# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Su Jing' _publ_contact_author_email sjing@njut.edu.cn _publ_section_title ; 1,5,9,13-Tetraselena[13]ferrocenophane: Synthesis, Complexation, Crystallographic and Electrochemical Study ; loop_ _publ_author_name 'Su Jing.' 'Christopher Morley' 'Cheng-Yun Gu.' 'M.Di Vaira' # Attachment '- Ag.cif' data_280521d _database_code_depnum_ccdc_archive 'CCDC 770358' #TrackingRef '- Ag.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 Ag Fe Se4 +, P F6 -' _chemical_formula_sum 'C19 H26 Ag F6 Fe P Se4' _chemical_formula_weight 878.93 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9497(12) _cell_length_b 23.326(4) _cell_length_c 15.469(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.971(2) _cell_angle_gamma 90.00 _cell_volume 2501.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 7.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3377 _exptl_absorpt_correction_T_max 0.3701 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1986)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13213 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 4883 _reflns_number_gt 4109 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.1073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00233(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4883 _refine_ls_number_parameters 354 _refine_ls_number_restraints 222 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.710 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.126 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 Ag Ag 0.05105(4) 0.081605(13) 0.77975(2) 0.04126(11) Uani 1 1 d . . . C1 C -0.0151(6) 0.23508(17) 0.7385(3) 0.0422(10) Uani 1 1 d . . . H1A H 0.1147 0.2270 0.7225 0.051 Uiso 1 1 calc R . . H1B H -0.0627 0.2679 0.7050 0.051 Uiso 1 1 calc R . . C2 C -0.0084(6) 0.25000(17) 0.8344(3) 0.0460(11) Uani 1 1 d . . . H2A H 0.0757 0.2829 0.8437 0.055 Uiso 1 1 calc R . . H2B H -0.1368 0.2620 0.8475 0.055 Uiso 1 1 calc R . . C3 C 0.0572(6) 0.20489(17) 0.8992(3) 0.0416(10) Uani 1 1 d . . . H3A H -0.0489 0.1789 0.9075 0.050 Uiso 1 1 calc R . . H3B H 0.0924 0.2231 0.9545 0.050 Uiso 1 1 calc R . . C4 C 0.3552(6) 0.12357(18) 0.9734(3) 0.0415(10) Uani 1 1 d . . . H4A H 0.4225 0.1509 1.0119 0.050 Uiso 1 1 calc R . . H4B H 0.2412 0.1107 1.0006 0.050 Uiso 1 1 calc R . . C5 C 0.4860(6) 0.07262(17) 0.9590(3) 0.0401(9) Uani 1 1 d . . . H5A H 0.5218 0.0546 1.0143 0.048 Uiso 1 1 calc R . . H5B H 0.4159 0.0447 0.9226 0.048 Uiso 1 1 calc R . . C6 C 0.6677(6) 0.09016(16) 0.9165(3) 0.0381(9) Uani 1 1 d . . . H6A H 0.7397 0.1168 0.9545 0.046 Uiso 1 1 calc R . . H6B H 0.6305 0.1103 0.8631 0.046 Uiso 1 1 calc R . . C7 C 0.6646(6) -0.01732(16) 0.8098(3) 0.0400(9) Uani 1 1 d . . . H7A H 0.7415 -0.0442 0.7790 0.048 Uiso 1 1 calc R . . H7B H 0.5784 -0.0395 0.8433 0.048 Uiso 1 1 calc R . . C8 C 0.5446(6) 0.01719(16) 0.7441(3) 0.0420(10) Uani 1 1 d . . . H8A H 0.6281 0.0356 0.7047 0.050 Uiso 1 1 calc R . . H8B H 0.4763 0.0469 0.7734 0.050 Uiso 1 1 calc R . . C9 C 0.4000(6) -0.02075(15) 0.6928(3) 0.0393(10) Uani 1 1 d . . . H9A H 0.3663 -0.0526 0.7291 0.047 Uiso 1 1 calc R . . H9B H 0.4608 -0.0364 0.6434 0.047 Uiso 1 1 calc R . . C10 C 0.2653(5) 0.07666(15) 0.5814(2) 0.0292(8) Uani 1 1 d . . . C11 C 0.3362(5) 0.13156(15) 0.6082(3) 0.0327(9) Uani 1 1 d . . . H11 H 0.3507 0.1449 0.6649 0.039 Uiso 1 1 calc R . . C12 C 0.3801(5) 0.16189(17) 0.5338(3) 0.0425(10) Uani 1 1 d . . . H12 H 0.4281 0.1991 0.5325 0.051 Uiso 1 1 calc R . . C13 C 0.3393(6) 0.12636(18) 0.4612(3) 0.0428(10) Uani 1 1 d . . . H13 H 0.3562 0.1361 0.4040 0.051 Uiso 1 1 calc R . . C14 C 0.2690(6) 0.07392(17) 0.4898(3) 0.0378(9) Uani 1 1 d . . . H14 H 0.2314 0.0428 0.4550 0.045 Uiso 1 1 calc R . . C15 C -0.1352(5) 0.16582(15) 0.5900(3) 0.0322(8) Uani 1 1 d . . . C16 C -0.0675(6) 0.21040(16) 0.5375(3) 0.0408(10) Uani 1 1 d . . . H16 H -0.0234 0.2462 0.5566 0.049 Uiso 1 1 calc R . . C17 C -0.0792(6) 0.19065(18) 0.4510(3) 0.0456(10) Uani 1 1 d . . . H17 H -0.0438 0.2113 0.4032 0.055 Uiso 1 1 calc R . . C18 C -0.1534(5) 0.13440(19) 0.4492(3) 0.0438(11) Uani 1 1 d . . . H18 H -0.1760 0.1117 0.4001 0.053 Uiso 1 1 calc R . . C19 C -0.1871(5) 0.11861(17) 0.5346(3) 0.0370(9) Uani 1 1 d . . . H19 H -0.2350 0.0835 0.5520 0.044 Uiso 1 1 calc R . . Fe Fe 0.09639(7) 0.13848(2) 0.52596(4) 0.02929(14) Uani 1 1 d . . . Se1 Se -0.18017(5) 0.168812(16) 0.70930(3) 0.03528(11) Uani 1 1 d . . . Se2 Se 0.27901(6) 0.160674(16) 0.86274(3) 0.03561(11) Uani 1 1 d . . . Se3 Se 0.83760(6) 0.026310(17) 0.89009(3) 0.03786(12) Uani 1 1 d . . . Se4 Se 0.16255(5) 0.019033(15) 0.65110(2) 0.03067(11) Uani 1 1 d . . . P1A P 0.4235(11) 0.3513(4) 0.6671(5) 0.056(3) Uani 0.403(15) 1 d PD A 1 F1A F 0.457(2) 0.3966(6) 0.5960(7) 0.100(5) Uani 0.403(15) 1 d PDU A 1 F2A F 0.389(2) 0.3023(8) 0.7325(12) 0.115(6) Uani 0.403(15) 1 d PDU A 1 F3A F 0.4510(18) 0.3984(6) 0.7378(8) 0.098(5) Uani 0.403(15) 1 d PDU A 1 F4A F 0.395(2) 0.3041(6) 0.5973(11) 0.151(7) Uani 0.403(15) 1 d PDU A 1 F5A F 0.2033(14) 0.3639(6) 0.6588(11) 0.125(5) Uani 0.403(15) 1 d PDU A 1 F6A F 0.6437(14) 0.3393(5) 0.6754(11) 0.115(5) Uani 0.403(15) 1 d PDU A 1 P1B P 0.4158(8) 0.3455(3) 0.6709(3) 0.058(2) Uani 0.597(15) 1 d PDU A 2 F1B F 0.3884(15) 0.4052(4) 0.6255(8) 0.161(5) Uani 0.597(15) 1 d PDU A 2 F2B F 0.4458(18) 0.2867(5) 0.7191(10) 0.123(4) Uani 0.597(15) 1 d PDU A 2 F3B F 0.5268(16) 0.3765(6) 0.7498(5) 0.142(5) Uani 0.597(15) 1 d PDU A 2 F4B F 0.3039(15) 0.3164(4) 0.5916(5) 0.099(3) Uani 0.597(15) 1 d PDU A 2 F5B F 0.2233(13) 0.3536(4) 0.7154(8) 0.120(4) Uani 0.597(15) 1 d PDU A 2 F6B F 0.6098(14) 0.3370(5) 0.6285(7) 0.157(5) Uani 0.597(15) 1 d PDU A 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 Ag 0.03985(19) 0.03943(18) 0.0455(2) -0.00875(14) 0.01037(14) 0.00108(13) C1 0.043(2) 0.031(2) 0.052(3) -0.0076(19) -0.001(2) -0.0008(16) C2 0.042(2) 0.034(2) 0.061(3) -0.022(2) -0.002(2) 0.0058(18) C3 0.036(2) 0.042(2) 0.048(2) -0.017(2) 0.0104(19) 0.0021(18) C4 0.047(2) 0.047(2) 0.032(2) -0.0009(19) 0.0143(19) 0.0014(19) C5 0.051(2) 0.037(2) 0.034(2) 0.0073(18) 0.0122(19) 0.0045(18) C6 0.047(2) 0.034(2) 0.034(2) -0.0016(17) 0.0044(18) -0.0017(17) C7 0.045(2) 0.036(2) 0.038(2) 0.0045(18) -0.0014(19) 0.0029(17) C8 0.045(2) 0.035(2) 0.045(2) 0.0073(19) -0.007(2) -0.0014(18) C9 0.044(2) 0.0271(19) 0.046(2) 0.0009(18) -0.0043(19) 0.0074(17) C10 0.0249(18) 0.0290(18) 0.034(2) 0.0014(16) 0.0026(15) 0.0014(14) C11 0.0223(18) 0.0318(19) 0.043(2) 0.0020(18) -0.0033(16) 0.0000(14) C12 0.0234(19) 0.039(2) 0.065(3) 0.012(2) 0.0063(19) -0.0027(16) C13 0.038(2) 0.045(2) 0.047(3) 0.014(2) 0.0151(19) 0.0086(18) C14 0.036(2) 0.038(2) 0.040(2) -0.0023(18) 0.0055(18) 0.0124(17) C15 0.0203(17) 0.0338(19) 0.042(2) -0.0019(17) -0.0018(16) 0.0060(14) C16 0.043(2) 0.0286(19) 0.050(3) 0.0011(19) -0.002(2) 0.0125(17) C17 0.047(2) 0.048(2) 0.042(2) 0.013(2) 0.002(2) 0.016(2) C18 0.029(2) 0.060(3) 0.041(2) -0.011(2) -0.0080(19) 0.0091(19) C19 0.0206(18) 0.038(2) 0.051(3) -0.0095(19) -0.0013(17) 0.0011(15) Fe 0.0243(3) 0.0273(3) 0.0361(3) 0.0014(2) 0.0003(2) 0.0021(2) Se1 0.0270(2) 0.0350(2) 0.0440(2) -0.00679(18) 0.00398(17) 0.00093(15) Se2 0.0337(2) 0.0373(2) 0.0363(2) -0.00563(17) 0.00516(17) 0.00170(16) Se3 0.0362(2) 0.0428(2) 0.0344(2) 