# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1242 data_global _publ_requested_journal 'ChemComm' _publ_contact_author ; Hiromi Tobita Department of Chemistry, Graduate School of Science, Tohoku University, Sendai 980-8578, JAPAN. ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 81-22-217-6541 ' _publ_contact_author_fax ' 81-22-217-6543 ' _publ_contact_author_email ' tobita@inorg.chem.tohoku.ac.jp ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; Synthesis and structures of heterometallic trinuclear clusters [CpFe(CO)2]2(m3-S2)W(CO)5 and Cp2Fe2(CO)3(m-CO)(m3-S)W(CO)5 and kinetic study of migration of the W(CO)5 moiety in the disulfido complex. ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 10 11:23:56 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 741.95 _chemical_formula_analytical ? _chemical_formula_sum 'C19 H10 Fe2 O9 S2 W ' _chemical_formula_moiety 'C19 H10 Fe2 O9 S2 W ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 17.174(6) _cell_length_b 7.096(4) _cell_length_c 19.452(4) _cell_angle_alpha 90 _cell_angle_beta 92.26(2) _cell_angle_gamma 90 _cell_volume 2368(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416.00 _exptl_absorpt_coefficient_mu 6.280 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.78 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 -1 2 -1 0 2 -1 1 _diffrn_reflns_number 5624 _reflns_number_total 5445 _reflns_number_gt 3508 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.055 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05506 _diffrn_orient_matrix_UB_12 -0.00195 _diffrn_orient_matrix_UB_13 0.01872 _diffrn_orient_matrix_UB_21 -0.01844 _diffrn_orient_matrix_UB_22 -0.04136 _diffrn_orient_matrix_UB_23 0.04573 _diffrn_orient_matrix_UB_31 0.00486 _diffrn_orient_matrix_UB_32 -0.13471 _diffrn_orient_matrix_UB_33 -0.01431 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'W' 'W' -0.849 6.872 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.19773(1) 0.00153(4) 0.54821(1) 0.03903(7) Uani 1.00 d . . . Fe1 Fe 0.42536(5) -0.2010(1) 0.37381(5) 0.0403(2) Uani 1.00 d . . . Fe2 Fe 0.16519(5) 0.0727(2) 0.33632(5) 0.0448(3) Uani 1.00 d . . . S1 S 0.35231(9) 0.0305(2) 0.42222(9) 0.0410(4) Uani 1.00 d . . . S2 S 0.23844(9) -0.0669(2) 0.42431(8) 0.0364(4) Uani 1.00 d . . . O1 O 0.4973(4) 0.090(1) 0.2913(4) 0.095(3) Uani 1.00 d . . . O2 O 0.3088(4) -0.306(1) 0.2692(4) 0.096(3) Uani 1.00 d . . . O3 O 0.1731(5) 0.439(1) 0.4023(4) 0.102(3) Uani 1.00 d . . . O4 O 0.2965(4) 0.161(1) 0.2524(3) 0.096(3) Uani 1.00 d . . . O5 O 0.0395(3) 0.2082(9) 0.5083(4) 0.078(2) Uani 1.00 d . . . O6 O 0.1129(4) -0.3946(9) 0.5550(4) 0.081(2) Uani 1.00 d . . . O7 O 0.3524(3) -0.191(1) 0.6108(3) 0.080(2) Uani 1.00 d . . . O8 O 0.2817(4) 0.4005(9) 0.5569(4) 0.088(2) Uani 1.00 d . . . O9 O 0.1498(4) 0.0534(10) 0.7000(3) 0.077(2) Uani 1.00 d . . . C1 C 0.4695(5) -0.028(1) 0.3238(4) 0.060(2) Uani 1.00 d . . . C2 C 0.3540(5) -0.260(1) 0.3099(4) 0.059(2) Uani 1.00 d . . . C3 C 0.1697(5) 0.293(1) 0.3774(5) 0.063(3) Uani 1.00 d . . . C4 C 0.2472(5) 0.124(1) 0.2867(4) 0.062(2) Uani 1.00 d . . . C5 C 0.0966(4) 0.132(1) 0.5197(4) 0.053(2) Uani 1.00 d . . . C6 C 0.1436(4) -0.255(1) 0.5496(4) 0.051(2) Uani 1.00 d . . . C7 C 0.2979(4) -0.125(1) 0.5854(4) 0.052(2) Uani 1.00 d . . . C8 C 0.2521(4) 0.258(1) 0.5516(4) 0.056(2) Uani 1.00 d . . . C9 C 0.1683(5) 0.0333(10) 0.6446(4) 0.051(2) Uani 1.00 d . . . C10 C 0.4553(9) -0.480(1) 0.3828(8) 0.106(5) Uani 1.00 d . . . C11 C 0.4147(7) -0.428(2) 0.4396(10) 0.114(5) Uani 1.00 d . . . C12 C 0.4581(9) -0.298(2) 0.4722(5) 0.099(4) Uani 1.00 d . . . C13 C 0.5231(6) -0.262(1) 0.4378(6) 0.079(3) Uani 1.00 d . . . C14 C 0.5209(6) -0.380(2) 0.3821(5) 0.080(3) Uani 1.00 d . . . C15 C 0.0782(5) -0.131(1) 0.3534(5) 0.072(3) Uani 1.00 d . . . C16 C 0.1181(6) -0.176(1) 0.2956(6) 0.081(3) Uani 1.00 d . . . C17 C 0.1049(7) -0.022(2) 0.2476(5) 0.100(4) Uani 1.00 d . . . C18 C 0.0601(5) 0.108(2) 0.2811(6) 0.083(3) Uani 1.00 d . . . C19 C 0.0449(5) 0.042(2) 0.3464(6) 0.076(3) Uani 1.00 d . . . H1 H 0.4405 -0.5772 0.3512 0.1268 Uiso 1.00 calc . . . H2 H 0.3676 -0.4816 0.4547 0.1362 Uiso 1.00 calc . . . H3 H 0.4449 -0.2374 0.5138 0.1192 Uiso 1.00 calc . . . H4 H 0.5639 -0.1773 0.4512 0.0944 Uiso 1.00 calc . . . H5 H 0.5603 -0.3923 0.3494 0.0955 Uiso 1.00 calc . . . H6 H 0.0761 -0.2076 0.3933 0.0864 Uiso 1.00 calc . . . H7 H 0.1452 -0.2898 0.2874 0.0976 Uiso 1.00 calc . . . H8 H 0.1216 -0.0146 0.2017 0.1200 Uiso 1.00 calc . . . H9 H 0.0416 0.2239 0.2620 0.0997 Uiso 1.00 calc . . . H10 H 0.0143 0.1038 0.3793 0.0908 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W 0.0366(1) 0.0405(1) 0.0402(1) -0.0005(1) 0.00449(9) -0.0021(1) Fe1 0.0358(5) 0.0474(6) 0.0377(5) 0.0061(4) 0.0016(4) 0.0031(4) Fe2 0.0333(5) 0.0523(6) 0.0483(6) 0.0006(4) -0.0053(4) 0.0094(5) S1 0.0333(7) 0.044(1) 0.0454(8) -0.0001(6) -0.0012(6) -0.0040(7) S2 0.0324(7) 0.0406(8) 0.0362(8) 0.0003(6) 0.0003(6) 0.0021(7) O1 0.108(6) 0.093(5) 0.086(5) -0.023(5) 0.025(4) 0.026(4) O2 0.073(4) 0.129(6) 0.084(5) 0.012(4) -0.022(4) -0.042(5) O3 0.132(7) 0.053(4) 0.121(7) -0.001(4) 0.002(5) 0.005(4) O4 0.067(4) 0.146(7) 0.077(4) -0.002(4) 0.015(3) 0.048(5) O5 0.046(3) 0.072(4) 0.115(5) 0.010(3) 0.004(3) 0.000(4) O6 0.079(4) 0.050(4) 0.115(6) -0.005(3) 0.007(4) 0.000(4) O7 0.057(3) 0.114(6) 0.067(4) 0.024(4) -0.007(3) 0.006(4) O8 0.067(4) 0.050(4) 0.147(7) -0.023(3) 0.003(4) -0.010(4) O9 0.094(5) 0.087(4) 0.051(3) -0.007(4) 0.022(3) -0.018(3) C1 0.058(4) 0.077(6) 0.045(4) 0.000(4) 0.005(3) 0.011(4) C2 0.054(4) 0.076(6) 0.048(4) 0.009(4) -0.008(3) -0.014(4) C3 0.062(5) 0.058(5) 0.069(5) 0.007(4) -0.001(4) 0.018(5) C4 0.050(4) 0.081(6) 0.054(5) 0.007(4) -0.006(4) 0.024(4) C5 0.037(4) 0.054(4) 0.069(5) -0.006(3) 0.012(3) -0.006(4) C6 0.051(4) 0.042(4) 0.062(5) -0.002(3) 0.007(3) 0.000(4) C7 0.047(4) 0.066(5) 0.044(4) -0.002(4) 0.005(3) -0.004(4) C8 0.039(4) 0.060(5) 0.070(5) 0.004(4) 0.001(3) -0.015(4) C9 