# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Stefanie Dehnen' _publ_contact_author_email DEHNEN@CHEMIE.UNI-MARBURG.DE _publ_section_title ; Synthesis and Reactivity of Ferrocenyl functionalized Sn/S Cages ; loop_ _publ_author_name 'Stefanie Dehnen' 'Christopher Pohlker' 'Rainer Pottgen' 'Inga Schellenberg' # end Validation Reply Form # Attachment '2-rev2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 755030' #TrackingRef '2-rev2.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C72 H90 FE6 NA6 O10 S12 SN6' _chemical_formula_sum 'C72 H90 Fe6 Na6 O10 S12 Sn6' _chemical_formula_weight 2685.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.830(3) _cell_length_b 18.538(4) _cell_length_c 20.011(4) _cell_angle_alpha 79.70(3) _cell_angle_beta 81.30(3) _cell_angle_gamma 81.10(3) _cell_volume 4588.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27921 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 54.46 _exptl_crystal_description rhombouses _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 2.872 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.187 _exptl_absorpt_correction_T_max 0.319 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1997)' _exptl_special_details ; The obtained crystal was weakly diffracting and therefore the quality of the X-ray data is limited. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDSII _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30816 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.00 _reflns_number_total 16699 _reflns_number_gt 12539 _reflns_threshold_expression >2sigma(I) _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^)+(0.0662P)^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_extinction_coef ? _refine_ls_number_reflns 16699 _refine_ls_number_parameters 1016 _refine_ls_number_restraints 549 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _computing_data_collection 'XAREA 1.38 (Stoe 2006)' _computing_cell_refinement 'XAREA 1.38 (Stoe 2006)' _computing_data_reduction 'XAREA 1.38 (Stoe 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005) SHELXTL-NT V5.1, Bruker AXS 1999' 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 Sn1 Sn 0.93543(4) 0.30127(3) 0.27645(2) 0.03085(12) Uani 1 1 d . . . Sn2 Sn 0.73972(5) 0.28961(3) 0.15356(2) 0.03516(13) Uani 1 1 d . . . Sn3 Sn 0.63469(3) 0.31956(2) 0.34092(2) 0.02271(10) Uani 1 1 d . . . Sn4 Sn 0.82719(3) 0.69789(2) 0.28424(2) 0.02117(10) Uani 1 1 d . . . Sn5 Sn 0.79639(3) 0.71765(2) 0.08661(2) 0.02173(10) Uani 1 1 d . . . Sn6 Sn 0.54732(3) 0.70521(2) 0.22681(2) 0.02056(10) Uani 1 1 d . . . Fe1 Fe 1.09614(7) 0.12923(5) 0.34941(5) 0.0259(2) Uani 1 1 d . . . Fe2 Fe 0.61184(10) 0.15153(6) 0.09205(5) 0.0419(3) Uani 1 1 d . . . Fe3 Fe 0.58904(7) 0.13863(5) 0.44116(5) 0.0271(2) Uani 1 1 d . . . Fe4 Fe 0.87155(7) 0.85985(5) 0.34305(5) 0.0254(2) Uani 1 1 d . . . Fe5 Fe 0.87636(8) 0.88920(5) -0.01526(5) 0.0302(2) Uani 1 1 d . . . Fe6 Fe 0.37542(7) 0.88133(5) 0.24365(5) 0.0240(2) Uani 1 1 d . . . S1 S 0.8704(2) 0.21554(12) 0.21725(11) 0.0595(7) Uani 1 1 d . A . S2 S 0.64882(13) 0.37987(9) 0.22336(8) 0.0281(4) Uani 1 1 d . . . S3 S 0.80862(12) 0.31234(9) 0.37866(7) 0.0238(3) Uani 1 1 d . A . S4 S 0.96750(15) 0.41504(10) 0.21134(9) 0.0360(4) Uani 1 1 d . . . S5 S 0.80777(14) 0.34888(9) 0.04707(8) 0.0290(4) Uani 1 1 d . A . S6 S 0.50949(13) 0.40052(10) 0.39732(9) 0.0311(4) Uani 1 1 d . . . S7 S 0.85759(13) 0.63473(8) 0.18528(8) 0.0232(3) Uani 1 1 d . . . S8 S 0.63743(13) 0.72950(10) 0.31658(8) 0.0270(3) Uani 1 1 d . . . S9 S 0.61150(13) 0.76597(9) 0.11433(8) 0.0274(3) Uani 1 1 d . . . S10 S 0.81260(13) 0.64728(9) -0.00039(8) 0.0259(3) Uani 1 1 d . . . S11 S 0.54572(13) 0.57844(9) 0.23464(8) 0.0249(3) Uani 1 1 d . . . S12 S 0.91111(13) 0.60954(9) 0.36397(8) 0.0263(3) Uani 1 1 d . . . Na1 Na 1.0416(2) 0.52018(18) 0.27289(15) 0.0433(7) Uani 1 1 d . . . Na2 Na 0.9883(3) 0.4020(2) 0.06995(18) 0.0562(9) Uani 1 1 d . . . Na3 Na 0.7626(2) 0.50251(14) 0.21673(12) 0.0249(5) Uani 1 1 d . . . Na4 Na 0.5830(2) 0.53834(16) 0.37060(14) 0.0379(7) Uani 1 1 d . . . Na5 Na 0.5514(2) 0.50983(16) 0.12016(13) 0.0321(6) Uani 1 1 d . . . Na6 Na 0.3738(3) 0.4974(2) 0.29772(18) 0.0658(12) Uani 1 1 d . . . O2 O 1.0244(6) 0.5314(4) 0.0550(5) 0.100(3) Uani 1 1 d . . . O3 O 0.7603(4) 0.4968(2) 0.3399(2) 0.0280(10) Uani 1 1 d . . . O4 O 0.7436(4) 0.5041(3) 0.1014(2) 0.0278(10) Uani 1 1 d . . . O5 O 0.5161(5) 0.6213(3) 0.4413(3) 0.0522(16) Uani 1 1 d . A . O6 O 0.5593(4) 0.6234(3) 0.0410(2) 0.0322(11) Uani 1 1 d . A . O7 O 0.5719(4) 0.4391(4) 0.0362(3) 0.0539(16) Uani 1 1 d . A . O8 O 0.3007(6) 0.5817(4) 0.3626(3) 0.071(2) Uani 1 1 d DU . . O9 O 0.3893(4) 0.4556(3) 0.1939(2) 0.0340(11) Uani 1 1 d U . . O10 O 0.1728(4) 0.4552(3) 0.3470(3) 0.0416(13) Uani 1 1 d U . . C1 C 1.0995(7) 0.0249(4) 0.4043(5) 0.051(2) Uani 1 1 d U . . H1 H 1.1513 0.0009 0.4330 0.061 Uiso 1 1 calc R . . C2 C 1.0042(6) 0.0689(4) 0.4242(4) 0.0393(18) Uani 1 1 d U . . H2 H 0.9803 0.0798 0.4691 0.047 Uiso 1 1 calc R . . C3 C 0.9510(5) 0.0938(4) 0.3673(4) 0.0319(15) Uani 1 1 d U . . H3 H 0.8848 0.1248 0.3667 0.038 Uiso 1 1 calc R . . C4 C 1.0110(5) 0.0655(4) 0.3105(4) 0.0295(14) Uani 1 1 d U . . H4 H 0.9922 0.0736 0.2653 0.035 Uiso 1 1 calc R . . C5 C 1.1039(6) 0.0230(4) 0.3327(5) 0.043(2) Uani 1 1 d U . . H5 H 1.1600 -0.0026 0.3049 0.052 Uiso 1 1 calc R . . C6 C 1.0744(5) 0.2395(4) 0.3138(3) 0.0297(15) Uani 1 1 d U . . C7 C 1.1599(5) 0.2036(4) 0.2730(4) 0.0304(15) Uani 1 1 d U . . H7 H 1.1639 0.2037 0.2252 0.036 Uiso 1 1 calc R . . C8 C 1.2379(6) 0.1677(4) 0.3147(4) 0.0300(15) Uani 1 1 d U . . H8 H 1.3029 0.1393 0.3002 0.036 Uiso 1 1 calc R . . C9 C 1.2020(6) 0.1816(4) 0.3816(4) 0.0334(16) Uani 1 1 d U . . H9 H 1.2388 0.1644 0.4204 0.040 Uiso 1 1 calc R . . C10 C 1.1015(6) 0.2258(4) 0.3813(4) 0.0319(15) Uani 1 1 d U . . H10 H 1.0595 0.2432 0.4199 0.038 Uiso 1 1 calc R . . C11A C 0.6006(7) 0.2395(5) 0.1431(4) 0.040(3) Uiso 0.631(13) 1 d PGU A 1 H11A H 0.6597 0.2605 0.1512 0.048 Uiso 0.631(13) 1 calc PR A 1 C12A C 0.5560(6) 0.1782(5) 0.1851(4) 0.024(2) Uiso 0.631(13) 1 d PGU A 1 H12A H 0.5802 0.1512 0.2261 0.029 Uiso 0.631(13) 1 calc PR A 1 C13A C 0.4687(7) 0.1646(6) 0.1547(5) 0.055(4) Uiso 0.631(13) 1 d PGU A 1 H13A H 0.4246 0.1270 0.1719 0.066 Uiso 0.631(13) 1 calc PR A 1 C14A C 0.4593(8) 0.2175(6) 0.0938(5) 0.057(4) Uiso 0.631(13) 1 d PGU A 1 H14A H 0.4079 0.2212 0.0634 0.068 Uiso 0.631(13) 1 calc PR A 1 C15A C 0.5409(8) 0.2638(6) 0.0866(5) 0.053(4) Uiso 0.631(13) 1 d PGU A 1 H15A H 0.5532 0.3037 0.0507 0.063 Uiso 0.631(13) 1 calc PR A 1 C16A C 0.7477(11) 0.1206(10) 0.0518(8) 0.158(11) Uiso 0.631(13) 1 d PGU A 1 H16A H 0.8138 0.1296 0.0624 0.189 Uiso 0.631(13) 1 calc PR A 1 C17A C 0.6919(13) 0.1654(8) 0.0005(7) 0.065(5) Uiso 0.631(13) 1 d PGU A 1 H17A H 0.7062 0.2109 -0.0272 0.078 Uiso 0.631(13) 1 calc PR A 1 C18A C 0.6088(12) 0.1232(9) 0.0018(7) 0.098(7) Uiso 0.631(13) 1 d PGU A 1 H18A H 0.5594 0.1360 -0.0306 0.118 Uiso 0.631(13) 1 calc PR A 1 C19A C 0.6033(14) 0.0676(8) 0.0484(8) 0.103(7) Uiso 0.631(13) 1 d PGU A 1 H19A H 0.5497 0.0358 0.0575 0.124 Uiso 0.631(13) 1 calc PR A 1 C20A C 0.6940(14) 0.0615(8) 0.0851(8) 0.129(9) Uiso 0.631(13) 1 d PGU A 1 H20A H 0.7126 0.0256 0.1231 0.155 Uiso 0.631(13) 1 calc PR A 1 C11B C 0.6194(17) 0.2116(11) 0.1622(9) 0.104(11) Uiso 0.369(13) 1 d PGU A 2 H11B H 0.6744 0.2420 0.1560 0.124 Uiso 0.369(13) 1 calc PR A 2 C12B C 0.6265(15) 0.1388(12) 0.1905(8) 0.136(14) Uiso 0.369(13) 1 d PGU A 2 H12B H 0.6873 0.1095 0.2075 0.163 Uiso 0.369(13) 1 calc PR A 2 C13B C 0.5310(16) 0.1154(11) 0.1902(8) 0.073(8) Uiso 0.369(13) 1 d PGU A 2 H13B H 0.5136 0.0668 0.2069 0.087 Uiso 0.369(13) 1 calc PR A 2 C14B C 0.4649(15) 0.1737(12) 0.1618(9) 0.116(14) Uiso 0.369(13) 1 d PGU A 2 H14B H 0.3933 0.1731 0.1551 0.139 Uiso 0.369(13) 1 calc PR A 2 C15B C 0.5195(17) 0.2332(11) 0.1445(9) 0.098(10) Uiso 0.369(13) 1 d PGU A 2 H15B H 0.4927 0.2813 0.1237 0.118 Uiso 0.369(13) 1 calc PR A 2 C16B C 0.7749(10) 0.1144(10) 0.0658(6) 0.077(8) Uiso 0.369(13) 1 d PGU A 2 H16B H 0.8365 0.1275 0.0792 0.092 Uiso 0.369(13) 1 calc PR A 2 C17B C 0.7265(15) 0.1517(8) 0.0087(6) 0.032(5) Uiso 0.369(13) 1 d PGU A 2 H17B H 0.7418 0.1956 -0.0216 0.039 Uiso 0.369(13) 1 calc PR A 2 C18B C 0.6492(12) 0.1057(8) 0.0089(6) 0.048(6) Uiso 0.369(13) 1 d PGU A 2 H18B H 0.6060 0.1131 -0.0270 0.058 Uiso 0.369(13) 1 calc PR A 2 C19B C 0.6400(13) 0.0544(8) 0.0588(6) 0.031(4) Uiso 0.369(13) 1 d PGU A 2 H19B H 0.5889 0.0208 0.0675 0.037 Uiso 0.369(13) 1 calc PR A 2 C20B C 0.7217(12) 0.0560(6) 0.1004(6) 0.073(8) Uiso 0.369(13) 1 d PGU A 2 H20B H 0.7359 0.0245 0.1419 0.088 Uiso 0.369(13) 1 calc PR A 2 C21 C 0.7064(6) 0.1283(5) 0.5019(3) 0.0369(17) Uani 1 1 d GU A . H21 H 0.7799 0.1303 0.4866 0.044 Uiso 1 1 calc R . . C22 C 0.6556(7) 0.0640(4) 0.5157(4) 0.0397(18) Uani 1 1 d U A . H22 H 0.6891 0.0153 0.5115 0.048 Uiso 1 1 calc R . . C23 C 0.5463(6) 0.0843(4) 0.5369(3) 0.0374(17) Uani 1 1 d U A . H23 H 0.4935 0.0519 0.5492 0.045 Uiso 1 1 calc R . . C24 C 0.5300(6) 0.1617(4) 0.5362(4) 0.0368(17) Uani 1 1 d U A . H24 H 0.4639 0.1904 0.5482 0.044 Uiso 1 1 calc R . . C25 C 0.6294(7) 0.1895(5) 0.5146(4) 0.0402(18) Uani 1 1 d U A . H25 H 0.6417 0.2395 0.5097 0.048 Uiso 1 1 calc R . . C26 C 0.4853(6) 0.1941(4) 0.3763(4) 0.0340(16) Uani 1 1 d U A . H26 H 0.4245 0.2281 0.3877 0.041 Uiso 1 1 calc R . . C27 C 0.4879(6) 0.1170(4) 0.3803(4) 0.0389(18) Uani 1 1 d U A . H27 H 0.4287 0.0904 0.3949 0.047 Uiso 1 1 calc R . . C28 C 0.5921(6) 0.0861(4) 0.3594(4) 0.0376(17) Uani 1 1 d U A . H28 H 0.6154 0.0352 0.3571 0.045 Uiso 1 1 calc R . . C29 C 0.6567(6) 0.1442(4) 0.3420(3) 0.0304(15) Uani 1 1 d U A . H29 H 0.7308 0.1388 0.3266 0.036 Uiso 1 1 calc R . . C30 C 0.5907(6) 0.2121(4) 0.3519(3) 0.0292(15) Uani 1 1 d U A . C31 C 0.7993(6) 0.8733(4) 0.2572(3) 0.0314(15) Uani 1 1 d U . . H31 H 0.7249 0.8777 0.2555 0.038 Uiso 1 1 calc R . . C32 C 0.8578(6) 0.9316(4) 0.2543(4) 0.0338(16) Uani 1 1 d U . . H32 H 0.8295 0.9824 0.2502 0.041 Uiso 1 1 calc R . . C33 C 0.9658(6) 0.9031(4) 0.2585(4) 0.0344(16) Uani 1 1 d U . . H33 H 1.0222 0.9309 0.2581 0.041 Uiso 1 1 calc R . . C34 C 0.9739(6) 0.8254(4) 0.2635(3) 0.0289(14) Uani 1 1 d U . . H34 H 1.0377 0.7919 0.2665 0.035 Uiso 1 1 calc R . . C35 C 0.8714(5) 0.8054(4) 0.2631(3) 0.0247(13) Uani 1 1 d U . . C36 C 0.8459(9) 0.9178(5) 0.4223(4) 0.058(3) Uani 1 1 d U . . H36 H 0.8419 0.9699 0.4184 0.070 Uiso 1 1 calc R . . C37 C 0.7597(7) 0.8790(5) 0.4244(4) 0.045(2) Uani 1 1 d U . . H37 H 0.6875 0.8995 0.4219 0.054 Uiso 1 1 calc R . . C38 C 0.8015(7) 0.8026(4) 0.4308(3) 0.0382(17) Uani 1 1 d U . . H38 H 0.7620 0.7625 0.4341 0.046 Uiso 1 1 calc R . . C39 C 0.9094(8) 0.7975(6) 0.4314(4) 0.056(3) Uani 1 1 d U . . H39 H 0.9570 0.7527 0.4344 0.068 Uiso 1 1 calc R . . C40 C 0.9389(8) 0.8675(7) 0.4270(4) 0.064(3) Uani 1 1 d U . . H40 H 1.0085 0.8789 0.4271 0.077 Uiso 1 1 calc R . . C41 C 0.9826(6) 0.8161(5) 0.0369(6) 0.060(3) Uani 1 1 d U B . H41 H 1.0307 0.7782 0.0184 0.072 Uiso 1 1 calc R . . C42 C 0.8788(6) 0.8101(4) 0.0696(4) 0.0347(16) Uani 1 1 d U B . C43 C 0.8367(7) 0.8807(4) 0.0872(4) 0.0403(18) Uani 1 1 d U B . H43 H 0.7671 0.8932 0.1095 0.048 Uiso 1 1 calc R . . C44 C 0.9134(8) 0.9291(5) 0.0668(5) 0.054(2) Uani 1 1 d U B . H44 H 0.9053 0.9795 0.0726 0.065 Uiso 1 1 calc R . . C45 C 1.0024(8) 0.8901(5) 0.0366(6) 0.066(3) Uani 1 1 d U B . H45 H 1.0672 0.9092 0.0184 0.079 Uiso 1 1 calc R . . C46A C 0.8841(12) 0.8748(8) -0.1166(7) 0.050(4) Uani 0.68(3) 1 d PGU B 1 H46A H 0.9359 0.8414 -0.1387 0.060 Uiso 0.68(3) 1 calc PR B 1 C47A C 0.7844(12) 0.8592(6) -0.0819(7) 0.042(4) Uani 0.68(3) 1 d PGU B 1 H47A H 0.7570 0.8134 -0.0764 0.050 Uiso 0.68(3) 1 calc PR B 1 C48A C 0.7324(11) 0.9232(7) -0.0566(7) 0.038(3) Uani 0.68(3) 1 d PGU B 1 H48A H 0.6636 0.9283 -0.0311 0.046 Uiso 0.68(3) 1 calc PR B 1 C49A C 0.7999(14) 0.9784(6) -0.0758(6) 0.041(4) Uani 0.68(3) 1 d PGU B 1 H49A H 0.7849 1.0273 -0.0655 0.049 Uiso 0.68(3) 1 calc PR B 1 C50A C 0.8937(14) 0.9484(8) -0.1128(5) 0.046(5) Uani 0.68(3) 1 d PGU B 1 H50A H 0.9531 0.9735 -0.1320 0.055 Uiso 0.68(3) 1 calc PR B 1 C46B C 0.909(2) 0.8513(14) -0.1012(13) 0.035(6) Uani 0.32(3) 1 d PGU B 2 H46B H 0.9507 0.8065 -0.1105 0.042 Uiso 0.32(3) 1 calc PR B 2 C47B C 0.804(2) 0.8588(13) -0.0737(16) 0.040(7) Uani 0.32(3) 1 d PGU B 2 H47B H 0.7610 0.8201 -0.0606 0.048 Uiso 0.32(3) 1 calc PR B 2 C48B C 0.773(3) 0.9314(15) -0.0685(15) 0.042(7) Uani 0.32(3) 1 d PGU B 2 H48B H 0.7041 0.9523 -0.0510 0.050 Uiso 0.32(3) 1 calc PR B 2 C49B C 0.858(3) 0.9689(13) -0.0927(13) 0.041(8) Uani 0.32(3) 1 d PGU B 2 H49B H 0.8586 1.0204 -0.0950 0.049 Uiso 0.32(3) 1 calc PR B 2 C50B C 0.942(3) 0.9194(17) -0.1128(12) 0.043(7) Uani 0.32(3) 1 d PGU B 2 H50B H 1.0110 0.9303 -0.1318 0.052 Uiso 0.32(3) 1 calc PR B 2 C51 C 0.3970(5) 0.7696(3) 0.2428(3) 0.0246(13) Uani 1 1 d U . . C52 C 0.3324(5) 0.8074(4) 0.1925(4) 0.0274(14) Uani 1 1 d U . . H52 H 0.3481 0.8064 0.1447 0.033 Uiso 1 1 calc R . . C53 C 0.2416(5) 0.8465(4) 0.2245(4) 0.0347(16) Uani 1 1 d U . . H53 H 0.1858 0.8764 0.2022 0.042 Uiso 1 1 calc R . . C54 C 0.2477(6) 0.8335(4) 0.2961(4) 0.0343(16) Uani 1 1 d U . . H54 H 0.1965 0.8532 0.3299 0.041 Uiso 1 1 calc R . . C55 C 0.3426(5) 0.7866(4) 0.3085(3) 0.0266(14) Uani 1 1 d U . . H55 H 0.3667 0.7692 0.3519 0.032 Uiso 1 1 calc R . . C56 C 0.5166(5) 0.9204(4) 0.2089(4) 0.0279(14) Uani 1 1 d U . . H56 H 0.5795 0.8929 0.1900 0.033 Uiso 1 1 calc R . . C57 C 0.4878(5) 0.9269(4) 0.2791(3) 0.0276(14) Uani 1 1 d U . . H57 H 0.5275 0.9049 0.3157 0.033 Uiso 1 1 calc R . . C58 C 0.3886(5) 0.9726(4) 0.2841(4) 0.0288(14) Uani 1 1 d U . . H58 H 0.3500 0.9869 0.3250 0.035 Uiso 1 1 calc R . . C59 C 0.3566(6) 0.9931(4) 0.2186(4) 0.0346(16) Uani 1 1 d U . . H59 H 0.2925 1.0231 0.2077 0.042 Uiso 1 1 calc R . . C60 C 0.4364(6) 0.9615(4) 0.1720(4) 0.0345(16) Uani 1 1 d U . . H60 H 0.4360 0.9670 0.1239 0.041 Uiso 1 1 calc R . . C01 C 0.1753(7) 0.6628(5) 0.4198(4) 0.048(2) Uani 1 1 d U . . H01C H 0.1897 0.6998 0.3791 0.058 Uiso 1 1 calc R A . H01D H 0.1784 0.6838 0.4610 0.058 Uiso 1 1 calc R . . H01E H 0.1044 0.6487 0.4212 0.058 Uiso 1 1 calc R . . C02 C 0.2564(7) 0.5964(5) 0.4168(4) 0.046(2) Uani 1 1 d DU A . C03 C 0.2771(7) 0.5496(5) 0.4832(4) 0.047(2) Uani 1 1 d U . . H03A H 0.3264 0.5053 0.4746 0.056 Uiso 1 1 calc R A . H03B H 0.2100 0.5349 0.5083 0.056 Uiso 1 1 calc R . . H03C H 0.3085 0.5776 0.5103 0.056 Uiso 1 1 calc R . . C04 C 0.0348(6) 0.4189(5) 0.4336(4) 0.0430(19) Uani 1 1 d U . . H04A H -0.0070 0.4639 0.4130 0.052 Uiso 1 1 calc R A . H04B H 0.0305 0.4183 0.4830 0.052 Uiso 1 1 calc R . . H04C H 0.0066 0.3754 0.4254 0.052 Uiso 1 1 calc R . . C05 C 0.1470(6) 0.4172(4) 0.4024(4) 0.0323(15) Uani 1 1 d U A . C06 C 0.2277(6) 0.3671(4) 0.4413(4) 0.0345(16) Uani 1 1 d U . . H06A H 0.2992 0.3771 0.4204 0.041 Uiso 1 1 calc R A . H06B H 0.2202 0.3156 0.4401 0.041 Uiso 1 1 calc R . . H06C H 0.2166 0.3758 0.4889 0.041 Uiso 1 1 calc R . . C07 C 0.3049(10) 0.3970(8) 0.1278(6) 0.083(4) Uani 1 1 d U A . H07A H 0.3233 0.4382 0.0920 0.100 Uiso 1 1 calc R . . H07B H 0.2273 0.3997 0.1378 0.100 Uiso 1 1 calc R . . H07C H 0.3342 0.3501 0.1119 0.100 Uiso 1 1 calc R . . C08 C 0.3501(6) 0.4015(4) 0.1910(4) 0.0363(17) Uani 1 1 d U . . C09 C 0.3413(8) 0.3400(5) 0.2494(5) 0.052(2) Uani 1 1 d U A . H09A H 0.3673 0.3528 0.2888 0.062 Uiso 1 1 calc R . . H09B H 0.3840 0.2949 0.2363 0.062 Uiso 1 1 calc R . . H09C H 0.2667 0.3317 0.2615 0.062 Uiso 1 1 calc R . . C010 C 1.2010(6) 0.6193(5) 0.1697(4) 0.051(2) Uani 1 1 d DU . . C011 C 1.2990(8) 0.6304(5) 0.1214(4) 0.058(3) Uani 1 1 d DU . . H01A H 1.3501 0.6479 0.1445 0.070 Uiso 1 1 calc R . . H01B H 1.2814 0.6672 0.0817 0.070 Uiso 1 1 calc R . . H11C H 1.3302 0.5835 0.1062 0.070 Uiso 1 1 calc R . . O1B O 1.2007(10) 0.5784(8) 0.2201(6) 0.051(5) Uani 0.436(14) 1 d PDU . 