0.00553(18) 0.00051(17) 0.00627(17) Se4 0.0300(2) 0.02517(19) 0.0372(2) -0.00264(16) 0.00509(16) -0.00111(14) P1A 0.066(6) 0.054(4) 0.051(5) 0.001(3) 0.025(4) -0.016(3) F1A 0.107(8) 0.113(8) 0.080(7) 0.040(6) 0.010(6) -0.039(6) F2A 0.131(11) 0.129(11) 0.086(7) 0.063(9) 0.005(8) -0.052(9) F3A 0.103(8) 0.103(8) 0.088(8) -0.060(7) 0.011(6) -0.001(6) F4A 0.192(15) 0.119(10) 0.142(12) -0.072(9) 0.021(11) -0.018(10) F5A 0.053(6) 0.178(12) 0.145(12) -0.014(10) 0.009(7) 0.003(6) F6A 0.069(6) 0.122(9) 0.153(13) 0.031(8) 0.007(8) 0.038(6) P1B 0.071(4) 0.061(3) 0.042(3) 0.002(2) 0.006(3) -0.028(3) F1B 0.249(12) 0.088(6) 0.142(9) 0.046(6) -0.016(8) -0.067(7) F2B 0.124(7) 0.101(6) 0.149(9) 0.041(6) 0.029(6) 0.040(5) F3B 0.166(9) 0.185(10) 0.073(5) 0.004(7) -0.013(6) -0.104(8) F4B 0.125(7) 0.098(5) 0.070(5) -0.006(4) -0.032(5) -0.026(5) F5B 0.117(7) 0.087(5) 0.164(9) -0.036(6) 0.078(7) -0.009(4) F6B 0.100(7) 0.280(12) 0.098(7) 0.043(7) 0.058(6) -0.009(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag Se4 2.6278(6) . ? Ag Se3 2.6698(6) 1_455 ? Ag Se2 2.6977(6) . ? Ag Se1 2.7686(6) . ? C1 C2 1.522(6) . ? C1 Se1 1.959(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.502(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 Se2 1.970(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.522(5) . ? C4 Se2 1.958(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.519(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 Se3 1.961(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.503(5) . ? C7 Se3 1.954(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.520(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 Se4 1.963(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.420(6) . ? C10 C11 1.423(5) . ? C10 Se4 1.894(4) . ? C10 Fe 2.013(3) . ? C11 C12 1.403(6) . ? C11 Fe 2.032(3) . ? C11 H11 0.9300 . ? C12 C13 1.408(6) . ? C12 Fe 2.042(4) . ? C12 H12 0.9300 . ? C13 C14 1.400(6) . ? C13 Fe 2.041(4) . ? C13 H13 0.9300 . ? C14 Fe 2.028(4) . ? C14 H14 0.9300 . ? C15 C16 1.420(5) . ? C15 C19 1.426(5) . ? C15 Se1 1.894(4) . ? C15 Fe 2.049(4) . ? C16 C17 1.412(6) . ? C16 Fe 2.042(4) . ? C16 H16 0.9300 . ? C17 C18 1.410(6) . ? C17 Fe 2.029(4) . ? C17 H17 0.9300 . ? C18 C19 1.407(6) . ? C18 Fe 2.036(4) . ? C18 H18 0.9300 . ? C19 Fe 2.038(4) . ? C19 H19 0.9300 . ? Se3 Ag 2.6698(6) 1_655 ? P1A F4A 1.545(9) . ? P1A F6A 1.552(9) . ? P1A F1A 1.553(9) . ? P1A F3A 1.555(9) . ? P1A F5A 1.555(9) . ? P1A F2A 1.556(8) . ? P1B F6B 1.552(7) . ? P1B F5B 1.558(7) . ? P1B F4B 1.562(6) . ? P1B F1B 1.566(7) . ? P1B F2B 1.568(7) . ? P1B F3B 1.574(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se4 Ag Se3 114.95(2) . 1_455 ? Se4 Ag Se2 123.084(19) . . ? Se3 Ag Se2 111.11(2) 1_455 . ? Se4 Ag Se1 107.669(19) . . ? Se3 Ag Se1 105.877(19) 1_455 . ? Se2 Ag Se1 89.467(19) . . ? C2 C1 Se1 112.5(3) . . ? C2 C1 H1A 109.1 . . ? Se1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? Se1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2A 107.7 . . ? C1 C2 H2A 107.7 . . ? C3 C2 H2B 107.7 . . ? C1 C2 H2B 107.7 . . ? H2A C2 H2B 107.1 . . ? C2 C3 Se2 112.5(3) . . ? C2 C3 H3A 109.1 . . ? Se2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? Se2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 Se2 110.2(3) . . ? C5 C4 H4A 109.6 . . ? Se2 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? Se2 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 112.1(3) . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 Se3 114.6(3) . . ? C5 C6 H6A 108.6 . . ? Se3 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? Se3 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 Se3 116.1(3) . . ? C8 C7 H7A 108.3 . . ? Se3 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? Se3 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 C9 110.9(3) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C8 C9 Se4 114.0(3) . . ? C8 C9 H9A 108.8 . . ? Se4 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? Se4 C9 H9B 108.8 . . ? H9A C9 H9B 107.6 . . ? C14 C10 C11 107.5(3) . . ? C14 C10 Se4 124.7(3) . . ? C11 C10 Se4 127.5(3) . . ? C14 C10 Fe 70.0(2) . . ? C11 C10 Fe 70.10(19) . . ? Se4 C10 Fe 121.28(18) . . ? C12 C11 C10 107.8(4) . . ? C12 C11 Fe 70.2(2) . . ? C10 C11 Fe 68.70(19) . . ? C12 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? Fe C11 H11 126.5 . . ? C11 C12 C13 108.3(3) . . ? C11 C12 Fe 69.5(2) . . ? C13 C12 Fe 69.8(2) . . ? C11 C12 H12 125.9 . . ? C13 C12 H12 125.9 . . ? Fe C12 H12 126.4 . . ? C14 C13 C12 108.5(4) . . ? C14 C13 Fe 69.4(2) . . ? C12 C13 Fe 69.8(2) . . ? C14 C13 H13 125.7 . . ? C12 C13 H13 125.7 . . ? Fe C13 H13 126.6 . . ? C13 C14 C10 107.9(4) . . ? C13 C14 Fe 70.4(2) . . ? C10 C14 Fe 68.9(2) . . ? C13 C14 H14 126.1 . . ? C10 C14 H14 126.1 . . ? Fe C14 H14 126.2 . . ? C16 C15 C19 107.6(4) . . ? C16 C15 Se1 127.9(3) . . ? C19 C15 Se1 124.1(3) . . ? C16 C15 Fe 69.4(2) . . ? C19 C15 Fe 69.2(2) . . ? Se1 C15 Fe 132.11(17) . . ? C17 C16 C15 107.7(3) . . ? C17 C16 Fe 69.2(2) . . ? C15 C16 Fe 69.9(2) . . ? C17 C16 H16 126.2 . . ? C15 C16 H16 126.2 . . ? Fe C16 H16 126.2 . . ? C18 C17 C16 108.6(4) . . ? C18 C17 Fe 70.0(2) . . ? C16 C17 Fe 70.2(2) . . ? C18 C17 H17 125.7 . . ? C16 C17 H17 125.7 . . ? Fe C17 H17 125.7 . . ? C19 C18 C17 108.0(4) . . ? C19 C18 Fe 69.8(2) . . ? C17 C18 Fe 69.4(2) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? Fe C18 H18 126.3 . . ? C18 C19 C15 108.1(4) . . ? C18 C19 Fe 69.7(2) . . ? C15 C19 Fe 70.0(2) . . ? C18 C19 H19 126.0 . . ? C15 C19 H19 126.0 . . ? Fe C19 H19 125.9 . . ? C10 Fe C14 41.13(15) . . ? C10 Fe C17 169.29(17) . . ? C14 Fe C17 129.16(17) . . ? C10 Fe C11 41.21(13) . . ? C14 Fe C11 68.80(16) . . ? C17 Fe C11 147.15(16) . . ? C10 Fe C18 131.53(16) . . ? C14 Fe C18 107.52(17) . . ? C17 Fe C18 40.57(17) . . ? C11 Fe C18 172.09(17) . . ? C10 Fe C19 110.30(15) . . ? C14 Fe C19 116.26(16) . . ? C17 Fe C19 68.18(18) . . ? C11 Fe C19 134.08(17) . . ? C18 Fe C19 40.42(17) . . ? C10 Fe C13 68.40(15) . . ? C14 Fe C13 40.25(16) . . ? C17 Fe C13 106.72(18) . . ? C11 Fe C13 68.02(17) . . ? C18 Fe C13 114.08(18) . . ? C19 Fe C13 146.84(17) . . ? C10 Fe C12 68.53(15) . . ? C14 Fe C12 68.13(17) . . ? C17 Fe C12 114.42(18) . . ? C11 Fe C12 40.29(16) . . ? C18 Fe C12 145.87(18) . . ? C19 Fe C12 172.48(18) . . ? C13 Fe C12 40.34(17) . . ? C10 Fe C16 149.72(16) . . ? C14 Fe C16 167.98(17) . . ? C17 Fe C16 40.57(17) . . ? C11 Fe C16 116.68(16) . . ? C18 Fe C16 68.36(16) . . ? C19 Fe C16 68.50(16) . . ? C13 Fe C16 129.92(17) . . ? C12 Fe C16 108.51(17) . . ? C10 Fe C15 118.13(15) . . ? C14 Fe C15 149.74(16) . . ? C17 Fe C15 68.18(17) . . ? C11 Fe C15 111.08(16) . . ? C18 Fe C15 68.29(16) . . ? C19 Fe C15 40.84(14) . . ? C13 Fe C15 169.80(16) . . ? C12 Fe C15 132.53(16) . . ? C16 Fe C15 40.61(15) . . ? C15 Se1 C1 96.89(17) . . ? C15 Se1 Ag 103.06(10) . . ? C1 Se1 Ag 100.04(12) . . ? C4 Se2 C3 98.64(18) . . ? C4 Se2 Ag 103.19(13) . . ? C3 Se2 Ag 92.80(12) . . ? C7 Se3 C6 100.08(17) . . ? C7 Se3 Ag 100.93(13) . 1_655 ? C6 Se3 Ag 97.79(12) . 