0.052(4) 0.049(5) 0.054(4) -0.006(3) 0.006(3) -0.001(3) C10 0.13(1) 0.049(6) 0.13(1) 0.017(7) -0.064(10) -0.006(6) C11 0.070(7) 0.12(1) 0.15(1) 0.007(7) 0.020(8) 0.10(1) C12 0.13(1) 0.12(1) 0.052(5) 0.086(9) 0.010(6) 0.032(6) C13 0.063(6) 0.074(6) 0.097(8) 0.007(5) -0.031(5) 0.010(6) C14 0.077(6) 0.098(8) 0.064(6) 0.049(6) 0.012(5) -0.003(6) C15 0.050(5) 0.088(7) 0.077(6) -0.029(5) -0.015(4) 0.010(6) C16 0.069(6) 0.078(7) 0.095(8) -0.013(5) -0.020(6) -0.020(6) C17 0.078(7) 0.17(1) 0.049(5) -0.049(8) -0.009(5) -0.009(7) C18 0.043(5) 0.108(8) 0.095(8) -0.006(5) -0.035(5) 0.026(7) C19 0.034(4) 0.098(8) 0.095(7) -0.004(4) -0.001(4) -0.001(6) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00093|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3508 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0437 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_shift/su_max 0.6105 _refine_ls_shift/su_mean 0.0501 _refine_diff_density_min -1.11 _refine_diff_density_max 0.88 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W S2 2.582(2) 1_555 1_555 yes W C5 2.026(8) 1_555 1_555 yes W C6 2.042(8) 1_555 1_555 yes W C7 2.047(8) 1_555 1_555 yes W C8 2.047(8) 1_555 1_555 yes W C9 1.974(8) 1_555 1_555 yes FE1 S1 2.292(2) 1_555 1_555 yes FE1 C1 1.756(8) 1_555 1_555 yes FE1 C2 1.763(7) 1_555 1_555 yes FE1 C10 2.054(9) 1_555 1_555 yes FE1 C11 2.07(1) 1_555 1_555 yes FE1 C12 2.089(9) 1_555 1_555 yes FE1 C13 2.094(8) 1_555 1_555 yes FE1 C14 2.078(8) 1_555 1_555 yes FE2 S2 2.307(2) 1_555 1_555 yes FE2 C3 1.756(10) 1_555 1_555 yes FE2 C4 1.776(9) 1_555 1_555 yes FE2 C15 2.114(8) 1_555 1_555 yes FE2 C16 2.084(9) 1_555 1_555 yes FE2 C17 2.088(9) 1_555 1_555 yes FE2 C18 2.080(7) 1_555 1_555 yes FE2 C19 2.095(8) 1_555 1_555 yes S1 S2 2.076(2) 1_555 1_555 yes O1 C1 1.162(10) 1_555 1_555 yes O2 C2 1.134(9) 1_555 1_555 yes O3 C3 1.14(1) 1_555 1_555 yes O4 C4 1.130(9) 1_555 1_555 yes O5 C5 1.133(9) 1_555 1_555 yes O6 C6 1.132(9) 1_555 1_555 yes O7 C7 1.141(9) 1_555 1_555 yes O8 C8 1.133(9) 1_555 1_555 yes O9 C9 1.144(9) 1_555 1_555 yes C10 C11 1.38(2) 1_555 1_555 yes C10 C14 1.33(2) 1_555 1_555 yes C11 C12 1.33(2) 1_555 1_555 yes C12 C13 1.35(2) 1_555 1_555 yes C13 C14 1.37(1) 1_555 1_555 yes C15 C16 1.38(1) 1_555 1_555 yes C15 C19 1.36(1) 1_555 1_555 yes C16 C17 1.45(1) 1_555 1_555 yes C17 C18 1.38(2) 1_555 1_555 yes C18 C19 1.39(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 W C5 95.3(2) 1_555 1_555 1_555 yes S2 W C6 89.1(2) 1_555 1_555 1_555 yes S2 W C7 89.6(2) 1_555 1_555 1_555 yes S2 W C8 93.3(2) 1_555 1_555 1_555 yes S2 W C9 175.6(2) 1_555 1_555 1_555 yes C5 W C6 91.4(3) 1_555 1_555 1_555 yes C5 W C7 175.2(3) 1_555 1_555 1_555 yes C5 W C8 89.3(3) 1_555 1_555 1_555 yes C5 W C9 87.6(3) 1_555 1_555 1_555 yes C6 W C7 89.0(3) 1_555 1_555 1_555 yes C6 W C8 177.4(3) 1_555 1_555 1_555 yes C6 W C9 87.4(3) 1_555 1_555 1_555 yes C7 W C8 90.2(3) 1_555 1_555 1_555 yes C7 W C9 87.6(3) 1_555 1_555 1_555 yes C8 W C9 90.1(3) 1_555 1_555 1_555 yes S1 FE1 C1 89.0(3) 1_555 1_555 1_555 yes S1 FE1 C2 94.9(3) 1_555 1_555 1_555 yes S1 FE1 C10 142.8(5) 1_555 1_555 1_555 yes S1 FE1 C11 103.9(5) 1_555 1_555 1_555 yes S1 FE1 C12 89.5(3) 1_555 1_555 1_555 yes S1 FE1 C13 110.0(3) 1_555 1_555 1_555 yes S1 FE1 C14 148.3(3) 1_555 1_555 1_555 yes C1 FE1 C2 94.6(4) 1_555 1_555 1_555 yes C1 FE1 C10 127.5(6) 1_555 1_555 1_555 yes C1 FE1 C11 159.5(4) 1_555 1_555 1_555 yes C1 FE1 C12 129.0(6) 1_555 1_555 1_555 yes C1 FE1 C13 96.8(4) 1_555 1_555 1_555 yes C1 FE1 C14 96.5(4) 1_555 1_555 1_555 yes C2 FE1 C10 89.7(4) 1_555 1_555 1_555 yes C2 FE1 C11 100.1(6) 1_555 1_555 1_555 yes C2 FE1 C12 136.3(6) 1_555 1_555 1_555 yes C2 FE1 C13 152.8(4) 1_555 1_555 1_555 yes C2 FE1 C14 115.7(4) 1_555 1_555 1_555 yes C10 FE1 C11 39.2(6) 1_555 1_555 1_555 yes C10 FE1 C12 63.1(5) 1_555 1_555 1_555 yes C10 FE1 C13 63.8(4) 1_555 1_555 1_555 yes C10 FE1 C14 37.6(5) 1_555 1_555 1_555 yes C11 FE1 C12 37.4(5) 1_555 1_555 1_555 yes C11 FE1 C13 64.0(5) 1_555 1_555 1_555 yes C11 FE1 C14 64.2(5) 1_555 1_555 1_555 yes C12 FE1 C13 37.6(4) 1_555 1_555 1_555 yes C12 FE1 C14 62.9(4) 1_555 1_555 1_555 yes C13 FE1 C14 38.4(4) 1_555 1_555 1_555 yes S2 FE2 C3 91.8(3) 1_555 1_555 1_555 yes S2 FE2 C4 94.0(2) 1_555 1_555 1_555 yes S2 FE2 C15 87.6(2) 1_555 1_555 1_555 yes S2 FE2 C16 96.3(3) 1_555 1_555 1_555 yes S2 FE2 C17 135.5(4) 1_555 1_555 1_555 yes S2 FE2 C18 150.7(3) 1_555 1_555 1_555 yes S2 FE2 C19 113.4(3) 1_555 1_555 1_555 yes C3 FE2 C4 92.6(4) 1_555 1_555 1_555 yes C3 FE2 C15 123.7(4) 1_555 1_555 1_555 yes C3 FE2 C16 159.4(4) 1_555 1_555 1_555 yes C3 FE2 C17 132.4(5) 1_555 1_555 1_555 yes C3 FE2 C18 98.6(4) 1_555 1_555 1_555 yes C3 FE2 C19 94.3(4) 1_555 1_555 1_555 yes C4 FE2 C15 143.6(4) 1_555 1_555 1_555 yes C4 FE2 C16 105.7(5) 1_555 1_555 1_555 yes C4 FE2 C17 89.7(4) 1_555 1_555 1_555 yes C4 FE2 C18 112.7(4) 1_555 1_555 1_555 yes C4 FE2 C19 151.5(4) 1_555 1_555 1_555 yes C15 FE2 C16 38.3(4) 1_555 1_555 1_555 yes C15 FE2 C17 65.1(4) 1_555 1_555 1_555 yes C15 FE2 C18 63.9(4) 1_555 1_555 1_555 yes C15 FE2 C19 37.7(4) 1_555 1_555 1_555 yes C16 FE2 C17 40.7(4) 1_555 1_555 1_555 yes C16 FE2 C18 65.8(4) 1_555 1_555 1_555 yes C16 FE2 C19 65.1(4) 1_555 1_555 1_555 yes C17 FE2 C18 38.7(4) 1_555 1_555 1_555 yes C17 FE2 C19 65.5(4) 1_555 1_555 1_555 yes C18 FE2 C19 38.9(4) 1_555 1_555 1_555 yes FE1 S1 S2 107.49(9) 1_555 1_555 1_555 yes W S2 FE2 116.86(7) 1_555 1_555 1_555 yes W S2 S1 104.21(8) 1_555 1_555 1_555 yes FE2 S2 S1 109.20(9) 1_555 1_555 1_555 yes FE1 C1 O1 178.1(8) 1_555 1_555 1_555 yes FE1 C2 O2 177.3(9) 1_555 1_555 1_555 yes FE2 C3 O3 177.8(8) 1_555 1_555 1_555 yes FE2 C4 O4 175.9(7) 1_555 1_555 1_555 yes W C5 O5 175.4(7) 1_555 1_555 1_555 yes W C6 O6 175.3(7) 1_555 1_555 1_555 yes W C7 O7 174.9(7) 1_555 1_555 1_555 yes W C8 O8 176.6(8) 1_555 1_555 1_555 yes W C9 O9 178.6(7) 1_555 1_555 1_555 yes FE1 C10 C11 71.0(7) 1_555 1_555 1_555 yes FE1 C10 C14 72.1(6) 1_555 1_555 1_555 yes FE1 