1 C02B C 1.1303(14) 0.6904(11) 0.1503(13) 0.065(7) Uani 0.436(14) 1 d PDU . 1 H02A H 1.1262 0.6984 0.1009 0.098 Uiso 0.436(14) 1 calc PR . 1 H02B H 1.1598 0.7316 0.1619 0.098 Uiso 0.436(14) 1 calc PR . 1 H02C H 1.0590 0.6874 0.1753 0.098 Uiso 0.436(14) 1 calc PR . 1 O1A O 1.1532(8) 0.5627(5) 0.1775(5) 0.040(3) Uani 0.564(14) 1 d PDU . 2 C02A C 1.1594(18) 0.6722(11) 0.2166(10) 0.081(7) Uani 0.564(14) 1 d PDU . 2 H02D H 1.1189 0.6475 0.2574 0.121 Uiso 0.564(14) 1 calc PR . 2 H02E H 1.1129 0.7131 0.1936 0.121 Uiso 0.564(14) 1 calc PR . 2 H02F H 1.2187 0.6916 0.2300 0.121 Uiso 0.564(14) 1 calc PR . 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 Sn1 0.0329(3) 0.0268(2) 0.0248(2) 0.00010(18) 0.00328(19) 0.00930(19) Sn2 0.0615(3) 0.0248(2) 0.0235(2) -0.00394(18) -0.0088(2) -0.0158(2) Sn3 0.0222(2) 0.0224(2) 0.0239(2) -0.00210(17) -0.00282(17) -0.00596(17) Sn4 0.0232(2) 0.0199(2) 0.02166(19) -0.00568(16) -0.00203(16) -0.00486(16) Sn5 0.0255(2) 0.0187(2) 0.0212(2) -0.00478(16) 0.00139(17) -0.00613(16) Sn6 0.0205(2) 0.0180(2) 0.0228(2) -0.00473(16) -0.00019(16) -0.00206(16) Fe1 0.0253(5) 0.0220(5) 0.0289(5) -0.0016(4) -0.0037(4) -0.0007(4) Fe2 0.0687(8) 0.0358(6) 0.0273(5) -0.0074(4) -0.0031(5) -0.0265(6) Fe3 0.0256(5) 0.0268(5) 0.0276(5) 0.0028(4) -0.0061(4) -0.0050(4) Fe4 0.0258(5) 0.0238(5) 0.0283(5) -0.0097(4) -0.0004(4) -0.0053(4) Fe5 0.0376(6) 0.0241(5) 0.0277(5) -0.0050(4) 0.0054(4) -0.0089(4) Fe6 0.0231(5) 0.0194(4) 0.0274(4) -0.0031(4) 0.0013(4) -0.0020(4) S1 0.101(2) 0.0361(11) 0.0401(11) -0.0176(9) -0.0277(12) 0.0254(12) S2 0.0274(8) 0.0270(8) 0.0281(8) 0.0036(7) -0.0054(7) -0.0051(7) S3 0.0225(8) 0.0281(8) 0.0212(7) -0.0043(6) -0.0022(6) -0.0039(6) S4 0.0331(10) 0.0348(10) 0.0297(8) 0.0057(7) 0.0060(7) 0.0053(7) S5 0.0352(9) 0.0280(9) 0.0257(8) -0.0063(7) -0.0049(7) -0.0061(7) S6 0.0240(8) 0.0338(9) 0.0336(8) -0.0058(7) 0.0018(7) -0.0030(7) S7 0.0278(8) 0.0197(7) 0.0227(7) -0.0061(6) -0.0011(6) -0.0041(6) S8 0.0236(8) 0.0339(9) 0.0252(7) -0.0109(7) -0.0001(6) -0.0048(7) S9 0.0302(9) 0.0246(8) 0.0239(7) -0.0026(6) 0.0027(7) 0.0003(6) S10 0.0298(9) 0.0258(8) 0.0236(7) -0.0094(6) 0.0031(6) -0.0078(6) S11 0.0260(8) 0.0191(7) 0.0299(8) -0.0065(6) 0.0008(6) -0.0047(6) S12 0.0298(9) 0.0247(8) 0.0258(7) -0.0050(6) -0.0072(7) -0.0027(6) Na1 0.0338(16) 0.0514(19) 0.0357(15) -0.0010(14) 0.0054(13) 0.0055(13) Na2 0.0382(18) 0.077(3) 0.062(2) -0.0356(19) 0.0119(16) -0.0233(17) Na3 0.0269(13) 0.0233(13) 0.0252(12) -0.0047(10) -0.0036(10) -0.0041(10) Na4 0.0474(18) 0.0359(16) 0.0291(14) -0.0103(12) 0.0003(12) -0.0007(13) Na5 0.0307(15) 0.0364(15) 0.0309(13) -0.0060(12) -0.0045(11) -0.0079(12) Na6 0.076(3) 0.081(3) 0.053(2) -0.0414(19) 0.0291(19) -0.049(2) O2 0.072(5) 0.060(5) 0.134(7) 0.024(5) 0.037(5) -0.004(4) O3 0.030(3) 0.025(2) 0.029(2) -0.0043(19) -0.0045(19) -0.0047(19) O4 0.031(2) 0.026(2) 0.027(2) -0.0044(19) -0.0027(19) -0.0043(19) O5 0.087(5) 0.034(3) 0.033(3) -0.010(2) 0.009(3) -0.013(3) O6 0.031(3) 0.037(3) 0.030(2) -0.007(2) -0.008(2) -0.002(2) O7 0.038(3) 0.084(5) 0.048(3) -0.034(3) -0.017(3) 0.002(3) O8 0.088(5) 0.061(4) 0.057(4) -0.027(3) 0.040(4) -0.016(4) O9 0.042(3) 0.031(3) 0.032(2) -0.005(2) -0.008(2) -0.012(2) O10 0.036(3) 0.044(3) 0.039(3) 0.001(2) 0.000(2) -0.001(2) C1 0.045(5) 0.031(4) 0.080(6) 0.015(4) -0.034(4) -0.014(3) C2 0.042(4) 0.045(4) 0.033(4) 0.000(3) -0.003(3) -0.019(4) C3 0.020(3) 0.037(4) 0.036(4) -0.002(3) -0.001(3) -0.004(3) C4 0.032(4) 0.024(3) 0.036(3) -0.007(3) -0.009(3) -0.004(3) C5 0.017(3) 0.033(4) 0.075(6) -0.012(4) 0.009(4) 0.001(3) C6 0.027(4) 0.026(3) 0.031(3) -0.001(3) 0.002(3) -0.002(3) C7 0.029(4) 0.026(3) 0.032(3) -0.004(3) 0.002(3) 0.000(3) C8 0.029(4) 0.021(3) 0.038(4) -0.006(3) -0.002(3) 0.000(3) C9 0.031(4) 0.025(4) 0.046(4) -0.006(3) -0.007(3) -0.004(3) C10 0.031(4) 0.026(3) 0.037(4) -0.006(3) 0.000(3) 0.001(3) C21 0.028(4) 0.052(5) 0.029(3) -0.008(3) -0.009(3) 0.005(3) C22 0.051(5) 0.037(4) 0.027(3) 0.000(3) -0.010(3) 0.006(3) C23 0.048(5) 0.035(4) 0.026(3) 0.001(3) -0.002(3) -0.005(3) C24 0.038(4) 0.034(4) 0.031(3) -0.003(3) 0.008(3) 0.004(3) C25 0.050(5) 0.040(4) 0.033(4) -0.007(3) -0.003(3) -0.014(4) C26 0.033(4) 0.027(4) 0.043(4) 0.007(3) -0.015(3) -0.012(3) C27 0.036(4) 0.036(4) 0.048(4) 0.010(3) -0.024(3) -0.014(3) C28 0.048(5) 0.028(4) 0.040(4) 0.000(3) -0.011(3) -0.015(3) C29 0.036(4) 0.025(3) 0.032(3) -0.003(3) -0.007(3) -0.010(3) C30 0.035(4) 0.024(3) 0.031(3) -0.001(3) -0.011(3) -0.011(3) C31 0.035(4) 0.031(4) 0.030(3) -0.009(3) -0.003(3) -0.006(3) C32 0.040(4) 0.027(4) 0.033(4) -0.002(3) -0.002(3) -0.006(3) C33 0.039(4) 0.033(4) 0.033(4) -0.011(3) 0.008(3) -0.015(3) C34 0.030(4) 0.026(3) 0.033(3) -0.013(3) 0.005(3) -0.011(3) C35 0.026(3) 0.023(3) 0.025(3) -0.006(3) 0.000(3) -0.005(3) C36 0.095(8) 0.044(5) 0.039(4) -0.020(4) 0.022(5) -0.032(5) C37 0.042(5) 0.050(5) 0.033(4) -0.001(3) 0.012(3) 0.005(4) C38 0.056(5) 0.033(4) 0.026(3) 0.000(3) -0.004(3) -0.014(3) C39 0.068(6) 0.073(6) 0.026(4) -0.014(4) -0.018(4) 0.019(5) C40 0.055(6) 0.118(9) 0.039(4) -0.034(5) -0.006(4) -0.046(6) C41 0.023(4) 0.035(4) 0.111(8) 0.010(5) 0.001(4) -0.004(3) C42 0.042(4) 0.028(4) 0.036(4) 0.000(3) -0.007(3) -0.011(3) C43 0.072(6) 0.023(4) 0.030(4) -0.003(3) -0.010(4) -0.015(3) C44 0.085(7) 0.029(4) 0.057(5) 0.008(4) -0.035(5) -0.028(4) C45 0.057(6) 0.039(5) 0.100(8) 0.017(5) -0.024(6) -0.022(4) C46A 0.064(10) 0.053(9) 0.029(7) -0.008(7) 0.002(7) -0.004(8) C47A 0.065(10) 0.041(7) 0.031(6) -0.007(5) -0.022(6) -0.027(7) C48A 0.024(7) 0.043(7) 0.046(7) 0.001(6) -0.009(6) -0.007(6) C49A 0.062(10) 0.032(7) 0.023(6) 0.007(5) -0.009(6) -0.002(7) C50A 0.074(12) 0.041(9) 0.019(6) 0.000(7) 0.010(7) -0.020(9) C46B 0.036(12) 0.047(14) 0.020(11) -0.003(10) -0.016(9) 0.007(11) C47B 0.030(11) 0.048(13) 0.042(13) 0.006(11) -0.023(11) -0.004(10) C48B 0.038(15) 0.044(13) 0.047(12) -0.006(11) -0.005(12) -0.016(13) C49B 0.073(19) 0.029(13) 0.024(13) -0.009(10) -0.002(14) -0.018(14) C50B 0.070(17) 0.043(15) 0.018(9) -0.007(10) -0.007(12) -0.010(13) C51 0.021(3) 0.020(3) 0.032(3) -0.003(3) 0.000(3) -0.004(2) C52 0.024(3) 0.025(3) 0.035(3) -0.007(3) -0.008(3) -0.005(3) C53 0.020(3) 0.026(4) 0.055(4) 0.000(3) -0.002(3) -0.006(3) C54 0.026(4) 0.023(3) 0.049(4) -0.003(3) 0.010(3) -0.005(3) C55 0.026(3) 0.022(3) 0.029(3) -0.003(3) 0.003(3) -0.001(3) C56 0.021(3) 0.024(3) 0.039(4) -0.008(3) 0.004(3) -0.009(3) C57 0.030(4) 0.024(3) 0.031(3) -0.004(3) -0.005(3) -0.008(3) C58 0.024(3) 0.024(3) 0.040(4) -0.015(3) 0.001(3) -0.001(3) C59 0.043(4) 0.016(3) 0.043(4) -0.002(3) -0.006(3) -0.001(3) C60 0.036(4) 0.033(4) 0.034(4) 0.001(3) -0.004(3) -0.010(3) C01 0.049(5) 0.049(5) 0.044(4) -0.001(4) 0.001(4) -0.014(4) C02 0.052(5) 0.038(4) 0.049(5) -0.013(4) 0.014(4) -0.025(4) C03 0.044(5) 0.044(5) 0.051(5) -0.013(4) 0.009(4) -0.009(4) C04 0.030(4) 0.041(4) 0.051(5) 0.005(4) 0.000(3) -0.003(3) C05 0.033(4) 0.028(4) 0.035(4) -0.004(3) -0.001(3) -0.007(3) C06 0.031(4) 0.036(4) 0.036(4) 0.000(3) -0.006(3) -0.007(3) C07 0.091(9) 0.110(10) 0.070(7) -0.041(7) -0.021(6) -0.042(7) C08 0.039(4) 0.043(4) 0.031(4) -0.017(3) 0.001(3) -0.007(3) C09 0.057(6) 0.033(4) 0.064(5) -0.006(4) 0.006(4) -0.014(4) C010 0.041(5) 0.070(6) 0.036(4) -0.008(4) -0.001(4) 0.008(4) C011 0.080(7) 0.046(5) 0.038(4) 0.001(4) 0.016(4) -0.009(5) O1B 0.031(7) 0.081(10) 0.034(7) -0.003(7) 0.005(5) 0.000(6) C02B 0.024(10) 0.093(18) 0.079(16) -0.028(13) 0.010(10) -0.010(10) O1A 0.045(6) 0.030(5) 0.042(6) -0.014(4) 0.017(5) -0.006(4) C02A 0.099(16) 0.075(13) 0.079(13) -0.051(11) 0.040(11) -0.051(12) 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 Sn1 C6 2.125(7) . ? Sn1 S4 2.332(2) . ? Sn1 S3 2.4315(17) . ? Sn1 S1 2.451(3) . ? Sn2 C11A 2.188(8) . ? Sn2 C11B 2.241(19) . ? Sn2 S5 2.3254(18) . ? Sn2 S1 2.372(2) . ? Sn2 S2 2.419(2) . ? Sn3 C30 2.118(7) . ? Sn3 S6 2.328(2) . ? Sn3 S2 2.4103(17) . ? Sn3 S3 2.4391(17) . ? Sn4 C35 2.110(6) . ? Sn4 S12 2.3295(18) . ? Sn4 S7 2.4286(17) . ? Sn4 S8 2.4304(18) . ? Sn5 C42 2.102(7) . ? Sn5 S10 2.3226(17) . ? Sn5 S9 2.4206(18) . ? Sn5 S7 2.4267(18) . ? Sn6 C51 2.118(6) . ? Sn6 S11 2.3303(17) . ? Sn6 S9 2.4151(17) . ? Sn6 S8 2.4176(18) . ? Fe1 C10 2.019(7) . ? Fe1 C9 2.024(7) . ? Fe1 C3 2.030(7) . ? Fe1 C7 2.031(7) . ? Fe1 C6 2.032(7) . ? Fe1 C8 2.035(7) . ? Fe1 C2 2.039(7) . ? Fe1 C5 2.040(8) . ? Fe1 C1 2.043(8) . ? Fe1 C4 2.045(7) . ? Fe2 C20A 1.847(14) . ? Fe2 C16A 1.857(14) . ? Fe2 C19A 1.940(13) . ? Fe2 C17A 1.956(13) . ? Fe2 C18B 1.965(13) . ? Fe2 C11B 1.964(16) . ? Fe2 C18A 1.975(13) . ? Fe2 C12B 1.976(16) . ? Fe2 C19B 1.993(15) . ? Fe2 C12A 2.010(8) . ? Fe2 C11A 2.050(10) . ? Fe2 C17B 2.051(15) . ? Fe3 C24 2.032(7) . ? Fe3 C29 2.033(7) . ? Fe3 C26 2.034(7) . ? Fe3 C27 2.035(7) . ? Fe3 C23 2.036(7) . ? Fe3 C22 2.038(7) . ? Fe3 C21 2.040(7) . ? Fe3 C28 2.042(8) . ? Fe3 C30 2.042(6) . ? Fe3 C25 2.049(8) . ? Fe4 C39 2.013(8) . ? Fe4 C36 2.030(8) . ? Fe4 C32 2.032(7) . ? Fe4 C31 2.033(7) . ? Fe4 C34 2.035(7) . ? Fe4 C40 2.038(8) . ? Fe4 C35 2.038(7) . ? Fe4 C33 2.040(7) . ? Fe4 C38 2.042(7) . ? Fe4 C37 2.044(7) . ? Fe5 C47B 1.81(3) . ? Fe5 C48B 1.82(3) . ? Fe5 C46B 1.94(3) . ? Fe5 C49B 1.95(2) . ? Fe5 C43 2.021(7) . ? Fe5 C50B 2.02(2) . ? Fe5 C41 2.033(9) . ? Fe5 C42 2.036(7) . ? Fe5 C45 2.054(10) . ? Fe5 C44 2.060(9) . ? Fe5 C50A 2.060(11) . ? Fe5 C49A 2.074(10) . ? Fe6 C59 2.029(7) . ? Fe6 C56 2.034(6) . ? Fe6 C60 2.034(7) . ? Fe6 C52 2.034(7) . ? Fe6 C53 2.036(7) . ? Fe6 C58 2.040(7) . ? Fe6 C54 2.041(7) . ? Fe6 C55 2.048(6) . ? Fe6 C57 2.049(7) . ? Fe6 C51 2.050(6) . ? S2 Na3 2.859(3) . ? S2 Na5 3.115(3) . ? S4 Na1 2.830(4) . ? S4 Na2 2.851(4) . ? S4 Na3 2.866(3) . ? S5 Na2 2.781(4) . ? S6 Na4 2.794(4) . ? S6 Na6 3.005(5) . ? S7 Na3 2.834(3) . ? S10 Na2 2.821(4) 2_765 ? S11 Na4 2.783(3) . ? S11 Na5 2.799(3) . ? S11 Na6 2.867(4) . ? S11 Na3 2.918(3) . ? S12 Na1 2.858(4) . ? Na1 O1A 2.301(9) . ? Na1 O10 2.443(6) 1_655 ? Na1 O1B 2.462(14) . ? Na1 Na3 3.988(4) . ? Na2 O2 2.471(9) . ? Na2 O2 2.600(10) 2_765 ? Na2 S10 2.821(4) 2_765 ? Na2 Na2 4.191(8) 2_765 ? Na3 O4 2.352(5) . ? Na3 O3 2.444(5) . ? Na3 Na5 3.531(4) . ? Na3 Na4 3.653(4) . ? Na4 O5 2.259(6) . ? Na4 O3 2.313(5) . ? Na4 Na6 3.480(5) . ? Na5 O7 2.273(6) . ? Na5 O6 2.404(5) . ? Na5 O4 2.426(5) . ? Na5 O9 2.590(6) . ? Na5 Na6 3.910(4) . ? Na6 O8 2.216(7) . ? Na6 O9 2.316(6) . ? Na6 O10 2.796(6) . ? Na6 O1B 2.963(13) 1_455 ? Na6 C08 3.087(8) . ? O2 Na2 2.600(10) 2_765 ? O8 C02 1.203(9) . ? O9 C08 1.201(9) . ? O10 C05 1.231(8) . ? O10 Na1 2.443(6) 1_455 ? C1 C2 1.407(12) . ? C1 C5 1.431(13) . ? C1 H1 0.9500 . ? C2 C3 1.388(10) . ? C2 H2 0.9500 . ? C3 C4 1.409(10) . ? C3 H3 0.9500 . ? C4 C5 1.408(10) . ? C4 H4 0.9500 . ? C5 H5 0.9600 . ? C6 C10 1.414(10) . ? C6 C7 1.419(10) . ? C7 C8 1.411(10) . ? C7 H7 0.9500 . ? C8 C9 1.403(10) . ? C8 H8 0.9500 . ? C9 C10 1.416(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11A C12A 1.428(7) . ? C11A C15A 1.428(7) . ? C11A H11A 0.9500 . ? C12A C13A 1.428(7) . ? C12A H12A 0.9500 . ? C13A C14A 1.428(7) . ? C13A H13A 0.9500 . ? C14A C15A 1.428(7) . ? C14A H14A 0.9500 . ? C15A H15A 0.9500 . ? C16A C20A 1.399(7) . ? C16A C17A 1.410(7) . ? C16A H16A 0.9500 . ? C17A C18A 1.411(7) . ? C17A H17A 0.9500 . ? C18A C19A 1.262(6) . ? C18A H18A 0.9500 . ? C19A C20A 1.447(7) . ? C19A H19A 0.9500 . ? C20A H20A 0.9500 . ? C11B C12B 1.362(7) . ? C11B C15B 1.363(7) . ? C11B H11B 0.9500 . ? C12B C13B 1.362(7) . ? C12B H12B 0.9500 . ? C13B C14B 1.362(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.362(7) . ? C14B H14B 0.9500 . ? C15B H15B 0.9500 . ? C16B C20B 1.392(2) . ? C16B C17B 1.403(2) . ? C16B H16B 0.9500 . ? C17B C18B 1.404(2) . ? C17B H17B 0.9500 . ? C18B C19B 1.2557(19) . ? C18B H18B 0.9500 . ? C19B C20B 1.440(2) . ? C19B H19B 0.9500 . ? C20B H20B 0.9500 . ? C21 C22 1.412(12) . ? C21 C25 1.417(11) . ? C21 H21 0.9500 . ? C22 C23 1.415(11) . ? C22 H22 0.9500 . ? C23 C24 1.417(11) . ? C23 H23 0.9500 . ? C24 C25 1.427(11) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.413(10) . ? C26 C30 1.435(9) . ? C26 H26 0.9500 . ? C27 C28 1.404(11) . ? C27 H27 0.9500 . ? C28 C29 1.422(10) . ? C28 H28 0.9500 . ? C29 C30 1.433(10) . ? C29 H29 0.9500 . ? C31 C32 1.396(10) . ? C31 C35 1.440(9) . ? C31 H31 0.9500 . ? C32 C33 1.413(10) . ? C32 H32 0.9500 . ? C33 C34 1.415(10) . ? C33 H33 0.9500 . ? C34 C35 1.422(9) . ? C34 H34 0.9500 . ? C36 C40 1.400(15) . ? C36 C37 1.403(13) . ? C36 H36 0.9500 . ? C37 C38 1.424(11) . ? C37 H37 0.9500 . ? C38 C39 1.375(12) . ? C38 H38 0.9500 . ? C39 C40 1.391(15) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.404(11) . ? C41 C45 1.432(13) . ? C41 H41 0.9500 . ? C42 C43 1.420(11) . ? C43 C44 1.400(11) . ? C43 H43 0.9500 . ? C44 C45 1.372(15) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46A C50A 1.406(9) . ? C46A C47A 1.406(9) . ? C46A H46A 0.9500 . ? C47A C48A 1.406(9) . ? C47A H47A 0.9500 . ? C48A C49A 1.406(9) . ? C48A H48A 0.9500 . ? C49A C50A 1.406(9) . ? C49A H49A 0.9500 . ? C50A H50A 0.9500 . ? C46B C47B 1.363(18) . ? C46B C50B 1.363(18) . ? C46B H46B 0.9500 . ? C47B C48B 1.363(18) . ? C47B H47B 0.9500 . ? C48B C49B 1.363(18) . ? C48B H48B 0.9500 . ? C49B C50B 1.363(18) . ? C49B H49B 0.9500 . ? C50B H50B 0.9500 . ? C51 C52 1.419(9) . ? C51 C55 1.455(9) . ? C52 C53 1.405(10) . ? C52 H52 0.9500 . ? C53 C54 1.423(11) . ? C53 H53 0.9500 . ? C54 C55 1.410(10) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C60 1.404(10) . ? C56 C57 1.420(9) . ? C56 H56 0.9500 . ? C57 C58 1.416(9) . ? C57 H57 0.9500 . ? C58 C59 1.401(10) . ? C58 H58 0.9500 . ? C59 C60 1.409(11) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C01 C02 1.488(12) . ? C01 H01C 0.9800 . ? C01 H01D 0.9800 . ? C01 H01E 0.9800 . ? C02 C03 1.487(12) . ? C03 H03A 0.9800 . ? C03 H03B 0.9800 . ? C03 H03C 0.9800 . ? C04 C05 1.478(10) . ? C04 H04A 0.9800 . ? C04 H04B 0.9800 . ? C04 H04C 0.9800 . ? C05 C06 1.493(10) . ? C06 H06A 0.9800 . ? C06 H06B 0.9800 . ? C06 H06C 0.9800 . ? C07 C08 1.491(12) . ? C07 H07A 0.9800 . ? C07 H07B 0.9800 . ? C07 H07C 0.9800 . ? C08 C09 1.483(11) . ? C09 H09A 0.9800 . ? C09 H09B 0.9800 . ? C09 H09C 0.9800 . ? C010 O1B 1.149(12) . ? C010 O1A 1.269(11) . ? C010 C02A 1.465(14) . ? C010 C011 1.482(10) . ? C010 C02B 1.504(16) . ? C011 H01A 0.9800 . ? C011 H01B 0.9800 . ? C011 H11C 0.9800 . ? O1B Na6 2.963(13) 1_655 ? C02B H02A 0.9800 . ? C02B H02B 0.9800 . ? C02B H02C 0.9800 . ? C02A H02D 0.9800 . ? C02A H02E 0.9800 . ? C02A H02F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Sn1 S4 112.58(19) . . ? C6 Sn1 S3 104.40(18) . . ? S4 Sn1 S3 113.35(7) . . ? C6 Sn1 S1 103.7(2) . . ? S4 Sn1 S1 116.05(8) . . ? S3 Sn1 S1 105.66(8) . . ? C11A Sn2 C11B 16.2(6) . . ? C11A Sn2 S5 109.5(2) . . ? C11B Sn2 S5 120.7(5) . . ? C11A Sn2 S1 117.6(2) . . ? C11B Sn2 S1 101.4(6) . . ? S5 Sn2 S1 114.19(9) . . ? C11A Sn2 S2 97.5(3) . . ? C11B Sn2 S2 102.6(5) . . ? S5 Sn2 S2 110.08(6) . . ? S1 Sn2 S2 106.43(7) . . ? C30 Sn3 S6 113.5(2) . . ? C30 Sn3 S2 112.01(19) . . ? S6 Sn3 S2 103.48(7) . . ? C30 Sn3 S3 109.98(19) . . ? S6 Sn3 S3 110.72(7) . . ? S2 Sn3 S3 106.86(6) . . ? C35 Sn4 S12 118.95(18) . . ? C35 Sn4 S7 113.85(17) . . ? S12 Sn4 S7 101.19(6) . . ? C35 Sn4 S8 