1_655 ? C10 Se4 C9 100.44(16) . . ? C10 Se4 Ag 100.35(11) . . ? C9 Se4 Ag 107.40(13) . . ? F4A P1A F6A 90.6(4) . . ? F4A P1A F1A 90.5(5) . . ? F6A P1A F1A 89.3(4) . . ? F4A P1A F3A 179.4(7) . . ? F6A P1A F3A 89.8(4) . . ? F1A P1A F3A 90.0(5) . . ? F4A P1A F5A 89.9(4) . . ? F6A P1A F5A 179.4(5) . . ? F1A P1A F5A 90.4(4) . . ? F3A P1A F5A 89.7(4) . . ? F4A P1A F2A 85.1(11) . . ? F6A P1A F2A 90.4(4) . . ? F1A P1A F2A 175.6(10) . . ? F3A P1A F2A 94.5(10) . . ? F5A P1A F2A 89.9(4) . . ? F6B P1B F5B 178.7(5) . . ? F6B P1B F4B 90.7(4) . . ? F5B P1B F4B 90.2(4) . . ? F6B P1B F1B 90.4(4) . . ? F5B P1B F1B 90.5(4) . . ? F4B P1B F1B 89.8(4) . . ? F6B P1B F2B 89.9(4) . . ? F5B P1B F2B 89.2(4) . . ? F4B P1B F2B 92.0(8) . . ? F1B P1B F2B 178.2(8) . . ? F6B P1B F3B 89.6(4) . . ? F5B P1B F3B 89.5(4) . . ? F4B P1B F3B 178.4(5) . . ? F1B P1B F3B 88.6(4) . . ? F2B P1B F3B 89.5(8) . . ? 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 Se1 C1 C2 C3 57.5(4) . . . . ? C1 C2 C3 Se2 41.2(5) . . . . ? Se2 C4 C5 C6 59.3(4) . . . . ? C4 C5 C6 Se3 -176.9(3) . . . . ? Se3 C7 C8 C9 -173.3(3) . . . . ? C7 C8 C9 Se4 150.8(3) . . . . ? C14 C10 C11 C12 0.7(4) . . . . ? Se4 C10 C11 C12 -174.3(3) . . . . ? Fe C10 C11 C12 -59.6(2) . . . . ? C14 C10 C11 Fe 60.3(2) . . . . ? Se4 C10 C11 Fe -114.7(3) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? Fe C11 C12 C13 -59.2(3) . . . . ? C10 C11 C12 Fe 58.6(2) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? Fe C12 C13 C14 -58.7(3) . . . . ? C11 C12 C13 Fe 59.0(3) . . . . ? C12 C13 C14 C10 0.1(4) . . . . ? Fe C13 C14 C10 -58.9(3) . . . . ? C12 C13 C14 Fe 59.0(3) . . . . ? C11 C10 C14 C13 -0.5(4) . . . . ? Se4 C10 C14 C13 174.7(3) . . . . ? Fe C10 C14 C13 59.8(3) . . . . ? C11 C10 C14 Fe -60.3(2) . . . . ? Se4 C10 C14 Fe 114.8(3) . . . . ? C19 C15 C16 C17 0.3(4) . . . . ? Se1 C15 C16 C17 -172.8(3) . . . . ? Fe C15 C16 C17 59.2(3) . . . . ? C19 C15 C16 Fe -58.8(2) . . . . ? Se1 C15 C16 Fe 128.0(3) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? Fe C16 C17 C18 59.7(3) . . . . ? C15 C16 C17 Fe -59.6(3) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? Fe C17 C18 C19 59.4(3) . . . . ? C16 C17 C18 Fe -59.8(3) . . . . ? C17 C18 C19 C15 0.6(4) . . . . ? Fe C18 C19 C15 59.7(2) . . . . ? C17 C18 C19 Fe -59.1(3) . . . . ? C16 C15 C19 C18 -0.6(4) . . . . ? Se1 C15 C19 C18 172.9(3) . . . . ? Fe C15 C19 C18 -59.6(3) . . . . ? C16 C15 C19 Fe 59.0(2) . . . . ? Se1 C15 C19 Fe -127.5(2) . . . . ? C11 C10 Fe C14 118.2(3) . . . . ? Se4 C10 Fe C14 -119.2(3) . . . . ? C14 C10 Fe C17 27.3(10) . . . . ? C11 C10 Fe C17 145.5(9) . . . . ? Se4 C10 Fe C17 -92.0(9) . . . . ? C14 C10 Fe C11 -118.2(3) . . . . ? Se4 C10 Fe C11 122.5(3) . . . . ? C14 C10 Fe C18 66.2(3) . . . . ? C11 C10 Fe C18 -175.5(3) . . . . ? Se4 C10 Fe C18 -53.0(3) . . . . ? C14 C10 Fe C19 107.1(2) . . . . ? C11 C10 Fe C19 -134.7(2) . . . . ? Se4 C10 Fe C19 -12.2(3) . . . . ? C14 C10 Fe C13 -37.4(2) . . . . ? C11 C10 Fe C13 80.9(3) . . . . ? Se4 C10 Fe C13 -156.6(3) . . . . ? C14 C10 Fe C12 -80.9(3) . . . . ? C11 C10 Fe C12 37.3(3) . . . . ? Se4 C10 Fe C12 159.9(3) . . . . ? C14 C10 Fe C16 -171.1(3) . . . . ? C11 C10 Fe C16 -52.8(4) . . . . ? Se4 C10 Fe C16 69.7(4) . . . . ? C14 C10 Fe C15 151.3(2) . . . . ? C11 C10 Fe C15 -90.5(3) . . . . ? Se4 C10 Fe C15 32.0(3) . . . . ? C13 C14 Fe C10 -119.1(3) . . . . ? C13 C14 Fe C17 67.2(3) . . . . ? C10 C14 Fe C17 -173.7(2) . . . . ? C13 C14 Fe C11 -80.6(3) . . . . ? C10 C14 Fe C11 38.5(2) . . . . ? C13 C14 Fe C18 106.8(3) . . . . ? C10 C14 Fe C18 -134.1(2) . . . . ? C13 C14 Fe C19 149.5(2) . . . . ? C10 C14 Fe C19 -91.3(2) . . . . ? C10 C14 Fe C13 119.1(3) . . . . ? C13 C14 Fe C12 -37.2(2) . . . . ? C10 C14 Fe C12 82.0(2) . . . . ? C13 C14 Fe C16 38.8(9) . . . . ? C10 C14 Fe C16 157.9(7) . . . . ? C13 C14 Fe C15 -176.4(3) . . . . ? C10 C14 Fe C15 -57.3(4) . . . . ? C18 C17 Fe C10 46.4(10) . . . . ? C16 C17 Fe C10 165.9(8) . . . . ? C18 C17 Fe C14 69.3(3) . . . . ? C16 C17 Fe C14 -171.2(3) . . . . ? C18 C17 Fe C11 -177.1(3) . . . . ? C16 C17 Fe C11 -57.6(4) . . . . ? C16 C17 Fe C18 119.5(4) . . . . ? C18 C17 Fe C19 -37.5(3) . . . . ? C16 C17 Fe C19 82.0(3) . . . . ? C18 C17 Fe C13 107.7(3) . . . . ? C16 C17 Fe C13 -132.8(3) . . . . ? C18 C17 Fe C12 150.2(3) . . . . ? C16 C17 Fe C12 -90.3(3) . . . . ? C18 C17 Fe C16 -119.5(4) . . . . ? C18 C17 Fe C15 -81.7(3) . . . . ? C16 C17 Fe C15 37.8(2) . . . . ? C12 C11 Fe C10 119.2(4) . . . . ? C12 C11 Fe C14 80.8(3) . . . . ? C10 C11 Fe C14 -38.4(2) . . . . ? C12 C11 Fe C17 -49.6(4) . . . . ? C10 C11 Fe C17 -168.8(3) . . . . ? C12 C11 Fe C18 144.3(12) . . . . ? C10 C11 Fe C18 25.1(14) . . . . ? C12 C11 Fe C19 -172.7(2) . . . . ? C10 C11 Fe C19 68.1(3) . . . . ? C12 C11 Fe C13 37.3(2) . . . . ? C10 C11 Fe C13 -81.9(3) . . . . ? C10 C11 Fe C12 -119.2(4) . . . . ? C12 C11 Fe C16 -87.5(3) . . . . ? C10 C11 Fe C16 153.3(2) . . . . ? C12 C11 Fe C15 -131.7(2) . . . . ? C10 C11 Fe C15 109.1(2) . . . . ? C19 C18 Fe C10 71.0(3) . . . . ? C17 C18 Fe C10 -169.6(3) . . . . ? C19 C18 Fe C14 110.2(3) . . . . ? C17 C18 Fe C14 -130.5(3) . . . . ? C19 C18 Fe C17 -119.3(4) . . . . ? C19 C18 Fe C11 49.1(14) . . . . ? C17 C18 Fe C11 168.4(12) . . . . ? C17 C18 Fe C19 119.3(4) . . . . ? C19 C18 Fe C13 152.8(2) . . . . ? C17 C18 Fe C13 -87.9(3) . . . . ? C19 C18 Fe C12 -173.2(3) . . . . ? C17 C18 Fe C12 -53.8(4) . . . . ? C19 C18 Fe C16 -81.8(3) . . . . ? C17 C18 Fe C16 37.5(3) . . . . ? C19 C18 Fe C15 -38.0(2) . . . . ? C17 C18 Fe C15 81.4(3) . . . . ? C18 C19 Fe C10 -131.0(2) . . . . ? C15 C19 Fe C10 109.9(2) . . . . ? C18 C19 Fe C14 -86.5(3) . . . . ? C15 C19 Fe C14 154.4(2) . . . . ? C18 C19 Fe C17 37.6(3) . . . . ? C15 C19 Fe C17 -81.4(2) . . . . ? C18 C19 Fe C11 -171.7(2) . . . . ? C15 C19 Fe C11 69.2(3) . . . . ? C15 C19 Fe C18 -119.1(3) . . . . ? C18 C19 Fe C13 -49.7(4) . . . . ? C15 C19 Fe C13 -168.8(3) . . . . ? C18 C19 Fe C12 149.3(12) . . . . ? C15 C19 Fe C12 30.2(13) . . . . ? C18 C19 Fe C16 81.4(3) . . . . ? C15 C19 Fe C16 -37.6(2) . . . . ? C18 C19 Fe C15 119.1(3) . . . . ? C14 C13 Fe C10 38.2(2) . . . . ? C12 C13 Fe C10 -81.8(2) . . . . ? C12 C13 Fe C14 -120.0(3) . . . . ? C14 C13 Fe C17 -131.7(3) . . . . ? C12 C13 Fe C17 108.3(3) . . . . ? C14 C13 Fe C11 82.7(2) . . . . ? C12 C13 Fe C11 -37.3(2) . . . . ? C14 C13 Fe C18 -89.0(3) . . . . ? C12 C13 Fe C18 151.0(2) . . . . ? C14 C13 Fe C19 -56.2(4) . . . . ? C12 C13 Fe C19 -176.2(3) . . . . ? C14 C13 Fe C12 120.0(3) . . . . ? C14 C13 Fe C16 -170.2(2) . . . . ? C12 C13 Fe C16 69.8(3) . . . . ? C14 C13 Fe C15 169.7(8) . . . . ? C12 C13 Fe C15 49.7(10) . . . . ? C11 C12 Fe C10 -38.2(2) . . . . ? C13 C12 Fe C10 81.5(2) . . . . ? C11 C12 Fe C14 -82.6(2) . . . . ? C13 C12 Fe C14 37.1(2) . . . . ? C11 C12 Fe C17 153.0(2) . . . . ? C13 C12 Fe C17 -87.3(3) . . . . ? C13 C12 Fe C11 119.7(3) . . . . ? C11 C12 Fe C18 -171.8(3) . . . . ? C13 C12 Fe C18 -52.1(4) . . . . ? C11 C12 Fe C19 44.4(13) . . . . ? C13 C12 Fe C19 164.0(12) . . . . ? C11 C12 Fe C13 -119.7(3) . . . . ? C11 C12 Fe C16 109.7(2) . . . . ? C13 C12 Fe C16 -130.6(2) . . . . ? C11 C12 Fe C15 70.9(3) . . . . ? C13 C12 Fe C15 -169.4(2) . . . . ? C17 C16 Fe C10 -174.8(3) . . . . ? C15 C16 Fe C10 -55.9(4) . . . . ? C17 C16 Fe C14 34.6(9) . . . . ? C15 C16 Fe C14 153.5(7) . . . . ? C15 C16 Fe C17 119.0(3) . . . . ? C17 C16 Fe C11 149.2(3) . . . . ? C15 C16 Fe C11 -91.9(2) . . . . ? C17 C16 Fe C18 -37.5(3) . . . . ? C15 C16 Fe C18 81.4(2) . . . . ? C17 C16 Fe C19 -81.1(3) . . . . ? C15 C16 Fe C19 