C10 H1 125.3(8) 1_555 1_555 1_555 no C11 C10 C14 108(1) 1_555 1_555 1_555 yes C11 C10 H1 126(1) 1_555 1_555 1_555 no C14 C10 H1 125(1) 1_555 1_555 1_555 no FE1 C11 C10 69.8(6) 1_555 1_555 1_555 yes FE1 C11 C12 72.1(7) 1_555 1_555 1_555 yes FE1 C11 H2 126.3(9) 1_555 1_555 1_555 no C10 C11 C12 106(1) 1_555 1_555 1_555 yes C10 C11 H2 127(2) 1_555 1_555 1_555 no C12 C11 H2 125(2) 1_555 1_555 1_555 no FE1 C12 C11 70.5(6) 1_555 1_555 1_555 yes FE1 C12 C13 71.4(5) 1_555 1_555 1_555 yes FE1 C12 H3 124.0(7) 1_555 1_555 1_555 no C11 C12 C13 110(1) 1_555 1_555 1_555 yes C11 C12 H3 125(1) 1_555 1_555 1_555 no C13 C12 H3 123(1) 1_555 1_555 1_555 no FE1 C13 C12 71.0(5) 1_555 1_555 1_555 yes FE1 C13 C14 70.1(5) 1_555 1_555 1_555 yes FE1 C13 H4 125.5(7) 1_555 1_555 1_555 no C12 C13 C14 106(1) 1_555 1_555 1_555 yes C12 C13 H4 127(1) 1_555 1_555 1_555 no C14 C13 H4 126(1) 1_555 1_555 1_555 no FE1 C14 C10 70.2(6) 1_555 1_555 1_555 yes FE1 C14 C13 71.4(5) 1_555 1_555 1_555 yes FE1 C14 H5 125.3(8) 1_555 1_555 1_555 no C10 C14 C13 108(1) 1_555 1_555 1_555 yes C10 C14 H5 125(1) 1_555 1_555 1_555 no C13 C14 H5 125(1) 1_555 1_555 1_555 no FE2 C15 C16 69.7(5) 1_555 1_555 1_555 yes FE2 C15 C19 70.4(5) 1_555 1_555 1_555 yes FE2 C15 H6 124.2(6) 1_555 1_555 1_555 no C16 C15 C19 110.5(9) 1_555 1_555 1_555 yes C16 C15 H6 124(1) 1_555 1_555 1_555 no C19 C15 H6 124(1) 1_555 1_555 1_555 no FE2 C16 C15 72.1(5) 1_555 1_555 1_555 yes FE2 C16 C17 69.8(5) 1_555 1_555 1_555 yes FE2 C16 H7 125.4(7) 1_555 1_555 1_555 no C15 C16 C17 106.3(10) 1_555 1_555 1_555 yes C15 C16 H7 127(1) 1_555 1_555 1_555 no C17 C16 H7 126(1) 1_555 1_555 1_555 no FE2 C17 C16 69.5(5) 1_555 1_555 1_555 yes FE2 C17 C18 70.3(5) 1_555 1_555 1_555 yes FE2 C17 H8 126.0(8) 1_555 1_555 1_555 no C16 C17 C18 106.0(9) 1_555 1_555 1_555 yes C16 C17 H8 126(1) 1_555 1_555 1_555 no C18 C17 H8 127(1) 1_555 1_555 1_555 no FE2 C18 C17 71.0(5) 1_555 1_555 1_555 yes FE2 C18 C19 71.1(5) 1_555 1_555 1_555 yes FE2 C18 H9 124.5(8) 1_555 1_555 1_555 no C17 C18 C19 109.5(10) 1_555 1_555 1_555 yes C17 C18 H9 125(1) 1_555 1_555 1_555 no C19 C18 H9 125(1) 1_555 1_555 1_555 no FE2 C19 C15 71.9(5) 1_555 1_555 1_555 yes FE2 C19 C18 70.0(5) 1_555 1_555 1_555 yes FE2 C19 H10 125.5(7) 1_555 1_555 1_555 no C15 C19 C18 107.6(9) 1_555 1_555 1_555 yes C15 C19 H10 126(1) 1_555 1_555 1_555 no C18 C19 H10 126(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag W S2 FE2 C3 47.9(3) 1_555 1_555 1_555 1_555 yes W S2 FE2 C4 140.6(3) 1_555 1_555 1_555 1_555 yes W S2 FE2 C15 -75.8(3) 1_555 1_555 1_555 1_555 yes W S2 FE2 C16 -113.1(3) 1_555 1_555 1_555 1_555 yes W S2 FE2 C17 -125.8(4) 1_555 1_555 1_555 1_555 yes W S2 FE2 C18 -63.3(8) 1_555 1_555 1_555 1_555 yes W S2 FE2 C19 -47.6(3) 1_555 1_555 1_555 1_555 yes W S2 S1 FE1 131.89(7) 1_555 1_555 1_555 1_555 yes FE1 S1 S2 FE2 -102.54(9) 1_555 1_555 1_555 1_555 yes FE1 C10 C11 C12 -63.5(8) 1_555 1_555 1_555 1_555 yes FE1 C10 C11 H2 120(1) 1_555 1_555 1_555 1_555 no FE1 C10 C14 C13 61.6(7) 1_555 1_555 1_555 1_555 yes FE1 C10 C14 H5 -119(1) 1_555 1_555 1_555 1_555 no FE1 C11 C10 C14 62.8(8) 1_555 1_555 1_555 1_555 yes FE1 C11 C10 H1 -120(1) 1_555 1_555 1_555 1_555 no FE1 C11 C12 C13 -60.3(7) 1_555 1_555 1_555 1_555 yes FE1 C11 C12 H3 118(1) 1_555 1_555 1_555 1_555 no FE1 C12 C11 C10 62.0(8) 1_555 1_555 1_555 1_555 yes FE1 C12 C11 H2 -122(1) 1_555 1_555 1_555 1_555 no FE1 C12 C13 C14 -61.7(7) 1_555 1_555 1_555 1_555 yes FE1 C12 C13 H4 120(1) 1_555 1_555 1_555 1_555 no FE1 C13 C12 C11 59.8(8) 1_555 1_555 1_555 1_555 yes FE1 C13 C12 H3 -119.0(9) 1_555 1_555 1_555 1_555 no FE1 C13 C14 C10 -60.8(7) 1_555 1_555 1_555 1_555 yes FE1 C13 C14 H5 120(1) 1_555 1_555 1_555 1_555 no FE1 C14 C10 C11 -62.0(8) 1_555 1_555 1_555 1_555 yes FE1 C14 C10 H1 121(1) 1_555 1_555 1_555 1_555 no FE1 C14 C13 C12 62.3(6) 1_555 1_555 1_555 1_555 yes FE1 C14 C13 H4 -120(1) 1_555 1_555 1_555 1_555 no FE2 S2 W C5 9.3(2) 1_555 1_555 1_555 1_555 yes FE2 S2 W C6 100.5(2) 1_555 1_555 1_555 1_555 yes FE2 S2 W C7 -170.5(2) 1_555 1_555 1_555 1_555 yes FE2 S2 W C8 -80.3(2) 1_555 1_555 1_555 1_555 yes FE2 S2 W C9 139(2) 1_555 1_555 1_555 1_555 yes FE2 C15 C16 C17 -61.8(6) 1_555 1_555 1_555 1_555 yes FE2 C15 C16 H7 121.2(10) 1_555 1_555 1_555 1_555 no FE2 C15 C19 C18 61.2(6) 1_555 1_555 1_555 1_555 yes FE2 C15 C19 H10 -121.2(10) 1_555 1_555 1_555 1_555 no FE2 C16 C15 C19 58.6(6) 1_555 1_555 1_555 1_555 yes FE2 C16 C15 H6 -118.2(8) 1_555 1_555 1_555 1_555 no FE2 C16 C17 C18 -61.2(6) 1_555 1_555 1_555 1_555 yes FE2 C16 C17 H8 120(1) 1_555 1_555 1_555 1_555 no FE2 C17 C16 C15 63.3(6) 1_555 1_555 1_555 1_555 yes FE2 C17 C16 H7 -119.7(10) 1_555 1_555 1_555 1_555 no FE2 C17 C18 C19 -61.0(6) 1_555 1_555 1_555 1_555 yes FE2 C17 C18 H9 119(1) 1_555 1_555 1_555 1_555 no FE2 C18 C17 C16 60.7(6) 1_555 1_555 1_555 1_555 yes FE2 C18 C17 H8 -120(1) 1_555 1_555 1_555 1_555 no FE2 C18 C19 C15 -62.5(6) 1_555 1_555 1_555 1_555 yes FE2 C18 C19 H10 119.9(10) 1_555 1_555 1_555 1_555 no FE2 C19 C15 C16 -58.2(6) 1_555 1_555 1_555 1_555 yes FE2 C19 C15 H6 118.6(8) 1_555 1_555 1_555 1_555 no FE2 C19 C18 C17 60.9(7) 1_555 1_555 1_555 1_555 yes FE2 C19 C18 H9 -119(1) 1_555 1_555 1_555 1_555 no S1 FE1 C1 O1 -11(23) 1_555 1_555 1_555 1_555 yes S1 FE1 C2 O2 -138(16) 1_555 1_555 1_555 1_555 yes S1 FE1 C10 C11 -8(1) 1_555 1_555 1_555 1_555 yes S1 FE1 C10 C14 -126.6(8) 1_555 1_555 1_555 1_555 yes S1 FE1 C10 H1 112(1) 1_555 1_555 1_555 1_555 no S1 FE1 C11 C10 174.5(8) 1_555 1_555 1_555 1_555 yes S1 FE1 C11 C12 -70.2(8) 1_555 1_555 1_555 1_555 yes S1 FE1 C11 H2 51(2) 1_555 1_555 1_555 1_555 no S1 FE1 C12 C11 114.1(9) 1_555 1_555 1_555 1_555 yes S1 FE1 C12 C13 -124.9(8) 1_555 1_555 1_555 1_555 yes S1 FE1 C12 H3 -6(1) 1_555 1_555 1_555 1_555 no S1 FE1 C13 C12 60.8(8) 1_555 1_555 1_555 1_555 yes S1 FE1 C13 C14 176.7(6) 1_555 1_555 1_555 1_555 yes S1 FE1 C13 H4 -62(1) 1_555 1_555 1_555 1_555 no S1 FE1 C14 C10 112(1) 1_555 1_555 1_555 1_555 yes S1 FE1 C14 