98.83(18) . . ? S12 Sn4 S8 114.40(6) . . ? S7 Sn4 S8 109.98(6) . . ? C42 Sn5 S10 118.5(2) . . ? C42 Sn5 S9 105.0(2) . . ? S10 Sn5 S9 109.60(7) . . ? C42 Sn5 S7 107.6(2) . . ? S10 Sn5 S7 106.53(6) . . ? S9 Sn5 S7 109.39(6) . . ? C51 Sn6 S11 116.03(18) . . ? C51 Sn6 S9 99.78(17) . . ? S11 Sn6 S9 114.30(6) . . ? C51 Sn6 S8 102.36(19) . . ? S11 Sn6 S8 110.17(7) . . ? S9 Sn6 S8 113.36(6) . . ? C10 Fe1 C9 41.0(3) . . ? C10 Fe1 C3 115.1(3) . . ? C9 Fe1 C3 147.8(3) . . ? C10 Fe1 C7 68.2(3) . . ? C9 Fe1 C7 68.1(3) . . ? C3 Fe1 C7 131.2(3) . . ? C10 Fe1 C6 40.9(3) . . ? C9 Fe1 C6 69.0(3) . . ? C3 Fe1 C6 107.5(3) . . ? C7 Fe1 C6 40.9(3) . . ? C10 Fe1 C8 68.6(3) . . ? C9 Fe1 C8 40.4(3) . . ? C3 Fe1 C8 170.4(3) . . ? C7 Fe1 C8 40.6(3) . . ? C6 Fe1 C8 69.0(3) . . ? C10 Fe1 C2 107.1(3) . . ? C9 Fe1 C2 116.0(3) . . ? C3 Fe1 C2 39.9(3) . . ? C7 Fe1 C2 168.3(3) . . ? C6 Fe1 C2 128.8(3) . . ? C8 Fe1 C2 149.1(3) . . ? C10 Fe1 C5 169.5(3) . . ? C9 Fe1 C5 131.5(3) . . ? C3 Fe1 C5 67.9(3) . . ? C7 Fe1 C5 118.2(3) . . ? C6 Fe1 C5 149.4(3) . . ? C8 Fe1 C5 110.2(3) . . ? C2 Fe1 C5 68.2(3) . . ? C10 Fe1 C1 129.4(4) . . ? C9 Fe1 C1 108.5(3) . . ? C3 Fe1 C1 67.7(3) . . ? C7 Fe1 C1 150.7(3) . . ? C6 Fe1 C1 167.5(4) . . ? C8 Fe1 C1 117.6(3) . . ? C2 Fe1 C1 40.3(4) . . ? C5 Fe1 C1 41.0(4) . . ? C10 Fe1 C4 148.0(3) . . ? C9 Fe1 C4 170.4(3) . . ? C3 Fe1 C4 40.4(3) . . ? C7 Fe1 C4 110.1(3) . . ? C6 Fe1 C4 116.2(3) . . ? C8 Fe1 C4 132.2(3) . . ? C2 Fe1 C4 67.8(3) . . ? C5 Fe1 C4 40.3(3) . . ? C1 Fe1 C4 68.2(3) . . ? C20A Fe2 C16A 44.4(3) . . ? C20A Fe2 C19A 44.9(3) . . ? C16A Fe2 C19A 72.4(4) . . ? C20A Fe2 C17A 75.4(4) . . ? C16A Fe2 C17A 43.3(2) . . ? C19A Fe2 C17A 71.5(3) . . ? C20A Fe2 C18B 54.0(5) . . ? C16A Fe2 C18B 53.2(6) . . ? C19A Fe2 C18B 33.4(7) . . ? C17A Fe2 C18B 38.2(7) . . ? C20A Fe2 C11B 123.9(7) . . ? C16A Fe2 C11B 110.1(6) . . ? C19A Fe2 C11B 161.6(7) . . ? C17A Fe2 C11B 123.5(6) . . ? C18B Fe2 C11B 160.4(7) . . ? C20A Fe2 C18A 69.6(4) . . ? C16A Fe2 C18A 68.6(3) . . ? C19A Fe2 C18A 37.6(2) . . ? C17A Fe2 C18A 42.1(2) . . ? C18B Fe2 C18A 17.2(5) . . ? C11B Fe2 C18A 160.8(7) . . ? C20A Fe2 C12B 90.6(5) . . ? C16A Fe2 C12B 103.8(6) . . ? C19A Fe2 C12B 121.2(6) . . ? C17A Fe2 C12B 143.0(7) . . ? C18B Fe2 C12B 144.6(7) . . ? C11B Fe2 C12B 40.5(2) . . ? C18A Fe2 C12B 158.2(7) . . ? C20A Fe2 C19B 28.9(7) . . ? C16A Fe2 C19B 61.1(7) . . ? C19A Fe2 C19B 16.0(6) . . ? C17A Fe2 C19B 71.9(6) . . ? C18B Fe2 C19B 37.0(2) . . ? C11B Fe2 C19B 150.0(8) . . ? C18A Fe2 C19B 47.4(6) . . ? C12B Fe2 C19B 110.8(7) . . ? C20A Fe2 C12A 119.5(5) . . ? C16A Fe2 C12A 132.4(5) . . ? C19A Fe2 C12A 133.5(5) . . ? C17A Fe2 C12A 154.9(5) . . ? C18B Fe2 C12A 166.9(5) . . ? C11B Fe2 C12A 31.9(6) . . ? C18A Fe2 C12A 158.2(5) . . ? C12B Fe2 C12A 31.3(6) . . ? C19B Fe2 C12A 131.4(4) . . ? C20A Fe2 C11A 139.8(6) . . ? C16A Fe2 C11A 115.0(6) . . ? C19A Fe2 C11A 172.6(5) . . ? C17A Fe2 C11A 114.1(5) . . ? C18B Fe2 C11A 151.6(5) . . ? C11B Fe2 C11A 17.7(7) . . ? C18A Fe2 C11A 144.1(5) . . ? C12B Fe2 C11A 57.6(6) . . ? C19B Fe2 C11A 167.6(5) . . ? C12A Fe2 C11A 41.2(2) . . ? C20A Fe2 C17B 65.0(7) . . ? C16A Fe2 C17B 29.0(6) . . ? C19A Fe2 C17B 71.9(6) . . ? C17A Fe2 C17B 14.4(6) . . ? C18B Fe2 C17B 40.9(2) . . ? C11B Fe2 C17B 119.6(7) . . ? C18A Fe2 C17B 50.1(6) . . ? C12B Fe2 C17B 130.0(7) . . ? C19B Fe2 C17B 68.1(4) . . ? C12A Fe2 C17B 150.8(5) . . ? C11A Fe2 C17B 114.8(4) . . ? C24 Fe3 C29 164.5(3) . . ? C24 Fe3 C26 107.1(3) . . ? C29 Fe3 C26 69.0(3) . . ? C24 Fe3 C27 119.0(3) . . ? C29 Fe3 C27 68.4(3) . . ? C26 Fe3 C27 40.7(3) . . ? C24 Fe3 C23 40.8(3) . . ? C29 Fe3 C23 153.8(3) . . ? C26 Fe3 C23 124.8(3) . . ? C27 Fe3 C23 106.4(3) . . ? C24 Fe3 C22 68.2(3) . . ? C29 Fe3 C22 120.0(3) . . ? C26 Fe3 C22 162.3(3) . . ? C27 Fe3 C22 125.4(3) . . ? C23 Fe3 C22 40.6(3) . . ? C24 Fe3 C21 68.3(3) . . ? C29 Fe3 C21 108.6(3) . . ? C26 Fe3 C21 155.4(3) . . ? C27 Fe3 C21 163.2(3) . . ? C23 Fe3 C21 68.4(3) . . ? C22 Fe3 C21 40.5(3) . . ? C24 Fe3 C28 153.1(3) . . ? C29 Fe3 C28 40.9(3) . . ? C26 Fe3 C28 68.5(3) . . ? C27 Fe3 C28 40.3(3) . . ? C23 Fe3 C28 118.6(3) . . ? C22 Fe3 C28 107.5(3) . . ? C21 Fe3 C28 126.8(3) . . ? C24 Fe3 C30 126.2(3) . . ? C29 Fe3 C30 41.2(3) . . ? C26 Fe3 C30 41.2(3) . . ? C27 Fe3 C30 68.8(3) . . ? C23 Fe3 C30 163.1(3) . . ? C22 Fe3 C30 155.1(3) . . ? C21 Fe3 C30 120.7(3) . . ? C28 Fe3 C30 69.0(3) . . ? C24 Fe3 C25 40.9(3) . . ? C29 Fe3 C25 127.0(3) . . ? C26 Fe3 C25 120.0(3) . . ? C27 Fe3 C25 154.3(3) . . ? C23 Fe3 C25 68.8(3) . . ? C22 Fe3 C25 68.4(3) . . ? C21 Fe3 C25 40.6(3) . . ? C28 Fe3 C25 164.4(3) . . ? C30 Fe3 C25 108.0(3) . . ? C39 Fe4 C36 67.2(4) . . ? C39 Fe4 C32 169.3(4) . . ? C36 Fe4 C32 109.0(4) . . ? C39 Fe4 C31 149.7(4) . . ? C36 Fe4 C31 131.2(4) . . ? C32 Fe4 C31 40.2(3) . . ? C39 Fe4 C34 109.4(3) . . ? C36 Fe4 C34 147.5(4) . . ? C32 Fe4 C34 68.0(3) . . ? C31 Fe4 C34 68.6(3) . . ? C39 Fe4 C40 40.1(4) . . ? C36 Fe4 C40 40.2(4) . . ? C32 Fe4 C40 130.6(4) . . ? C31 Fe4 C40 169.2(4) . . ? C34 Fe4 C40 115.6(4) . . ? C39 Fe4 C35 116.7(3) . . ? C36 Fe4 C35 170.7(4) . . ? C32 Fe4 C35 68.6(3) . . ? C31 Fe4 C35 41.4(3) . . ? C34 Fe4 C35 40.9(3) . . ? C40 Fe4 C35 147.9(4) . . ? C39 Fe4 C33 130.8(4) . . ? C36 Fe4 C33 115.5(3) . . ? C32 Fe4 C33 40.6(3) . . ? C31 Fe4 C33 68.5(3) . . ? C34 Fe4 C33 40.6(3) . . ? C40 Fe4 C33 107.7(3) . . ? C35 Fe4 C33 69.0(3) . . ? C39 Fe4 C38 39.6(4) . . ? C36 Fe4 C38 67.6(3) . . ? C32 Fe4 C38 149.6(3) . . ? C31 Fe4 C38 117.9(3) . . ? C34 Fe4 C38 131.6(3) . . ? C40 Fe4 C38 67.6(4) . . ? C35 Fe4 C38 109.5(3) . . ? C33 Fe4 C38 169.4(3) . . ? C39 Fe4 C37 67.6(4) . . ? C36 Fe4 C37 40.3(4) . . ? C32 Fe4 C37 116.5(3) . . ? C31 Fe4 C37 109.3(3) . . ? C34 Fe4 C37 171.0(3) . . ? C40 Fe4 C37 68.1(4) . . ? C35 Fe4 C37 131.9(3) . . ? C33 Fe4 C37 147.7(3) . . ? C38 Fe4 C37 40.8(3) . . ? C47B Fe5 C48B 44.1(8) . . ? C47B Fe5 C46B 42.5(6) . . ? C48B Fe5 C46B 71.8(10) . . ? C47B Fe5 C49B 71.6(10) . . ? C48B Fe5 C49B 42.1(6) . . ? C46B Fe5 C49B 69.1(8) . . ? C47B Fe5 C43 126.0(9) . . ? C48B Fe5 C43 117.1(10) . . ? C46B Fe5 C43 154.5(8) . . ? C49B Fe5 C43 134.5(10) . . ? C47B Fe5 C50B 70.1(9) . . ? C48B Fe5 C50B 69.8(9) . . ? C46B Fe5 C50B 40.2(5) . . ? C49B Fe5 C50B 40.0(5) . . ? C43 Fe5 C50B 163.3(7) . . ? C47B Fe5 C41 120.2(9) . . ? C48B Fe5 C41 164.2(9) . . ? C46B Fe5 C41 97.6(8) . . ? C49B Fe5 C41 145.7(12) . . ? C43 Fe5 C41 67.8(4) . . ? C50B Fe5 C41 110.0(11) . . ? C47B Fe5 C42 107.2(8) . . ? C48B Fe5 C42 132.9(11) . . ? C46B Fe5 C42 114.6(8) . . ? C49B Fe5 C42 173.7(12) . . ? C43 Fe5 C42 41.0(3) . . ? C50B Fe5 C42 145.9(11) . . ? C41 Fe5 C42 40.4(3) . . ? C47B Fe5 C45 156.5(10) . . ? C48B Fe5 C45 154.4(10) . . ? C46B Fe5 C45 116.8(8) . . ? C49B Fe5 C45 115.7(10) . . ? C43 Fe5 C45 66.4(4) . . ? C50B Fe5 C45 100.7(9) . . ? C41 Fe5 C45 41.0(4) . . ? C42 Fe5 C45 67.9(3) . . ? C47B Fe5 C44 162.8(10) . . ? C48B Fe5 C44 126.1(9) . . ? C46B Fe5 C44 154.6(8) . . ? C49B Fe5 C44 110.7(8) . . ? C43 Fe5 C44 40.1(3) . . ? C50B Fe5 C44 123.2(7) . . ? C41 Fe5 C44 68.0(4) . . ? C42 Fe5 C44 68.5(3) . . ? C45 Fe5 C44 39.0(4) . . ? C47B Fe5 C50A 66.5(9) . . ? C48B Fe5 C50A 51.8(9) . . ? C46B Fe5 C50A 52.1(7) . . ? C49B Fe5 C50A 19.3(7) . . ? C43 Fe5 C50A 152.9(5) . . ? C50B Fe5 C50A 21.2(8) . . ? C41 Fe5 C50A 130.6(6) . . ? C42 Fe5 C50A 166.0(5) . . ? C45 Fe5 C50A 112.5(5) . . ? C44 Fe5 C50A 121.3(4) . . ? C47B Fe5 C49A 68.7(9) . . ? C48B Fe5 C49A 27.7(10) . . ? C46B Fe5 C49A 82.1(6) . . ? C49B Fe5 C49A 22.0(8) . . ? C43 Fe5 C49A 117.3(5) . . ? C50B Fe5 C49A 61.0(7) . . ? C41 Fe5 C49A 165.7(5) . . ? C42 Fe5 C49A 151.7(5) . . ? C45 Fe5 C49A 126.8(4) . . ? C44 Fe5 C49A 106.7(4) . . ? C50A Fe5 C49A 39.8(2) . . ? C59 Fe6 C56 68.2(3) . . ? C59 Fe6 C60 40.6(3) . . ? C56 Fe6 C60 40.4(3) . . ? C59 Fe6 C52 127.3(3) . . ? C56 Fe6 C52 117.5(3) . . ? C60 Fe6 C52 107.1(3) . . ? C59 Fe6 C53 106.9(3) . . ? C56 Fe6 C53 149.8(3) . . ? C60 Fe6 C53 116.3(3) . . ? C52 Fe6 C53 40.4(3) . . ? C59 Fe6 C58 40.3(3) . . ? C56 Fe6 C58 67.9(3) . . ? C60 Fe6 C58 67.8(3) . . ? C52 Fe6 C58 165.7(3) . . ? C53 Fe6 C58 128.5(3) . . ? C59 Fe6 C54 117.4(3) . . ? C56 Fe6 C54 168.4(3) . . ? C60 Fe6 C54 150.2(3) . . ? C52 Fe6 C54 68.3(3) . . ? C53 Fe6 C54 40.8(3) . . ? C58 Fe6 C54 109.1(3) . . ? C59 Fe6 C55 151.0(3) . . ? C56 Fe6 C55 130.2(3) . . ? C60 Fe6 C55 167.7(3) . . ? C52 Fe6 C55 68.8(3) . . ? C53 Fe6 C55 68.5(3) . . ? C58 Fe6 C55 119.0(3) . . ? C54 Fe6 C55 40.3(3) . . ? C59 Fe6 C57 68.4(3) . . ? C56 Fe6 C57 40.7(3) . . ? C60 Fe6 C57 68.3(3) . . ? C52 Fe6 C57 151.7(3) . . ? C53 Fe6 C57 167.4(3) . . ? C58 Fe6 C57 40.5(3) . . ? C54 Fe6 C57 129.8(3) . . ? C55 Fe6 C57 109.6(3) . . ? C59 Fe6 C51 165.6(3) . . ? C56 Fe6 C51 108.4(3) . . ? C60 Fe6 C51 127.9(3) . . ? C52 Fe6 C51 40.7(3) . . ? C53 Fe6 C51 68.6(3) . . ? C58 Fe6 C51 152.9(3) . . ? C54 Fe6 C51 68.8(3) . . ? C55 Fe6 C51 41.6(3) . . ? C57 Fe6 C51 118.9(3) . . ? Sn2 S1 Sn1 104.89(8) . . ? Sn3 S2 Sn2 107.49(7) . . ? Sn3 S2 Na3 106.26(8) . . ? Sn2 S2 Na3 113.38(8) . . ? Sn3 S2 Na5 144.85(9) . . ? Sn2 S2 Na5 104.84(8) . . ? Na3 S2 Na5 72.32(8) . . ? Sn1 S3 Sn3 104.91(6) . . ? Sn1 S4 Na1 119.32(9) . . ? Sn1 S4 Na2 108.59(11) . . ? Na1 S4 Na2 128.78(11) . . ? Sn1 S4 Na3 104.12(8) . . ? Na1 S4 Na3 88.88(10) . . ? Na2 S4 Na3 96.52(11) . . ? Sn2 S5 Na2 105.09(10) . . ? Sn3 S6 Na4 107.57(9) . . ? Sn3 S6 Na6 110.12(9) . . ? Na4 S6 Na6 73.66(10) . . ? Sn5 S7 Sn4 110.11(6) . . ? Sn5 S7 Na3 113.27(8) . . ? Sn4 S7 Na3 110.05(8) . . ? Sn6 S8 Sn4 107.44(7) . . ? Sn6 S9 Sn5 108.60(7) . . ? Sn5 S10 Na2 122.24(10) . 2_765 ? Sn6 S11 Na4 97.36(9) . . ? Sn6 S11 Na5 122.89(9) . . ? Na4 S11 Na5 138.18(10) . . ? Sn6 S11 Na6 126.27(11) . . ? Na4 S11 Na6 76.04(11) . . ? Na5 S11 Na6 87.27(10) . . ? Sn6 S11 Na3 110.36(8) . . ? Na4 S11 Na3 79.65(9) . . ? Na5 S11 Na3 76.25(9) . . ? Na6 S11 Na3 120.21(12) . . ? Sn4 S12 Na1 99.30(8) . . ? O1A Na1 O10 100.0(3) . 1_655 ? O1A Na1 O1B 29.4(4) . . ? O10 Na1 O1B 78.8(3) 1_655 . ? O1A Na1 S4 95.3(3) . . ? O10 Na1 S4 108.43(18) 1_655 . ? O1B Na1 S4 121.3(4) . . ? O1A Na1 S12 125.7(3) . . ? O10 Na1 S12 100.17(17) 1_655 . ? O1B Na1 S12 110.3(4) . . ? S4 Na1 S12 124.41(12) . . ? O1A Na1 Na3 109.1(3) . . ? O10 Na1 Na3 141.71(18) 1_655 . ? O1B Na1 Na3 136.3(3) . . ? S4 Na1 Na3 45.93(7) . . ? S12 Na1 Na3 82.79(9) . . ? O2 Na2 O2 68.5(4) . 2_765 ? O2 Na2 S5 128.8(3) . . ? O2 Na2 S5 81.1(2) 2_765 . ? O2 Na2 S10 93.9(2) . 2_765 ? O2 Na2 S10 77.3(2) 2_765 2_765 ? S5 Na2 S10 119.06(13) . 2_765 ? O2 Na2 S4 82.3(3) . . ? O2 Na2 S4 147.4(3) 2_765 . ? S5 Na2 S4 108.02(12) . . ? S10 Na2 S4 120.48(15) 2_765 . ? O2 Na2 Na2 35.3(3) . 2_765 ? O2 Na2 Na2 33.3(2) 2_765 2_765 ? S5 Na2 Na2 105.86(16) . 2_765 ? S10 Na2 Na2 84.44(11) 2_765 2_765 ? S4 Na2 Na2 116.35(15) . 2_765 ? O4 Na3 O3 173.00(19) . . ? O4 Na3 S7 92.37(14) . . ? O3 Na3 S7 92.73(14) . . ? O4 Na3 S2 77.08(14) . . ? O3 Na3 S2 97.42(14) . . ? S7 Na3 S2 168.48(11) . . ? O4 Na3 S4 95.21(15) . . ? O3 Na3 S4 89.49(14) . . ? S7 Na3 S4 91.01(9) . . ? S2 Na3 S4 94.49(9) . . ? O4 Na3 S11 88.28(14) . . ? O3 Na3 S11 86.55(14) . . ? S7 Na3 S11 94.35(9) . . ? S2 Na3 S11 80.90(8) . . ? S4 Na3 S11 173.48(10) . . ? O4 Na3 Na5 43.16(13) . . ? O3 Na3 Na5 130.11(15) . . ? S7 Na3 Na5 111.80(9) . . ? S2 Na3 Na5 57.19(7) . . ? S4 Na3 Na5 130.46(10) . . ? S11 Na3 Na5 50.35(7) . . ? O4 Na3 Na4 135.51(15) . . ? O3 Na3 Na4 38.54(12) . . ? S7 Na3 Na4 100.05(9) . . ? S2 Na3 Na4 84.73(9) . . ? S4 Na3 Na4 126.75(10) . . ? S11 Na3 Na4 48.54(7) . . ? Na5 Na3 Na4 93.06(9) . . ? O4 Na3 Na1 121.31(15) . . ? O3 Na3 Na1 65.62(13) . . ? S7 Na3 Na1 56.71(7) . . ? S2 Na3 Na1 133.02(10) . . ? S4 Na3 Na1 45.19(7) . . ? S11 Na3 Na1 136.44(10) . . ? Na5 Na3 Na1 163.23(9) . . ? Na4 Na3 Na1 100.81(9) . . ? O5 Na4 O3 127.2(3) . . ? O5 Na4 S11 116.63(19) . . ? O3 Na4 S11 92.40(15) . . ? O5 Na4 S6 118.58(18) . . ? O3 Na4 S6 97.21(16) . . ? S11 Na4 S6 98.58(11) . . ? O5 Na4 Na6 108.1(2) . . ? O3 Na4 Na6 124.32(17) . . ? S11 Na4 Na6 53.08(9) . . ? S6 Na4 Na6 55.95(10) . . ? O5 Na4 Na3 145.96(19) . . ? O3 Na4 Na3 41.18(13) . . ? S11 Na4 Na3 51.81(7) . . ? S6 Na4 Na3 95.44(10) . . ? Na6 Na4 Na3 89.33(9) . . ? O7 Na5 O6 93.8(2) . . ? O7 Na5 O4 85.9(2) . . ? O6 Na5 O4 82.94(18) . . ? O7 Na5 O9 97.6(2) . . ? O6 Na5 O9 130.0(2) . . ? O4 Na5 O9 146.17(19) . . ? O7 Na5 S11 171.0(2) . . ? O6 Na5 S11 93.46(15) . . ? O4 Na5 S11 89.65(14) . . ? O9 Na5 S11 81.75(14) . . ? O7 Na5 S2 92.68(19) . . ? O6 Na5 S2 152.74(16) . . ? O4 Na5 S2 71.13(13) . . ? O9 Na5 S2 75.10(13) . . ? S11 Na5 S2 78.47(8) . . ? O7 Na5 Na3 119.40(18) . . ? O6 Na5 Na3 103.93(15) . . ? O4 Na5 Na3 41.54(12) . . ? O9 Na5 Na3 111.91(14) . . ? S11 Na5 Na3 53.40(7) . . ? S2 Na5 Na3 50.49(7) . . ? O7 Na5 Na6 131.3(2) . . ? O6 Na5 Na6 122.77(16) . . ? O4 Na5 Na6 126.00(16) . . ? O9 Na5 Na6 34.78(13) . . ? S11 Na5 Na6 47.09(7) . . ? S2 Na5 Na6 69.85(10) . . ? Na3 Na5 Na6 84.59(10) . . ? O8 Na6 O9 148.2(3) . . ? O8 Na6 O10 76.8(2) . . ? O9 Na6 O10 96.0(2) . . ? O8 Na6 S11 93.9(2) . . ? O9 Na6 S11 85.15(16) . . ? O10 Na6 S11 164.2(2) . . ? O8 Na6 O1B 78.1(4) . 1_455 ? O9 Na6 O1B 70.9(3) . 1_455 ? O10 Na6 O1B 65.4(3) . 1_455 ? S11 Na6 O1B 100.4(3) . 1_455 ? O8 Na6 S6 98.4(3) . . ? O9 Na6 S6 113.4(2) . . ? O10 Na6 S6 101.86(16) . . ? S11 Na6 S6 92.06(13) . . ? O1B Na6 S6 167.2(3) 1_455 . ? O8 Na6 C08 148.7(3) . . ? O9 Na6 C08 19.83(19) . . ? O10 Na6 C08 79.4(2) . . ? S11 Na6 C08 104.05(17) . . ? O1B Na6 C08 73.7(4) 1_455 . ? S6 Na6 C08 106.2(2) . . ? O8 Na6 Na4 74.9(2) . . ? O9 Na6 Na4 125.41(19) . . ? O10 Na6 Na4 135.54(17) . . ? S11 Na6 Na4 50.89(8) . . ? O1B Na6 Na4 138.0(4) 1_455 . ? S6 Na6 Na4 50.39(9) . . ? C08 Na6 Na4 136.1(2) . . ? O8 Na6 Na5 132.6(2) . . ? O9 Na6 Na5 39.64(14) . . ? O10 Na6 Na5 134.51(17) . . ? S11 Na6 Na5 45.64(7) . . ? O1B Na6 Na5 85.6(2) 1_455 . ? S6 Na6 Na5 105.43(12) . . ? C08 Na6 Na5 58.45(16) . . ? Na4 Na6 Na5 89.54(10) . . ? Na2 O2 Na2 111.5(4) . 2_765 ? Na4 O3 Na3 100.28(19) . . ? Na3 O4 Na5 95.30(18) . . ? C02 O8 Na6 149.4(6) . . ? C08 O9 Na6 119.3(5) . . ? C08 O9 Na5 130.5(5) . . ? Na6 O9 Na5 105.6(2) . . ? C05 O10 Na1 122.1(5) . 