37.8(2) . . . . ? C17 C16 Fe C13 66.4(3) . . . . ? C15 C16 Fe C13 -174.6(2) . . . . ? C17 C16 Fe C12 106.2(3) . . . . ? C15 C16 Fe C12 -134.8(2) . . . . ? C17 C16 Fe C15 -119.0(3) . . . . ? C16 C15 Fe C10 151.7(2) . . . . ? C19 C15 Fe C10 -89.0(2) . . . . ? Se1 C15 Fe C10 28.7(3) . . . . ? C16 C15 Fe C14 -169.4(3) . . . . ? C19 C15 Fe C14 -50.2(4) . . . . ? Se1 C15 Fe C14 67.6(4) . . . . ? C16 C15 Fe C17 -37.8(2) . . . . ? C19 C15 Fe C17 81.4(3) . . . . ? Se1 C15 Fe C17 -160.8(3) . . . . ? C16 C15 Fe C11 106.8(2) . . . . ? C19 C15 Fe C11 -133.9(2) . . . . ? Se1 C15 Fe C11 -16.2(3) . . . . ? C16 C15 Fe C18 -81.6(2) . . . . ? C19 C15 Fe C18 37.6(2) . . . . ? Se1 C15 Fe C18 155.3(3) . . . . ? C16 C15 Fe C19 -119.2(3) . . . . ? Se1 C15 Fe C19 117.7(4) . . . . ? C16 C15 Fe C13 23.9(10) . . . . ? C19 C15 Fe C13 143.1(8) . . . . ? Se1 C15 Fe C13 -99.2(9) . . . . ? C16 C15 Fe C12 65.9(3) . . . . ? C19 C15 Fe C12 -174.9(2) . . . . ? Se1 C15 Fe C12 -57.1(3) . . . . ? C19 C15 Fe C16 119.2(3) . . . . ? Se1 C15 Fe C16 -123.0(3) . . . . ? C16 C15 Se1 C1 -21.0(3) . . . . ? C19 C15 Se1 C1 166.9(3) . . . . ? Fe C15 Se1 C1 75.0(3) . . . . ? C16 C15 Se1 Ag -123.0(3) . . . . ? C19 C15 Se1 Ag 64.9(3) . . . . ? Fe C15 Se1 Ag -27.0(3) . . . . ? C2 C1 Se1 C15 -178.0(3) . . . . ? C2 C1 Se1 Ag -73.4(3) . . . . ? Se4 Ag Se1 C15 -13.07(11) . . . . ? Se3 Ag Se1 C15 -136.50(11) 1_455 . . . ? Se2 Ag Se1 C15 111.67(11) . . . . ? Se4 Ag Se1 C1 -112.64(13) . . . . ? Se3 Ag Se1 C1 123.93(13) 1_455 . . . ? Se2 Ag Se1 C1 12.11(13) . . . . ? C5 C4 Se2 C3 162.8(3) . . . . ? C5 C4 Se2 Ag 67.8(3) . . . . ? C2 C3 Se2 C4 166.1(3) . . . . ? C2 C3 Se2 Ag -90.1(3) . . . . ? Se4 Ag Se2 C4 -105.36(13) . . . . ? Se3 Ag Se2 C4 36.93(13) 1_455 . . . ? Se1 Ag Se2 C4 143.77(13) . . . . ? Se4 Ag Se2 C3 155.08(13) . . . . ? Se3 Ag Se2 C3 -62.62(13) 1_455 . . . ? Se1 Ag Se2 C3 44.21(13) . . . . ? C8 C7 Se3 C6 42.0(4) . . . . ? C8 C7 Se3 Ag -58.0(3) . . . 1_655 ? C5 C6 Se3 C7 61.2(3) . . . . ? C5 C6 Se3 Ag 163.9(3) . . . 1_655 ? C14 C10 Se4 C9 99.3(3) . . . . ? C11 C10 Se4 C9 -86.5(3) . . . . ? Fe C10 Se4 C9 -174.5(2) . . . . ? C14 C10 Se4 Ag -150.7(3) . . . . ? C11 C10 Se4 Ag 23.5(3) . . . . ? Fe C10 Se4 Ag -64.5(2) . . . . ? C8 C9 Se4 C10 59.9(3) . . . . ? C8 C9 Se4 Ag -44.6(3) . . . . ? Se3 Ag Se4 C10 170.34(10) 1_455 . . . ? Se2 Ag Se4 C10 -48.66(10) . . . . ? Se1 Ag Se4 C10 52.64(10) . . . . ? Se3 Ag Se4 C9 -85.16(13) 1_455 . . . ? Se2 Ag Se4 C9 55.84(13) . . . . ? Se1 Ag Se4 C9 157.13(13) . . . . ? ######################################################## # END of CIF ######################################################## # Attachment '- Cu.cif' data_l _database_code_depnum_ccdc_archive 'CCDC 770359' #TrackingRef '- Cu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H26 Cu F6 Fe P Se4' _chemical_formula_weight 834.60 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 19.221(4) _cell_length_b 10.995(2) _cell_length_c 12.001(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2536.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 7.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3244 _exptl_absorpt_correction_T_max 0.5303 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1986)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart Apex CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2429 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.27 _reflns_number_total 2429 _reflns_number_gt 1506 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.060(16) _refine_ls_number_reflns 2429 _refine_ls_number_parameters 277 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.74872(7) -0.08544(10) 0.13103(12) 0.0457(3) Uani 1 1 d . . . Se2 Se 0.87423(6) 0.00382(13) 0.37210(14) 0.0519(3) Uani 1 1 d . . . Se3 Se 0.94823(5) -0.13290(13) 0.09482(12) 0.0487(4) Uani 1 1 d . . . Se4 Se 0.85200(6) -0.34448(12) 0.30100(12) 0.0475(4) Uani 1 1 d . . . Cu Cu 0.85452(6) -0.14148(14) 0.22749(13) 0.0434(4) Uani 1 1 d . . . Fe Fe 0.68581(7) -0.36598(16) 0.20555(15) 0.0392(5) Uani 1 1 d . . . C11 C 0.7328(5) -0.5141(12) 0.2765(11) 0.055(4) Uani 1 1 d D . . H11A H 0.7307 -0.5407 0.3544 0.067 Uiso 1 1 calc R . . C12 C 0.6901(6) -0.5498(12) 0.1884(11) 0.051(4) Uani 1 1 d D . . H12A H 0.6502 -0.6048 0.1950 0.062 Uiso 1 1 calc R . . C13 C 0.7088(6) -0.4922(11) 0.0957(13) 0.050(3) Uani 1 1 d D . . H13A H 0.6851 -0.5015 0.0239 0.060 Uiso 1 1 calc R . . C14 C 0.7649(6) -0.4183(12) 0.1122(11) 0.051(4) Uani 1 1 d D . . H14A H 0.7896 -0.3700 0.0561 0.061 Uiso 1 1 calc R . . C10 C 0.7810(5) -0.4283(10) 0.2262(13) 0.045(3) Uani 1 1 d D . . C16 C 0.6780(5) -0.2209(10) 0.3194(11) 0.050(3) Uani 1 1 d DU . . H16A H 0.7117 -0.1987 0.3772 0.060 Uiso 1 1 calc R . . C17 C 0.6199(6) -0.2976(11) 0.3314(12) 0.061(4) Uani 1 1 d DU . . H17A H 0.6064 -0.3406 0.3996 0.073 Uiso 1 1 calc R . . C18 C 0.5863(6) -0.3079(11) 0.2247(15) 0.065(4) Uani 1 1 d DU . . H18A H 0.5457 -0.3597 0.2113 0.078 Uiso 1 1 calc R . . C19 C 0.6213(5) -0.2407(10) 0.1379(13) 0.051(3) Uani 1 1 d DU . . H19A H 0.6078 -0.2296 0.0598 0.061 Uiso 1 1 calc R . . C15 C 0.6788(5) -0.1826(10) 0.2010(11) 0.038(3) Uani 1 1 d DU . . C1 C 0.7206(6) 0.0738(12) 0.1954(15) 0.077 Uani 1 1 d U . . H1B H 0.6997 0.1223 0.1367 0.092 Uiso 1 1 calc R . . H1A H 0.6850 0.0593 0.2512 0.092 Uiso 1 1 calc R . . C2 C 0.7746(7) 0.1427(15) 0.2449(16) 0.098(5) Uani 1 1 d U . . H2B H 0.7601 0.2267 0.2364 0.117 Uiso 1 1 calc R . . H2A H 0.8141 0.1324 0.1955 0.117 Uiso 1 1 calc R . . C3 C 0.8041(6) 0.1361(13) 0.3578(14) 0.085(5) Uani 1 1 d U . . H3B H 0.7669 0.1224 0.4109 0.102 Uiso 1 1 calc R . . H3A H 0.8258 0.2133 0.3758 0.102 Uiso 1 1 calc R . . C4 C 0.9514(5) 0.0965(10) 0.3194(10) 0.043(3) Uani 1 1 d . . . H4B H 0.9366 0.1474 0.2578 0.051 Uiso 1 1 calc R . . H4A H 0.9679 0.1493 0.3785 0.051 Uiso 1 1 calc R . . C5 C 1.0117(5) 0.0131(11) 0.2804(11) 0.044(4) Uani 1 1 d . . . H5B H 1.0554 0.0504 0.3018 0.052 Uiso 1 1 calc R . . H5A H 1.0081 -0.0638 0.3196 0.052 Uiso 1 1 calc R . . C6 C 1.0138(6) -0.0129(12) 0.1547(12) 0.059(4) Uani 1 1 d . . . H6B H 1.0604 -0.0396 0.1361 0.071 Uiso 1 1 calc R . . H6A H 1.0059 0.0633 0.1159 0.071 Uiso 1 1 calc R . . C7 C 1.0035(6) -0.2742(10) 0.1313(14) 0.060(4) Uani 1 1 d U . . H7B H 1.0387 -0.2838 0.0739 0.072 Uiso 1 1 calc R . . H7A H 1.0276 -0.2580 0.2007 0.072 Uiso 1 1 calc R . . C8 C 0.9655(6) -0.3938(12) 0.1432(14) 0.073(4) Uani 1 1 d U . . H8B H 0.9974 -0.4573 0.1200 0.087 Uiso 1 1 calc R . . H8A H 0.9277 -0.3932 0.0895 0.087 Uiso 1 1 calc R . . C9 C 0.9347(6) -0.4332(12) 0.2542(11) 0.056(4) Uani 1 1 d U . . H9B H 0.9701 -0.4241 0.3112 0.067 Uiso 1 1 calc R . . H9A H 0.9232 -0.5190 0.2496 0.067 Uiso 1 1 calc R . . P P 0.89849(19) -0.7245(4) -0.0187(3) 0.0531(10) Uani 1 1 d . . . F1 F 0.9793(4) -0.7519(9) -0.0348(9) 0.103(3) Uani 1 1 d . . . F2 F 0.9112(4) -0.5860(8) -0.0555(7) 0.091 Uani 1 1 d . . . F3 F 0.8177(3) -0.6972(8) -0.0011(8) 0.088(3) Uani 1 1 d . . . F4 F 0.9099(4) -0.6889(7) 0.1075(8) 0.092(3) Uani 1 1 d . . . F5 F 0.8875(4) -0.7563(8) -0.1421(6) 0.098(3) Uani 1 1 d . . . F6 F 0.8867(4) -0.8624(6) 0.0203(8) 0.079(2) 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 Se1 0.0300(5) 0.0541(7) 0.0528(8) 0.0073(8) -0.0052(6) 0.0014(8) Se2 0.0421(6) 0.0668(8) 0.0470(8) -0.0037(10) 