C13 -5(1) 1_555 1_555 1_555 1_555 yes S1 FE1 C14 H5 -127.1(9) 1_555 1_555 1_555 1_555 no S1 S2 W C5 129.8(2) 1_555 1_555 1_555 1_555 yes S1 S2 W C6 -138.9(2) 1_555 1_555 1_555 1_555 yes S1 S2 W C7 -49.9(2) 1_555 1_555 1_555 1_555 yes S1 S2 W C8 40.2(2) 1_555 1_555 1_555 1_555 yes S1 S2 W C9 -99(2) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C3 -70.0(3) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C4 22.7(3) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C15 166.3(3) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C16 129.0(3) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C17 116.3(4) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C18 178.8(8) 1_555 1_555 1_555 1_555 yes S1 S2 FE2 C19 -165.5(3) 1_555 1_555 1_555 1_555 yes S2 W C5 O5 -171(8) 1_555 1_555 1_555 1_555 yes S2 W C6 O6 170(8) 1_555 1_555 1_555 1_555 yes S2 W C7 O7 170(8) 1_555 1_555 1_555 1_555 yes S2 W C8 O8 -167(11) 1_555 1_555 1_555 1_555 yes S2 W C9 O9 -128(26) 1_555 1_555 1_555 1_555 yes S2 FE2 C3 O3 135(22) 1_555 1_555 1_555 1_555 yes S2 FE2 C4 O4 -177(13) 1_555 1_555 1_555 1_555 yes S2 FE2 C15 C16 -103.4(6) 1_555 1_555 1_555 1_555 yes S2 FE2 C15 C19 134.8(6) 1_555 1_555 1_555 1_555 yes S2 FE2 C15 H6 15(1) 1_555 1_555 1_555 1_555 no S2 FE2 C16 C15 78.0(6) 1_555 1_555 1_555 1_555 yes S2 FE2 C16 C17 -166.3(7) 1_555 1_555 1_555 1_555 yes S2 FE2 C16 H7 -45(1) 1_555 1_555 1_555 1_555 no S2 FE2 C17 C16 19.6(9) 1_555 1_555 1_555 1_555 yes S2 FE2 C17 C18 136.1(7) 1_555 1_555 1_555 1_555 yes S2 FE2 C17 H8 -101(1) 1_555 1_555 1_555 1_555 no S2 FE2 C18 C17 -96(1) 1_555 1_555 1_555 1_555 yes S2 FE2 C18 C19 23(1) 1_555 1_555 1_555 1_555 yes S2 FE2 C18 H9 143.5(7) 1_555 1_555 1_555 1_555 no S2 FE2 C19 C15 -50.6(6) 1_555 1_555 1_555 1_555 yes S2 FE2 C19 C18 -167.8(6) 1_555 1_555 1_555 1_555 yes S2 FE2 C19 H10 71(1) 1_555 1_555 1_555 1_555 no S2 S1 FE1 C1 135.2(3) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C2 40.7(3) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C10 -55.2(5) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C11 -60.9(5) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C12 -95.8(5) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C13 -127.9(3) 1_555 1_555 1_555 1_555 yes S2 S1 FE1 C14 -124.0(7) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C2 83(23) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C10 176(23) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C11 -141(23) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C12 -100(23) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C13 -121(23) 1_555 1_555 1_555 1_555 yes O1 C1 FE1 C14 -160(23) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C1 132(16) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C10 4(16) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C11 -32(16) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C12 -43(17) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C13 18(17) 1_555 1_555 1_555 1_555 yes O2 C2 FE1 C14 33(17) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C4 41(22) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C15 -136(22) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C16 -111(22) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C17 -50(22) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C18 -72(22) 1_555 1_555 1_555 1_555 yes O3 C3 FE2 C19 -111(22) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C3 -85(13) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C15 91(13) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C16 84(13) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C17 46(13) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C18 14(13) 1_555 1_555 1_555 1_555 yes O4 C4 FE2 C19 18(14) 1_555 1_555 1_555 1_555 yes O5 C5 W C6 99(8) 1_555 1_555 1_555 1_555 yes O5 C5 W C7 5(10) 1_555 1_555 1_555 1_555 yes O5 C5 W C8 -78(8) 1_555 1_555 1_555 1_555 yes O5 C5 W C9 12(8) 1_555 1_555 1_555 1_555 yes O6 C6 W C5 -94(8) 1_555 1_555 1_555 1_555 yes O6 C6 W C7 80(8) 1_555 1_555 1_555 1_555 yes O6 C6 W C8 9(12) 1_555 1_555 1_555 1_555 yes O6 C6 W C9 -6(8) 1_555 1_555 1_555 1_555 yes O7 C7 W C5 -7(10) 1_555 1_555 1_555 1_555 yes O7 C7 W C6 -100(8) 1_555 1_555 1_555 1_555 yes O7 C7 W C8 76(8) 1_555 1_555 1_555 1_555 yes O7 C7 W C9 -13(8) 1_555 1_555 1_555 1_555 yes O8 C8 W C5 97(11) 1_555 1_555 1_555 1_555 yes O8 C8 W C6 -7(15) 1_555 1_555 1_555 1_555 yes O8 C8 W C7 -78(11) 1_555 1_555 1_555 1_555 yes O8 C8 W C9 9(11) 1_555 1_555 1_555 1_555 yes O9 C9 W C5 2(27) 1_555 1_555 1_555 1_555 yes O9 C9 W C6 -88(27) 1_555 1_555 1_555 1_555 yes O9 C9 W C7 -178(27) 1_555 1_555 1_555 1_555 yes O9 C9 W C8 91(27) 1_555 1_555 1_555 1_555 yes C1 FE1 C10 C11 158.0(9) 1_555 1_555 1_555 1_555 yes C1 FE1 C10 C14 40.3(10) 1_555 1_555 1_555 1_555 yes C1 FE1 C10 H1 -80(1) 1_555 1_555 1_555 1_555 no C1 FE1 C11 C10 -58(2) 1_555 1_555 1_555 1_555 yes C1 FE1 C11 C12 57(2) 1_555 1_555 1_555 1_555 yes C1 FE1 C11 H2 179.1(9) 1_555 1_555 1_555 1_555 no C1 FE1 C12 C11 -157.7(9) 1_555 1_555 1_555 1_555 yes C1 FE1 C12 C13 -36.6(9) 1_555 1_555 1_555 1_555 yes C1 FE1 C12 H3 81(1) 1_555 1_555 1_555 1_555 no C1 FE1 C13 C12 152.2(8) 1_555 1_555 1_555 1_555 yes C1 FE1 C13 C14 -91.9(7) 1_555 1_555 1_555 1_555 yes C1 FE1 C13 H4 29(1) 1_555 1_555 1_555 1_555 no C1 FE1 C14 C10 -148.9(9) 1_555 1_555 1_555 1_555 yes C1 FE1 C14 C13 92.8(7) 1_555 1_555 1_555 1_555 yes C1 FE1 C14 H5 -28(1) 1_555 1_555 1_555 1_555 no C2 FE1 C10 C11 -106.5(9) 1_555 1_555 1_555 1_555 yes C2 FE1 C10 C14 135.8(8) 1_555 1_555 1_555 1_555 yes C2 FE1 C10 H1 14(1) 1_555 1_555 1_555 1_555 no C2 FE1 C11 C10 76.9(9) 1_555 1_555 1_555 1_555 yes C2 FE1 C11 C12 -167.8(8) 1_555 1_555 1_555 1_555 yes C2 FE1 C11 H2 -45(2) 1_555 1_555 1_555 1_555 no C2 FE1 C12 C11 17(1) 1_555 1_555 1_555 1_555 yes C2 FE1 C12 C13 138.6(8) 1_555 1_555 1_555 1_555 yes C2 FE1 C12 H3 -103(1) 1_555 1_555 1_555 1_555 no C2 FE1 C13 C12 -93(1) 1_555 1_555 