1_455 ? C05 O10 Na6 126.7(5) . . ? Na1 O10 Na6 110.6(2) 1_455 . ? C2 C1 C5 107.3(7) . . ? C2 C1 Fe1 69.7(4) . . ? C5 C1 Fe1 69.4(4) . . ? C2 C1 H1 126.4 . . ? C5 C1 H1 126.4 . . ? Fe1 C1 H1 126.2 . . ? C3 C2 C1 108.4(7) . . ? C3 C2 Fe1 69.7(4) . . ? C1 C2 Fe1 70.0(4) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe1 C2 H2 126.1 . . ? C2 C3 C4 109.0(6) . . ? C2 C3 Fe1 70.4(4) . . ? C4 C3 Fe1 70.4(4) . . ? C2 C3 H3 125.5 . . ? C4 C3 H3 125.5 . . ? Fe1 C3 H3 125.3 . . ? C5 C4 C3 107.6(7) . . ? C5 C4 Fe1 69.6(4) . . ? C3 C4 Fe1 69.2(4) . . ? C5 C4 H4 126.2 . . ? C3 C4 H4 126.2 . . ? Fe1 C4 H4 126.5 . . ? C4 C5 C1 107.7(7) . . ? C4 C5 Fe1 70.0(4) . . ? C1 C5 Fe1 69.6(5) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe1 C5 H5 125.8 . . ? C10 C6 C7 106.6(6) . . ? C10 C6 Fe1 69.1(4) . . ? C7 C6 Fe1 69.5(4) . . ? C10 C6 Sn1 128.8(5) . . ? C7 C6 Sn1 124.6(5) . . ? Fe1 C6 Sn1 126.4(4) . . ? C8 C7 C6 109.1(6) . . ? C8 C7 Fe1 69.8(4) . . ? C6 C7 Fe1 69.6(4) . . ? C8 C7 H7 125.5 . . ? C6 C7 H7 125.5 . . ? Fe1 C7 H7 126.7 . . ? C9 C8 C7 107.6(6) . . ? C9 C8 Fe1 69.4(4) . . ? C7 C8 Fe1 69.5(4) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? Fe1 C8 H8 126.4 . . ? C8 C9 C10 108.3(6) . . ? C8 C9 Fe1 70.2(4) . . ? C10 C9 Fe1 69.3(4) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe1 C9 H9 126.2 . . ? C6 C10 C9 108.5(6) . . ? C6 C10 Fe1 70.1(4) . . ? C9 C10 Fe1 69.7(4) . . ? C6 C10 H10 125.7 . . ? C9 C10 H10 125.7 . . ? Fe1 C10 H10 126.1 . . ? C12A C11A C15A 108.0 . . ? C12A C11A Fe2 67.9(4) . . ? C15A C11A Fe2 73.0(3) . . ? C12A C11A Sn2 129.5(5) . . ? C15A C11A Sn2 122.4(5) . . ? Fe2 C11A Sn2 122.4(4) . . ? C12A C11A H11A 126.0 . . ? C15A C11A H11A 126.0 . . ? Fe2 C11A H11A 124.6 . . ? C13A C12A C11A 108.0 . . ? C13A C12A Fe2 71.7(4) . . ? C11A C12A Fe2 70.9(4) . . ? C13A C12A H12A 126.0 . . ? C11A C12A H12A 126.0 . . ? Fe2 C12A H12A 123.1 . . ? C12A C13A C14A 108.0 . . ? C12A C13A Fe2 67.4(3) . . ? C14A C13A Fe2 72.9(3) . . ? C12A C13A H13A 126.0 . . ? C14A C13A H13A 126.0 . . ? Fe2 C13A H13A 125.3 . . ? C15A C14A C13A 108.0 . . ? C15A C14A Fe2 70.1(4) . . ? C13A C14A Fe2 67.4(3) . . ? C15A C14A H14A 126.0 . . ? C13A C14A H14A 126.0 . . ? Fe2 C14A H14A 128.0 . . ? C14A C15A C11A 108.0 . . ? C14A C15A Fe2 70.9(4) . . ? C11A C15A Fe2 67.1(3) . . ? C14A C15A H15A 126.0 . . ? C11A C15A H15A 126.0 . . ? Fe2 C15A H15A 127.6 . . ? C20A C16A C17A 111.8 . . ? C20A C16A Fe2 67.4(4) . . ? C17A C16A Fe2 72.1(4) . . ? C20A C16A H16A 124.1 . . ? C17A C16A H16A 124.1 . . ? Fe2 C16A H16A 128.1 . . ? C16A C17A C18A 100.1 . . ? C16A C17A Fe2 64.6(4) . . ? C18A C17A Fe2 69.7(4) . . ? C16A C17A H17A 130.0 . . ? C18A C17A H17A 130.0 . . ? Fe2 C17A H17A 127.1 . . ? C19A C18A C17A 116.6 . . ? C19A C18A Fe2 69.7(4) . . ? C17A C18A Fe2 68.2(3) . . ? C19A C18A H18A 121.7 . . ? C17A C18A H18A 121.7 . . ? Fe2 C18A H18A 133.2 . . ? C18A C19A C20A 107.1 . . ? C18A C19A Fe2 72.7(4) . . ? C20A C19A Fe2 64.2(4) . . ? C18A C19A H19A 126.4 . . ? C20A C19A H19A 126.4 . . ? Fe2 C19A H19A 128.1 . . ? C16A C20A C19A 104.0 . . ? C16A C20A Fe2 68.2(4) . . ? C19A C20A Fe2 71.0(4) . . ? C16A C20A H20A 128.0 . . ? C19A C20A H20A 128.0 . . ? Fe2 C20A H20A 124.5 . . ? C12B C11B C15B 108.0 . . ? C12B C11B Fe2 70.2(4) . . ? C15B C11B Fe2 76.2(4) . . ? C12B C11B Sn2 128.3(10) . . ? C15B C11B Sn2 123.4(10) . . ? Fe2 C11B Sn2 123.9(9) . . ? C12B C11B H11B 126.0 . . ? C15B C11B H11B 126.0 . . ? Fe2 C11B H11B 119.4 . . ? C13B C12B C11B 108.0 . . ? C13B C12B Fe2 76.6(4) . . ? C11B C12B Fe2 69.3(4) . . ? C13B C12B H12B 126.0 . . ? C11B C12B H12B 126.0 . . ? Fe2 C12B H12B 119.9 . . ? C12B C13B C14B 108.0 . . ? C12B C13B Fe2 64.8(3) . . ? C14B C13B Fe2 74.7(3) . . ? C12B C13B H13B 126.0 . . ? C14B C13B H13B 126.0 . . ? Fe2 C13B H13B 125.9 . . ? C15B C14B C13B 108.0 . . ? C15B C14B Fe2 67.9(3) . . ? C13B C14B Fe2 68.6(3) . . ? C15B C14B H14B 126.0 . . ? C13B C14B H14B 126.0 . . ? Fe2 C14B H14B 129.1 . . ? C14B C15B C11B 108.0 . . ? C14B C15B Fe2 75.3(3) . . ? C11B C15B Fe2 64.9(3) . . ? C14B C15B H15B 126.0 . . ? C11B C15B H15B 126.0 . . ? Fe2 C15B H15B 125.2 . . ? C20B C16B C17B 111.8 . . ? C20B C16B Fe2 69.4(4) . . ? C17B C16B Fe2 67.9(3) . . ? C20B C16B H16B 124.1 . . ? C17B C16B H16B 124.1 . . ? Fe2 C16B H16B 130.5 . . ? C16B C17B C18B 100.1 . . ? C16B C17B Fe2 72.8(3) . . ? C18B C17B Fe2 66.3(5) . . ? C16B C17B H17B 130.0 . . ? C18B C17B H17B 130.0 . . ? Fe2 C17B H17B 122.9 . . ? C19B C18B C17B 116.6 . . ? C19B C18B Fe2 72.7(4) . . ? C17B C18B Fe2 72.9(5) . . ? C19B C18B H18B 121.7 . . ? C17B C18B H18B 121.7 . . ? Fe2 C18B H18B 124.3 . . ? C18B C19B C20B 107.1 . . ? C18B C19B Fe2 70.3(4) . . ? C20B C19B Fe2 72.7(4) . . ? C18B C19B H19B 126.4 . . ? C20B C19B H19B 126.4 . . ? Fe2 C19B H19B 122.2 . . ? C16B C20B C19B 104.0 . . ? C16B C20B Fe2 71.9(5) . . ? C19B C20B Fe2 66.0(4) . . ? C16B C20B H20B 128.0 . . ? C19B C20B H20B 128.0 . . ? Fe2 C20B H20B 125.7 . . ? C22 C21 C25 108.5(7) . . ? C22 C21 Fe3 69.6(4) . . ? C25 C21 Fe3 70.0(4) . . ? C22 C21 H21 125.7 . . ? C25 C21 H21 125.7 . . ? Fe3 C21 H21 126.2 . . ? C21 C22 C23 108.4(7) . . ? C21 C22 Fe3 69.8(4) . . ? C23 C22 Fe3 69.6(4) . . ? C21 C22 H22 125.8 . . ? C23 C22 H22 125.8 . . ? Fe3 C22 H22 126.3 . . ? C22 C23 C24 107.5(7) . . ? C22 C23 Fe3 69.7(4) . . ? C24 C23 Fe3 69.5(4) . . ? C22 C23 H23 126.2 . . ? C24 C23 H23 126.2 . . ? Fe3 C23 H23 126.1 . . ? C23 C24 C25 108.6(7) . . ? C23 C24 Fe3 69.8(4) . . ? C25 C24 Fe3 70.1(4) . . ? C23 C24 H24 125.7 . . ? C25 C24 H24 125.7 . . ? Fe3 C24 H24 125.9 . . ? C21 C25 C24 107.0(7) . . ? C21 C25 Fe3 69.4(4) . . ? C24 C25 Fe3 68.9(4) . . ? C21 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? Fe3 C25 H25 126.7 . . ? C27 C26 C30 108.0(7) . . ? C27 C26 Fe3 69.7(4) . . ? C30 C26 Fe3 69.7(4) . . ? C27 C26 H26 126.0 . . ? C30 C26 H26 126.0 . . ? Fe3 C26 H26 126.1 . . ? C28 C27 C26 109.0(6) . . ? C28 C27 Fe3 70.1(4) . . ? C26 C27 Fe3 69.6(4) . . ? C28 C27 H27 125.5 . . ? C26 C27 H27 125.5 . . ? Fe3 C27 H27 126.3 . . ? C27 C28 C29 108.0(7) . . ? C27 C28 Fe3 69.6(5) . . ? C29 C28 Fe3 69.2(4) . . ? C27 C28 H28 126.0 . . ? C29 C28 H28 126.0 . . ? Fe3 C28 H28 126.8 . . ? C28 C29 C30 108.2(6) . . ? C28 C29 Fe3 69.9(4) . . ? C30 C29 Fe3 69.8(4) . . ? C28 C29 H29 125.9 . . ? C30 C29 H29 125.9 . . ? Fe3 C29 H29 126.0 . . ? C29 C30 C26 106.9(6) . . ? C29 C30 Fe3 69.1(4) . . ? C26 C30 Fe3 69.1(4) . . ? C29 C30 Sn3 128.8(5) . . ? C26 C30 Sn3 124.2(5) . . ? Fe3 C30 Sn3 123.7(3) . . ? C32 C31 C35 108.0(6) . . ? C32 C31 Fe4 69.9(4) . . ? C35 C31 Fe4 69.5(4) . . ? C32 C31 H31 126.0 . . ? C35 C31 H31 126.0 . . ? Fe4 C31 H31 126.2 . . ? C31 C32 C33 109.4(7) . . ? C31 C32 Fe4 69.9(4) . . ? C33 C32 Fe4 70.0(4) . . ? C31 C32 H32 125.3 . . ? C33 C32 H32 125.3 . . ? Fe4 C32 H32 126.3 . . ? C32 C33 C34 107.1(6) . . ? C32 C33 Fe4 69.4(4) . . ? C34 C33 Fe4 69.5(4) . . ? C32 C33 H33 126.5 . . ? C34 C33 H33 126.5 . . ? Fe4 C33 H33 126.2 . . ? C33 C34 C35 109.1(6) . . ? C33 C34 Fe4 69.9(4) . . ? C35 C34 Fe4 69.7(4) . . ? C33 C34 H34 125.5 . . ? C35 C34 H34 125.5 . . ? Fe4 C34 H34 126.6 . . ? C34 C35 C31 106.5(6) . . ? C34 C35 Fe4 69.5(4) . . ? C31 C35 Fe4 69.1(4) . . ? C34 C35 Sn4 127.1(5) . . ? C31 C35 Sn4 125.7(5) . . ? Fe4 C35 Sn4 118.6(3) . . ? C40 C36 C37 109.2(8) . . ? C40 C36 Fe4 70.2(5) . . ? C37 C36 Fe4 70.4(5) . . ? C40 C36 H36 125.4 . . ? C37 C36 H36 125.4 . . ? Fe4 C36 H36 125.6 . . ? C36 C37 C38 106.5(8) . . ? C36 C37 Fe4 69.3(5) . . ? C38 C37 Fe4 69.5(4) . . ? C36 C37 H37 126.7 . . ? C38 C37 H37 126.7 . . ? Fe4 C37 H37 125.9 . . ? C39 C38 C37 107.5(8) . . ? C39 C38 Fe4 69.1(5) . . ? C37 C38 Fe4 69.7(4) . . ? C39 C38 H38 126.2 . . ? C37 C38 H38 126.2 . . ? Fe4 C38 H38 126.6 . . ? C38 C39 C40 110.2(9) . . ? C38 C39 Fe4 71.3(4) . . ? C40 C39 Fe4 70.9(5) . . ? C38 C39 H39 124.9 . . ? C40 C39 H39 124.9 . . ? Fe4 C39 H39 124.5 . . ? C39 C40 C36 106.6(8) . . ? C39 C40 Fe4 69.0(5) . . ? C36 C40 Fe4 69.6(5) . . ? C39 C40 H40 126.7 . . ? C36 C40 H40 126.7 . . ? Fe4 C40 H40 126.3 . . ? C42 C41 C45 107.2(8) . . ? C42 C41 Fe5 69.9(4) . . ? C45 C41 Fe5 70.3(5) . . ? C42 C41 H41 126.4 . . ? C45 C41 H41 126.4 . . ? Fe5 C41 H41 125.0 . . ? C41 C42 C43 106.5(7) . . ? C41 C42 Fe5 69.7(5) . . ? C43 C42 Fe5 68.9(4) . . ? C41 C42 Sn5 127.9(6) . . ? C43 C42 Sn5 125.6(6) . . ? Fe5 C42 Sn5 124.2(4) . . ? C44 C43 C42 109.6(8) . . ? C44 C43 Fe5 71.5(5) . . ? C42 C43 Fe5 70.1(4) . . ? C44 C43 H43 125.2 . . ? C42 C43 H43 125.2 . . ? Fe5 C43 H43 124.8 . . ? C45 C44 C43 107.2(8) . . ? C45 C44 Fe5 70.3(6) . . ? C43 C44 Fe5 68.4(5) . . ? C45 C44 H44 126.4 . . ? C43 C44 H44 126.4 . . ? Fe5 C44 H44 126.5 . . ? C44 C45 C41 109.4(8) . . ? C44 C45 Fe5 70.8(5) . . ? C41 C45 Fe5 68.7(5) . . ? C44 C45 H45 125.3 . . ? C41 C45 H45 125.3 . . ? Fe5 C45 H45 126.8 . . ? C50A C46A C47A 108.0 . . ? C50A C46A Fe5 69.4(4) . . ? C47A C46A Fe5 71.3(5) . . ? C50A C46A H46A 126.0 . . ? C47A C46A H46A 126.0 . . ? Fe5 C46A H46A 124.8 . . ? C48A C47A C46A 108.0 . . ? C48A C47A Fe5 70.4(4) . . ? C46A C47A Fe5 69.4(4) . . ? C48A C47A H47A 126.0 . . ? C46A C47A H47A 126.0 . . ? Fe5 C47A H47A 125.8 . . ? C49A C48A C47A 108.0 . . ? C49A C48A Fe5 69.3(4) . . ? C47A C48A Fe5 70.6(4) . . ? C49A C48A H48A 126.0 . . ? C47A C48A H48A 126.0 . . ? Fe5 C48A H48A 125.7 . . ? C50A C49A C48A 108.0 . . ? C50A C49A Fe5 69.6(4) . . ? C48A C49A Fe5 71.3(5) . . ? C50A C49A H49A 126.0 . . ? C48A C49A H49A 126.0 . . ? Fe5 C49A H49A 124.7 . . ? C49A C50A C46A 108.0 . . ? C49A C50A Fe5 70.6(4) . . ? C46A C50A Fe5 70.8(4) . . ? C49A C50A H50A 126.0 . . ? C46A C50A H50A 126.0 . . ? Fe5 C50A H50A 124.1 . . ? C47B C46B C50B 108.0 . . ? C47B C46B Fe5 63.7(11) . . ? C50B C46B Fe5 73.3(10) . . ? C47B C46B H46B 126.0 . . ? C50B C46B H46B 126.0 . . ? Fe5 C46B H46B 128.4 . . ? C46B C47B C48B 108.0 . . ? C46B C47B Fe5 73.8(10) . . ? C48B C47B Fe5 68.4(10) . . ? C46B C47B H47B 126.0 . . ? C48B C47B H47B 126.0 . . ? Fe5 C47B H47B 123.4 . . ? C49B C48B C47B 108.0 . . ? C49B C48B Fe5 74.2(10) . . ? C47B C48B Fe5 67.4(10) . . ? C49B C48B H48B 126.0 . . ? C47B C48B H48B 126.0 . . ? Fe5 C48B H48B 123.9 . . ? C50B C49B C48B 108.0 . . ? C50B C49B Fe5 72.6(9) . . ? C48B C49B Fe5 63.7(11) . . ? C50B C49B H49B 126.0 . . ? C48B C49B H49B 126.0 . . ? Fe5 C49B H49B 129.2 . . ? C49B C50B C46B 108.0 . . ? C49B C50B Fe5 67.3(9) . . ? C46B C50B Fe5 66.5(9) . . ? C49B C50B H50B 126.0 . . ? C46B C50B H50B 126.0 . . ? Fe5 C50B H50B 131.9 . . ? C52 C51 C55 106.7(6) . . ? C52 C51 Fe6 69.1(4) . . ? C55 C51 Fe6 69.1(4) . . ? C52 C51 Sn6 127.5(5) . . ? C55 C51 Sn6 125.8(5) . . ? Fe6 C51 Sn6 124.3(3) . . ? C53 C52 C51 109.2(6) . . ? C53 C52 Fe6 69.9(4) . . ? C51 C52 Fe6 70.3(4) . . ? C53 C52 H52 125.4 . . ? C51 C52 H52 125.4 . . ? Fe6 C52 H52 126.1 . . ? C52 C53 C54 108.0(6) . . ? C52 C53 Fe6 69.8(4) . . ? C54 C53 Fe6 69.8(4) . . ? C52 C53 H53 126.0 . . ? C54 C53 H53 126.0 . . ? Fe6 C53 H53 126.0 . . ? C55 C54 C53 108.6(6) . . ? C55 C54 Fe6 70.1(4) . . ? C53 C54 Fe6 69.4(4) . . ? C55 C54 H54 125.7 . . ? C53 C54 H54 125.7 . . ? Fe6 C54 H54 126.4 . . ? C54 C55 C51 107.6(6) . . ? C54 C55 Fe6 69.6(4) . . ? C51 C55 Fe6 69.3(3) . . ? C54 C55 H55 126.2 . . ? C51 C55 H55 126.2 . . ? Fe6 C55 H55 126.5 . . ? C60 C56 C57 108.4(6) . . ? C60 C56 Fe6 69.8(4) . . ? C57 C56 Fe6 70.2(4) . . ? C60 C56 H56 125.8 . . ? C57 C56 H56 125.8 . . ? Fe6 C56 H56 125.8 . . ? C58 C57 C56 106.7(6) . . ? C58 C57 Fe6 69.4(4) . . ? C56 C57 Fe6 69.1(4) . . ? C58 C57 H57 126.6 . . ? C56 C57 H57 126.6 . . ? Fe6 C57 H57 126.4 . . ? C59 C58 C57 108.8(6) . . ? C59 C58 Fe6 69.4(4) . . ? C57 C58 Fe6 70.1(4) . . ? C59 C58 H58 125.6 . . ? C57 C58 H58 125.6 . . ? Fe6 C58 H58 126.5 . . ? C58 C59 C60 107.9(6) . . ? C58 C59 Fe6 70.3(4) . . ? C60 C59 Fe6 69.9(4) . . ? C58 C59 H59 126.1 . . ? C60 C59 H59 126.1 . . ? Fe6 C59 H59 125.3 . . ? C56 C60 C59 108.1(6) . . ? C56 C60 Fe6 69.8(4) . . ? C59 C60 Fe6 69.5(4) . . ? C56 C60 H60 125.9 . . ? C59 C60 H60 125.9 . . ? Fe6 C60 H60 126.3 . . ? C02 C01 H01C 109.5 . . ? C02 C01 H01D 109.5 . . ? H01C C01 H01D 109.5 . . ? C02 C01 H01E 109.5 . . ? H01C C01 H01E 109.5 . . ? H01D C01 H01E 109.5 . . ? O8 C02 C03 122.7(9) . . ? O8 C02 C01 120.4(8) . . ? C03 C02 C01 116.9(7) . . ? C02 C03 H03A 109.5 . . ? C02 C03 H03B 109.5 . . ? H03A C03 H03B 109.5 . . ? C02 C03 H03C 109.5 . . ? H03A C03 H03C 109.5 . . ? H03B C03 H03C 109.5 . . ? C05 C04 H04A 109.5 . . ? C05 C04 H04B 109.5 . . ? H04A C04 H04B 109.5 . . ? C05 C04 H04C 109.5 . . ? H04A C04 H04C 109.5 . . ? H04B C04 H04C 109.5 . . ? O10 C05 C04 121.7(7) . . ? O10 C05 C06 121.6(7) . . ? C04 C05 C06 116.7(6) . . ? C05 C06 H06A 109.5 . . ? C05 C06 H06B 109.5 . . ? H06A C06 H06B 109.5 . . ? C05 C06 H06C 109.5 . . ? H06A C06 H06C 109.5 . . ? H06B C06 H06C 109.5 . . ? C08 C07 H07A 109.5 . . ? C08 C07 H07B 109.5 . . ? H07A C07 H07B 109.5 . . ? C08 C07 H07C 109.5 . . ? H07A C07 H07C 109.5 . . ? H07B C07 H07C 109.5 . . ? O9 C08 C09 122.3(7) . . ? O9 C08 C07 119.2(8) . . ? C09 C08 C07 118.4(8) . . ? C09 C08 Na6 86.2(5) . . ? C07 C08 Na6 147.3(7) . . ? C08 C09 H09A 109.5 . . ? C08 C09 H09B 109.5 . . ? H09A C09 H09B 109.5 . . ? C08 C09 H09C 109.5 . . ? H09A C09 H09C 109.5 . . ? H09B C09 H09C 109.5 . . ? O1B C010 O1A 60.2(10) . . ? O1B C010 C02A 82.0(13) . . ? O1A C010 C02A 115.8(10) . . ? O1B C010 C011 122.8(10) . . ? O1A C010 C011 124.2(8) . . ? C02A C010 C011 119.8(11) . . ? O1B C010 C02B 130.8(13) . . ? O1A C010 C02B 112.8(12) . . ? C02A C010 C02B 56.3(13) . . ? C011 C010 C02B 101.6(10) . . ? C010 C011 H01A 109.5 . . ? C010 C011 H01B 109.5 . . ? H01A C011 H01B 109.5 . . ? C010 C011 H11C 109.5 . . ? H01A C011 H11C 109.5 . . ? H01B C011 H11C 109.5 . . ? C010 O1B Na1 121.6(10) . . ? C010 O1B Na6 132.3(9) . 1_655 ? Na1 O1B Na6 104.9(4) . 1_655 ? C010 C02B H02A 109.5 . . ? C010 C02B H02B 109.5 . . ? C010 C02B H02C 109.5 . . ? C010 O1A Na1 126.1(7) . . ? C010 C02A H02D 109.5 . . ? C010 C02A H02E 109.5 . . ? H02D C02A H02E 109.5 . . ? C010 C02A H02F 109.5 . . ? H02D C02A H02F 109.5 . . ? H02E C02A H02F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 3.03 _refine_diff_density_min -2.02 _refine_diff_density_rms 0.14 # start Validation Reply Form _vrf_PLAT029_2 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: The obtained crystal was weakly diffracting and therefore the quality of the X-ray data is limited. ; _vrf_PLAT220_2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.58 Ratio RESPONSE: The problem is connected with complicated disorder, which could not be properly handled due to the limited X-ray data quality. ; _vrf_PLAT222_2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.52 Ratio RESPONSE: The problem is connected with complicated disorder, which could not be properly handled due to the limited X-ray data quality. ; _vrf_PLAT780_2 ; PROBLEM: Coordinates do not Form a Properly Connected Set RESPONSE: The problem arises probably due to the lack of water H atoms, which could not be found. ; # end Validation Reply Form # Attachment '3-rev2.cif' data_3abs _database_code_depnum_ccdc_archive 'CCDC 755031' #TrackingRef '3-rev2.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C40 H36 Fe4 S6 Sn4' _chemical_formula_sum 'C40 H36 Fe4 S6 Sn4' _chemical_formula_weight 1407.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 13.967(3) _cell_length_b 13.967(3) _cell_length_c 11.064(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2158.