0.0029(7) -0.0008(7) Se3 0.0337(6) 0.0710(9) 0.0413(8) 0.0010(8) 0.0007(6) 0.0061(7) Se4 0.0448(7) 0.0542(8) 0.0436(8) 0.0056(9) -0.0081(7) -0.0020(7) Cu 0.0251(7) 0.0542(9) 0.0508(11) -0.0017(10) -0.0021(8) 0.0004(7) Fe 0.0269(9) 0.0525(11) 0.0384(12) 0.0006(11) 0.0040(8) 0.0002(8) C11 0.042(8) 0.069(9) 0.055(10) 0.024(9) -0.019(7) 0.005(7) C12 0.038(7) 0.072(10) 0.044(10) 0.006(8) 0.009(7) -0.003(7) C13 0.044(8) 0.048(8) 0.058(10) -0.010(9) -0.012(7) -0.006(7) C14 0.055(9) 0.075(9) 0.021(8) -0.003(8) -0.008(7) -0.002(7) C10 0.032(6) 0.036(7) 0.067(11) -0.010(9) 0.010(7) 0.002(6) C16 0.044(6) 0.056(7) 0.051(6) 0.001(6) 0.012(5) -0.003(5) C17 0.052(6) 0.070(7) 0.059(6) -0.014(6) 0.021(5) -0.005(6) C18 0.053(6) 0.063(7) 0.081(8) -0.001(7) 0.005(6) -0.010(5) C19 0.042(6) 0.049(6) 0.062(6) 0.007(6) -0.015(5) 0.005(5) C15 0.022(5) 0.046(6) 0.046(6) 0.005(5) -0.013(5) 0.012(4) C1 0.048 0.054 0.128 0.016 -0.008 0.020 C2 0.100(8) 0.087(8) 0.107(9) 0.006(8) -0.026(7) 0.010(7) C3 0.066(7) 0.098(9) 0.090(8) -0.006(8) 0.006(6) 0.004(7) C4 0.044(7) 0.058(8) 0.026(7) 0.003(7) -0.016(6) -0.012(6) C5 0.029(7) 0.031(7) 0.071(11) -0.003(8) -0.010(7) -0.022(6) C6 0.032(8) 0.072(9) 0.073(12) -0.028(10) -0.009(7) 0.021(7) C7 0.049(6) 0.073(7) 0.059(7) -0.013(7) 0.010(6) 0.003(5) C8 0.074(7) 0.070(7) 0.074(8) 0.000(7) -0.006(7) 0.011(6) C9 0.049(6) 0.066(7) 0.053(7) 0.005(6) -0.034(5) 0.004(5) P 0.056(2) 0.066(3) 0.038(3) 0.008(2) -0.0042(18) 0.008(2) F1 0.058(4) 0.133(9) 0.118(9) 0.038(7) -0.014(5) 0.022(5) F2 0.091 0.091 0.091 0.000 0.000 0.000 F3 0.047(4) 0.112(7) 0.104(8) 0.033(7) 0.003(5) 0.022(5) F4 0.123(7) 0.112(7) 0.042(6) 0.002(6) 0.000(5) -0.007(6) F5 0.118(7) 0.140(8) 0.037(6) -0.016(7) -0.022(5) 0.022(6) F6 0.111(6) 0.052(5) 0.073(6) 0.017(5) -0.007(5) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 C15 1.910(12) . ? Se1 C1 1.989(14) . ? Se1 Cu 2.4197(19) . ? Se2 C4 1.908(10) . ? Se2 C3 1.990(13) . ? Se2 Cu 2.389(2) . ? Se3 C7 1.933(12) . ? Se3 C6 1.960(12) . ? Se3 Cu 2.4059(19) . ? Se4 C10 1.875(12) . ? Se4 C9 1.948(12) . ? Se4 Cu 2.400(2) . ? Fe C13 1.965(13) . ? Fe C10 1.970(10) . ? Fe C14 1.974(12) . ? Fe C15 2.022(11) . ? Fe C19 2.024(11) . ? Fe C18 2.029(11) . ? Fe C12 2.034(13) . ? Fe C11 2.048(11) . ? Fe C16 2.106(12) . ? Fe C17 2.109(12) . ? C11 C12 1.394(16) . ? C11 C10 1.455(15) . ? C11 H11A 0.9800 . ? C12 C13 1.331(17) . ? C12 H12A 0.9800 . ? C13 C14 1.364(15) . ? C13 H13A 0.9800 . ? C14 C10 1.407(19) . ? C14 H14A 0.9800 . ? C16 C17 1.406(15) . ? C16 C15 1.483(17) . ? C16 H16A 0.9800 . ? C17 C18 1.44(2) . ? C17 H17A 0.9800 . ? C18 C19 1.443(18) . ? C18 H18A 0.9800 . ? C19 C15 1.485(15) . ? C19 H19A 0.9800 . ? C1 C2 1.415(17) . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C2 C3 1.47(2) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? C4 C5 1.549(15) . ? C4 H4B 0.9700 . ? C4 H4A 0.9700 . ? C5 C6 1.536(17) . ? C5 H5B 0.9700 . ? C5 H5A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6A 0.9700 . ? C7 C8 1.512(15) . ? C7 H7B 0.9700 . ? C7 H7A 0.9700 . ? C8 C9 1.520(19) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9A 0.9700 . ? P F5 1.537(8) . ? P F4 1.580(10) . ? P F1 1.593(8) . ? P F3 1.596(7) . ? P F6 1.603(8) . ? P F2 1.604(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Se1 C1 97.5(5) . . ? C15 Se1 Cu 103.8(3) . . ? C1 Se1 Cu 105.5(4) . . ? C4 Se2 C3 96.2(5) . . ? C4 Se2 Cu 103.9(4) . . ? C3 Se2 Cu 108.6(5) . . ? C7 Se3 C6 96.0(5) . . ? C7 Se3 Cu 103.3(4) . . ? C6 Se3 Cu 105.4(4) . . ? C10 Se4 C9 102.1(5) . . ? C10 Se4 Cu 107.2(4) . . ? C9 Se4 Cu 110.1(4) . . ? Se2 Cu Se4 110.97(8) . . ? Se2 Cu Se3 109.62(7) . . ? Se4 Cu Se3 107.14(7) . . ? Se2 Cu Se1 108.09(7) . . ? Se4 Cu Se1 113.31(7) . . ? Se3 Cu Se1 107.61(8) . . ? C13 Fe C10 68.2(5) . . ? C13 Fe C14 40.5(4) . . ? C10 Fe C14 41.8(5) . . ? C13 Fe C15 134.5(6) . . ? C10 Fe C15 114.3(4) . . ? C14 Fe C15 109.0(5) . . ? C13 Fe C19 110.4(6) . . ? C10 Fe C19 148.9(5) . . ? C14 Fe C19 116.3(6) . . ? C15 Fe C19 43.1(4) . . ? C13 Fe C18 120.7(6) . . ? C10 Fe C18 166.1(7) . . ? C14 Fe C18 151.8(6) . . ? C15 Fe C18 68.1(5) . . ? C19 Fe C18 41.7(5) . . ? C13 Fe C12 38.8(5) . . ? C10 Fe C12 68.2(4) . . ? C14 Fe C12 67.8(5) . . ? C15 Fe C12 172.5(6) . . ? C19 Fe C12 131.4(5) . . ? C18 Fe C12 111.3(5) . . ? C13 Fe C11 67.5(6) . . ? C10 Fe C11 42.4(4) . . ? C14 Fe C11 70.4(5) . . ? C15 Fe C11 146.5(5) . . ? C19 Fe C11 168.1(4) . . ? C18 Fe C11 128.2(5) . . ? C12 Fe C11 39.9(5) . . ? C13 Fe C16 170.6(5) . . ? C10 Fe C16 104.4(5) . . ? C14 Fe C16 130.1(5) . . ? C15 Fe C16 42.0(5) . . ? C19 Fe C16 72.6(5) . . ? C18 Fe C16 67.7(5) . . ? C12 Fe C16 145.2(5) . . ? C11 Fe C16 111.4(5) . . ? C13 Fe C17 150.2(5) . . ? C10 Fe C17 126.3(6) . . ? C14 Fe C17 166.5(5) . . ? C15 Fe C17 67.9(5) . . ? C19 Fe C17 71.2(6) . . ? C18 Fe C17 40.6(6) . . ? C12 Fe C17 116.8(5) . . ? C11 Fe C17 104.5(5) . . ? C16 Fe C17 39.0(4) . . ? C12 C11 C10 104.1(11) . . ? C12 C11 Fe 69.5(7) . . ? C10 C11 Fe 65.9(6) . . ? C12 C11 H11A 128.0 . . ? C10 C11 H11A 128.0 . . ? Fe C11 H11A 128.0 . . ? C13 C12 C11 109.9(12) . . ? C13 C12 Fe 67.8(7) . . ? C11 C12 Fe 70.6(7) . . ? C13 C12 H12A 125.0 . . ? C11 C12 H12A 125.0 . . ? Fe C12 H12A 125.0 . . ? C12 C13 C14 112.1(14) . . ? C12 C13 Fe 73.4(8) . . ? C14 C13 Fe 70.1(7) . . ? C12 C13 H13A 124.0 . . ? C14 C13 H13A 124.0 . . ? Fe C13 H13A 124.0 . . ? C13 C14 C10 105.6(12) . . ? C13 C14 Fe 69.4(7) . . ? C10 C14 Fe 68.9(7) . . ? C13 C14 H14A 127.2 . . ? C10 C14 H14A 127.2 . . ? Fe C14 H14A 127.2 . . ? C14 C10 C11 108.3(11) . . ? C14 C10 Se4 126.0(10) . . ? C11 C10 Se4 125.8(11) . . ? C14 C10 Fe 69.3(7) . . ? C11 C10 Fe 71.7(6) . . ? Se4 C10 Fe 124.4(6) . . ? C17 C16 C15 106.1(11) . . ? C17 C16 Fe 70.6(7) . . ? C15 C16 Fe 65.9(6) . . ? C17 C16 H16A 126.9 . . ? C15 C16 H16A 126.9 . . ? Fe C16 H16A 126.9 . . ? C16 C17 C18 108.2(12) . . ? C16 C17 Fe 70.4(7) . . ? C18 C17 Fe 66.7(7) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? Fe C17 H17A 125.9 . . ? C17 C18 C19 113.2(11) . . ? C17 C18 Fe 72.7(6) . . ? C19 C18 Fe 68.9(6) . . ? C17 C18 H18A 123.4 . . ? C19 C18 H18A 123.4 . . ? Fe C18 H18A 123.4 . . ? C18 C19 C15 101.5(12) . . ? C18 C19 Fe 69.3(7) . . ? C15 C19 Fe 68.4(6) . . ? C18 C19 H19A 129.1 . . ? C15 C19 H19A 129.1 . . ? Fe C19 H19A 129.1 . . ? C16 C15 C19 111.0(11) . . ? C16 C15 Se1 126.0(8) . . ? C19 C15 Se1 122.7(10) . . ? C16 C15 Fe 72.0(7) . . ? C19 C15 Fe 68.5(6) . . ? Se1 C15 Fe 121.5(6) . . ? C2 C1 Se1 115.8(9) . . ? C2 C1 H1B 108.3 . . ? Se1 C1 H1B 108.3 . . ? C2 C1 H1A 108.3 . . ? Se1 C1 H1A 108.3 . . ? H1B C1 H1A 107.4 . . ? C1 C2 C3 130.1(17) . . ? C1 C2 H2B 104.8 . . ? C3 C2 H2B 104.8 . . ? C1 C2 H2A 104.8 . . ? C3 C2 H2A 104.8 . . ? H2B C2 H2A 105.8 . . ? C2 C3 Se2 112.1(11) . . ? C2 C3 H3B 109.2 . . ? Se2 C3 H3B 109.2 . . ? C2 C3 H3A 109.2 . . ? Se2 C3 H3A 109.2 . . ? H3B C3 H3A 107.9 . . ? C5 C4 Se2 111.4(7) . . ? C5 C4 H4B 109.3 . . ? Se2 C4 H4B 109.3 . . ? C5 C4 H4A 109.3 . . ? Se2 C4 H4A 109.3 . . ? H4B C4 H4A 108.0 . . ? C6 C5 C4 115.3(10) . . ? C6 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? H5B C5 H5A 107.5 . . ? C5 C6 Se3 117.9(9) . . ? C5 C6 H6B 107.8 . . ? Se3 C6 H6B 107.8 . . ? C5 C6 H6A 107.8 . . ? Se3 C6 H6A 107.8 . . ? H6B C6 H6A 107.2 . . ? C8 C7 Se3 117.1(9) . . ? C8 C7 H7B 108.0 . . ? Se3 C7 H7B 108.0 . . ? C8 C7 H7A 108.0 . . ? Se3 C7 H7A 108.0 . . ? H7B C7 H7A 107.3 . . ? C7 C8 C9 121.2(14) . . ? C7 C8 H8B 107.0 . . ? C9 C8 H8B 107.0 . . ? C7 C8 H8A 107.0 . . ? C9 C8 H8A 107.0 . . ? H8B C8 H8A 106.8 . . ? C8 C9 Se4 115.3(9) . . ? C8 C9 H9B 108.4 . . ? Se4 C9 H9B 108.4 . . ? C8 C9 H9A 108.4 . . ? Se4 C9 H9A 108.4 . . ? H9B C9 H9A 107.5 . . ? F5 P F4 178.8(6) . . ? F5 P F1 88.5(5) . . ? F4 P F1 91.6(5) . . ? F5 P F3 92.1(5) . . ? F4 P F3 87.8(5) . . ? F1 P F3 179.4(6) . . ? F5 P F6 92.7(5) . . ? F4 P F6 88.5(5) . . ? F1 P F6 89.7(5) . . ? F3 P F6 90.1(5) . . ? F5 P F2 88.4(5) . . ? F4 P F2 90.4(5) . . ? F1 P F2 89.8(5) . . ? F3 P F2 90.4(5) . . ? F6 P F2 178.9(5) . . ? 