1_555 1_555 yes C2 FE1 C13 C14 22(1) 1_555 1_555 1_555 1_555 yes C2 FE1 C13 H4 143.4(9) 1_555 1_555 1_555 1_555 no C2 FE1 C14 C10 -50.6(9) 1_555 1_555 1_555 1_555 yes C2 FE1 C14 C13 -168.9(7) 1_555 1_555 1_555 1_555 yes C2 FE1 C14 H5 69(1) 1_555 1_555 1_555 1_555 no C3 FE2 C15 C16 166.0(6) 1_555 1_555 1_555 1_555 yes C3 FE2 C15 C19 44.2(7) 1_555 1_555 1_555 1_555 yes C3 FE2 C15 H6 -75(1) 1_555 1_555 1_555 1_555 no C3 FE2 C16 C15 -34(1) 1_555 1_555 1_555 1_555 yes C3 FE2 C16 C17 80(1) 1_555 1_555 1_555 1_555 yes C3 FE2 C16 H7 -158.0(9) 1_555 1_555 1_555 1_555 no C3 FE2 C17 C16 -151.9(7) 1_555 1_555 1_555 1_555 yes C3 FE2 C17 C18 -35.4(9) 1_555 1_555 1_555 1_555 yes C3 FE2 C17 H8 87(1) 1_555 1_555 1_555 1_555 no C3 FE2 C18 C17 154.4(7) 1_555 1_555 1_555 1_555 yes C3 FE2 C18 C19 -86.2(7) 1_555 1_555 1_555 1_555 yes C3 FE2 C18 H9 33(1) 1_555 1_555 1_555 1_555 no C3 FE2 C19 C15 -144.5(6) 1_555 1_555 1_555 1_555 yes C3 FE2 C19 C18 98.3(7) 1_555 1_555 1_555 1_555 yes C3 FE2 C19 H10 -22(1) 1_555 1_555 1_555 1_555 no C4 FE2 C15 C16 -9.9(9) 1_555 1_555 1_555 1_555 yes C4 FE2 C15 C19 -131.8(7) 1_555 1_555 1_555 1_555 yes C4 FE2 C15 H6 109(1) 1_555 1_555 1_555 1_555 no C4 FE2 C16 C15 173.9(6) 1_555 1_555 1_555 1_555 yes C4 FE2 C16 C17 -70.4(7) 1_555 1_555 1_555 1_555 yes C4 FE2 C16 H7 50(1) 1_555 1_555 1_555 1_555 no C4 FE2 C17 C16 114.9(7) 1_555 1_555 1_555 1_555 yes C4 FE2 C17 C18 -128.6(7) 1_555 1_555 1_555 1_555 yes C4 FE2 C17 H8 -5(1) 1_555 1_555 1_555 1_555 no C4 FE2 C18 C17 57.9(8) 1_555 1_555 1_555 1_555 yes C4 FE2 C18 C19 177.4(7) 1_555 1_555 1_555 1_555 yes C4 FE2 C18 H9 -62(1) 1_555 1_555 1_555 1_555 no C4 FE2 C19 C15 112.1(10) 1_555 1_555 1_555 1_555 yes C4 FE2 C19 C18 -5(1) 1_555 1_555 1_555 1_555 yes C4 FE2 C19 H10 -126(1) 1_555 1_555 1_555 1_555 no C10 FE1 C11 C12 115(1) 1_555 1_555 1_555 1_555 yes C10 FE1 C11 H2 -122(2) 1_555 1_555 1_555 1_555 no C10 FE1 C12 C11 -39.8(8) 1_555 1_555 1_555 1_555 yes C10 FE1 C12 C13 81.3(8) 1_555 1_555 1_555 1_555 yes C10 FE1 C12 H3 -160(2) 1_555 1_555 1_555 1_555 no C10 FE1 C13 C12 -79.2(9) 1_555 1_555 1_555 1_555 yes C10 FE1 C13 C14 36.8(8) 1_555 1_555 1_555 1_555 yes C10 FE1 C13 H4 157(1) 1_555 1_555 1_555 1_555 no C10 FE1 C14 C13 -118(1) 1_555 1_555 1_555 1_555 yes C10 FE1 C14 H5 120(1) 1_555 1_555 1_555 1_555 no C10 C11 FE1 C12 -115(1) 1_555 1_555 1_555 1_555 yes C10 C11 FE1 C13 -79.8(8) 1_555 1_555 1_555 1_555 yes C10 C11 FE1 C14 -36.9(7) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C13 1(1) 1_555 1_555 1_555 1_555 yes C10 C11 C12 H3 -179.6(9) 1_555 1_555 1_555 1_555 no C10 C14 FE1 C11 38.4(9) 1_555 1_555 1_555 1_555 yes C10 C14 FE1 C12 80.3(9) 1_555 1_555 1_555 1_555 yes C10 C14 FE1 C13 118(1) 1_555 1_555 1_555 1_555 yes C10 C14 C13 C12 1(1) 1_555 1_555 1_555 1_555 yes C10 C14 C13 H4 179.1(10) 1_555 1_555 1_555 1_555 no C11 FE1 C10 C14 -117(1) 1_555 1_555 1_555 1_555 yes C11 FE1 C10 H1 121(2) 1_555 1_555 1_555 1_555 no C11 FE1 C12 C13 121(1) 1_555 1_555 1_555 1_555 yes C11 FE1 C12 H3 -120(2) 1_555 1_555 1_555 1_555 no C11 FE1 C13 C12 -35.4(8) 1_555 1_555 1_555 1_555 yes C11 FE1 C13 C14 80.6(9) 1_555 1_555 1_555 1_555 yes C11 FE1 C13 H4 -158(1) 1_555 1_555 1_555 1_555 no C11 FE1 C14 C13 -79.9(8) 1_555 1_555 1_555 1_555 yes C11 FE1 C14 H5 158(1) 1_555 1_555 1_555 1_555 no C11 C10 FE1 C12 37.9(7) 1_555 1_555 1_555 1_555 yes C11 C10 FE1 C13 80.1(8) 1_555 1_555 1_555 1_555 yes C11 C10 FE1 C14 117(1) 1_555 1_555 1_555 1_555 yes C11 C10 C14 C13 0(1) 1_555 1_555 1_555 1_555 yes C11 C10 C14 H5 178.1(10) 1_555 1_555 1_555 1_555 no C11 C12 FE1 C13 -121(1) 1_555 1_555 1_555 1_555 yes C11 C12 FE1 C14 -82.2(9) 1_555 1_555 1_555 1_555 yes C11 C12 C13 C14 -1(1) 1_555 1_555 1_555 1_555 yes C11 C12 C13 H4 -179.6(10) 1_555 1_555 1_555 1_555 no C12 FE1 C10 C14 -79.8(8) 1_555 1_555 1_555 1_555 yes C12 FE1 C10 H1 159(2) 1_555 1_555 1_555 1_555 no C12 FE1 C11 H2 121(2) 1_555 1_555 1_555 1_555 no C12 FE1 C13 C14 115(1) 1_555 1_555 1_555 1_555 yes C12 FE1 C13 H4 -122(1) 1_555 1_555 1_555 1_555 no C12 FE1 C14 C13 -38.0(7) 1_555 1_555 1_555 1_555 yes C12 FE1 C14 H5 -159(1) 1_555 1_555 1_555 1_555 no C12 C11 FE1 C13 35.6(7) 1_555 1_555 1_555 1_555 yes C12 C11 FE1 C14 78.5(8) 1_555 1_555 1_555 1_555 yes C12 C11 C10 C14 0(1) 1_555 1_555 1_555 1_555 yes C12 C11 C10 H1 176(1) 1_555 1_555 1_555 1_555 no C12 C13 FE1 C14 -115(1) 1_555 1_555 1_555 1_555 yes C12 C13 C14 H5 -177.1(9) 1_555 1_555 1_555 1_555 no C13 FE1 C10 C14 -37.6(6) 1_555 1_555 1_555 1_555 yes C13 FE1 C10 H1 -158(2) 1_555 1_555 1_555 1_555 no C13 FE1 C11 H2 157(2) 1_555 1_555 1_555 1_555 no C13 FE1 C12 H3 118(2) 1_555 1_555 1_555 1_555 no C13 FE1 C14 H5 -121(1) 1_555 1_555 1_555 1_555 no C13 C12 FE1 C14 38.9(7) 1_555 1_555 1_555 1_555 yes C13 C12 C11 H2 177(1) 1_555 1_555 1_555 1_555 no C13 C14 C10 H1 -177.4(10) 1_555 1_555 1_555 1_555 no C14 FE1 C10 H1 -121(2) 1_555 1_555 1_555 1_555 no C14 FE1 C11 H2 -159(2) 1_555 1_555 1_555 1_555 no C14 FE1 C12 H3 157(1) 1_555 1_555 1_555 1_555 no C14 FE1 C13 H4 121(1) 1_555 1_555 1_555 1_555 no C14 C10 C11 H2 -176(1) 1_555 1_555 1_555 1_555 no C14 C13 C12 H3 179.3(8) 1_555 1_555 1_555 1_555 no C15 FE2 C16 C17 115.7(9) 1_555 1_555 1_555 1_555 yes C15 FE2 C16 H7 -123(1) 1_555 1_555 1_555 1_555 no C15 FE2 C17 C16 -37.9(6) 1_555 1_555 1_555 1_555 yes C15 FE2 C17 C18 78.6(7) 1_555 1_555 1_555 1_555 yes C15 FE2 C17 H8 -158(1) 1_555 1_555 1_555 1_555 no C15 FE2 C18 C17 -82.1(7) 1_555 1_555 1_555 1_555 yes C15 FE2 C18 C19 37.3(6) 1_555 1_555 1_555 1_555 yes C15 FE2 C18 H9 157(1) 1_555 1_555 1_555 1_555 no C15 FE2 C19 C18 -117.2(9) 1_555 1_555 1_555 1_555 yes C15 FE2 C19 H10 121(1) 1_555 1_555 1_555 1_555 no C15 C16 FE2 C17 -115.7(9) 1_555 1_555 1_555 1_555 yes C15 C16 FE2 C18 -77.9(7) 1_555 1_555 1_555 1_555 yes C15 C16 FE2 C19 -34.9(6) 1_555 1_555 1_555 1_555 yes C15 C16 C17 C18 2.0(10) 1_555 1_555 1_555 1_555 yes C15 C16 C17 H8 -176.5(9) 1_555 1_555 1_555 1_555 no C15 C19 FE2 C16 35.4(6) 1_555 1_555 