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25222 _cell_measurement_theta_min 9.83 _cell_measurement_theta_max 54.12 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 3.899 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.235 _exptl_absorpt_correction_T_max 0.281 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS2 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8638 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.92 _diffrn_reflns_theta_max 26.77 _reflns_number_total 2256 _reflns_number_gt 2228 _reflns_threshold_expression >2sigma(I) _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^)+(0.0300P)^2^+1.3140P] 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 0.00(2) _refine_ls_number_reflns 2256 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0162 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0431 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _computing_data_collection 'XAREA 1.38 (Stoe 2006)' _computing_cell_refinement 'XAREA 1.38 (Stoe 2006)' _computing_data_reduction 'XAREA 1.38 (Stoe 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005) SHELXTL-NT V5.1, Bruker AXS 1999' 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 Sn1 Sn 0.376377(11) 0.555988(11) 0.378609(18) 0.01595(6) Uani 1 1 d . . . Fe1 Fe 0.21124(3) 0.53134(3) 0.13116(4) 0.02261(10) Uani 1 1 d . . . S1 S 0.31154(5) 0.43119(5) 0.50158(6) 0.02112(15) Uani 1 1 d . . . S2 S 0.5000 0.5000 0.24543(8) 0.02164(19) Uani 1 2 d S . . C1 C 0.2586(2) 0.6047(2) 0.2788(2) 0.0196(6) Uani 1 1 d . . . C2 C 0.1617(2) 0.5727(3) 0.2958(3) 0.0278(7) Uani 1 1 d . . . H2 H 0.1399 0.5313 0.3581 0.033 Uiso 1 1 calc R . . C3 C 0.1047(2) 0.6133(3) 0.2037(3) 0.0360(8) Uani 1 1 d . . . H3 H 0.0378 0.6039 0.1935 0.043 Uiso 1 1 calc R . . C4 C 0.1647(2) 0.6709(2) 0.1283(4) 0.0333(6) Uani 1 1 d . . . H4 H 0.1447 0.7066 0.0597 0.040 Uiso 1 1 calc R . . C5 C 0.2598(2) 0.6652(2) 0.1744(3) 0.0256(7) Uani 1 1 d . . . H5 H 0.3145 0.6962 0.1415 0.031 Uiso 1 1 calc R . . C6 C 0.2839(2) 0.4034(2) 0.1168(4) 0.0330(7) Uani 1 1 d . . . H6 H 0.3256 0.3761 0.1753 0.040 Uiso 1 1 calc R . . C7 C 0.1840(3) 0.3886(2) 0.1092(4) 0.0425(9) Uani 1 1 d . . . H7 H 0.1466 0.3504 0.1623 0.051 Uiso 1 1 calc R . . C8 C 0.1495(3) 0.4402(3) 0.0093(4) 0.0493(11) Uani 1 1 d . . . H8 H 0.0850 0.4419 -0.0179 0.059 Uiso 1 1 calc R . . C9 C 0.2274(3) 0.4892(3) -0.0435(3) 0.0447(10) Uani 1 1 d . . . H9 H 0.2244 0.5306 -0.1115 0.054 Uiso 1 1 calc R . . C10 C 0.3108(3) 0.4655(3) 0.0229(3) 0.0341(8) Uani 1 1 d . . . H10 H 0.3738 0.4878 0.0068 0.041 Uiso 1 1 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 Sn1 0.01251(9) 0.01708(9) 0.01826(9) 0.00052(8) -0.00091(8) 0.00116(6) Fe1 0.02143(19) 0.01939(18) 0.0270(2) -0.00247(17) -0.00550(19) 0.00199(14) S1 0.0151(3) 0.0203(3) 0.0280(3) 0.0047(3) -0.0003(3) -0.0014(3) S2 0.0161(4) 0.0323(5) 0.0165(4) 0.000 0.000 0.0044(4) C1 0.0161(13) 0.0212(14) 0.0214(13) 0.0004(11) -0.0027(11) 0.0033(11) C2 0.0165(14) 0.0380(18) 0.0289(14) -0.0026(13) 0.0016(12) 0.0039(13) C3 0.0195(16) 0.044(2) 0.0446(18) -0.0160(16) -0.0083(13) 0.0115(15) C4 0.045(2) 0.0220(15) 0.0326(14) -0.0022(16) -0.0139(19) 0.0157(11) C5 0.0319(17) 0.0175(14) 0.0276(14) 0.0035(11) -0.0038(13) -0.0008(12) C6 0.0361(16) 0.0192(14) 0.0437(16) -0.0057(16) -0.0090(17) 0.0069(12) C7 0.0423(19) 0.0185(15) 0.067(3) -0.0112(17) -0.001(2) -0.0051(13) C8 0.042(2) 0.038(2) 0.069(2) -0.027(2) -0.032(2) 0.0092(17) C9 0.065(3) 0.042(2) 0.0274(15) -0.0130(15) -0.0136(16) 0.021(2) C10 0.0368(19) 0.0334(18) 0.0322(16) -0.0114(14) 0.0048(14) 0.0067(15) 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 Sn1 C1 2.095(3) . ? Sn1 S1 2.3894(8) . ? Sn1 S2 2.4009(7) . ? Sn1 S1 2.4014(8) 3_566 ? Fe1 C2 2.032(3) . ? Fe1 C9 2.033(3) . ? Fe1 C1 2.039(3) . ? Fe1 C3 2.042(3) . ? Fe1 C7 2.044(3) . ? Fe1 C8 2.045(3) . ? Fe1 C5 2.046(3) . ? Fe1 C10 2.052(3) . ? Fe1 C4 2.055(3) . ? Fe1 C6 2.061(3) . ? S1 Sn1 2.4014(8) 4_656 ? S2 Sn1 2.4009(7) 2_665 ? C1 C5 1.432(4) . ? C1 C2 1.437(4) . ? C2 C3 1.412(5) . ? C2 H2 0.9500 . ? C3 C4 1.431(5) . ? C3 H3 0.9500 . ? C4 C5 1.426(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.405(5) . ? C6 C7 1.413(5) . ? C6 H6 0.9500 . ? C7 C8 1.405(6) . ? C7 H7 0.9500 . ? C8 C9 1.411(7) . ? C8 H8 0.9500 . ? C9 C10 1.417(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 S1 103.85(9) . . ? C1 Sn1 S2 110.32(8) . . ? S1 Sn1 S2 112.61(2) . . ? C1 Sn1 S1 106.92(8) . 3_566 ? S1 Sn1 S1 111.63(2) . 3_566 ? S2 Sn1 S1 111.13(2) . 3_566 ? C2 Fe1 C9 166.45(16) . . ? C2 Fe1 C1 41.34(12) . . ? C9 Fe1 C1 150.63(17) . . ? C2 Fe1 C3 40.57(14) . . ? C9 Fe1 C3 128.07(15) . . ? C1 Fe1 C3 68.89(12) . . ? C2 Fe1 C7 108.68(17) . . ? C9 Fe1 C7 67.98(19) . . ? C1 Fe1 C7 130.23(16) . . ? C3 Fe1 C7 117.23(16) . . ? C2 Fe1 C8 128.63(18) . . ? C9 Fe1 C8 40.50(19) . . ? C1 Fe1 C8 167.96(17) . . ? C3 Fe1 C8 107.47(16) . . ? C7 Fe1 C8 40.19(18) . . ? C2 Fe1 C5 69.12(14) . . ? C9 Fe1 C5 116.76(17) . . ? C1 Fe1 C5 41.04(12) . . ? C3 Fe1 C5 68.75(15) . . ? C7 Fe1 C5 168.81(15) . . ? C8 Fe1 C5 149.63(16) . . ? C2 Fe1 C10 151.75(14) . . ? C9 Fe1 C10 40.57(15) . . ? C1 Fe1 C10 118.23(14) . . ? C3 Fe1 C10 166.95(15) . . ? C7 Fe1 C10 67.67(16) . . ? C8 Fe1 C10 67.81(17) . . ? C5 Fe1 C10 108.73(15) . . ? C2 Fe1 C4 68.70(15) . . ? C9 Fe1 C4 107.16(17) . . ? C1 Fe1 C4 68.80(14) . . ? C3 Fe1 C4 40.87(16) . . ? C7 Fe1 C4 149.79(14) . . ? C8 Fe1 C4 116.51(15) . . ? C5 Fe1 C4 40.68(13) . . ? C10 Fe1 C4 129.05(16) . . ? C2 Fe1 C6 118.87(15) . . ? C9 Fe1 C6 67.74(16) . . ? C1 Fe1 C6 109.75(13) . . ? C3 Fe1 C6 151.04(16) . . ? C7 Fe1 C6 40.25(13) . . ? C8 Fe1 C6 67.50(15) . . ? C5 Fe1 C6 130.35(13) . . ? C10 Fe1 C6 39.95(16) . . ? C4 Fe1 C6 167.69(15) . . ? Sn1 S1 Sn1 104.77(3) . 4_656 ? Sn1 S2 Sn1 104.28(4) . 2_665 ? C5 C1 C2 107.5(3) . . ? C5 C1 Fe1 69.75(17) . . ? C2 C1 Fe1 69.06(17) . . ? C5 C1 Sn1 127.4(2) . . ? C2 C1 Sn1 124.7(2) . . ? Fe1 C1 Sn1 120.91(14) . . ? C3 C2 C1 108.2(3) . . ? C3 C2 Fe1 70.09(18) . . ? C1 C2 Fe1 69.60(17) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe1 C2 H2 126.0 . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Fe1 69.33(19) . . ? C4 C3 Fe1 70.1(2) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Fe1 C3 H3 126.4 . . ? C5 C4 C3 107.8(3) . . ? C5 C4 Fe1 69.31(18) . . ? C3 C4 Fe1 69.05(19) . . ? C5 C4 H4 126.1 . . ? C3 C4 H4 126.1 . . ? Fe1 C4 H4 127.1 . . ? C4 C5 C1 108.1(3) . . ? C4 C5 Fe1 70.01(17) . . ? C1 C5 Fe1 69.21(17) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe1 C5 H5 126.4 . . ? C10 C6 C7 108.1(4) . . ? C10 C6 Fe1 69.68(18) . . ? C7 C6 Fe1 69.23(18) . . ? C10 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Fe1 C6 H6 126.7 . . ? C8 C7 C6 108.1(4) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 70.52(18) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe1 C7 H7 125.2 . . ? C7 C8 C9 108.1(3) . . ? C7 C8 Fe1 69.9(2) . . ? C9 C8 Fe1 69.3(2) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe1 C8 H8 126.4 . . ? C8 C9 C10 107.8(3) . . ? C8 C9 Fe1 70.2(2) . . ? C10 C9 Fe1 70.45(19) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 124.9 . . ? C6 C10 C9 107.9(4) . . ? C6 C10 Fe1 70.37(19) . . ? C9 C10 Fe1 69.0(2) . . ? C6 C10 H10 126.0 . . ? C9 C10 H10 126.0 . . ? Fe1 C10 H10 126.2 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.77 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.25 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.07 # Attachment '4-rev2.cif' data_4abs _database_code_depnum_ccdc_archive 'CCDC 755032' #TrackingRef '4-rev2.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C108 H128 Fe8 Na2 Ni3 O7 S16 Sn8, 2(C4 H8 O)' _chemical_formula_sum 'C116 H144 Fe8 Na2 Ni3 O9 S16 Sn8' _chemical_formula_weight 3813.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.989(3) _cell_length_b 15.435(3) _cell_length_c 20.444(4) _cell_angle_alpha 72.39(3) _cell_angle_beta 79.23(3) _cell_angle_gamma 77.20(3) _cell_volume 3486.9(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8222 _cell_measurement_theta_min 5.99 _cell_measurement_theta_max 54.45 _exptl_crystal_description needles _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1882 _exptl_absorpt_coefficient_mu 2.896 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.470 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS2 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32920 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 26.74 _reflns_number_total 14586 _reflns_number_gt 11929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XAREA 1.38 (Stoe 2006)' _computing_cell_refinement 'XAREA 1.38 (Stoe 2006)' _computing_data_reduction 'XAREA 1.38 (Stoe 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005) SHELXTL-NT V5.1, Bruker AXS 1999' _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^)+(0.0863P)^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_extinction_coef ? _refine_ls_number_reflns 14586 _refine_ls_number_parameters 719 _refine_ls_number_restraints 1075 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_special_details ; The space group choice was carefully considered and also a solution in P1 space group was taken into consideration. It seems, that the most plausible model is obtained when assuming P-1 space group and THF molecule disorder. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.94230(6) -0.00845(4) 0.64542(4) 0.02838(15) Uani 1 1 d U . . Fe2 Fe 0.47780(7) 0.84074(5) 0.61038(4) 0.03450(17) Uani 1 1 d U . . Fe3 Fe 1.03016(7) 0.15890(5) 0.89185(4) 0.03544(17) Uani 1 1 d U . . Fe4 Fe 0.76348(7) 0.60283(6) 0.89913(4) 0.03955(18) Uani 1 1 d U . . Ni1 Ni 0.78596(5) 0.45488(4) 0.59212(3) 0.02659(13) Uani 1 1 d U . . Ni2 Ni 1.0000 0.5000 0.5000 0.02921(19) Uani 1 2 d SU . . Sn1 Sn 0.76408(3) 0.70221(2) 0.562878(17) 0.03022(9) Uani 1 1 d U . . Sn2 Sn 0.77442(3) 0.55341(2) 0.735002(17) 0.02918(9) Uani 1 1 d U . . Sn3 Sn 0.90247(3) 0.29931(2) 0.739907(16) 0.02699(9) Uani 1 1 d U . . Sn4 Sn 0.98075(3) 0.23433(2) 0.581516(17) 0.02897(9) Uani 1 1 d U . . S1 S 1.14083(15) 0.17144(9) 0.50926(8) 0.0487(4) Uani 1 1 d U . . S2 S 0.84891(11) 0.68834(8) 0.66530(7) 0.0352(3) Uani 1 1 d U . . S3 S 0.92996(13) 0.43040(9) 0.77125(8) 0.0403(3) Uani 1 1 d U . . S4 S 1.07364(11) 0.24114(9) 0.67357(7) 0.0351(3) Uani 1 1 d U . . S5 S 0.82097(12) 0.57705(8) 0.50703(6) 0.0310(2) Uani 1 1 d U . . S6 S 0.66345(10) 0.53961(8) 0.65515(6) 0.0279(2) Uani 1 1 d U . . S7 S 0.75587(10) 0.32266(8) 0.67050(6) 0.0277(2) Uani 1 1 d U . . S8 S 0.89950(12) 0.38848(8) 0.51590(6) 0.0310(3) Uani 1 1 d U . . Na1 Na 0.5093(2) 0.41022(16) 0.70584(14) 0.0482(6) Uani 1 1 d U C . C1 C 0.5905(5) 0.7678(4) 0.5505(3) 0.0359(10) Uani 1 1 d U . . C2 C 0.4877(5) 0.7294(4) 0.5739(3) 0.0437(13) Uani 1 1 d U . . H2 H 0.4833 0.6678 0.6007 0.052 Uiso 1 1 calc R . . C3 C 0.3926(6) 0.7990(4) 0.5505(4) 0.0519(15) Uani 1 1 d U . . H3 H 0.3140 0.7920 0.5594 0.062 Uiso 1 1 calc R . . C4 C 0.4356(6) 0.8798(4) 0.5118(3) 0.0493(14) Uani 1 1 d U . . H4 H 0.3910 0.9366 0.4896 0.059 Uiso 1 1 calc R . . C5 C 0.5579(6) 0.8618(4) 0.5117(3) 0.0434(12) Uani 1 1 d U . . H5 H 0.6086 0.9046 0.4899 0.052 Uiso 1 1 calc R . . C6 C 0.5606(5) 0.8444(5) 0.6878(3) 0.0463(13) Uani 1 1 d U . . H6 H 0.6396 0.8206 0.6930 0.056 Uiso 1 1 calc R . . C7 C 0.4672(6) 0.7954(5) 0.7151(3) 0.0504(13) Uani 1 1 d U . . H7 H 0.4730 0.7329 0.7421 0.060 Uiso 1 1 calc R . . C8 C 0.3644(5) 0.8552(5) 0.6953(3) 0.0504(13) Uani 1 1 d U . . H8 H 0.2893 0.8400 0.7064 0.060 Uiso 1 1 calc R . . C9 C 0.3933(5) 0.9428(4) 0.6557(3) 0.0424(11) Uani 1 1 d U . . H9 H 0.3408 0.9963 0.6360 0.051 Uiso 1 1 calc R . . C10 C 0.5140(5) 0.9356(4) 0.6512(3) 0.0449(12) Uani 1 1 d U . . H10 H 0.5567 0.9835 0.6276 0.054 Uiso 1 1 calc R . . C11 C 0.6833(5) 0.5741(5) 0.8305(3) 0.0492(13) Uani 1 1 d U . . C12 C 0.6820(9) 0.5038(7) 0.8954(4) 0.082(2) Uani 1 1 d U . . H12 H 0.7136 0.4402 0.9014 0.098 Uiso 1 1 calc R . . C13 C 0.6267(11) 0.5442(10) 0.9483(5) 0.099(3) Uani 1 1 d U . . H13 H 0.6180 0.5131 0.9963 0.119 Uiso 1 1 calc R . . C14 C 0.5885(7) 0.6330(10) 0.9207(5) 0.092(3) Uani 1 1 d U . . H14 H 0.5439 0.6749 0.9453 0.110 Uiso 1 1 calc R . . C15 C 0.6261(7) 0.6559(7) 0.8462(4) 0.078(2) Uani 1 1 d U . . H15 H 0.6139 0.7154 0.8144 0.094 Uiso 1 1 calc R . . C16 C 0.9252(7) 0.6232(8) 0.8512(5) 0.083(2) Uani 1 1 d U . . H16 H 0.9566 0.6203 0.8055 0.100 Uiso 1 1 calc R . . C17 C 0.9318(8) 0.5512(9) 0.9091(6) 0.101(3) Uani 1 1 d U . . H17 H 0.9707 0.4901 0.9104 0.122 Uiso 1 1 calc R . . C18 C 0.8697(9) 0.5818(9) 0.9698(5) 0.094(3) Uani 1 1 d U . . H18 H 0.8567 0.5453 1.0163 0.113 Uiso 1 1 calc R . . C19 C 0.8352(8) 0.6750(8) 0.9438(5) 0.084(2) Uani 1 1 d U . . H19 H 0.7971 0.7159 0.9709 0.101 Uiso 1 1 calc R . . C20 C 0.8646(9) 0.7023(8) 0.8700(5) 0.090(2) Uani 1 1 d U . . H20 H 0.8465 0.7624 0.8399 0.109 Uiso 1 1 calc R . . C21 C 0.8948(4) 0.1951(3) 0.8342(3) 0.0323(10) Uani 1 1 d U . . C22 C 0.9486(5) 0.1008(3) 0.8413(3) 0.0367(11) Uani 1 1 d U . . H22 H 0.9840 0.0743 0.8046 0.044 Uiso 1 1 calc R . . C23 C 0.9397(5) 0.0536(4) 0.9133(3) 0.0431(12) Uani 1 1 d U . . H23 H 0.9673 -0.0102 0.9326 0.052 Uiso 1 1 calc R . . C24 C 0.8834(5) 0.1169(4) 0.9509(3) 0.0442(12) Uani 1 1 d U . . H24 H 0.8667 0.1037 0.9998 0.053 Uiso 1 1 calc R . . C25 C 0.8558(5) 0.2046(4) 0.9027(3) 0.0379(10) Uani 1 1 d U . . H25 H 0.8178 0.2601 0.9140 0.045 Uiso 1 1 calc R . . C26 C 1.1493(5) 0.2415(4) 0.8425(3) 0.0449(13) Uani 1 1 d U . . H26 H 1.1446 0.2871 0.7993 0.054 Uiso 1 1 calc R . . C27 C 1.2018(5) 0.1467(5) 0.8516(4) 0.0518(13) Uani 1 1 d U . . H27 H 1.2385 0.1174 0.8166 0.062 Uiso 1 1 calc R . . C28 C 1.1876(6) 0.1050(5) 0.9254(4) 0.0577(16) Uani 1 1 d U . . H28 H 1.2141 0.0419 0.9475 0.069 Uiso 1 1 calc R . . C29 C 1.1286(7) 0.1715(5) 0.9595(4) 0.0588(16) Uani 1 1 d U . . H29 H 1.1081 0.1616 1.0081 0.071 Uiso 1 1 calc R . . C30 C 1.1055(6) 0.2562(5) 0.9079(3) 0.0502(13) Uani 1 1 d U . . H30 H 1.0669 0.3134 0.9161 0.060 Uiso 1 1 calc R . . C31 C 0.8807(4) 0.1287(3) 0.6033(3) 0.0312(10) Uani 1 1 d U . . C32 C 0.8819(5) 0.0765(3) 0.5564(3) 0.0373(11) Uani 1 1 d U . . H32 H 0.9229 0.0852 0.5110 0.045 Uiso 1 1 calc R . . C33 C 0.8101(5) 0.0083(4) 0.5899(3) 0.0440(13) Uani 1 1 d U . . H33 H 0.7941 -0.0355 0.5704 0.053 Uiso 1 1 calc R . . C34 C 0.7672(5) 0.0179(4) 0.6573(4) 0.0431(12) Uani 1 1 d U . . H34 H 0.7187 -0.0192 0.6911 0.052 Uiso 1 1 calc R . . C35 C 0.8092(4) 0.0923(3) 0.6654(3) 0.0358(10) Uani 1 1 d U . . H35 H 0.7927 0.1143 0.7055 0.043 Uiso 1 1 calc R . . C36 C 1.0944(5) -0.0228(4) 0.6813(3) 0.0405(11) Uani 1 1 d U . . H36 H 1.1269 0.0262 0.6847 0.049 Uiso 1 1 calc R . . C37 C 1.1121(5) -0.0588(4) 0.6226(3) 0.0385(11) Uani 1 1 d U . . H37 H 1.1592 -0.0379 0.5803 0.046 Uiso 1 1 calc R . . C38 C 1.0478(5) -0.1304(3) 0.6383(3) 0.0382(11) Uani 1 1 d U . . H38 H 1.0443 -0.1662 0.6085 0.046 Uiso 1 1 calc R . . C39 C 0.9903(6) -0.1393(4) 0.7052(3) 0.0431(12) Uani 1 1 d U . . H39 H 0.9400 -0.1820 0.7285 0.052 Uiso 1 1 calc R . . C40 C 1.0194(6) -0.0736(4) 0.7332(3) 0.0430(12) Uani 1 1 d U . . H40 H 0.9932 -0.0658 0.7782 0.052 Uiso 1 1 calc R . . C41 C 0.3929(7) 0.3408(7) 0.8668(5) 0.088(3) Uani 1 1 d DU C . H41A H 0.3409 0.3311 0.8384 0.106 Uiso 1 1 calc R . . H41B H 0.3524 0.3902 0.8888 0.106 Uiso 1 1 calc R . . C42 C 0.4286(7) 0.2550(7) 0.9195(4) 0.084(3) Uani 1 1 d DU . . H42A H 0.4337 0.2002 0.9028 0.100 Uiso 1 1 calc R A 1 H42B H 0.3747 0.2497 0.9630 0.100 Uiso 1 1 calc R A 1 C43 C 0.5919(7) 0.3099(7) 0.8593(5) 0.092(3) Uani 1 1 d DU . . H43A H 0.6475 0.3488 0.8592 0.110 Uiso 1 1 calc R B 1 H43B H 0.6321 0.2625 0.8353 0.110 Uiso 1 1 calc R B 1 C44A C 0.5482(10) 0.2660(10) 0.9296(6) 0.066(4) Uiso 0.65(3) 1 d PDU C 1 H44A H 0.5423 0.3057 0.9605 0.079 Uiso 0.65(3) 1 calc PR C 1 H44B H 0.5967 0.2055 0.9480 0.079 Uiso 0.65(3) 1 calc PR C 1 C44B C 0.5564(12) 0.2252(12) 0.9066(13) 0.067(7) Uiso 0.35(3) 1 d PDU C 2 H44C H 0.5919 0.2064 0.9499 0.080 Uiso 0.35(3) 1 calc PR C 2 H44D H 0.5764 0.1738 0.8846 0.080 Uiso 0.35(3) 1 calc PR C 2 C45 C 0.3556(7) 0.2812(6) 0.6646(5) 0.072(2) Uani 1 1 d DU . . H45A H 0.3425 0.3387 0.6267 0.086 Uiso 1 1 calc R D 1 H45B H 0.2812 0.2727 0.6941 0.086 Uiso 1 1 calc R D 1 C46A C 0.4004(15) 0.2035(12) 0.6363(11) 0.055(5) Uiso 0.39(3) 1 d PDU E 1 H46A H 0.4280 0.2237 0.5863 0.065 Uiso 0.39(3) 1 calc PR E 1 H46B H 0.3418 0.1641 0.6437 0.065 Uiso 0.39(3) 1 calc PR E 1 C47A C 0.4958(17) 0.1554(14) 0.6764(10) 0.063(6) Uiso 0.39(3) 1 d PDU E 1 H47C H 0.5700 0.1590 0.6457 0.075 Uiso 0.39(3) 1 calc PR E 1 H47D H 0.4894 0.0894 0.6964 0.075 Uiso 0.39(3) 1 calc PR E 1 C46B C 0.3758(14) 0.1784(8) 0.6658(10) 0.074(4) Uiso 0.61(3) 1 d PDU E 2 H46C H 0.3027 0.1544 0.6827 0.089 Uiso 0.61(3) 1 calc PR E 2 H46D H 0.4025 0.1719 0.6184 0.089 Uiso 0.61(3) 1 calc PR E 2 C47B C 0.4637(12) 0.1249(9) 0.7119(9) 0.068(4) Uiso 0.61(3) 1 d PDU E 2 H47A H 0.4313 0.0785 0.7518 0.082 Uiso 0.61(3) 1 calc PR E 2 H47B H 0.5315 0.0938 0.6866 0.082 Uiso 0.61(3) 1 calc PR E 2 C48 C 0.4931(7) 0.1990(5) 0.7340(5) 0.072(2) Uani 1 1 d DU . . H48A H 0.4483 0.1685 0.7775 