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 C4 Se2 Cu Se4 127.2(3) . . . . ? C3 Se2 Cu Se4 -131.3(5) . . . . ? C4 Se2 Cu Se3 9.1(3) . . . . ? C3 Se2 Cu Se3 110.6(5) . . . . ? C4 Se2 Cu Se1 -108.0(3) . . . . ? C3 Se2 Cu Se1 -6.4(5) . . . . ? C10 Se4 Cu Se2 140.3(4) . . . . ? C9 Se4 Cu Se2 -109.5(4) . . . . ? C10 Se4 Cu Se3 -100.1(4) . . . . ? C9 Se4 Cu Se3 10.2(4) . . . . ? C10 Se4 Cu Se1 18.4(4) . . . . ? C9 Se4 Cu Se1 128.7(4) . . . . ? C7 Se3 Cu Se2 103.2(4) . . . . ? C6 Se3 Cu Se2 3.0(4) . . . . ? C7 Se3 Cu Se4 -17.4(4) . . . . ? C6 Se3 Cu Se4 -117.5(4) . . . . ? C7 Se3 Cu Se1 -139.5(4) . . . . ? C6 Se3 Cu Se1 120.3(4) . . . . ? C15 Se1 Cu Se2 -95.7(4) . . . . ? C1 Se1 Cu Se2 6.2(5) . . . . ? C15 Se1 Cu Se4 27.7(4) . . . . ? C1 Se1 Cu Se4 129.7(4) . . . . ? C15 Se1 Cu Se3 146.0(4) . . . . ? C1 Se1 Cu Se3 -112.1(4) . . . . ? C13 Fe C11 C12 -35.0(6) . . . . ? C10 Fe C11 C12 -116.8(10) . . . . ? C14 Fe C11 C12 -78.4(8) . . . . ? C15 Fe C11 C12 -173.6(9) . . . . ? C19 Fe C11 C12 48(3) . . . . ? C18 Fe C11 C12 77.2(9) . . . . ? C16 Fe C11 C12 155.1(7) . . . . ? C17 Fe C11 C12 114.6(7) . . . . ? C13 Fe C11 C10 81.8(8) . . . . ? C14 Fe C11 C10 38.4(8) . . . . ? C15 Fe C11 C10 -56.7(12) . . . . ? C19 Fe C11 C10 164(3) . . . . ? C18 Fe C11 C10 -166.0(8) . . . . ? C12 Fe C11 C10 116.8(10) . . . . ? C16 Fe C11 C10 -88.1(8) . . . . ? C17 Fe C11 C10 -128.5(8) . . . . ? C10 C11 C12 C13 -0.8(12) . . . . ? Fe C11 C12 C13 56.3(8) . . . . ? C10 C11 C12 Fe -57.1(7) . . . . ? C10 Fe C12 C13 -81.9(8) . . . . ? C14 Fe C12 C13 -36.7(7) . . . . ? C15 Fe C12 C13 29(4) . . . . ? C19 Fe C12 C13 69.4(9) . . . . ? C18 Fe C12 C13 113.0(9) . . . . ? C11 Fe C12 C13 -122.3(10) . . . . ? C16 Fe C12 C13 -165.8(8) . . . . ? C17 Fe C12 C13 157.3(7) . . . . ? C13 Fe C12 C11 122.3(10) . . . . ? C10 Fe C12 C11 40.4(7) . . . . ? C14 Fe C12 C11 85.6(8) . . . . ? C15 Fe C12 C11 152(3) . . . . ? C19 Fe C12 C11 -168.3(8) . . . . ? C18 Fe C12 C11 -124.7(8) . . . . ? C16 Fe C12 C11 -43.5(11) . . . . ? C17 Fe C12 C11 -80.4(8) . . . . ? C11 C12 C13 C14 1.8(13) . . . . ? Fe C12 C13 C14 59.7(8) . . . . ? C11 C12 C13 Fe -58.0(8) . . . . ? C10 Fe C13 C12 81.9(8) . . . . ? C14 Fe C13 C12 121.7(12) . . . . ? C15 Fe C13 C12 -174.8(7) . . . . ? C19 Fe C13 C12 -131.4(7) . . . . ? C18 Fe C13 C12 -86.3(10) . . . . ? C11 Fe C13 C12 35.9(7) . . . . ? C16 Fe C13 C12 121(3) . . . . ? C17 Fe C13 C12 -43.9(14) . . . . ? C10 Fe C13 C14 -39.8(8) . . . . ? C15 Fe C13 C14 63.5(10) . . . . ? C19 Fe C13 C14 106.9(9) . . . . ? C18 Fe C13 C14 152.1(8) . . . . ? C12 Fe C13 C14 -121.7(12) . . . . ? C11 Fe C13 C14 -85.7(8) . . . . ? C16 Fe C13 C14 0(4) . . . . ? C17 Fe C13 C14 -165.5(10) . . . . ? C12 C13 C14 C10 -1.9(14) . . . . ? Fe C13 C14 C10 59.7(8) . . . . ? C12 C13 C14 Fe -61.7(9) . . . . ? C10 Fe C14 C13 116.9(12) . . . . ? C15 Fe C14 C13 -137.5(8) . . . . ? C19 Fe C14 C13 -91.3(9) . . . . ? C18 Fe C14 C13 -58.6(15) . . . . ? C12 Fe C14 C13 35.2(8) . . . . ? C11 Fe C14 C13 78.0(9) . . . . ? C16 Fe C14 C13 179.9(8) . . . . ? C17 Fe C14 C13 148(2) . . . . ? C13 Fe C14 C10 -116.9(12) . . . . ? C15 Fe C14 C10 105.5(8) . . . . ? C19 Fe C14 C10 151.8(7) . . . . ? C18 Fe C14 C10 -175.5(9) . . . . ? C12 Fe C14 C10 -81.7(8) . . . . ? C11 Fe C14 C10 -38.9(7) . . . . ? C16 Fe C14 C10 63.0(10) . . . . ? C17 Fe C14 C10 31(3) . . . . ? C13 C14 C10 C11 1.3(13) . . . . ? Fe C14 C10 C11 61.4(8) . . . . ? C13 C14 C10 Se4 -178.2(7) . . . . ? Fe C14 C10 Se4 -118.2(9) . . . . ? C13 C14 C10 Fe -60.0(8) . . . . ? C12 C11 C10 C14 -0.4(12) . . . . ? Fe C11 C10 C14 -59.8(8) . . . . ? C12 C11 C10 Se4 179.2(8) . . . . ? Fe C11 C10 Se4 119.7(9) . . . . ? C12 C11 C10 Fe 59.5(7) . . . . ? C9 Se4 C10 C14 -76.5(11) . . . . ? Cu Se4 C10 C14 39.2(11) . . . . ? C9 Se4 C10 C11 104.1(10) . . . . ? Cu Se4 C10 C11 -140.2(8) . . . . ? C9 Se4 C10 Fe -164.6(9) . . . . ? Cu Se4 C10 Fe -48.9(9) . . . . ? C13 Fe C10 C14 38.6(8) . . . . ? C15 Fe C10 C14 -91.8(9) . . . . ? C19 Fe C10 C14 -55.2(13) . . . . ? C18 Fe C10 C14 171.2(19) . . . . ? C12 Fe C10 C14 80.5(8) . . . . ? C11 Fe C10 C14 118.6(11) . . . . ? C16 Fe C10 C14 -135.3(8) . . . . ? C17 Fe C10 C14 -171.4(8) . . . . ? C13 Fe C10 C11 -80.0(8) . . . . ? C14 Fe C10 C11 -118.6(11) . . . . ? C15 Fe C10 C11 149.6(7) . . . . ? C19 Fe C10 C11 -173.8(10) . . . . ? C18 Fe C10 C11 53(2) . . . . ? C12 Fe C10 C11 -38.1(7) . . . . ? C16 Fe C10 C11 106.1(8) . . . . ? C17 Fe C10 C11 70.0(9) . . . . ? C13 Fe C10 Se4 158.7(11) . . . . ? C14 Fe C10 Se4 120.1(12) . . . . ? C15 Fe C10 Se4 28.3(11) . . . . ? C19 Fe C10 Se4 64.9(15) . . . . ? C18 Fe C10 Se4 -69(2) . . . . ? C12 Fe C10 Se4 -159.3(11) . . . . ? C11 Fe C10 Se4 -121.3(13) . . . . ? C16 Fe C10 Se4 -15.2(10) . . . . ? C17 Fe C10 Se4 -51.3(11) . . . . ? C13 Fe C16 C17 -168(3) . . . . ? C10 Fe C16 C17 -130.9(8) . . . . ? C14 Fe C16 C17 -168.6(8) . . . . ? C15 Fe C16 C17 118.6(10) . . . . ? C19 Fe C16 C17 81.3(8) . . . . ? C18 Fe C16 C17 37.1(8) . . . . ? C12 Fe C16 C17 -58.4(11) . . . . ? C11 Fe C16 C17 -86.8(8) . . . . ? C13 Fe C16 C15 73(4) . . . . ? C10 Fe C16 C15 110.5(7) . . . . ? C14 Fe C16 C15 72.7(9) . . . . ? C19 Fe C16 C15 -37.3(6) . . . . ? C18 Fe C16 C15 -81.5(8) . . . . ? C12 Fe C16 C15 -177.1(7) . . . . ? C11 Fe C16 C15 154.6(6) . . . . ? C17 Fe C16 C15 -118.6(10) . . . . ? C15 C16 C17 C18 0.6(11) . . . . ? Fe C16 C17 C18 -56.0(7) . . . . ? C15 C16 C17 Fe 56.6(7) . . . . ? C13 Fe C17 C16 176.2(10) . . . . ? C10 Fe C17 C16 65.3(9) . . . . ? C14 Fe C17 C16 40(3) . . . . ? C15 Fe C17 C16 -39.4(7) . . . . ? C19 Fe C17 C16 -85.4(8) . . . . ? C18 Fe C17 C16 -121.0(11) . . . . ? C12 Fe C17 C16 147.0(8) . . . . ? C11 Fe C17 C16 106.2(8) . . . . ? C13 Fe C17 C18 -62.9(14) . . . . ? C10 Fe C17 C18 -173.7(7) . . . . ? C14 Fe C17 C18 161(2) . . . . ? C15 Fe C17 C18 81.6(8) . . . . ? C19 Fe C17 C18 35.6(7) . . . . ? C12 Fe C17 C18 -92.0(9) . . . . ? C11 Fe C17 C18 -132.8(8) . . . . ? C16 Fe C17 C18 121.0(11) . . . . ? C16 C17 C18 C19 1.1(12) . . . . ? Fe C17 C18 C19 -57.1(8) . . . . ? C16 C17 C18 Fe 58.2(7) . . . . ? C13 Fe C18 C17 149.0(8) . . . . ? C10 Fe C18 C17 22(2) . . . . ? C14 Fe C18 C17 -170.8(11) . . . . ? C15 Fe C18 C17 -81.2(8) . . . . ? C19 Fe C18 C17 -124.2(11) . . . . ? C12 Fe C18 C17 106.8(8) . . . . ? C11 Fe C18 C17 64.6(10) . . . . ? C16 Fe C18 C17 -35.7(7) . . . . ? C13 Fe C18 C19 -86.8(9) . . . . ? C10 Fe C18 C19 145.8(19) . . . . ? C14 Fe C18 C19 -46.6(14) . . . . ? C15 Fe C18 C19 43.0(8) . . . . ? C12 Fe C18 C19 -129.0(8) . . . . ? C11 Fe C18 C19 -171.2(8) . . . . ? C16 Fe