1_555 1_555 yes C15 C19 FE2 C17 80.4(7) 1_555 1_555 1_555 1_555 yes C15 C19 FE2 C18 117.2(9) 1_555 1_555 1_555 1_555 yes C15 C19 C18 C17 -1(1) 1_555 1_555 1_555 1_555 yes C15 C19 C18 H9 178.0(8) 1_555 1_555 1_555 1_555 no C16 FE2 C15 C19 -121.9(9) 1_555 1_555 1_555 1_555 yes C16 FE2 C15 H6 118(1) 1_555 1_555 1_555 1_555 no C16 FE2 C17 C18 116.5(9) 1_555 1_555 1_555 1_555 yes C16 FE2 C17 H8 -120(1) 1_555 1_555 1_555 1_555 no C16 FE2 C18 C17 -39.7(7) 1_555 1_555 1_555 1_555 yes C16 FE2 C18 C19 79.7(7) 1_555 1_555 1_555 1_555 yes C16 FE2 C18 H9 -160(1) 1_555 1_555 1_555 1_555 no C16 FE2 C19 C18 -81.7(7) 1_555 1_555 1_555 1_555 yes C16 FE2 C19 H10 157(1) 1_555 1_555 1_555 1_555 no C16 C15 FE2 C17 40.3(6) 1_555 1_555 1_555 1_555 yes C16 C15 FE2 C18 83.4(7) 1_555 1_555 1_555 1_555 yes C16 C15 FE2 C19 121.9(9) 1_555 1_555 1_555 1_555 yes C16 C15 C19 C18 3.0(10) 1_555 1_555 1_555 1_555 yes C16 C15 C19 H10 -179.4(9) 1_555 1_555 1_555 1_555 no C16 C17 FE2 C18 -116.5(9) 1_555 1_555 1_555 1_555 yes C16 C17 FE2 C19 -79.6(7) 1_555 1_555 1_555 1_555 yes C16 C17 C18 C19 0(1) 1_555 1_555 1_555 1_555 yes C16 C17 C18 H9 -179.9(9) 1_555 1_555 1_555 1_555 no C17 FE2 C15 C19 -81.5(7) 1_555 1_555 1_555 1_555 yes C17 FE2 C15 H6 159(1) 1_555 1_555 1_555 1_555 no C17 FE2 C16 H7 120(1) 1_555 1_555 1_555 1_555 no C17 FE2 C18 C19 119.4(10) 1_555 1_555 1_555 1_555 yes C17 FE2 C18 H9 -120(1) 1_555 1_555 1_555 1_555 no C17 FE2 C19 C18 -36.8(7) 1_555 1_555 1_555 1_555 yes C17 FE2 C19 H10 -157(1) 1_555 1_555 1_555 1_555 no C17 C16 FE2 C18 37.8(6) 1_555 1_555 1_555 1_555 yes C17 C16 FE2 C19 80.8(7) 1_555 1_555 1_555 1_555 yes C17 C16 C15 C19 -3.1(10) 1_555 1_555 1_555 1_555 yes C17 C16 C15 H6 -180.0(8) 1_555 1_555 1_555 1_555 no C17 C18 FE2 C19 -119.4(10) 1_555 1_555 1_555 1_555 yes C17 C18 C19 H10 -179.2(9) 1_555 1_555 1_555 1_555 no C18 FE2 C15 C19 -38.5(6) 1_555 1_555 1_555 1_555 yes C18 FE2 C15 H6 -157(1) 1_555 1_555 1_555 1_555 no C18 FE2 C16 H7 158(1) 1_555 1_555 1_555 1_555 no C18 FE2 C17 H8 122(1) 1_555 1_555 1_555 1_555 no C18 FE2 C19 H10 -120(1) 1_555 1_555 1_555 1_555 no C18 C17 FE2 C19 36.9(6) 1_555 1_555 1_555 1_555 yes C18 C17 C16 H7 179.1(9) 1_555 1_555 1_555 1_555 no C18 C19 C15 H6 179.8(8) 1_555 1_555 1_555 1_555 no C19 FE2 C15 H6 -119(1) 1_555 1_555 1_555 1_555 no C19 FE2 C16 H7 -158(1) 1_555 1_555 1_555 1_555 no C19 FE2 C17 H8 159(1) 1_555 1_555 1_555 1_555 no C19 FE2 C18 H9 120(1) 1_555 1_555 1_555 1_555 no C19 C15 C16 H7 179.8(9) 1_555 1_555 1_555 1_555 no C19 C18 C17 H8 178.2(10) 1_555 1_555 1_555 1_555 no H1 C10 C11 H2 0(2) 1_555 1_555 1_555 1_555 no H1 C10 C14 H5 1(1) 1_555 1_555 1_555 1_555 no H2 C11 C12 H3 -3(1) 1_555 1_555 1_555 1_555 no H3 C12 C13 H4 1(1) 1_555 1_555 1_555 1_555 no H4 C13 C14 H5 0(1) 1_555 1_555 1_555 1_555 no H6 C15 C16 H7 2(1) 1_555 1_555 1_555 1_555 no H6 C15 C19 H10 -2(1) 1_555 1_555 1_555 1_555 no H7 C16 C17 H8 0(1) 1_555 1_555 1_555 1_555 no H8 C17 C18 H9 -1(1) 1_555 1_555 1_555 1_555 no H9 C18 C19 H10 0(1) 1_555 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W S2 2.582(2) 1_555 1_555 ? O1 O7 3.228(10) 1_555 3_656 ? O1 C14 3.38(1) 1_555 2_655 ? O1 C2 3.45(1) 1_555 2_655 ? O1 C10 3.55(2) 1_555 2_655 ? O1 C1 3.58(1) 1_555 2_655 ? O2 O7 3.201(9) 1_555 4_544 ? O2 O9 3.473(10) 1_555 4_544 ? O3 O6 3.39(1) 1_555 1_565 ? O3 C16 3.54(1) 1_555 1_565 ? O3 C15 3.57(1) 1_555 1_565 ? O4 O9 3.359(10) 1_555 4_554 ? O5 O6 3.141(9) 1_555 3_556 ? O5 O6 3.204(9) 1_555 1_565 ? O5 O5 3.26(1) 1_555 3_556 ? O5 C6 3.314(9) 1_555 3_556 ? O5 C5 3.389(9) 1_555 3_556 ? O5 C15 3.47(1) 1_555 3_556 ? O6 O8 3.241(10) 1_555 1_545 ? O6 C8 3.434(10) 1_555 1_545 ? O6 C5 3.438(10) 1_555 1_545 ? O7 O8 3.301(9) 1_555 1_545 ? O8 C6 3.41(1) 1_555 1_565 ? O8 C7 3.42(1) 1_555 1_565 ? O8 C13 3.49(1) 1_555 3_656 ? O8 C11 3.51(1) 1_555 1_565 ? O8 C14 3.55(1) 1_555 3_656 ? O9 C4 3.267(10) 1_555 4_555 ? O9 C18 3.29(1) 1_555 4_555 ? O9 C16 3.32(1) 1_555 4_545 ? O9 C19 3.49(1) 1_555 3_556 ? O9 C17 3.54(2) 1_555 4_555 ? C10 C12 3.51(1) 1_555 3_646 ? C11 C12 3.35(1) 1_555 3_646 ? C11 C13 3.39(1) 1_555 3_646 ? C12 C12 3.37(2) 1_555 3_646 ? C12 C13 3.59(2) 1_555 3_646 ? #------------------------------------------------------------------------------ #===END data_2 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 17 16:57:39 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 681.88 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H10 Fe2 O8 S W ' _chemical_formula_moiety 'C18 H10 Fe2 O8 S W ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 16.896(9) _cell_length_b 9.848(5) _cell_length_c 12.815(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2132(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.5 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_Int_Tables_number 29 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,y,1/2+z 1/2+x,-y,z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1296.00 _exptl_absorpt_coefficient_mu 6.868 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.619 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.49 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 1 -1 -2 1 -1 -3 -1 -1 _diffrn_reflns_number 2795 _reflns_number_total 2790 _reflns_number_observed 1372 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.456 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02297 _diffrn_orient_matrix_UB_12 -0.09049 _diffrn_orient_matrix_UB_13 -0.01842 _diffrn_orient_matrix_UB_21 -0.05237 _diffrn_orient_matrix_UB_22 0.04378 _diffrn_orient_matrix_UB_23 -0.01372 _diffrn_orient_matrix_UB_31 0.01527 _diffrn_orient_matrix_UB_32 0.01438 _diffrn_orient_matrix_UB_33 -0.07458 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 72 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 32 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 8 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; W 0 4 -0.849 6.872 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags W 0.5390 0.2216 0.1772 0.0439 Uani d . 