0.086 Uiso 1 1 calc R E 1 H48B H 0.5717 0.1984 0.7429 0.086 Uiso 1 1 calc R E 1 C49 C 0.2237(7) 0.5082(6) 0.7038(7) 0.092(3) Uani 1 1 d DU . . H49A H 0.1765 0.4750 0.7450 0.111 Uiso 1 1 calc R . . H49B H 0.2302 0.4791 0.6659 0.111 Uiso 1 1 calc R . . C50 C 0.1723(9) 0.6092(6) 0.6819(7) 0.111(4) Uani 1 1 d DU . . H50A H 0.1971 0.6369 0.6323 0.134 Uiso 1 1 calc R . . H50B H 0.0869 0.6188 0.6902 0.134 Uiso 1 1 calc R . . C51 C 0.2187(9) 0.6488(7) 0.7266(7) 0.104(3) Uani 1 1 d DU . . H51A H 0.2391 0.7098 0.7005 0.124 Uiso 1 1 calc R . . H51B H 0.1613 0.6563 0.7671 0.124 Uiso 1 1 calc R . . C52 C 0.3217(8) 0.5823(6) 0.7489(6) 0.087(3) Uani 1 1 d DU . . H52A H 0.3906 0.6123 0.7332 0.104 Uiso 1 1 calc R . . H52B H 0.3132 0.5595 0.8000 0.104 Uiso 1 1 calc R . . O1 O 0.4979(4) 0.3648(4) 0.8252(3) 0.0649(13) Uani 1 1 d DU C . O2 O 0.4381(4) 0.2873(3) 0.7049(3) 0.0645(14) Uani 1 1 d U C . O3 O 0.3346(4) 0.5079(3) 0.7195(3) 0.0638(13) Uani 1 1 d DU . . C55A C 0.5114(11) 0.9621(9) 0.9027(7) 0.052(3) Uiso 0.50 1 d PDU . . H55A H 0.4358 0.9724 0.8861 0.063 Uiso 0.50 1 calc PR . . H55B H 0.5057 0.9245 0.9516 0.063 Uiso 0.50 1 calc PR . . C56A C 0.6043(12) 0.9140(13) 0.8588(10) 0.083(5) Uiso 0.50 1 d PDU . . H56A H 0.5868 0.9303 0.8107 0.099 Uiso 0.50 1 calc PR . . H56B H 0.6152 0.8461 0.8783 0.099 Uiso 0.50 1 calc PR . . C57A C 0.7095(11) 0.9515(9) 0.8623(7) 0.053(3) Uiso 0.50 1 d PDU . . H57A H 0.7666 0.9026 0.8880 0.063 Uiso 0.50 1 calc PR . . H57B H 0.7470 0.9796 0.8155 0.063 Uiso 0.50 1 calc PR . . C58A C 0.6593(16) 1.0201(14) 0.8991(11) 0.096(6) Uiso 0.50 1 d PDU . . H58A H 0.6737 0.9948 0.9480 0.115 Uiso 0.50 1 calc PR . . H58B H 0.6973 1.0748 0.8786 0.115 Uiso 0.50 1 calc PR . . C59A C 0.1353(15) 0.7490(9) 0.9099(10) 0.080(5) Uiso 0.50 1 d PDU . . H59A H 0.1061 0.7283 0.8759 0.096 Uiso 0.50 1 calc PR . . H59B H 0.0975 0.7209 0.9566 0.096 Uiso 0.50 1 calc PR . . C60A C 0.2648(16) 0.7171(16) 0.9068(14) 0.105(7) Uiso 0.50 1 d PDU . . H60A H 0.2867 0.6757 0.9516 0.126 Uiso 0.50 1 calc PR . . H60B H 0.2958 0.6856 0.8699 0.126 Uiso 0.50 1 calc PR . . C61A C 0.3034(11) 0.8051(8) 0.8908(7) 0.049(3) Uiso 0.50 1 d PDU . . H61A H 0.3733 0.8065 0.8562 0.058 Uiso 0.50 1 calc PR . . H61B H 0.3222 0.8142 0.9331 0.058 Uiso 0.50 1 calc PR . . C62A C 0.2085(10) 0.8788(9) 0.8628(7) 0.057(3) Uiso 0.50 1 d PDU . . H62A H 0.2099 0.9367 0.8738 0.069 Uiso 0.50 1 calc PR . . H62B H 0.2145 0.8910 0.8120 0.069 Uiso 0.50 1 calc PR . . O5A O 0.5430(14) 1.0469(10) 0.8967(9) 0.115(5) Uiso 0.50 1 d PDU . . O6A O 0.1081(8) 0.8445(6) 0.8953(5) 0.054(2) Uiso 0.50 1 d PDU . . O4 O 0.4825(9) 0.4550(7) 0.5831(5) 0.056(2) Uiso 0.50 1 d PU . . C53A C 0.5348(9) 0.4204(7) 0.5270(5) 0.085(3) Uiso 0.50 1 d PU . 1 H53A H 0.5870 0.3966 0.5632 0.101 Uiso 0.50 1 calc PR . 1 H53B H 0.4954 0.3710 0.5259 0.101 Uiso 0.50 1 calc PR . 1 C54A C 0.3986(14) 0.5310(10) 0.5500(8) 0.051(3) Uiso 0.50 1 d PU F 1 H54A H 0.3257 0.5173 0.5427 0.062 Uiso 0.50 1 calc PR F 1 H54B H 0.3931 0.5922 0.5578 0.062 Uiso 0.50 1 calc PR F 1 C53B C 0.5348(9) 0.4204(7) 0.5270(5) 0.085(3) Uiso 0.50 1 d PU F -1 H53C H 0.5052 0.3700 0.5189 0.101 Uiso 0.50 1 calc PR F -1 H53D H 0.6168 0.4243 0.5096 0.101 Uiso 0.50 1 calc PR F -1 C54B C 0.4446(14) 0.5141(10) 0.5352(8) 0.052(3) Uiso 0.50 1 d PU F -1 H54C H 0.4961 0.5601 0.5139 0.063 Uiso 0.50 1 calc PR F -1 H54D H 0.4311 0.4878 0.4994 0.063 Uiso 0.50 1 calc PR F -1 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 Fe1 0.0284(3) 0.0232(3) 0.0340(4) -0.0065(3) -0.0065(3) -0.0053(3) Fe2 0.0317(4) 0.0334(4) 0.0413(4) -0.0100(3) -0.0105(3) -0.0071(3) Fe3 0.0354(4) 0.0377(4) 0.0337(4) -0.0008(3) -0.0132(3) -0.0126(3) Fe4 0.0391(4) 0.0479(4) 0.0367(4) -0.0170(3) -0.0111(3) -0.0052(3) Ni1 0.0335(3) 0.0227(3) 0.0253(3) -0.0057(2) -0.0061(2) -0.0079(2) Ni2 0.0394(5) 0.0213(4) 0.0271(4) -0.0066(3) -0.0017(4) -0.0079(3) Sn1 0.03664(19) 0.02468(16) 0.03045(17) -0.00887(13) -0.00275(13) -0.00709(13) Sn2 0.03130(18) 0.03008(17) 0.02989(17) -0.01014(13) -0.00800(13) -0.00692(13) Sn3 0.02947(17) 0.02636(16) 0.02674(16) -0.00556(12) -0.00699(12) -0.00775(13) Sn4 0.03729(19) 0.02244(15) 0.02827(17) -0.00606(12) -0.00424(13) -0.00868(13) S1 0.0651(10) 0.0272(6) 0.0493(8) -0.0142(6) 0.0194(7) -0.0163(6) S2 0.0346(7) 0.0296(6) 0.0466(7) -0.0099(5) -0.0131(5) -0.0105(5) S3 0.0449(8) 0.0297(6) 0.0541(8) -0.0139(6) -0.0262(6) -0.0026(5) S4 0.0288(6) 0.0428(7) 0.0376(6) -0.0147(5) -0.0055(5) -0.0081(5) S5 0.0420(7) 0.0231(5) 0.0282(6) -0.0063(4) -0.0031(5) -0.0086(5) S6 0.0300(6) 0.0275(5) 0.0292(5) -0.0081(4) -0.0075(4) -0.0073(4) S7 0.0315(6) 0.0251(5) 0.0288(5) -0.0047(4) -0.0089(5) -0.0089(4) S8 0.0439(7) 0.0226(5) 0.0276(6) -0.0067(4) -0.0049(5) -0.0083(5) Na1 0.0351(11) 0.0403(11) 0.0669(15) -0.0070(11) -0.0059(10) -0.0130(9) C1 0.040(3) 0.031(2) 0.040(3) -0.0128(19) -0.014(2) -0.0001(19) C2 0.047(3) 0.030(2) 0.062(4) -0.014(2) -0.027(3) -0.005(2) C3 0.047(3) 0.041(3) 0.080(4) -0.021(3) -0.037(3) -0.001(2) C4 0.065(4) 0.034(3) 0.051(3) -0.012(2) -0.032(3) 0.008(2) C5 0.057(3) 0.029(2) 0.039(2) -0.008(2) -0.008(2) 0.002(2) C6 0.032(3) 0.064(3) 0.052(3) -0.032(3) -0.013(2) 0.003(2) C7 0.042(3) 0.060(3) 0.043(3) -0.010(3) -0.005(2) -0.002(3) C8 0.035(3) 0.058(3) 0.049(3) -0.006(3) -0.002(2) -0.006(2) C9 0.036(3) 0.047(3) 0.048(3) -0.020(2) -0.007(2) -0.003(2) C10 0.040(3) 0.052(3) 0.054(3) -0.031(2) -0.005(2) -0.010(2) C11 0.038(3) 0.079(4) 0.046(3) -0.036(3) -0.006(2) -0.013(3) C12 0.125(6) 0.095(4) 0.048(3) -0.025(3) 0.013(4) -0.079(4) C13 0.111(6) 0.162(7) 0.058(4) -0.049(4) 0.009(4) -0.083(6) C14 0.041(3) 0.188(8) 0.074(5) -0.087(5) -0.007(3) -0.003(5) C15 0.065(4) 0.115(5) 0.066(4) -0.060(4) -0.034(3) 0.032(4) C16 0.048(4) 0.144(7) 0.085(4) -0.066(5) -0.002(3) -0.033(4) C17 0.061(4) 0.151(7) 0.102(6) -0.063(5) -0.049(4) 0.032(5) C18 0.078(5) 0.149(7) 0.076(4) -0.050(5) -0.044(4) -0.006(5) C19 0.080(5) 0.128(6) 0.081(5) -0.068(5) -0.001(4) -0.046(5) C20 0.108(6) 0.105(5) 0.089(5) -0.055(4) 0.022(5) -0.068(5) C21 0.033(2) 0.033(2) 0.031(2) -0.0015(18) -0.0109(18) -0.011(2) C22 0.040(3) 0.029(2) 0.042(3) -0.0028(19) -0.013(2) -0.011(2) C23 0.047(3) 0.037(2) 0.046(3) 0.003(2) -0.016(2) -0.019(2) C24 0.042(3) 0.055(3) 0.033(2) 0.002(2) -0.009(2) -0.018(2) C25 0.034(2) 0.044(3) 0.034(2) -0.007(2) -0.006(2) -0.007(2) C26 0.048(3) 0.045(3) 0.042(3) 0.006(2) -0.016(2) -0.024(2) C27 0.034(2) 0.053(3) 0.065(3) -0.009(3) -0.010(2) -0.009(2) C28 0.039(3) 0.049(3) 0.075(4) 0.018(3) -0.029(3) -0.016(2) C29 0.066(4) 0.076(4) 0.043(3) 0.000(3) -0.028(3) -0.035(3) C30 0.047(3) 0.055(3) 0.058(3) -0.013(3) -0.022(3) -0.020(3) C31 0.030(2) 0.0232(19) 0.042(3) -0.0061(18) -0.0099(19) -0.0055(17) C32 0.045(3) 0.026(2) 0.043(3) -0.0077(19) -0.020(2) -0.003(2) C33 0.039(3) 0.035(3) 0.069(4) -0.021(2) -0.027(3) -0.001(2) C34 0.029(2) 0.035(3) 0.069(3) -0.016(3) -0.006(2) -0.011(2) C35 0.030(2) 0.027(2) 0.052(3) -0.015(2) -0.001(2) -0.0059(17) C36 0.035(3) 0.037(3) 0.053(3) -0.014(2) -0.018(2) 0.001(2) C37 0.031(2) 0.036(3) 0.046(3) -0.011(2) -0.007(2) 0.0016(19) C38 0.044(3) 0.027(2) 0.045(3) -0.013(2) -0.013(2) 0.0010(19) C39 0.062(4) 0.025(2) 0.040(3) -0.003(2) -0.013(2) -0.006(2) C40 0.057(3) 0.034(3) 0.039(3) -0.009(2) -0.017(2) -0.002(2) C41 0.046(4) 0.119(7) 0.082(5) -0.010(5) -0.003(4) -0.008(5) C42 0.051(4) 0.113(7) 0.065(5) 0.003(4) 0.005(4) -0.016(4) C43 0.060(4) 0.113(7) 0.098(6) 0.015(5) -0.041(4) -0.043(5) C45 0.065(5) 0.078(5) 0.082(5) -0.010(4) -0.032(4) -0.031(4) C48 0.067(5) 0.053(3) 0.110(6) -0.023(4) -0.041(4) -0.016(3) C49 0.041(4) 0.072(5) 0.161(10) -0.022(5) -0.021(5) -0.011(4) C50 0.063(6) 0.080(6) 0.182(12) -0.019(7) -0.050(6) 0.013(5) C51 0.072(6) 0.072(5) 0.163(11) -0.030(6) -0.031(6) 0.006(4) C52 0.064(5) 0.066(5) 0.135(9) -0.042(5) -0.014(5) 0.001(4) O1 0.049(3) 0.078(3) 0.061(3) -0.001(2) -0.011(2) -0.019(2) O2 0.055(3) 0.050(2) 0.100(4) -0.022(3) -0.032(3) -0.014(2) O3 0.042(2) 0.054(3) 0.092(4) -0.012(2) -0.019(2) -0.0042(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C34 2.030(6) . ? Fe1 C37 2.032(6) . ? Fe1 C36 2.033(5) . ? Fe1 C39 2.040(5) . ? Fe1 C35 2.042(5) . ? Fe1 C33 2.044(5) . ? Fe1 C32 2.046(5) . ? Fe1 C40 2.050(6) . ? Fe1 C38 2.051(5) . ? Fe1 C31 2.052(5) . ? Fe2 C5 2.028(6) . ? Fe2 C7 2.029(6) . ? Fe2 C8 2.033(7) . ? Fe2 C1 2.034(6) . ? Fe2 C6 2.039(6) . ? Fe2 C2 2.043(6) . ? Fe2 C10 2.045(6) . ? Fe2 C4 2.047(6) . ? Fe2 C9 2.048(6) . ? Fe2 C3 2.048(6) . ? Fe3 C22 2.038(5) . ? Fe3 C28 2.041(6) . ? Fe3 C26 2.043(5) . ? Fe3 C23 2.045(5) . ? Fe3 C25 2.046(6) . ? Fe3 C30 2.047(6) . ? Fe3 C24 2.052(6) . ? Fe3 C29 2.054(6) . ? Fe3 C27 2.058(7) . ? Fe3 C21 2.061(5) . ? Fe4 C13 2.002(10) . ? Fe4 C18 2.010(7) . ? Fe4 C12 2.014(7) . ? Fe4 C15 2.021(7) . ? Fe4 C17 2.023(9) . ? Fe4 C19 2.037(7) . ? Fe4 C14 2.039(8) . ? Fe4 C11 2.040(6) . ? Fe4 C20 2.046(8) . ? Fe4 C16 2.048(8) . ? Ni1 S5 2.2025(15) . ? Ni1 S8 2.2106(16) . ? Ni1 S6 2.2336(16) . ? Ni1 S7 2.2348(14) . ? Ni1 Ni2 2.9679(12) . ? Ni2 S5 2.2134(16) 2_766 ? Ni2 S5 2.2134(15) . ? Ni2 S8 2.2259(13) . ? Ni2 S8 2.2259(13) 2_766 ? Ni2 Ni1 2.9680(12) 2_766 ? Sn1 C1 2.128(5) . ? Sn1 S2 2.4274(15) . ? Sn1 S1 2.4279(16) 2_766 ? Sn1 S5 2.4413(14) . ? Sn2 C11 2.129(6) . ? Sn2 S6 2.3725(13) . ? Sn2 S2 2.3913(15) . ? Sn2 S3 2.3932(17) . ? Sn3 C21 2.107(5) . ? Sn3 S7 2.3610(13) . ? Sn3 S4 2.3953(16) . ? Sn3 S3 2.4026(14) . ? Sn4 C31 2.127(5) . ? Sn4 S4 2.3974(14) . ? Sn4 S1 2.4063(18) . ? Sn4 S8 2.4371(15) . ? S1 Sn1 2.4279(16) 2_766 ? S6 Na1 2.854(3) . ? S7 Na1 3.018(3) . ? Na1 O2 2.253(5) . ? Na1 O1 2.312(6) . ? Na1 O3 2.319(6) . ? Na1 O4 2.456(10) . ? C1 C2 1.424(8) . ? C1 C5 1.434(7) . ? C2 C3 1.426(8) . ? C2 H2 0.9500 . ? C3 C4 1.408(9) . ? C3 H3 0.9500 . ? C4 C5 1.431(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.423(9) . ? C6 C10 1.423(9) . ? C6 H6 0.9500 . ? C7 C8 1.410(9) . ? C7 H7 0.9500 . ? C8 C9 1.430(9) . ? C8 H8 0.9500 . ? C9 C10 1.414(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C15 1.395(11) . ? C11 C12 1.437(11) . ? C12 C13 1.398(14) . ? C12 H12 0.9500 . ? C13 C14 1.325(16) . ? C13 H13 0.9500 . ? C14 C15 1.461(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.358(15) . ? C16 C20 1.398(14) . ? C16 H16 0.9500 . ? C17 C18 1.473(15) . ? C17 H17 0.9500 . ? C18 C19 1.372(15) . ? C18 H18 0.9500 . ? C19 C20 1.435(13) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C25 1.431(8) . ? C21 C22 1.431(7) . ? C22 C23 1.426(8) . ? C22 H22 0.9500 . ? C23 C24 1.404(9) . ? C23 H23 0.9500 . ? C24 C25 1.424(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.408(10) . ? C26 C27 1.429(9) . ? C26 H26 0.9500 . ? C27 C28 1.443(10) . ? C27 H27 0.9500 . ? C28 C29 1.403(12) . ? C28 H28 0.9500 . ? C29 C30 1.419(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.425(7) . ? C31 C35 1.427(8) . ? C32 C33 1.436(8) . ? C32 H32 0.9500 . ? C33 C34 1.417(10) . ? C33 H33 0.9500 . ? C34 C35 1.415(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C40 1.416(9) . ? C36 C37 1.430(8) . ? C36 H36 0.9500 . ? C37 C38 1.411(8) . ? C37 H37 0.9500 . ? C38 C39 1.393(9) . ? C38 H38 0.9500 . ? C39 C40 1.436(8) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 O1 1.436(8) . ? C41 C42 1.468(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C44B 1.496(13) . ? C42 C44A 1.539(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O1 1.410(8) . ? C43 C44A 1.443(11) . ? C43 C44B 1.466(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45 O2 1.434(8) . ? C45 C46A 1.442(12) . ? C45 C46B 1.543(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46A C47A 1.461(13) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A C48 1.516(13) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C46B C47B 1.481(12) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B C48 1.480(11) . ? C47B H47A 0.9900 . ? C47B H47B 0.9900 . ? C48 O2 1.380(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O3 1.424(8) . ? C49 C50 1.506(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.483(11) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.467(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O3 1.416(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C55A O5A 1.406(13) . ? C55A C56A 1.503(13) . ? C55A H55A 0.9900 . ? C55A H55B 0.9900 . ? C56A C57A 1.521(13) . ? C56A H56A 0.9900 . ? C56A H56B 0.9900 . ? C57A C58A 1.442(13) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C58A O5A 1.370(14) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C59A O6A 1.389(12) . ? C59A C60A 1.517(14) . ? C59A H59A 0.9900 . ? C59A H59B 0.9900 . ? C60A C61A 1.46(3) . ? C60A H60A 0.9900 . ? C60A H60B 0.9900 . ? C61A C62A 1.480(12) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? C62A O6A 1.393(12) . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? O4 C54B 1.201(16) . ? O4 C54A 1.448(18) . ? C53A C54A 1.661(18) 2_666 ? C53A C54B 1.636(19) . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C54A C54B 0.621(18) . ? C54A H54A 0.9900 . ? C54A H54B 0.9900 . ? C54B H54C 0.9900 . ? C54B H54D 0.9900 . ? 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 C34 Fe1 C37 165.7(2) . . ? C34 Fe1 C36 150.8(3) . . ? C37 Fe1 C36 41.2(2) . . ? C34 Fe1 C39 106.7(3) . . ? C37 Fe1 C39 67.7(2) . . ? C36 Fe1 C39 68.6(2) . . ? C34 Fe1 C35 40.7(2) . . ? C37 Fe1 C35 152.8(2) . . ? C36 Fe1 C35 118.9(2) . . ? C39 Fe1 C35 129.4(2) . . ? C34 Fe1 C33 40.7(3) . . ? C37 Fe1 C33 128.3(3) . . ? C36 Fe1 C33 168.1(3) . . ? C39 Fe1 C33 115.2(2) . . ? C35 Fe1 C33 68.3(2) . . ? C34 Fe1 C32 69.0(3) . . ? C37 Fe1 C32 108.4(2) . . ? C36 Fe1 C32 130.2(2) . . ? C39 Fe1 C32 148.6(2) . . ? C35 Fe1 C32 68.5(2) . . ? C33 Fe1 C32 41.1(2) . . ? C34 Fe1 C40 116.8(3) . . ? C37 Fe1 C40 68.4(3) . . ? C36 Fe1 C40 40.6(3) . . ? C39 Fe1 C40 41.1(2) . . ? C35 Fe1 C40 109.2(2) . . ? C33 Fe1 C40 149.1(3) . . ? C32 Fe1 C40 169.0(2) . . ? C34 Fe1 C38 127.0(2) . . ? C37 Fe1 C38 40.5(2) . . ? C36 Fe1 C38 68.8(2) . . ? C39 Fe1 C38 39.8(2) . . ? C35 Fe1 C38 166.0(2) . . ? C33 Fe1 C38 106.4(2) . . ? C32 Fe1 C38 116.6(2) . . ? C40 Fe1 C38 68.3(2) . . ? C34 Fe1 C31 68.8(2) . . ? C37 Fe1 C31 119.1(2) . . ? C36 Fe1 C31 109.9(2) . . ? C39 Fe1 C31 168.8(2) . . ? C35 Fe1 C31 40.8(2) . . ? C33 Fe1 C31 68.7(2) . . ? C32 Fe1 C31 40.7(2) . . ? C40 Fe1 C31 130.7(2) . . ? C38 Fe1 C31 151.0(2) . . ? C5 Fe2 C7 155.8(3) . . ? C5 Fe2 C8 162.3(2) . . ? C7 Fe2 C8 40.6(3) . . ? C5 Fe2 C1 41.4(2) . . ? C7 Fe2 C1 120.3(2) . . ? C8 Fe2 C1 154.6(2) . . ? C5 Fe2 C6 120.6(3) . . ? C7 Fe2 C6 40.9(3) . . ? C8 Fe2 C6 68.8(3) . . ? C1 Fe2 C6 108.0(2) . . ? C5 Fe2 C2 68.8(2) . . ? C7 Fe2 C2 107.8(3) . . ? C8 Fe2 C2 119.4(3) . . ? C1 Fe2 C2 40.9(2) . . ? C6 Fe2 C2 126.4(2) . . ? C5 Fe2 C10 107.9(3) . . ? C7 Fe2 C10 68.5(3) . . ? C8 Fe2 C10 68.5(3) . . ? C1 Fe2 C10 126.4(2) . . ? C6 Fe2 C10 40.8(3) . . ? C2 Fe2 C10 164.1(2) . . ? C5 Fe2 C4 41.1(3) . . ? C7 Fe2 C4 161.8(3) . . ? C8 Fe2 C4 124.5(3) . . ? C1 Fe2 C4 69.2(2) . . ? C6 Fe2 C4 155.5(3) . . ? C2 Fe2 C4 68.2(2) . . ? C10 Fe2 C4 120.2(3) . . ? C5 Fe2 C9 125.1(2) . . ? C7 Fe2 C9 68.6(3) . . ? C8 Fe2 C9 41.0(3) . . ? C1 Fe2 C9 163.3(2) . . ? C6 Fe2 C9 68.6(2) . . ? C2 Fe2 C9 154.2(2) . . ? C10 Fe2 C9 40.4(2) . . ? C4 Fe2 C9 106.8(2) . . ? C5 Fe2 C3 68.7(3) . . ? C7 Fe2 C3 125.3(3) . . ? C8 Fe2 C3 106.5(3) . . ? C1 Fe2 C3 69.0(3) . . ? C6 Fe2 C3 163.3(3) . . ? C2 Fe2 C3 40.8(2) . . ? C10 Fe2 C3 154.0(2) . . ? C4 Fe2 C3 40.2(3) . . ? C9 Fe2 C3 119.1(3) . . ? C22 Fe3 C28 125.5(3) . . ? C22 Fe3 C26 123.1(2) . . ? C28 Fe3 C26 68.1(2) . . ? C22 Fe3 C23 40.9(2) . . ? C28 Fe3 C23 