C18 C19 88.5(8) . . . . ? C17 Fe C18 C19 124.2(11) . . . . ? C17 C18 C19 C15 -2.2(12) . . . . ? Fe C18 C19 C15 -61.4(7) . . . . ? C17 C18 C19 Fe 59.2(8) . . . . ? C13 Fe C19 C18 113.6(9) . . . . ? C10 Fe C19 C18 -164.9(10) . . . . ? C14 Fe C19 C18 157.5(8) . . . . ? C15 Fe C19 C18 -112.2(12) . . . . ? C12 Fe C19 C18 74.8(10) . . . . ? C11 Fe C19 C18 36(3) . . . . ? C16 Fe C19 C18 -75.8(8) . . . . ? C17 Fe C19 C18 -34.7(8) . . . . ? C13 Fe C19 C15 -134.2(8) . . . . ? C10 Fe C19 C15 -52.6(13) . . . . ? C14 Fe C19 C15 -90.3(9) . . . . ? C18 Fe C19 C15 112.2(12) . . . . ? C12 Fe C19 C15 -173.0(7) . . . . ? C11 Fe C19 C15 148(3) . . . . ? C16 Fe C19 C15 36.4(7) . . . . ? C17 Fe C19 C15 77.5(8) . . . . ? C17 C16 C15 C19 -2.0(12) . . . . ? Fe C16 C15 C19 57.5(7) . . . . ? C17 C16 C15 Se1 -175.9(8) . . . . ? Fe C16 C15 Se1 -116.3(8) . . . . ? C17 C16 C15 Fe -59.6(7) . . . . ? C18 C19 C15 C16 2.5(12) . . . . ? Fe C19 C15 C16 -59.6(8) . . . . ? C18 C19 C15 Se1 176.6(7) . . . . ? Fe C19 C15 Se1 114.5(8) . . . . ? C18 C19 C15 Fe 62.1(7) . . . . ? C1 Se1 C15 C16 -75.4(10) . . . . ? Cu Se1 C15 C16 32.6(10) . . . . ? C1 Se1 C15 C19 111.4(9) . . . . ? Cu Se1 C15 C19 -140.6(7) . . . . ? C1 Se1 C15 Fe -165.3(7) . . . . ? Cu Se1 C15 Fe -57.3(7) . . . . ? C13 Fe C15 C16 -167.3(7) . . . . ? C10 Fe C15 C16 -84.6(8) . . . . ? C14 Fe C15 C16 -129.4(7) . . . . ? C19 Fe C15 C16 122.2(10) . . . . ? C18 Fe C15 C16 80.6(8) . . . . ? C12 Fe C15 C16 167(3) . . . . ? C11 Fe C15 C16 -46.3(12) . . . . ? C17 Fe C15 C16 36.6(7) . . . . ? C13 Fe C15 C19 70.5(9) . . . . ? C10 Fe C15 C19 153.3(8) . . . . ? C14 Fe C15 C19 108.5(8) . . . . ? C18 Fe C15 C19 -41.6(8) . . . . ? C12 Fe C15 C19 45(4) . . . . ? C11 Fe C15 C19 -168.5(9) . . . . ? C16 Fe C15 C19 -122.2(10) . . . . ? C17 Fe C15 C19 -85.6(8) . . . . ? C13 Fe C15 Se1 -45.6(10) . . . . ? C10 Fe C15 Se1 37.1(10) . . . . ? C14 Fe C15 Se1 -7.7(9) . . . . ? C19 Fe C15 Se1 -116.1(11) . . . . ? C18 Fe C15 Se1 -157.7(9) . . . . ? C12 Fe C15 Se1 -71(3) . . . . ? C11 Fe C15 Se1 75.4(12) . . . . ? C16 Fe C15 Se1 121.7(9) . . . . ? C17 Fe C15 Se1 158.3(8) . . . . ? C15 Se1 C1 C2 129.9(14) . . . . ? Cu Se1 C1 C2 23.3(14) . . . . ? Se1 C1 C2 C3 -84(2) . . . . ? C1 C2 C3 Se2 81.8(19) . . . . ? C4 Se2 C3 C2 85.5(12) . . . . ? Cu Se2 C3 C2 -21.4(13) . . . . ? C3 Se2 C4 C5 -160.6(9) . . . . ? Cu Se2 C4 C5 -49.7(8) . . . . ? Se2 C4 C5 C6 96.2(11) . . . . ? C4 C5 C6 Se3 -77.7(12) . . . . ? C7 Se3 C6 C5 -83.0(10) . . . . ? Cu Se3 C6 C5 22.6(10) . . . . ? C6 Se3 C7 C8 156.8(14) . . . . ? Cu Se3 C7 C8 49.4(14) . . . . ? Se3 C7 C8 C9 -88.3(16) . . . . ? C7 C8 C9 Se4 72.3(14) . . . . ? C10 Se4 C9 C8 84.4(10) . . . . ? Cu Se4 C9 C8 -29.2(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.541 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.130 ######################################################## # END of CIF ######################################################## # Attachment '- Pt.cif' data_js139 _database_code_depnum_ccdc_archive 'CCDC 770360' #TrackingRef '- Pt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 Fe Pt Se4 2+, 2(P F6) 2-' _chemical_formula_sum 'C19 H26 F12 Fe P2 Pt Se4' _chemical_formula_weight 1111.12 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 10.1013(4) _cell_length_b 18.6014(6) _cell_length_c 16.1256(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.735(4) _cell_angle_gamma 90.00 _cell_volume 2916.43(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9390 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 28.86 _exptl_crystal_description 'irregular prism' _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 10.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.132 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Oxford Diffraction software, CrysAlisPro 171.29.2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.4547 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24022 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 5113 _reflns_number_gt 3477 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Oxford Diffraction software, CrysAlisPro 171.29.2' _computing_cell_refinement 'Oxford Diffraction software, CrysAlisPro, Version 171.33.41' _computing_data_reduction 'Oxford Diffraction software, CrysAlisPro 171.29.2' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+37.9709P] 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 5113 _refine_ls_number_parameters 480 _refine_ls_number_restraints 504 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.721 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.192 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 Pt Pt 0.82521(5) 0.04894(2) 0.24886(3) 0.04392(15) Uani 1 1 d . . . Se1 Se 0.74374(14) -0.03268(6) 0.34452(8) 0.0520(3) Uani 1 1 d D . . Se2 Se 0.66004(18) -0.00205(9) 0.12648(9) 0.0791(5) Uani 1 1 d D . . Se3 Se 0.88153(17) 0.14267(8) 0.16295(10) 0.0743(5) Uani 1 1 d D . . Se4 Se 0.98685(13) 0.08336(7) 0.38371(9) 0.0594(4) Uani 1 1 d D . . C1 C 0.5853(14) -0.0852(8) 0.2731(9) 0.082(5) Uani 1 1 d D . . H11 H 0.5453 -0.1134 0.3107 0.098 Uiso 1 1 calc R . . H12 H 0.5168 -0.0504 0.2440 0.098 Uiso 1 1 calc R . . C2 C 0.6140(18) -0.1331(8) 0.2084(10) 0.095(5) Uani 1 1 d D . . H21 H 0.6634 -0.1744 0.2382 0.114 Uiso 1 1 calc R . . H22 H 0.5266 -0.1504 0.1725 0.114 Uiso 1 1 calc R . . C3 C 0.691(2) -0.1047(7) 0.1525(11) 0.113(7) Uani 1 1 d D . . H31 H 0.6669 -0.1314 0.0988 0.135 Uiso 1 1 calc R . . H32 H 0.7884 -0.1123 0.1793 0.135 Uiso 1 1 calc R . . C4 C 0.755(3) -0.0062(12) 0.0344(11) 0.152(7) Uani 1 1 d DU . . H41 H 0.8330 -0.0382 0.0531 0.182 Uiso 1 1 calc R . . H42 H 0.6923 -0.0276 -0.0161 0.182 Uiso 1 1 calc R . . C5 C 0.803(3) 0.0606(12) 0.0092(13) 0.152(6) Uani 1 1 d DU . . H51 H 0.7253 0.0935 -0.0017 0.182 Uiso 1 1 calc R . . H52 H 0.8210 0.0520 -0.0460 0.182 Uiso 1 1 calc R . . C6 C 0.919(2) 0.0995(11) 0.0605(10) 0.134(6) Uani 1 1 d DU . . H61 H 0.9438 0.1371 0.0258 0.161 Uiso 1 1 calc R . . H62 H 0.9969 0.0671 0.0785 0.161 Uiso 1 1 calc R . . C7 C 1.0730(15) 0.1739(11) 0.2123(12) 0.117(7) Uani 1 1 d D . . H71 H 1.1331 0.1351 0.2051 0.141 Uiso 1 1 calc R . . H72 H 1.0903 0.2144 0.1787 0.141 Uiso 1 1 calc R . . C8 C 1.1125(17) 0.1952(9) 0.3041(12) 0.113(7) Uani 1 1 d D . . H81 H 1.1929 0.2259 0.3138 0.135 Uiso 1 1 calc R . . H82 H 1.0386 0.2242 0.3143 0.135 Uiso 1 1 calc R . . C9 C 1.1432(14) 0.1382(9) 0.3688(11) 0.091(5) Uani 1 1 d D . . H91 H 1.1900 0.1596 0.4238 0.110 Uiso 1 1 calc R . . H92 H 1.2070 0.1049 0.3539 0.110 Uiso 1 1 calc R . . Fe Fe 0.70114(18) 0.13293(8) 0.43696(11) 0.0476(4) Uani 1 1 d . . . C10 C 0.8897(12) 0.1556(6) 0.4256(8) 0.053(3) Uani 1 1 d . . . C11 C 0.7940(14) 0.2068(6) 0.3802(9) 0.061(3) Uani 1 1 d . . . H111 H 0.7733 0.2164 0.3215 0.073 Uiso 1 1 calc R . . C12 C 0.7358(16) 0.2404(7) 0.4400(11) 0.075(4) Uani 1 1 d . . . H121 H 0.6703 0.2768 0.4280 0.090 Uiso 1 1 calc R . . C13 C 0.7935(19) 0.2093(8) 0.5207(11) 0.090(5) Uani 1 1 d . . . H131 H 0.7708 0.2212 0.5711 0.108 Uiso 1 1 calc R . . C14 C 0.8888(15) 0.1585(8) 0.5141(9) 0.071(4) Uani 1 1 d . . . H141 H 0.9428 0.1310 0.5588 0.085 Uiso 1 1 calc R . . C15 C 0.6400(12) 0.0337(6) 0.3900(8) 0.049(3) Uani 1 1 d . . . C16 C 0.5497(13) 0.0856(7) 0.3444(10) 0.065(4) Uani 1 1 d . . . H161 H 0.5291 