1.00 . Fe1 0.3156 0.1997 0.3362 0.0452 Uani d . 1.00 . Fe2 0.3586 0.4516 0.3190 0.0425 Uani d . 1.00 . S 0.3952 0.2839 0.2125 0.0401 Uani d . 1.00 . O1 0.4432 0.0863 0.4543 0.0912 Uani d . 1.00 . O2 0.5075 0.4578 0.4367 0.0854 Uani d . 1.00 . O3 0.2914 0.3734 0.5164 0.1065 Uani d . 1.00 . O4 0.4843 0.2194 -0.0560 0.0848 Uani d . 1.00 . O5 0.5695 0.5387 0.1742 0.0816 Uani d . 1.00 . O6 0.6171 0.2070 0.4043 0.0909 Uani d . 1.00 . O7 0.4958 -0.0915 0.1982 0.1268 Uani d . 1.00 . O8 0.7052 0.1637 0.0846 0.0853 Uani d . 1.00 . C1 0.3954 0.1377 0.4066 0.0583 Uani d . 1.00 . C2 0.4507 0.4525 0.3912 0.0455 Uani d . 1.00 . C3 0.3121 0.3474 0.4340 0.0524 Uani d . 1.00 . C4 0.5029 0.2202 0.0273 0.0529 Uani d . 1.00 . C5 0.5593 0.4245 0.1743 0.0521 Uani d . 1.00 . C6 0.5838 0.2146 0.3301 0.0580 Uani d . 1.00 . C7 0.5103 0.0175 0.1894 0.0692 Uani d . 1.00 . C8 0.6468 0.1871 0.1207 0.0505 Uani d . 1.00 . C9 0.1953 0.2153 0.2882 0.1154 Uani d . 1.00 . C10 0.2031 0.1507 0.3851 0.1325 Uani d . 1.00 . C11 0.2409 0.0479 0.3828 0.1288 Uani d . 1.00 . C12 0.2672 0.0260 0.2768 0.1154 Uani d . 1.00 . C13 0.2334 0.1345 0.2162 0.1235 Uani d . 1.00 . C14 0.2545 0.5724 0.3270 0.0888 Uani d . 1.00 . C15 0.3217 0.6444 0.3583 0.0998 Uani d . 1.00 . C16 0.3727 0.6479 0.2742 0.0908 Uani d . 1.00 . C17 0.3419 0.5815 0.1863 0.0901 Uani d . 1.00 . C18 0.2677 0.5347 0.2200 0.0701 Uani d . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W 0.0427 0.0435 0.0454 0.0059 0.0080 0.0002 Fe1 0.0444 0.0470 0.0443 -0.0035 0.0017 0.0074 Fe2 0.0410 0.0404 0.0460 0.0029 -0.0065 -0.0086 S 0.0393 0.0404 0.0404 0.0019 0.0003 -0.0009 O1 0.0665 0.1036 0.1036 -0.0085 -0.0311 0.0616 O2 0.0553 0.0959 0.1049 -0.0048 -0.0418 -0.0259 O3 0.1324 0.1407 0.0463 -0.0190 0.0235 -0.0456 O4 0.0899 0.1159 0.0487 -0.0176 -0.0020 0.0086 O5 0.0836 0.0526 0.1087 -0.0191 -0.0260 0.0109 O6 0.0756 0.1327 0.0643 0.0270 -0.0182 0.0138 O7 0.2250 0.0625 0.0929 -0.0375 0.0151 0.0135 O8 0.0621 0.1187 0.0750 0.0419 0.0320 0.0287 C1 0.0570 0.0636 0.0544 -0.0040 -0.0090 0.0225 C2 0.0362 0.0350 0.0654 0.0047 -0.0074 -0.0236 C3 0.0462 0.0803 0.0307 -0.0029 -0.0118 -0.0098 C4 0.0378 0.0705 0.0503 -0.0026 -0.0020 -0.0128 C5 0.0416 0.0500 0.0646 -0.0150 -0.0166 0.0174 C6 0.0296 0.0818 0.0624 0.0190 -0.0133 -0.0059 C7 0.0924 0.0645 0.0507 -0.0126 -0.0136 0.0119 C8 0.0367 0.0577 0.0572 0.0039 -0.0021 0.0362 C9 0.0517 0.0646 0.2300 -0.0279 -0.0491 0.0392 C10 0.0689 0.1546 0.1741 -0.0732 0.0308 0.0140 C11 0.1453 0.0945 0.1465 -0.0942 -0.0376 0.0667 C12 0.0617 0.0984 0.1862 -0.0112 -0.0268 -0.0859 C13 0.0796 0.2438 0.0471 -0.1209 -0.0336 0.0144 C14 0.0870 0.0579 0.1215 0.0577 -0.0312 -0.0338 C15 0.1184 0.0590 0.1219 0.0342 -0.0352 -0.0640 C16 0.0671 0.0475 0.1579 -0.0025 -0.0285 0.0161 C17 0.1029 0.0514 0.1161 0.0169 -0.0112 0.0409 C18 0.0684 0.0446 0.0974 0.0244 -0.0424 0.0015 #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00216|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1372 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0387 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0513 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.852 _refine_ls_shift/esd_max 0.8950 _refine_ls_shift/esd_mean 0.2230 _refine_diff_density_min -0.84 _refine_diff_density_max 0.55 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W S 2.547(6) 1_555 1_555 yes W C4 2.02(2) 1_555 1_555 yes W C5 2.02(2) 1_555 1_555 yes W C6 2.09(3) 1_555 1_555 yes W C7 2.07(2) 1_555 1_555 yes W C8 1.99(2) 1_555 1_555 yes FE1 FE2 2.592(4) 1_555 1_555 yes FE1 S 2.239(6) 1_555 1_555 yes FE1 C1 1.75(2) 1_555 1_555 yes FE1 C3 1.94(2) 1_555 1_555 yes FE1 C9 2.16(3) 1_555 1_555 yes FE1 C10 2.03(3) 1_555 1_555 yes FE1 C11 2.03(3) 1_555 1_555 yes FE1 C12 2.02(3) 1_555 1_555 yes FE1 C13 2.12(3) 1_555 1_555 yes FE2 S 2.228(6) 1_555 1_555 yes FE2 C2 1.81(2) 1_555 1_555 yes FE2 C3 1.95(3) 1_555 1_555 yes FE2 C14 2.11(2) 1_555 1_555 yes FE2 C15 2.09(2) 1_555 1_555 yes FE2 C16 2.04(3) 1_555 1_555 yes FE2 C17 2.10(3) 1_555 1_555 yes FE2 C18 2.13(2) 1_555 1_555 yes O1 C1 1.11(3) 1_555 1_555 yes O2 C2 1.13(3) 1_555 1_555 yes O3 C3 1.13(3) 1_555 1_555 yes O4 C4 1.10(3) 1_555 1_555 yes O5 C5 1.15(2) 1_555 1_555 yes O6 C6 1.11(3) 1_555 1_555 yes O7 C7 1.11(3) 1_555 1_555 yes O8 C8 1.11(2) 1_555 1_555 yes C9 C10 1.36(7) 1_555 1_555 yes C9 C13 1.29(6) 1_555 1_555 yes C10 C11 1.20(7) 1_555 1_555 yes C11 C12 1.43(6) 1_555 1_555 yes C12 C13 1.42(6) 1_555 1_555 yes C14 C15 1.40(4) 1_555 1_555 yes C14 C18 1.40(4) 1_555 1_555 yes C15 C16 1.34(5) 1_555 1_555 yes C16 C17 1.37(5) 1_555 1_555 yes C17 C18 1.36(4) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S W C4 83.3(7) 1_555 1_555 1_555 yes S W C5 86.0(6) 1_555 1_555 1_555 yes S W C6 100.5(6) 1_555 1_555 1_555 yes S W C7 90.1(9) 1_555 1_555 1_555 yes S W C8 168.0(7) 1_555 1_555 1_555 yes C4 W C5 92(1) 1_555 1_555 1_555 yes C4 W C6 175.8(9) 1_555 1_555 1_555 yes C4 W C7 90(1) 1_555 1_555 1_555 yes C4 W C8 85.4(10) 1_555 1_555 1_555 yes C5 W C6 89(1) 1_555 1_555 1_555 yes C5 W C7 174(1) 1_555 1_555 1_555 yes C5 W C8 90.6(9) 1_555 1_555 1_555 yes C6 W C7 87(1) 1_555 1_555 1_555 yes C6 W C8 91.0(9) 1_555 1_555 1_555 yes C7 W C8 93(1) 1_555 1_555 1_555 yes FE2 FE1 S 54.4(2) 1_555 1_555 1_555 yes FE2 FE1 C1 99.9(8) 1_555 1_555 1_555 yes FE2 FE1 C3 48.5(8) 1_555 1_555 1_555 yes FE2 FE1 C9 101.0(9) 1_555 1_555 1_555 yes FE2 FE1 C10 121(1) 1_555 1_555 1_555 yes FE2 FE1 C11 154(2) 1_555 1_555 1_555 yes FE2 FE1 C12 150(1) 1_555 1_555 1_555 yes FE2 FE1 C13 113(1) 1_555 1_555 1_555 yes S FE1 C1 91.8(8) 1_555 1_555 1_555 yes S FE1 C3 101.5(8) 1_555 1_555 1_555 yes S FE1 C9 110(1) 1_555 1_555 1_555 yes S FE1 C10 148(1) 1_555 1_555 1_555 yes S FE1 C11 147(1) 1_555 1_555 1_555 yes S FE1 C12 106(1) 1_555 1_555 1_555 yes S FE1 C13 90.3(10) 1_555 1_555 1_555 yes C1 FE1 C3 88(1) 1_555 1_555 1_555 yes C1 FE1 C9 155(1) 1_555 1_555 1_555 yes C1 FE1 C10 119(2) 1_555 1_555 1_555 yes