108.2(2) . . ? C26 Fe3 C23 158.9(3) . . ? C22 Fe3 C25 68.5(2) . . ? C28 Fe3 C25 155.5(3) . . ? C26 Fe3 C25 124.3(2) . . ? C23 Fe3 C25 68.0(2) . . ? C22 Fe3 C30 158.0(2) . . ? C28 Fe3 C30 67.5(3) . . ? C26 Fe3 C30 40.3(3) . . ? C23 Fe3 C30 159.4(3) . . ? C25 Fe3 C30 107.1(3) . . ? C22 Fe3 C24 68.4(2) . . ? C28 Fe3 C24 120.7(2) . . ? C26 Fe3 C24 160.1(3) . . ? C23 Fe3 C24 40.1(3) . . ? C25 Fe3 C24 40.7(2) . . ? C30 Fe3 C24 123.2(3) . . ? C22 Fe3 C29 160.7(3) . . ? C28 Fe3 C29 40.1(3) . . ? C26 Fe3 C29 68.3(2) . . ? C23 Fe3 C29 123.2(2) . . ? C25 Fe3 C29 120.2(3) . . ? C30 Fe3 C29 40.5(3) . . ? C24 Fe3 C29 106.1(3) . . ? C22 Fe3 C27 108.5(3) . . ? C28 Fe3 C27 41.2(3) . . ? C26 Fe3 C27 40.8(3) . . ? C23 Fe3 C27 122.6(3) . . ? C25 Fe3 C27 161.4(2) . . ? C30 Fe3 C27 68.4(3) . . ? C24 Fe3 C27 157.0(3) . . ? C29 Fe3 C27 68.9(3) . . ? C22 Fe3 C21 40.8(2) . . ? C28 Fe3 C21 162.5(3) . . ? C26 Fe3 C21 108.4(2) . . ? C23 Fe3 C21 68.5(2) . . ? C25 Fe3 C21 40.8(2) . . ? C30 Fe3 C21 121.8(2) . . ? C24 Fe3 C21 68.6(2) . . ? C29 Fe3 C21 156.3(3) . . ? C27 Fe3 C21 125.0(3) . . ? C13 Fe4 C18 107.0(5) . . ? C13 Fe4 C12 40.7(4) . . ? C18 Fe4 C12 122.3(5) . . ? C13 Fe4 C15 68.7(5) . . ? C18 Fe4 C15 160.0(4) . . ? C12 Fe4 C15 68.0(5) . . ? C13 Fe4 C17 127.7(6) . . ? C18 Fe4 C17 42.8(4) . . ? C12 Fe4 C17 110.4(5) . . ? C15 Fe4 C17 154.8(4) . . ? C13 Fe4 C19 121.1(4) . . ? C18 Fe4 C19 39.6(4) . . ? C12 Fe4 C19 156.9(4) . . ? C15 Fe4 C19 124.6(4) . . ? C17 Fe4 C19 67.0(5) . . ? C13 Fe4 C14 38.3(5) . . ? C18 Fe4 C14 122.6(4) . . ? C12 Fe4 C14 66.3(5) . . ? C15 Fe4 C14 42.2(4) . . ? C17 Fe4 C14 162.2(5) . . ? C19 Fe4 C14 108.6(4) . . ? C13 Fe4 C11 69.6(3) . . ? C18 Fe4 C11 158.5(4) . . ? C12 Fe4 C11 41.5(3) . . ? C15 Fe4 C11 40.2(3) . . ? C17 Fe4 C11 121.5(4) . . ? C19 Fe4 C11 160.2(4) . . ? C14 Fe4 C11 68.6(3) . . ? C13 Fe4 C20 155.8(5) . . ? C18 Fe4 C20 69.4(5) . . ? C12 Fe4 C20 161.1(3) . . ? C15 Fe4 C20 106.1(5) . . ? C17 Fe4 C20 66.7(6) . . ? C19 Fe4 C20 41.1(4) . . ? C14 Fe4 C20 122.3(5) . . ? C11 Fe4 C20 122.5(4) . . ? C13 Fe4 C16 163.1(5) . . ? C18 Fe4 C16 69.7(4) . . ? C12 Fe4 C16 126.0(4) . . ? C15 Fe4 C16 120.1(4) . . ? C17 Fe4 C16 39.0(4) . . ? C19 Fe4 C16 67.6(4) . . ? C14 Fe4 C16 157.3(5) . . ? C11 Fe4 C16 107.0(3) . . ? C20 Fe4 C16 39.9(4) . . ? S5 Ni1 S8 79.25(5) . . ? S5 Ni1 S6 93.01(6) . . ? S8 Ni1 S6 171.25(5) . . ? S5 Ni1 S7 174.16(5) . . ? S8 Ni1 S7 95.25(5) . . ? S6 Ni1 S7 92.33(6) . . ? S5 Ni1 Ni2 47.93(5) . . ? S8 Ni1 Ni2 48.23(4) . . ? S6 Ni1 Ni2 128.28(4) . . ? S7 Ni1 Ni2 129.12(5) . . ? S5 Ni2 S5 179.998(1) 2_766 . ? S5 Ni2 S8 101.31(5) 2_766 . ? S5 Ni2 S8 78.69(5) . . ? S5 Ni2 S8 78.69(5) 2_766 2_766 ? S5 Ni2 S8 101.31(5) . 2_766 ? S8 Ni2 S8 179.998(1) . 2_766 ? S5 Ni2 Ni1 132.38(4) 2_766 . ? S5 Ni2 Ni1 47.61(4) . . ? S8 Ni2 Ni1 47.79(4) . . ? S8 Ni2 Ni1 132.21(4) 2_766 . ? S5 Ni2 Ni1 47.62(4) 2_766 2_766 ? S5 Ni2 Ni1 132.39(4) . 2_766 ? S8 Ni2 Ni1 132.21(4) . 2_766 ? S8 Ni2 Ni1 47.79(4) 2_766 2_766 ? Ni1 Ni2 Ni1 180.0 . 2_766 ? C1 Sn1 S2 122.07(15) . . ? C1 Sn1 S1 98.36(15) . 2_766 ? S2 Sn1 S1 94.52(6) . 2_766 ? C1 Sn1 S5 110.62(15) . . ? S2 Sn1 S5 118.76(5) . . ? S1 Sn1 S5 107.09(5) 2_766 . ? C11 Sn2 S6 116.82(16) . . ? C11 Sn2 S2 111.0(2) . . ? S6 Sn2 S2 98.27(5) . . ? C11 Sn2 S3 102.76(19) . . ? S6 Sn2 S3 118.14(5) . . ? S2 Sn2 S3 109.90(6) . . ? C21 Sn3 S7 116.81(13) . . ? C21 Sn3 S4 103.45(16) . . ? S7 Sn3 S4 103.85(5) . . ? C21 Sn3 S3 104.09(15) . . ? S7 Sn3 S3 117.48(5) . . ? S4 Sn3 S3 110.31(6) . . ? C31 Sn4 S4 117.33(14) . . ? C31 Sn4 S1 98.15(15) . . ? S4 Sn4 S1 101.72(6) . . ? C31 Sn4 S8 117.42(13) . . ? S4 Sn4 S8 111.11(5) . . ? S1 Sn4 S8 108.47(6) . . ? Sn4 S1 Sn1 107.69(6) . 2_766 ? Sn2 S2 Sn1 95.98(5) . . ? Sn2 S3 Sn3 107.20(5) . . ? Sn3 S4 Sn4 96.50(5) . . ? Ni1 S5 Ni2 84.46(6) . . ? Ni1 S5 Sn1 103.02(5) . . ? Ni2 S5 Sn1 121.78(6) . . ? Ni1 S6 Sn2 104.71(6) . . ? Ni1 S6 Na1 94.09(7) . . ? Sn2 S6 Na1 117.19(7) . . ? Ni1 S7 Sn3 100.81(5) . . ? Ni1 S7 Na1 89.74(7) . . ? Sn3 S7 Na1 123.57(7) . . ? Ni1 S8 Ni2 83.98(5) . . ? Ni1 S8 Sn4 106.15(6) . . ? Ni2 S8 Sn4 116.80(6) . . ? O2 Na1 O1 92.2(2) . . ? O2 Na1 O3 97.6(2) . . ? O1 Na1 O3 87.0(2) . . ? O2 Na1 O4 81.1(3) . . ? O1 Na1 O4 169.0(3) . . ? O3 Na1 O4 85.3(3) . . ? O2 Na1 S6 153.6(2) . . ? O1 Na1 S6 107.33(16) . . ? O3 Na1 S6 100.97(15) . . ? O4 Na1 S6 81.9(2) . . ? O2 Na1 S7 93.42(17) . . ? O1 Na1 S7 99.21(15) . . ? O3 Na1 S7 167.18(16) . . ? O4 Na1 S7 89.9(3) . . ? S6 Na1 S7 66.52(6) . . ? C2 C1 C5 107.2(5) . . ? C2 C1 Fe2 69.9(3) . . ? C5 C1 Fe2 69.1(3) . . ? C2 C1 Sn1 128.9(4) . . ? C5 C1 Sn1 123.8(4) . . ? Fe2 C1 Sn1 128.5(3) . . ? C1 C2 C3 108.5(5) . . ? C1 C2 Fe2 69.2(3) . . ? C3 C2 Fe2 69.8(3) . . ? C1 C2 H2 125.7 . . ? C3 C2 H2 125.7 . . ? Fe2 C2 H2 126.8 . . ? C4 C3 C2 108.1(6) . . ? C4 C3 Fe2 69.8(3) . . ? C2 C3 Fe2 69.4(3) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe2 C3 H3 126.4 . . ? C3 C4 C5 108.3(5) . . ? C3 C4 Fe2 70.0(4) . . ? C5 C4 Fe2 68.7(3) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe2 C4 H4 127.0 . . ? C4 C5 C1 107.9(5) . . ? C4 C5 Fe2 70.2(4) . . ? C1 C5 Fe2 69.5(3) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe2 C5 H5 125.8 . . ? C7 C6 C10 107.3(5) . . ? C7 C6 Fe2 69.2(3) . . ? C10 C6 Fe2 69.8(3) . . ? C7 C6 H6 126.3 . . ? C10 C6 H6 126.3 . . ? Fe2 C6 H6 126.3 . . ? C8 C7 C6 108.6(6) . . ? C8 C7 Fe2 69.8(4) . . ? C6 C7 Fe2 69.9(3) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? Fe2 C7 H7 126.1 . . ? C7 C8 C9 107.9(6) . . ? C7 C8 Fe2 69.6(4) . . ? C9 C8 Fe2 70.1(4) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe2 C8 H8 125.9 . . ? C10 C9 C8 107.7(6) . . ? C10 C9 Fe2 69.7(3) . . ? C8 C9 Fe2 68.9(4) . . ? C10 C9 H9 126.2 . . ? C8 C9 H9 126.2 . . ? Fe2 C9 H9 126.8 . . ? C9 C10 C6 108.5(5) . . ? C9 C10 Fe2 69.9(3) . . ? C6 C10 Fe2 69.4(3) . . ? C9 C10 H10 125.7 . . ? C6 C10 H10 125.7 . . ? Fe2 C10 H10 126.5 . . ? C15 C11 C12 105.7(7) . . ? C15 C11 Fe4 69.2(4) . . ? C12 C11 Fe4 68.3(4) . . ? C15 C11 Sn2 129.4(6) . . ? C12 C11 Sn2 124.5(6) . . ? Fe4 C11 Sn2 121.2(3) . . ? C13 C12 C11 109.0(10) . . ? C13 C12 Fe4 69.2(5) . . ? C11 C12 Fe4 70.2(4) . . ? C13 C12 H12 125.5 . . ? C11 C12 H12 125.5 . . ? Fe4 C12 H12 126.7 . . ? C14 C13 C12 108.9(9) . . ? C14 C13 Fe4 72.4(6) . . ? C12 C13 Fe4 70.1(5) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Fe4 C13 H13 123.6 . . ? C13 C14 C15 109.0(9) . . ? C13 C14 Fe4 69.4(6) . . ? C15 C14 Fe4 68.3(4) . . ? C13 C14 H14 125.5 . . ? C15 C14 H14 125.5 . . ? Fe4 C14 H14 128.5 . . ? C11 C15 C14 107.2(9) . . ? C11 C15 Fe4 70.6(4) . . ? C14 C15 Fe4 69.5(4) . . ? C11 C15 H15 126.4 . . ? C14 C15 H15 126.4 . . ? Fe4 C15 H15 125.0 . . ? C17 C16 C20 108.5(9) . . ? C17 C16 Fe4 69.5(6) . . ? C20 C16 Fe4 69.9(5) . . ? C17 C16 H16 125.7 . . ? C20 C16 H16 125.7 . . ? Fe4 C16 H16 126.4 . . ? C16 C17 C18 110.0(10) . . ? C16 C17 Fe4 71.5(5) . . ? C18 C17 Fe4 68.1(5) . . ? C16 C17 H17 125.0 . . ? C18 C17 H17 125.0 . . ? Fe4 C17 H17 127.0 . . ? C19 C18 C17 104.0(10) . . ? C19 C18 Fe4 71.3(5) . . ? C17 C18 Fe4 69.1(4) . . ? C19 C18 H18 128.0 . . ? C17 C18 H18 128.0 . . ? Fe4 C18 H18 123.4 . . ? C18 C19 C20 110.6(9) . . ? C18 C19 Fe4 69.1(5) . . ? C20 C19 Fe4 69.8(4) . . ? C18 C19 H19 124.7 . . ? C20 C19 H19 124.7 . . ? Fe4 C19 H19 128.1 . . ? C16 C20 C19 106.6(10) . . ? C16 C20 Fe4 70.1(5) . . ? C19 C20 Fe4 69.1(5) . . ? C16 C20 H20 126.7 . . ? C19 C20 H20 126.7 . . ? Fe4 C20 H20 125.7 . . ? C25 C21 C22 106.9(4) . . ? C25 C21 Fe3 69.0(3) . . ? C22 C21 Fe3 68.7(3) . . ? C25 C21 Sn3 128.6(4) . . ? C22 C21 Sn3 123.7(4) . . ? Fe3 C21 Sn3 119.2(2) . . ? C23 C22 C21 108.0(5) . . ? C23 C22 Fe3 69.8(3) . . ? C21 C22 Fe3 70.4(3) . . ? C23 C22 H22 126.0 . . ? C21 C22 H22 126.0 . . ? Fe3 C22 H22 125.3 . . ? C24 C23 C22 108.7(5) . . ? C24 C23 Fe3 70.2(3) . . ? C22 C23 Fe3 69.3(3) . . ? C24 C23 H23 125.7 . . ? C22 C23 H23 125.7 . . ? Fe3 C23 H23 126.4 . . ? C23 C24 C25 107.9(5) . . ? C23 C24 Fe3 69.7(3) . . ? C25 C24 Fe3 69.4(3) . . ? C23 C24 H24 126.1 . . ? C25 C24 H24 126.1 . . ? Fe3 C24 H24 126.4 . . ? C24 C25 C21 108.6(5) . . ? C24 C25 Fe3 69.9(3) . . ? C21 C25 Fe3 70.2(3) . . ? C24 C25 H25 125.7 . . ? C21 C25 H25 125.7 . . ? Fe3 C25 H25 125.8 . . ? C30 C26 C27 108.8(5) . . ? C30 C26 Fe3 70.0(3) . . ? C27 C26 Fe3 70.2(3) . . ? C30 C26 H26 125.6 . . ? C27 C26 H26 125.6 . . ? Fe3 C26 H26 125.8 . . ? C26 C27 C28 105.5(6) . . ? C26 C27 Fe3 69.0(4) . . ? C28 C27 Fe3 68.8(4) . . ? C26 C27 H27 127.2 . . ? C28 C27 H27 127.2 . . ? Fe3 C27 H27 126.5 . . ? C29 C28 C27 109.7(6) . . ? C29 C28 Fe3 70.5(4) . . ? C27 C28 Fe3 70.0(3) . . ? C29 C28 H28 125.1 . . ? C27 C28 H28 125.1 . . ? Fe3 C28 H28 126.0 . . ? C28 C29 C30 107.1(6) . . ? C28 C29 Fe3 69.5(4) . . ? C30 C29 Fe3 69.5(3) . . ? C28 C29 H29 126.4 . . ? C30 C29 H29 126.4 . . ? Fe3 C29 H29 126.2 . . ? C26 C30 C29 108.8(7) . . ? C26 C30 Fe3 69.7(3) . . ? C29 C30 Fe3 70.0(3) . . ? C26 C30 H30 125.6 . . ? C29 C30 H30 125.6 . . ? Fe3 C30 H30 126.3 . . ? C32 C31 C35 107.7(4) . . ? C32 C31 Fe1 69.4(3) . . ? C35 C31 Fe1 69.3(3) . . ? C32 C31 Sn4 123.2(4) . . ? C35 C31 Sn4 129.0(4) . . ? Fe1 C31 Sn4 123.4(2) . . ? C31 C32 C33 107.7(5) . . ? C31 C32 Fe1 69.9(3) . . ? C33 C32 Fe1 69.4(3) . . ? C31 C32 H32 126.2 . . ? C33 C32 H32 126.2 . . ? Fe1 C32 H32 126.1 . . ? C34 C33 C32 108.0(5) . . ? C34 C33 Fe1 69.1(3) . . ? C32 C33 Fe1 69.5(3) . . ? C34 C33 H33 126.0 . . ? C32 C33 H33 126.0 . . ? Fe1 C33 H33 126.9 . . ? C35 C34 C33 108.2(5) . . ? C35 C34 Fe1 70.1(3) . . ? C33 C34 Fe1 70.2(3) . . ? C35 C34 H34 125.9 . . ? C33 C34 H34 125.9 . . ? Fe1 C34 H34 125.4 . . ? C34 C35 C31 108.5(5) . . ? C34 C35 Fe1 69.2(3) . . ? C31 C35 Fe1 70.0(3) . . ? C34 C35 H35 125.8 . . ? C31 C35 H35 125.8 . . ? Fe1 C35 H35 126.7 . . ? C40 C36 C37 107.4(5) . . ? C40 C36 Fe1 70.4(3) . . ? C37 C36 Fe1 69.4(3) . . ? C40 C36 H36 126.3 . . ? C37 C36 H36 126.3 . . ? Fe1 C36 H36 125.5 . . ? C38 C37 C36 108.6(5) . . ? C38 C37 Fe1 70.5(3) . . ? C36 C37 Fe1 69.4(3) . . ? C38 C37 H37 125.7 . . ? C36 C37 H37 125.7 . . ? Fe1 C37 H37 125.9 . . ? C39 C38 C37 107.9(5) . . ? C39 C38 Fe1 69.7(3) . . ? C37 C38 Fe1 69.0(3) . . ? C39 C38 H38 126.0 . . ? C37 C38 H38 126.0 . . ? Fe1 C38 H38 126.8 . . ? C38 C39 C40 108.9(5) . . ? C38 C39 Fe1 70.5(3) . . ? C40 C39 Fe1 69.8(3) . . ? C38 C39 H39 125.5 . . ? C40 C39 H39 125.5 . . ? Fe1 C39 H39 125.7 . . ? C36 C40 C39 107.2(5) . . ? C36 C40 Fe1 69.0(3) . . ? C39 C40 Fe1 69.1(3) . . ? C36 C40 H40 126.4 . . ? C39 C40 H40 126.4 . . ? Fe1 C40 H40 127.0 . . ? O1 C41 C42 105.3(6) . . ? O1 C41 H41A 110.7 . . ? C42 C41 H41A 110.7 . . ? O1 C41 H41B 110.7 . . ? C42 C41 H41B 110.7 . . ? H41A C41 H41B 108.8 . . ? C41 C42 C44B 109.4(8) . . ? C41 C42 C44A 102.4(8) . . ? C41 C42 H42A 111.3 . . ? C44B C42 H42A 78.6 . . ? C44A C42 H42A 111.3 . . ? C41 C42 H42B 111.3 . . ? C44B C42 H42B 131.4 . . ? C44A C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? O1 C43 C44A 108.3(8) . . ? O1 C43 C44B 109.3(9) . . ? O1 C43 H43A 110.0 . . ? C44A C43 H43A 110.0 . . ? C44B C43 H43A 134.8 . . ? O1 C43 H43B 110.0 . . ? C44A C43 H43B 110.0 . . ? C44B C43 H43B 77.6 . . ? H43A C43 H43B 108.4 . . ? C43 C44A C42 100.6(8) . . ? C43 C44A H44A 111.7 . . ? C42 C44A H44A 111.7 . . ? C43 C44A H44B 111.7 . . ? C42 C44A H44B 111.7 . . ? H44A C44A H44B 109.4 . . ? C43 C44B C42 101.5(10) . . ? C43 C44B H44C 111.5 . . ? C42 C44B H44C 111.5 . . ? C43 C44B H44D 111.5 . . ? C42 C44B H44D 111.5 . . ? H44C C44B H44D 109.3 . . ? O2 C45 C46A 108.3(9) . . ? O2 C45 C46B 105.3(7) . . ? O2 C45 H45A 110.0 . . ? C46A C45 H45A 110.0 . . ? C46B C45 H45A 131.8 . . ? O2 C45 H45B 110.0 . . ? C46A C45 H45B 110.0 . . ? C46B C45 H45B 88.3 . . ? H45A C45 H45B 108.4 . . ? C45 C46A C47A 101.8(12) . . ? C45 C46A H46A 111.4 . . ? C47A C46A H46A 111.4 . . ? C45 C46A H46B 111.4 . . ? C47A C46A H46B 111.4 . . ? H46A C46A H46B 109.3 . . ? C46A C47A C48 109.9(12) . . ? C46A C47A H47C 109.7 . . ? C48 C47A H47C 109.7 . . ? C46A C47A H47D 109.7 . . ? C48 C47A H47D 109.7 . . ? H47C C47A H47D 108.2 . . ? C47B C46B C45 109.5(10) . . ? C47B C46B H46C 109.8 . . ? C45 C46B H46C 109.8 . . ? C47B C46B H46D 109.8 . . ? C45 C46B H46D 109.8 . . ? H46C C46B H46D 108.2 . . ? C48 C47B C46B 101.0(9) . . ? C48 C47B H47A 111.6 . . ? C46B C47B H47A 111.6 . . ? C48 C47B H47B 111.6 . . ? C46B C47B H47B 111.6 . . ? H47A C47B H47B 109.4 . . ? O2 C48 C47B 115.5(7) . . ? O2 C48 C47A 99.7(9) . . ? O2 C48 H48A 111.8 . . ? C47B C48 H48A 80.4 . . ? C47A C48 H48A 111.8 . . ? O2 C48 H48B 111.8 . . ? C47B C48 H48B 122.9 . . ? C47A C48 H48B 111.8 . . ? H48A C48 H48B 109.6 . . ? O3 C49 C50 103.6(7) . . ? O3 C49 H49A 111.0 . . ? C50 C49 H49A 111.0 . . ? O3 C49 H49B 111.0 . . ? C50 C49 H49B 111.0 . . ? H49A C49 H49B 109.0 . . ? C51 C50 C49 103.1(8) . . ? C51 C50 H50A 111.1 . . ? C49 C50 H50A 111.1 . . ? C51 C50 H50B 111.1 . . ? C49 C50 H50B 111.1 . . ? H50A C50 H50B 109.1 . . ? C52 C51 C50 105.3(8) . . ? C52 C51 H51A 110.7 . . ? C50 C51 H51A 110.7 . . ? C52 C51 H51B 110.7 . . ? C50 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? O3 C52 C51 108.2(8) . . ? O3 C52 H52A 110.1 . . ? C51 C52 H52A 110.1 . . ? O3 C52 H52B 110.1 . . ? C51 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C43 O1 C41 108.6(6) . . ? C43 O1 Na1 121.8(5) . . ? C41 O1 Na1 120.1(5) . . ? C48 O2 C45 108.2(5) . . ? C48 O2 Na1 120.1(4) . . ? C45 O2 Na1 130.1(4) . . ? C52 O3 C49 106.5(7) . . ? C52 O3 Na1 122.5(4) . . ? C49 O3 Na1 131.0(5) . . ? O5A C55A C56A 106.3(13) . . ? O5A C55A H55A 110.5 . . ? C56A C55A H55A 110.5 . . ? O5A C55A H55B 110.5 . . ? C56A C55A H55B 110.5 . . ? H55A C55A H55B 108.7 . . ? C55A C56A C57A 102.1(12) . . ? C55A C56A H56A 111.4 . . ? C57A C56A H56A 111.4 . . ? C55A C56A H56B 111.4 . . ? C57A C56A H56B 111.4 . . ? H56A C56A H56B 109.2 . . ? C58A C57A C56A 101.8(13) . . ? C58A C57A H57A 111.4 . . ? C56A C57A H57A 111.4 . . ? C58A C57A H57B 111.4 . . ? C56A C57A H57B 111.4 . . ? H57A C57A H57B 109.3 . . ? O5A C58A C57A 112.2(16) . . ? O5A C58A H58A 109.2 . . ? C57A C58A H58A 109.2 . . ? O5A C58A H58B 109.2 . . ? C57A C58A H58B 109.2 . . ? H58A C58A H58B 107.9 . . ? O6A C59A C60A 110.5(15) . . ? O6A C59A H59A 109.6 . . ? C60A C59A H59A 109.6 . . ? O6A C59A H59B 109.6 . . ? C60A C59A H59B 109.6 . . ? H59A C59A H59B 108.1 . . ? C61A C60A C59A 100.7(15) . . ? C61A C60A H60A 111.6 . . ? C59A C60A H60A 111.6 . . ? C61A C60A H60B 111.6 . . ? C59A C60A H60B 111.6 . . ? H60A C60A H60B 109.4 . . ? C60A C61A C62A 107.6(12) . . ? C60A C61A H61A 110.2 . . ? C62A C61A H61A 110.2 . . ? C60A C61A H61B 110.2 . . ? C62A C61A H61B 110.2 . . ? H61A C61A H61B 108.5 . . ? O6A C62A C61A 104.8(10) . . ? O6A C62A H62A 110.8 . . ? C61A C62A H62A 110.8 . . ? O6A C62A H62B 110.8 . . ? C61A C62A H62B 110.8 . . ? H62A C62A H62B 108.9 . . ? C58A O5A C55A 100.7(15) . . ? C59A O6A C62A 107.1(11) . . ? C54B O4 Na1 147.2(10) . . ? C54A O4 Na1 125.7(9) . . ? C54A C53A C54B 95.7(11) 2_666 . ? C54A C53A H53A 112.6 2_666 . ? C54B C53A H53A 112.6 . . ? C54A C53A H53B 112.6 2_666 . ? C54B C53A H53B 112.6 . . ? H53A C53A H53B 110.1 . . ? C54B C54A O4 55(2) . . ? C54B C54A H54A 118.3 . . ? O4 C54A H54A 118.3 . . ? C54B C54A H54B 118.3 . . ? O4 C54A H54B 118.3 . . ? H54A C54A H54B 115.5 . . ? C54A C54B O4 100(2) . . ? C54A C54B C53A 147(3) . . ? O4 C54B C53A 56.5(9) . . ? C54A C54B H54C 111.7 . . ? O4 C54B H54C 111.7 . . ? C53A C54B H54C 99.5 . . ? C54A C54B H54D 111.7 . . ? O4 C54B H54D 111.7 . . ? C53A C54B H54D 64.9 . . ? H54C C54B H54D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.96 _refine_diff_density_min -1.09 _refine_diff_density_rms 0.15 # Attachment '1-rev2.