5 C7 3.566(5) . 3_655 no C6 O3 3.151(2) . 8_555 no C6 As1 3.091(3) . . no C6 C5 2.724(5) . . no C6 As1 3.091(3) . 3_655 no C6 C5 2.724(5) . 3_655 no C6 O3 3.151(2) . 6_555 no C7 O5 3.232(5) . 5_445 no C7 O3 3.284(5) . 6_555 no C2 H7C 3.0400 . 7_545 no H7A O5 2.7600 . 5_445 no H7A O3 2.5800 . 6_555 no H7B O4 2.7200 . 5_445 no H7B O4 2.7200 . 7_545 no H7C C2 3.0400 . 7_555 no #===END