C1 FE1 C11 93(1) 1_555 1_555 1_555 yes C1 FE1 C12 102(1) 1_555 1_555 1_555 yes C1 FE1 C13 140(2) 1_555 1_555 1_555 yes C3 FE1 C9 96(1) 1_555 1_555 1_555 yes C3 FE1 C10 88(1) 1_555 1_555 1_555 yes C3 FE1 C11 110(2) 1_555 1_555 1_555 yes C3 FE1 C12 149(1) 1_555 1_555 1_555 yes C3 FE1 C13 129(2) 1_555 1_555 1_555 yes C9 FE1 C10 37(1) 1_555 1_555 1_555 yes C9 FE1 C11 62(1) 1_555 1_555 1_555 yes C9 FE1 C12 62(1) 1_555 1_555 1_555 yes C9 FE1 C13 35(1) 1_555 1_555 1_555 yes C10 FE1 C11 34(1) 1_555 1_555 1_555 yes C10 FE1 C12 61(1) 1_555 1_555 1_555 yes C10 FE1 C13 61(1) 1_555 1_555 1_555 yes C11 FE1 C12 41(1) 1_555 1_555 1_555 yes C11 FE1 C13 65(1) 1_555 1_555 1_555 yes C12 FE1 C13 39(1) 1_555 1_555 1_555 yes FE1 FE2 S 54.7(2) 1_555 1_555 1_555 yes FE1 FE2 C2 101.6(7) 1_555 1_555 1_555 yes FE1 FE2 C3 47.9(7) 1_555 1_555 1_555 yes FE1 FE2 C14 108.2(9) 1_555 1_555 1_555 yes FE1 FE2 C15 141(1) 1_555 1_555 1_555 yes FE1 FE2 C16 166.0(10) 1_555 1_555 1_555 yes FE1 FE2 C17 128.1(9) 1_555 1_555 1_555 yes FE1 FE2 C18 102.8(7) 1_555 1_555 1_555 yes S FE2 C2 94.5(6) 1_555 1_555 1_555 yes S FE2 C3 101.3(8) 1_555 1_555 1_555 yes S FE2 C14 132.2(9) 1_555 1_555 1_555 yes S FE2 C15 155(1) 1_555 1_555 1_555 yes S FE2 C16 120(1) 1_555 1_555 1_555 yes S FE2 C17 91.2(9) 1_555 1_555 1_555 yes S FE2 C18 97.1(8) 1_555 1_555 1_555 yes C2 FE2 C3 88(1) 1_555 1_555 1_555 yes C2 FE2 C14 133(1) 1_555 1_555 1_555 yes C2 FE2 C15 97(1) 1_555 1_555 1_555 yes C2 FE2 C16 91(1) 1_555 1_555 1_555 yes C2 FE2 C17 120(1) 1_555 1_555 1_555 yes C2 FE2 C18 155(1) 1_555 1_555 1_555 yes C3 FE2 C14 86(1) 1_555 1_555 1_555 yes C3 FE2 C15 100(1) 1_555 1_555 1_555 yes C3 FE2 C16 137(1) 1_555 1_555 1_555 yes C3 FE2 C17 147(1) 1_555 1_555 1_555 yes C3 FE2 C18 110(1) 1_555 1_555 1_555 yes C14 FE2 C15 38(1) 1_555 1_555 1_555 yes C14 FE2 C16 63(1) 1_555 1_555 1_555 yes C14 FE2 C17 63(1) 1_555 1_555 1_555 yes C14 FE2 C18 38(1) 1_555 1_555 1_555 yes C15 FE2 C16 37(1) 1_555 1_555 1_555 yes C15 FE2 C17 64(1) 1_555 1_555 1_555 yes C15 FE2 C18 64(1) 1_555 1_555 1_555 yes C16 FE2 C17 38(1) 1_555 1_555 1_555 yes C16 FE2 C18 63(1) 1_555 1_555 1_555 yes C17 FE2 C18 37(1) 1_555 1_555 1_555 yes W S FE1 127.6(2) 1_555 1_555 1_555 yes W S FE2 123.5(2) 1_555 1_555 1_555 yes FE1 S FE2 70.9(2) 1_555 1_555 1_555 yes FE1 C1 O1 174(2) 1_555 1_555 1_555 yes FE2 C2 O2 177(1) 1_555 1_555 1_555 yes FE1 C3 FE2 83.5(9) 1_555 1_555 1_555 yes FE1 C3 O3 140(2) 1_555 1_555 1_555 yes FE2 C3 O3 136(2) 1_555 1_555 1_555 yes W C4 O4 178(2) 1_555 1_555 1_555 yes W C5 O5 177(3) 1_555 1_555 1_555 yes W C6 O6 170(2) 1_555 1_555 1_555 yes W C7 O7 178(3) 1_555 1_555 1_555 yes W C8 O8 177(2) 1_555 1_555 1_555 yes FE1 C9 C10 65(2) 1_555 1_555 1_555 yes FE1 C9 C13 70(1) 1_555 1_555 1_555 yes FE1 C9 H1 123(3) 1_555 1_555 1_555 no C10 C9 C13 105(3) 1_555 1_555 1_555 yes C10 C9 H1 120(10) 1_555 1_555 1_555 no C13 C9 H1 133(10) 1_555 1_555 1_555 no FE1 C10 C9 76(2) 1_555 1_555 1_555 yes FE1 C10 C11 72(2) 1_555 1_555 1_555 yes FE1 C10 H2 121(3) 1_555 1_555 1_555 no C9 C10 C11 116(5) 1_555 1_555 1_555 yes C9 C10 H2 124(7) 1_555 1_555 1_555 no C11 C10 H2 118(7) 1_555 1_555 1_555 no FE1 C11 C10 72(2) 1_555 1_555 1_555 yes FE1 C11 C12 69(1) 1_555 1_555 1_555 yes FE1 C11 H3 126(3) 1_555 1_555 1_555 no C10 C11 C12 104(4) 1_555 1_555 1_555 yes C10 C11 H3 123(8) 1_555 1_555 1_555 no C12 C11 H3 131(8) 1_555 1_555 1_555 no FE1 C12 C11 69(1) 1_555 1_555 1_555 yes FE1 C12 C13 73(1) 1_555 1_555 1_555 yes FE1 C12 H4 125(3) 1_555 1_555 1_555 no C11 C12 C13 105(3) 1_555 1_555 1_555 yes C11 C12 H4 120(10) 1_555 1_555 1_555 no C13 C12 H4 133(10) 1_555 1_555 1_555 no FE1 C13 C9 73(2) 1_555 1_555 1_555 yes FE1 C13 C12 66(1) 1_555 1_555 1_555 yes FE1 C13 H5 126(2) 1_555 1_555 1_555 no C9 C13 C12 107(3) 1_555 1_555 1_555 yes C9 C13 H5 126(7) 1_555 1_555 1_555 no C12 C13 H5 126(7) 1_555 1_555 1_555 no FE2 C14 C15 69(1) 1_555 1_555 1_555 yes FE2 C14 C18 71(1) 1_555 1_555 1_555 yes FE2 C14 H6 123(3) 1_555 1_555 1_555 no C15 C14 C18 107(3) 1_555 1_555 1_555 yes C15 C14 H6 121(6) 1_555 1_555 1_555 no C18 C14 H6 130(6) 1_555 1_555 1_555 no FE2 C15 C14 71(1) 1_555 1_555 1_555 yes FE2 C15 C16 69(1) 1_555 1_555 1_555 yes FE2 C15 H7 124(3) 1_555 1_555 1_555 no C14 C15 C16 106(2) 1_555 1_555 1_555 yes C14 C15 H7 124(4) 1_555 1_555 1_555 no C16 C15 H7 129(4) 1_555 1_555 1_555 no FE2 C16 C15 73(2) 1_555 1_555 1_555 yes FE2 C16 C17 72(1) 1_555 1_555 1_555 yes FE2 C16 H8 122(3) 1_555 1_555 1_555 no C15 C16 C17 110(2) 1_555 1_555 1_555 yes C15 C16 H8 117(8) 1_555 1_555 1_555 no C17 C16 H8 131(9) 1_555 1_555 1_555 no FE2 C17 C16 68(1) 1_555 1_555 1_555 yes FE2 C17 C18 72(1) 1_555 1_555 1_555 yes FE2 C17 H9 124(3) 1_555 1_555 1_555 no C16 C17 C18 107(3) 1_555 1_555 1_555 yes C16 C17 H9 122(5) 1_555 1_555 1_555 no C18 C17 H9 129(4) 1_555 1_555 1_555 no FE2 C18 C14 69(1) 1_555 1_555 1_555 yes FE2 C18 C17 69(1) 1_555 1_555 1_555 yes FE2 C18 H10 124(3) 1_555 1_555 1_555 no C14 C18 C17 107(2) 1_555 1_555 1_555 yes C14 C18 H10 121(7) 1_555 1_555 1_555 no C17 C18 H10 130(7) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W S 2.547(6) 1_555 1_555 ? FE1 FE2 2.592(4) 1_555 1_555 ? O1 O4 3.24(3) 1_555 2_655 ? O1 C4 3.28(3) 1_555 2_655 ? O1 C7 3.31(4) 1_555 2_655 ? O1 O7 3.31(3) 1_555 2_655 ? O2 O4 3.19(3) 1_555 2_665 ? O2 O5 3.32(4) 1_555 2_665 ? O2 C4 3.39(3) 1_555 2_665 ? O2 C5 3.46(5) 1_555 2_665 ? O3 O5 3.24(3) 1_555 2_665 ? O3 C18 3.24(3) 1_555 3_555 ? O3 C13 3.51(6) 1_555 3_555 ? O4 C10 3.37(5) 1_555 3_554 ? O4 O7 3.41(3) 1_555 2_654 ? O4 C16 3.47(4) 1_555 2_664 ? O4 C2 3.48(3) 1_555 2_664 ? O5 C18 3.50(3) 1_555 4_565 ? O5 C9 3.53(4) 1_555 4_565 ? O6 C11 3.29(4) 1_555 4_555 ? O6 C14 3.37(3) 1_555 4_565 ? O7 C16 3.44(4) 1_555 1_545 ? O8 C12 3.26(4) 1_555 4_555 ? O8 C11 3.44(5) 1_555 2_654 ? O8 C13 3.48(6) 1_555 4_555 ? O8 C15 3.49(4) 1_555 2_664 ? C8 C12 3.56(4) 1_555 4_555 ? #------------------------------------------------------------------------------