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 755188' #TrackingRef '1-rev2.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C10 H9 Cl3 Fe Sn' _chemical_formula_sum 'C10 H9 Cl3 Fe Sn' _chemical_formula_weight 410.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 6.8102(5) _cell_length_b 9.7487(6) _cell_length_c 18.6877(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.404(6) _cell_angle_gamma 90.00 _cell_volume 1220.29(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8759 _cell_measurement_theta_min 6.15 _cell_measurement_theta_max 54.47 _exptl_crystal_description 'thin plates' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 3.853 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDSII _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5375 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2141 _reflns_number_gt 1248 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XAREA 1.38 (Stoe 2006)' _computing_cell_refinement 'XAREA 1.38 (Stoe 2006)' _computing_data_reduction 'XAREA 1.38 (Stoe 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005) SHELXTL-NT V5.1, Bruker AXS 1999' _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^)+(0.0519P)^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_extinction_coef ? _refine_ls_number_reflns 2141 _refine_ls_number_parameters 137 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; 'For all C atoms SIMU and DELU restraints were applied' ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5402(9) 0.255(2) 0.8659(3) 0.0213(12) Uani 1 1 d U . . C2 C 0.576(2) 0.1342(16) 0.9125(6) 0.0214(19) Uani 1 1 d U . . H2 H 0.5732 0.0412 0.8971 0.026 Uiso 1 1 calc R . . C3 C 0.618(3) 0.1837(14) 0.9869(6) 0.0191(18) Uani 1 1 d U . . H3 H 0.6479 0.1300 1.0299 0.023 Uiso 1 1 calc R . . C4 C 0.606(3) 0.3290(14) 0.9820(6) 0.0222(19) Uani 1 1 d U . . H4 H 0.6303 0.3885 1.0230 0.027 Uiso 1 1 calc R . . C5 C 0.555(2) 0.3738(16) 0.9111(6) 0.020(2) Uani 1 1 d U . . H5 H 0.5337 0.4662 0.8955 0.024 Uiso 1 1 calc R . . C6 C 0.0547(10) 0.250(3) 0.8759(3) 0.0284(12) Uani 1 1 d U . . H6 H 0.0178 0.2553 0.8244 0.034 Uiso 1 1 calc R . . C7 C 0.084(3) 0.1273(16) 0.9167(6) 0.028(2) Uani 1 1 d U . . H7 H 0.0736 0.0363 0.8982 0.033 Uiso 1 1 calc R . . C8 C 0.133(2) 0.1674(13) 0.9911(6) 0.025(2) Uani 1 1 d U . . H8 H 0.1575 0.1057 1.0311 0.030 Uiso 1 1 calc R . . C9 C 0.139(2) 0.3128(13) 0.9972(6) 0.024(2) Uani 1 1 d U . . H9 H 0.1692 0.3657 1.0405 0.029 Uiso 1 1 calc R . . C10 C 0.089(3) 0.3624(16) 0.9243(6) 0.027(2) Uani 1 1 d U . . H10 H 0.0811 0.4563 0.9104 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.2296(8) 0.4370(4) 0.71907(16) 0.0297(9) Uani 1 1 d . . . Cl2 Cl 0.6560(2) 0.2522(6) 0.67424(7) 0.0287(3) Uani 1 1 d . . . Cl3 Cl 0.2322(7) 0.0642(5) 0.71801(18) 0.0296(9) Uani 1 1 d . . . Fe1 Fe 0.33923(11) 0.2508(3) 0.93504(3) 0.01688(19) Uani 1 1 d . . . Sn1 Sn 0.43458(6) 0.24976(16) 0.755422(15) 0.01975(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(2) 0.021(2) 0.0223(17) 0.000(2) 0.0042(16) -0.002(3) C2 0.020(3) 0.020(2) 0.025(3) 0.001(2) 0.005(2) 0.001(3) C3 0.016(3) 0.021(3) 0.019(2) -0.002(2) 0.000(2) 0.002(3) C4 0.023(3) 0.021(3) 0.022(2) 0.002(2) 0.002(2) -0.001(3) C5 0.019(3) 0.019(2) 0.022(2) -0.0017(19) 0.003(2) 0.000(2) C6 0.025(2) 0.028(2) 0.0311(18) -0.002(2) 0.0017(18) 0.000(3) C7 0.024(3) 0.029(3) 0.030(3) -0.003(2) 0.004(2) -0.004(3) C8 0.021(3) 0.026(3) 0.027(2) -0.001(2) 0.008(2) -0.002(3) C9 0.019(3) 0.026(3) 0.027(2) 0.000(2) 0.004(2) 0.002(3) C10 0.024(3) 0.028(3) 0.029(3) 0.001(2) 0.007(2) 0.002(3) Cl1 0.040(2) 0.025(2) 0.0236(12) 0.0032(12) 0.0031(15) 0.004(2) Cl2 0.0320(9) 0.0315(8) 0.0263(6) -0.0013(19) 0.0147(5) -0.002(3) Cl3 0.017(2) 0.026(2) 0.0471(17) -0.0133(14) 0.0096(15) -0.010(2) Fe1 0.0128(4) 0.0166(4) 0.0218(3) -0.0017(9) 0.0048(3) 0.0008(16) Sn1 0.0212(2) 0.0184(2) 0.01975(18) 0.0014(5) 0.00392(13) 0.0006(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.42(2) . ? C1 C2 1.46(2) . ? C1 Fe1 2.046(6) . ? C1 Sn1 2.060(5) . ? C2 C3 1.450(17) . ? C2 Fe1 2.080(16) . ? C2 H2 0.9500 . ? C3 C4 1.421(10) . ? C3 Fe1 2.077(15) . ? C3 H3 0.9500 . ? C4 C5 1.379(17) . ? C4 Fe1 2.020(16) . ? C4 H4 0.9500 . ? C5 Fe1 2.008(15) . ? C5 H5 0.9500 . ? C6 C7 1.41(3) . ? C6 C10 1.42(3) . ? C6 Fe1 2.050(6) . ? C6 H6 0.9500 . ? C7 C8 1.425(16) . ? C7 Fe1 2.091(17) . ? C7 H7 0.9500 . ? C8 C9 1.422(11) . ? C8 Fe1 2.067(15) . ? C8 H8 0.9500 . ? C9 C10 1.428(16) . ? C9 Fe1 2.037(15) . ? C9 H9 0.9500 . ? C10 Fe1 1.999(17) . ? C10 H10 0.9500 . ? Cl1 Sn1 2.324(5) . ? Cl2 Sn1 2.3243(13) . ? Cl3 Sn1 2.305(4) . ? 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 C5 C1 C2 108.3(4) . . ? C5 C1 Fe1 68.0(7) . . ? C2 C1 Fe1 70.5(7) . . ? C5 C1 Sn1 126.3(11) . . ? C2 C1 Sn1 124.5(11) . . ? Fe1 C1 Sn1 118.7(3) . . ? C3 C2 C1 106.6(12) . . ? C3 C2 Fe1 69.5(9) . . ? C1 C2 Fe1 68.0(7) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? Fe1 C2 H2 127.3 . . ? C4 C3 C2 105.8(12) . . ? C4 C3 Fe1 67.5(12) . . ? C2 C3 Fe1 69.7(9) . . ? C4 C3 H3 127.1 . . ? C2 C3 H3 127.1 . . ? Fe1 C3 H3 127.2 . . ? C5 C4 C3 112.2(13) . . ? C5 C4 Fe1 69.5(9) . . ? C3 C4 Fe1 71.9(12) . . ? C5 C4 H4 123.9 . . ? C3 C4 H4 123.9 . . ? Fe1 C4 H4 126.3 . . ? C4 C5 C1 107.0(12) . . ? C4 C5 Fe1 70.4(10) . . ? C1 C5 Fe1 70.9(7) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Fe1 C5 H5 123.9 . . ? C7 C6 C10 108.7(5) . . ? C7 C6 Fe1 71.7(8) . . ? C10 C6 Fe1 67.6(8) . . ? C7 C6 H6 125.7 . . ? C10 C6 H6 125.7 . . ? Fe1 C6 H6 126.6 . . ? C6 C7 C8 106.3(13) . . ? C6 C7 Fe1 68.5(8) . . ? C8 C7 Fe1 69.0(9) . . ? C6 C7 H7 126.8 . . ? C8 C7 H7 126.8 . . ? Fe1 C7 H7 127.1 . . ? C9 C8 C7 110.5(13) . . ? C9 C8 Fe1 68.6(11) . . ? C7 C8 Fe1 70.9(9) . . ? C9 C8 H8 124.8 . . ? C7 C8 H8 124.8 . . ? Fe1 C8 H8 127.4 . . ? C8 C9 C10 105.2(13) . . ? C8 C9 Fe1 70.8(11) . . ? C10 C9 Fe1 67.8(9) . . ? C8 C9 H9 127.4 . . ? C10 C9 H9 127.4 . . ? Fe1 C9 H9 125.5 . . ? C6 C10 C9 109.3(13) . . ? C6 C10 Fe1 71.5(8) . . ? C9 C10 Fe1 70.7(9) . . ? C6 C10 H10 125.4 . . ? C9 C10 H10 125.4 . . ? Fe1 C10 H10 124.0 . . ? C10 Fe1 C5 107.2(6) . . ? C10 Fe1 C4 121.4(6) . . ? C5 Fe1 C4 40.0(5) . . ? C10 Fe1 C9 41.4(5) . . ? C5 Fe1 C9 122.8(6) . . ? C4 Fe1 C9 106.4(6) . . ? C10 Fe1 C1 125.4(5) . . ? C5 Fe1 C1 41.1(6) . . ? C4 Fe1 C1 67.3(5) . . ? C9 Fe1 C1 161.3(7) . . ? C10 Fe1 C6 40.9(8) . . ? C5 Fe1 C6 122.8(6) . . ? C4 Fe1 C6 157.7(9) . . ? C9 Fe1 C6 69.2(5) . . ? C1 Fe1 C6 109.5(2) . . ? C10 Fe1 C8 67.7(6) . . ? C5 Fe1 C8 160.1(5) . . ? C4 Fe1 C8 124.7(5) . . ? C9 Fe1 C8 40.6(3) . . ? C1 Fe1 C8 157.4(7) . . ? C6 Fe1 C8 66.9(5) . . ? C10 Fe1 C3 155.4(5) . . ? C5 Fe1 C3 69.3(6) . . ? C4 Fe1 C3 40.6(3) . . ? C9 Fe1 C3 118.6(5) . . ? C1 Fe1 C3 69.0(4) . . ? C6 Fe1 C3 161.0(9) . . ? C8 Fe1 C3 106.8(6) . . ? C10 Fe1 C2 162.8(5) . . ? C5 Fe1 C2 69.8(3) . . ? C4 Fe1 C2 67.9(6) . . ? C9 Fe1 C2 154.5(5) . . ? C1 Fe1 C2 41.5(6) . . ? C6 Fe1 C2 125.5(6) . . ? C8 Fe1 C2 120.8(6) . . ? C3 Fe1 C2 40.8(5) . . ? C5 Fe1 C7 158.0(5) . . ? C4 Fe1 C7 160.8(5) . . ? C9 Fe1 C7 69.0(6) . . ? C1 Fe1 C7 122.7(5) . . ? C6 Fe1 C7 39.8(8) . . ? C8 Fe1 C7 40.1(5) . . ? C3 Fe1 C7 123.9(6) . . ? C2 Fe1 C7 107.7(6) . . ? C1 Sn1 Cl3 114.0(5) . . ? C1 Sn1 Cl1 110.8(5) . . ? C1 Sn1 Cl2 120.23(18) . . ? Cl3 Sn1 Cl2 103.47(17) . . ? Cl1 Sn1 Cl2 103.15(18) . . ? 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 C5 C1 C2 C3 -1.4(11) . . . . ? Fe1 C1 C2 C3 -59.0(11) . . . . ? Sn1 C1 C2 C3 -171.0(9) . . . . ? C5 C1 C2 Fe1 57.6(6) . . . . ? Sn1 C1 C2 Fe1 -112.0(6) . . . . ? C1 C2 C3 C4 0(2) . . . . ? Fe1 C2 C3 C4 -58.1(16) . . . . ? C1 C2 C3 Fe1 58.1(9) . . . . ? C2 C3 C4 C5 2(3) . . . . ? Fe1 C3 C4 C5 -57.9(16) . . . . ? C2 C3 C4 Fe1 59.5(14) . . . . ? C3 C4 C5 C1 -2(2) . . . . ? Fe1 C4 C5 C1 -61.8(9) . . . . ? C3 C4 C5 Fe1 59.3(18) . . . . ? C2 C1 C5 C4 2.4(11) . . . . ? Fe1 C1 C5 C4 61.5(12) . . . . ? Sn1 C1 C5 C4 171.8(10) . . . . ? C2 C1 C5 Fe1 -59.1(6) . . . . ? Sn1 C1 C5 Fe1 110.3(6) . . . . ? C10 C6 C7 C8 1.4(11) . . . . ? Fe1 C6 C7 C8 58.9(12) . . . . ? C10 C6 C7 Fe1 -57.6(6) . . . . ? C6 C7 C8 C9 -1(2) . . . . ? Fe1 C7 C8 C9 57.2(16) . . . . ? C6 C7 C8 Fe1 -58.6(10) . . . . ? C7 C8 C9 C10 1(3) . . . . ? Fe1 C8 C9 C10 59.4(13) . . . . ? C7 C8 C9 Fe1 -58.5(14) . . . . ? C7 C6 C10 C9 -0.9(12) . . . . ? Fe1 C6 C10 C9 -60.9(12) . . . . ? C7 C6 C10 Fe1 60.1(7) . . . . ? C8 C9 C10 C6 0(2) . . . . ? Fe1 C9 C10 C6 61.4(11) . . . . ? C8 C9 C10 Fe1 -61.4(15) . . . . ? C6 C10 Fe1 C5 120.5(9) . . . . ? C9 C10 Fe1 C5 -120.4(9) . . . . ? C6 C10 Fe1 C4 162.0(8) . . . . ? C9 C10 Fe1 C4 -79.0(10) . . . . ? C6 C10 Fe1 C9 -119.1(13) . . . . ? C6 C10 Fe1 C1 78.9(11) . . . . ? C9 C10 Fe1 C1 -162.1(8) . . . . ? C9 C10 Fe1 C6 119.1(13) . . . . ? C6 C10 Fe1 C8 -80.0(9) . . . . ? C9 C10 Fe1 C8 39.1(8) . . . . ? C6 C10 Fe1 C3 -161.6(13) . . . . ? C9 C10 Fe1 C3 -42.5(19) . . . . ? C6 C10 Fe1 C2 43(2) . . . . ? C9 C10 Fe1 C2 162.2(18) . . . . ? C6 C10 Fe1 C7 -36.6(8) . . . . ? C9 C10 Fe1 C7 82.5(9) . . . . ? C4 C5 Fe1 C10 118.6(9) . . . . ? C1 C5 Fe1 C10 -124.5(7) . . . . ? C1 C5 Fe1 C4 116.9(12) . . . . ? C4 C5 Fe1 C9 75.8(11) . . . . ? C1 C5 Fe1 C9 -167.3(6) . . . . ? C4 C5 Fe1 C1 -116.9(12) . . . . ? C4 C5 Fe1 C6 160.8(10) . . . . ? C1 C5 Fe1 C6 -82.3(10) . . . . ? C4 C5 Fe1 C8 47(2) . . . . ? C1 C5 Fe1 C8 163.6(15) . . . . ? C4 C5 Fe1 C3 -35.6(9) . . . . ? C1 C5 Fe1 C3 81.3(7) . . . . ? C4 C5 Fe1 C2 -79.3(10) . . . . ? C1 C5 Fe1 C2 37.6(6) . . . . ? C4 C5 Fe1 C7 -166.8(15) . . . . ? C1 C5 Fe1 C7 -49.9(19) . . . . ? C5 C4 Fe1 C10 -79.2(10) . . . . ? C3 C4 Fe1 C10 157.6(9) . . . . ? C3 C4 Fe1 C5 -123.1(15) . . . . ? C5 C4 Fe1 C9 -121.9(9) . . . . ? C3 C4 Fe1 C9 115.0(10) . . . . ? C5 C4 Fe1 C1 39.4(10) . . . . ? C3 C4 Fe1 C1 -83.7(11) . . . . ? C5 C4 Fe1 C6 -46.9(17) . . . . ? C3 C4 Fe1 C6 -170.0(7) . . . . ? C5 C4 Fe1 C8 -162.4(9) . . . . ? C3 C4 Fe1 C8 74.4(12) . . . . ? C5 C4 Fe1 C3 123.1(15) . . . . ? C5 C4 Fe1 C2 84.5(7) . . . . ? C3 C4 Fe1 C2 -38.6(9) . . . . ? C5 C4 Fe1 C7 164.9(16) . . . . ? C3 C4 Fe1 C7 42(2) . . . . ? C8 C9 Fe1 C10 116.2(14) . . . . ? C8 C9 Fe1 C5 -165.2(8) . . . . ? C10 C9 Fe1 C5 78.6(10) . . . . ? C8 C9 Fe1 C4 -124.6(10) . . . . ? C10 C9 Fe1 C4 119.1(9) . . . . ? C8 C9 Fe1 C1 167.9(7) . . . . ? C10 C9 Fe1 C1 51.7(17) . . . . ? C8 C9 Fe1 C6 78.4(12) . . . . ? C10 C9 Fe1 C6 -37.8(11) . . . . ? C10 C9 Fe1 C8 -116.2(14) . . . . ? C8 C9 Fe1 C3 -82.5(11) . . . . ? C10 C9 Fe1 C3 161.3(9) . . . . ? C8 C9 Fe1 C2 -51.7(18) . . . . ? C10 C9 Fe1 C2 -167.9(12) . . . . ? C8 C9 Fe1 C7 35.7(9) . . . . ? C10 C9 Fe1 C7 -80.5(7) . . . . ? C5 C1 Fe1 C10 74.9(8) . . . . ? C2 C1 Fe1 C10 -164.9(8) . . . . ? Sn1 C1 Fe1 C10 -45.5(13) . . . . ? C2 C1 Fe1 C5 120.2(5) . . . . ? Sn1 C1 Fe1 C5 -120.4(14) . . . . ? C5 C1 Fe1 C4 -38.4(8) . . . . ? C2 C1 Fe1 C4 81.8(8) . . . . ? Sn1 C1 Fe1 C4 -158.9(13) . . . . ? C5 C1 Fe1 C9 35.4(14) . . . . ? C2 C1 Fe1 C9 155.6(13) . . . . ? Sn1 C1 Fe1 C9 -85.1(16) . . . . ? C5 C1 Fe1 C6 117.9(10) . . . . ? C2 C1 Fe1 C6 -121.9(10) . . . . ? Sn1 C1 Fe1 C6 -2.5(13) . . . . ? C5 C1 Fe1 C8 -165.5(11) . . . . ? C2 C1 Fe1 C8 -45.3(12) . . . . ? Sn1 C1 Fe1 C8 74.1(16) . . . . ? C5 C1 Fe1 C3 -82.3(7) . . . . ? C2 C1 Fe1 C3 37.9(7) . . . . ? Sn1 C1 Fe1 C3 157.3(12) . . . . ? C5 C1 Fe1 C2 -120.2(5) . . . . ? Sn1 C1 Fe1 C2 119.4(14) . . . . ? C5 C1 Fe1 C7 160.1(8) . . . . ? C2 C1 Fe1 C7 -79.7(8) . . . . ? Sn1 C1 Fe1 C7 39.7(13) . . . . ? C7 C6 Fe1 C10 -120.1(6) . . . . ? C7 C6 Fe1 C5 161.7(8) . . . . ? C10 C6 Fe1 C5 -78.2(8) . . . . ? C7 C6 Fe1 C4 -164.3(12) . . . . ? C10 C6 Fe1 C4 -44.2(13) . . . . ? C7 C6 Fe1 C9 -81.9(8) . . . . ? C10 C6 Fe1 C9 38.2(8) . . . . ? C7 C6 Fe1 C1 118.0(9) . . . . ? C10 C6 Fe1 C1 -121.9(9) . . . . ? C7 C6 Fe1 C8 -38.0(7) . . . . ? C10 C6 Fe1 C8 82.1(8) . . . . ? C7 C6 Fe1 C3 36.0(14) . . . . ? C10 C6 Fe1 C3 156.1(13) . . . . ? C7 C6 Fe1 C2 74.3(9) . . . . ? C10 C6 Fe1 C2 -165.6(8) . . . . ? C10 C6 Fe1 C7 120.1(6) . . . . ? C9 C8 Fe1 C10 -39.9(9) . . . . ? C7 C8 Fe1 C10 82.3(7) . . . . ? C9 C8 Fe1 C5 39(2) . . . . ? C7 C8 Fe1 C5 161.3(15) . . . . ? C9 C8 Fe1 C4 73.7(12) . . . . ? C7 C8 Fe1 C4 -164.0(9) . . . . ? C7 C8 Fe1 C9 122.2(14) . . . . ? C9 C8 Fe1 C1 -169.9(7) . . . . ? C7 C8 Fe1 C1 -47.7(16) . . . . ? C9 C8 Fe1 C6 -84.5(12) . . . . ? C7 C8 Fe1 C6 37.8(11) . . . . ? C9 C8 Fe1 C3 114.6(10) . . . . ? C7 C8 Fe1 C3 -123.2(9) . . . . ? C9 C8 Fe1 C2 156.8(8) . . . . ? C7 C8 Fe1 C2 -80.9(10) . . . . ? C9 C8 Fe1 C7 -122.2(14) . . . . ? C4 C3 Fe1 C10 -51(2) . . . . ? C2 C3 Fe1 C10 -169.1(13) . . . . ? C4 C3 Fe1 C5 35.1(10) . . . . ? C2 C3 Fe1 C5 -82.7(7) . . . . ? C2 C3 Fe1 C4 -117.8(15) . . . . ? C4 C3 Fe1 C9 -81.9(11) . . . . ? C2 C3 Fe1 C9 160.3(9) . . . . ? C4 C3 Fe1 C1 79.3(11) . . . . ? C2 C3 Fe1 C1 -38.6(9) . . . . ? C4 C3 Fe1 C6 168.3(8) . . . . ? C2 C3 Fe1 C6 50.5(17) . . . . ? C4 C3 Fe1 C8 -124.2(10) . . . . ? C2 C3 Fe1 C8 118.0(9) . . . . ? C4 C3 Fe1 C2 117.8(15) . . . . ? C4 C3 Fe1 C7 -164.7(9) . . . . ? C2 C3 Fe1 C7 77.5(10) . . . . ? C3 C2 Fe1 C10 164.5(19) . . . . ? C1 C2 Fe1 C10 46(2) . . . . ? C3 C2 Fe1 C5 81.4(9) . . . . ? C1 C2 Fe1 C5 -37.3(6) . . . . ? C3 C2 Fe1 C4 38.4(8) . . . . ? C1 C2 Fe1 C4 -80.3(8) . . . . ? C3 C2 Fe1 C9 -43.4(18) . . . . ? C1 C2 Fe1 C9 -162.1(12) . . . . ? C3 C2 Fe1 C1 118.6(12) . . . . ? C3 C2 Fe1 C6 -162.1(10) . . . . ? C1 C2 Fe1 C6 79.3(11) . . . . ? C3 C2 Fe1 C8 -79.9(10) . . . . ? C1 C2 Fe1 C8 161.5(7) . . . . ? C1 C2 Fe1 C3 -118.6(12) . . . . ? C3 C2 Fe1 C7 -121.8(9) . . . . ? C1 C2 Fe1 C7 119.6(7) . . . . ? C6 C7 Fe1 C10 37.6(7) . . . . ? C8 C7 Fe1 C10 -80.7(9) . . . . ? C6 C7 Fe1 C5 -45(2) . . . . ? C8 C7 Fe1 C5 -163.0(14) . . . . ? C6 C7 Fe1 C4 161.8(17) . . . . ? C8 C7 Fe1 C4 44(2) . . . . ? C6 C7 Fe1 C9 82.2(8) . . . . ? C8 C7 Fe1 C9 -36.1(8) . . . . ? C6 C7 Fe1 C1 -81.4(10) . . . . ? C8 C7 Fe1 C1 160.3(9) . . . . ? C8 C7 Fe1 C6 -118.3(12) . . . . ? C6 C7 Fe1 C8 118.3(12) . . . . ? C6 C7 Fe1 C3 -166.7(8) . . . . ? C8 C7 Fe1 C3 75.0(10) . . . . ? C6 C7 Fe1 C2 -124.6(8) . . . . ? C8 C7 Fe1 C2 117.1(9) . . . . ? C5 C1 Sn1 Cl3 -138.3(9) . . . . ? C2 C1 Sn1 Cl3 29.4(9) . . . . ? Fe1 C1 Sn1 Cl3 -55.7(11) . . . . ? C5 C1 Sn1 Cl1 -22.1(10) . . . . ? C2 C1 Sn1 Cl1 145.6(9) . . . . ? Fe1 C1 Sn1 Cl1 60.5(11) . . . . ? C5 C1 Sn1 Cl2 98.0(9) . . . . ? C2 C1 Sn1 Cl2 -94.2(9) . . . . ? Fe1 C1 Sn1 Cl2 -179.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 0.76 _refine_diff_density_min -0.62 _refine_diff_density_rms 0.11 # start Validation Reply Form _vrf_PLAT113_1 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P21/m RESPONSE: The crystals show systematic intergrowth and pseudo- merohedral twinning. Therefore, we have performed an according twin integration and considered two individuals measured at once. >From this data set (the best we could get) it was not possible to perform the structure solution and refinement in P21/m. An absorption correction did not seem reasonable based on the poor crystal quality. ; _vrf_PLAT057_1 ; PROBLEM: Correction for Absorption Required RT(exp) RESPONSE: The crystals show systematic intergrowth and pseudo- merohedral twinning. Therefore no reliable absorption correction could have been applied. ; _vrf_PLAT029_1 ; PROBLEM: _diffrn_measured_fraction_theta_full Low RESPONSE: The crystals show systematic intergrowth and pseudo- merohedral twinning. Therefore the collected data provide only a crystal structure model and are not considered complete. ;