0.0945 0.2856 0.078 Uiso 1 1 calc R . . C17 C 0.4950(14) 0.1221(9) 0.4050(13) 0.089(5) Uani 1 1 d . . . H171 H 0.4301 0.1588 0.3923 0.107 Uiso 1 1 calc R . . C18 C 0.5555(18) 0.0935(9) 0.4878(12) 0.087(5) Uani 1 1 d . . . H181 H 0.5397 0.1088 0.5393 0.104 Uiso 1 1 calc R . . C19 C 0.6427(15) 0.0384(7) 0.4782(9) 0.066(4) Uani 1 1 d . . . H191 H 0.6942 0.0094 0.5222 0.080 Uiso 1 1 calc R . . P1A P 0.4027(19) 0.2072(8) 0.0940(10) 0.078(6) Uani 0.38(2) 1 d PDU A 1 F1A F 0.391(4) 0.1298(12) 0.120(2) 0.173(16) Uani 0.38(2) 1 d PDU A 1 F2A F 0.538(3) 0.214(2) 0.162(2) 0.201(19) Uani 0.38(2) 1 d PDU A 1 F3A F 0.413(5) 0.2845(12) 0.068(2) 0.154(15) Uani 0.38(2) 1 d PDU A 1 F4A F 0.267(3) 0.2008(19) 0.0261(18) 0.152(16) Uani 0.38(2) 1 d PDU A 1 F5A F 0.328(3) 0.2309(16) 0.1589(19) 0.130(15) Uani 0.38(2) 1 d PDU A 1 F6A F 0.477(3) 0.1834(19) 0.029(2) 0.18(2) Uani 0.38(2) 1 d PDU A 1 P1B P 0.3843(10) 0.2136(4) 0.0863(6) 0.073(4) Uani 0.62(2) 1 d PDU A 2 F1B F 0.4831(17) 0.1490(8) 0.0835(12) 0.160(10) Uani 0.62(2) 1 d PDU A 2 F2B F 0.5123(18) 0.2636(9) 0.1221(10) 0.128(8) Uani 0.62(2) 1 d PDU A 2 F3B F 0.284(2) 0.2776(10) 0.0891(10) 0.145(10) Uani 0.62(2) 1 d PDU A 2 F4B F 0.2568(15) 0.1631(10) 0.0506(11) 0.131(9) Uani 0.62(2) 1 d PDU A 2 F5B F 0.3856(18) 0.1928(9) 0.1808(8) 0.133(9) Uani 0.62(2) 1 d PDU A 2 F6B F 0.382(2) 0.2344(8) -0.0082(8) 0.126(8) Uani 0.62(2) 1 d PDU A 2 P2A P 1.1693(18) -0.0900(8) 0.2487(12) 0.074(5) Uani 0.38(2) 1 d PDU B 1 F7A F 1.207(5) -0.0150(13) 0.223(2) 0.170(16) Uani 0.38(2) 1 d PDU B 1 F8A F 1.087(3) -0.0562(17) 0.3056(17) 0.118(11) Uani 0.38(2) 1 d PDU B 1 F9A F 1.120(5) -0.1651(15) 0.267(3) 0.138(14) Uani 0.38(2) 1 d PDU B 1 F10A F 1.252(3) -0.1242(15) 0.1917(18) 0.119(13) Uani 0.38(2) 1 d PDU B 1 F11A F 1.298(3) -0.090(2) 0.3254(15) 0.118(12) Uani 0.38(2) 1 d PDU B 1 F12A F 1.040(3) -0.090(2) 0.1717(18) 0.169(17) Uani 0.38(2) 1 d PDU B 1 P2B P 1.1529(11) -0.0909(5) 0.2338(7) 0.074(4) Uani 0.62(2) 1 d PDU B 2 F7B F 1.094(2) -0.0189(8) 0.1878(10) 0.112(8) Uani 0.62(2) 1 d PDU B 2 F8B F 1.0372(17) -0.0912(11) 0.2824(11) 0.136(8) Uani 0.62(2) 1 d PDU B 2 F9B F 1.213(3) -0.1627(12) 0.2812(15) 0.153(11) Uani 0.62(2) 1 d PDU B 2 F10B F 1.2687(16) -0.0911(12) 0.1854(12) 0.146(10) Uani 0.62(2) 1 d PDU B 2 F11B F 1.250(2) -0.0476(12) 0.3101(11) 0.181(12) Uani 0.62(2) 1 d PDU B 2 F12B F 1.057(2) -0.1349(10) 0.1577(11) 0.131(8) Uani 0.62(2) 1 d PDU B 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 Pt 0.0477(3) 0.0407(3) 0.0476(3) 0.0040(2) 0.0202(2) 0.0060(2) Se1 0.0661(9) 0.0390(6) 0.0551(7) 0.0039(5) 0.0234(6) 0.0034(5) Se2 0.0982(13) 0.0780(10) 0.0516(8) -0.0024(7) 0.0040(8) -0.0070(9) Se3 0.0895(11) 0.0573(8) 0.0915(11) 0.0293(8) 0.0507(9) 0.0133(7) Se4 0.0405(7) 0.0615(8) 0.0729(9) -0.0032(7) 0.0096(6) -0.0017(6) C1 0.096(12) 0.065(9) 0.092(11) -0.019(8) 0.037(9) -0.035(8) C2 0.110(14) 0.074(11) 0.095(12) -0.024(10) 0.017(11) -0.023(10) C3 0.18(2) 0.070(11) 0.102(13) -0.045(10) 0.065(14) -0.017(12) C4 0.26(2) 0.142(14) 0.067(9) -0.015(9) 0.072(11) -0.001(14) C5 0.254(19) 0.147(13) 0.073(9) -0.006(9) 0.076(10) 0.000(13) C6 0.23(2) 0.133(14) 0.068(9) 0.004(9) 0.089(11) 0.002(13) C7 0.114(16) 0.109(15) 0.157(19) 0.027(14) 0.085(15) -0.029(12) C8 0.064(11) 0.093(13) 0.18(2) 0.001(14) 0.038(13) -0.046(10) C9 0.074(11) 0.093(12) 0.116(14) -0.003(11) 0.041(10) -0.022(9) Fe 0.0521(11) 0.0373(9) 0.0578(10) -0.0081(7) 0.0225(8) -0.0063(7) C10 0.043(7) 0.042(7) 0.072(9) -0.011(6) 0.015(6) -0.010(5) C11 0.070(9) 0.041(7) 0.075(9) 0.001(6) 0.027(7) -0.012(6) C12 0.092(12) 0.036(7) 0.110(13) -0.004(8) 0.050(10) -0.006(7) C13 0.128(15) 0.067(10) 0.092(12) -0.041(9) 0.058(11) -0.043(10) C14 0.067(10) 0.077(10) 0.067(9) -0.026(8) 0.016(8) -0.019(8) C15 0.046(7) 0.048(7) 0.058(7) 0.002(6) 0.022(6) 0.001(5) C16 0.049(8) 0.057(8) 0.087(10) -0.022(7) 0.016(7) -0.013(7) C17 0.027(8) 0.092(12) 0.145(16) -0.043(12) 0.019(9) -0.001(7) C18 0.083(12) 0.094(12) 0.100(13) -0.033(10) 0.053(11) -0.032(10) C19 0.087(11) 0.050(8) 0.080(10) -0.009(7) 0.052(8) -0.024(7) P1A 0.077(10) 0.087(11) 0.073(11) -0.004(9) 0.025(8) -0.029(9) F1A 0.20(3) 0.11(2) 0.21(3) 0.00(2) 0.05(3) -0.01(2) F2A 0.16(3) 0.23(3) 0.18(3) 0.00(3) -0.01(2) -0.03(3) F3A 0.17(3) 0.11(2) 0.18(3) 0.04(2) 0.05(2) -0.05(2) F4A 0.12(2) 0.16(3) 0.18(3) -0.01(2) 0.04(2) -0.03(2) F5A 0.15(3) 0.14(3) 0.14(3) -0.07(2) 0.11(2) -0.04(2) F6A 0.20(3) 0.24(4) 0.14(3) -0.04(2) 0.10(2) 0.01(3) P1B 0.094(7) 0.063(6) 0.068(6) -0.012(5) 0.033(6) -0.015(5) F1B 0.129(17) 0.103(14) 0.26(2) 0.011(16) 0.078(17) 0.064(13) F2B 0.100(14) 0.130(16) 0.152(17) -0.030(14) 0.031(12) -0.045(13) F3B 0.155(18) 0.124(15) 0.134(15) -0.014(12) 0.002(13) 0.071(14) F4B 0.120(15) 0.129(17) 0.152(17) -0.044(13) 0.049(13) -0.076(13) F5B 0.148(19) 0.16(2) 0.098(13) 0.047(14) 0.047(12) 0.021(15) F6B 0.20(2) 0.110(13) 0.078(11) 0.000(10) 0.047(12) -0.028(13) P2A 0.077(10) 0.096(11) 0.057(9) 0.003(8) 0.033(8) 0.019(9) F7A 0.22(3) 0.12(2) 0.15(3) 0.02(2) 0.02(3) -0.02(2) F8A 0.13(2) 0.14(2) 0.105(17) -0.007(16) 0.053(16) 0.072(18) F9A 0.16(3) 0.13(2) 0.14(2) 0.003(19) 0.07(2) -0.04(2) F10A 0.16(3) 0.11(2) 0.11(2) -0.036(16) 0.071(19) 0.012(18) F11A 0.12(2) 0.16(3) 0.061(15) -0.004(17) -0.004(14) 0.032(19) F12A 0.14(3) 0.22(4) 0.14(3) -0.01(3) 0.01(2) -0.01(3) P2B 0.082(6) 0.082(6) 0.050(5) 0.003(4) 0.002(5) 0.041(5) F7B 0.139(17) 0.098(12) 0.101(12) 0.046(10) 0.034(11) 0.064(12) F8B 0.150(14) 0.149(15) 0.131(13) 0.021(11) 0.076(11) 0.034(11) F9B 0.17(2) 0.157(18) 0.128(15) 0.045(14) 0.033(16) 0.111(16) F10B 0.085(13) 0.22(3) 0.147(17) 0.002(17) 0.048(12) 0.008(14) F11B 0.21(2) 0.17(2) 0.117(17) -0.045(17) -0.026(16) 0.007(19) F12B 0.142(17) 0.132(16) 0.108(13) -0.032(12) 0.013(11) -0.018(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt Se3 2.3895(13) . ? Pt Se2 2.4066(15) . ? Pt Se4 2.4247(14) . ? Pt Se1 2.4598(12) . ? Se1 C15 1.892(11) . ? Se1 C1 1.960(11) . ? Se2 C3 1.962(13) . ? Se2 C4 1.974(13) . ? Se3 C6 1.964(13) . ? Se3 C7 1.969(14) . ? Se4 C10 1.893(12) . ? Se4 C9 1.949(11) . ? C1 C2 1.459(13) . ? C1 H11 0.9700 . ? C1 H12 0.9700 . ? C2 C3 1.443(14) . ? C2 H21 0.9700 . ? C2 H22 0.9700 . ? C3 H31 0.9700 . ? C3 H32 0.9700 . ? C4 C5 1.431(15) . ? C4 H41 0.9700 . ? C4 H42 0.9700 . ? C5 C6 1.438(15) . ? C5 H51 0.9700 . ? C5 H52 0.9700 . ? C6 H61 0.9700 . ? C6 H62 0.9700 . ? C7 C8 1.480(14) . ? C7 H71 0.9700 . ? C7 H72 0.9700 . ? C8 C9 1.461(14) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? Fe C13 2.006(14) . ? Fe C10 2.008(12) . ? Fe C18 2.008(14) . ? Fe C17 2.015(13) . ? Fe C11 2.017(12) . ? Fe C14 2.022(14) . ? Fe C19 2.024(12) . ? Fe C15 2.026(12) . ? Fe C16 2.026(13) . ? Fe C12 2.027(13) . ? C10 C11 1.411(17) . ? C10 C14 1.430(18) . ? C11 C12 1.405(18) . ? C11 H111 0.9300 . ? C12 C13 1.40(2) . ? C12 H121 0.9300 . ? C13 C14 1.37(2) . ? C13 H131 0.9300 . ? C14 H141 0.9300 . ? C15 C16 1.393(17) . ? C15 C19 1.418(17) . ? C16 C17 1.419(19) . ? C16 H161 0.9300 . ? C17 C18 1.41(2) . ? C17 H171 0.9300 . ? C18 C19 1.39(2) . ? C18 H181 0.9300 . ? C19 H191 0.9300 . ? P1A F6A 1.509(16) . ? P1A F2A 1.510(16) . ? P1A F3A 1.510(16) . ? P1A F1A 1.510(16) . ? P1A F4A 1.512(16) . ? P1A F5A 1.512(16) . ? P1B F6B 1.567(10) . ? P1B F5B 1.570(10) . ? P1B F1B 1.570(10) . ? P1B F2B 1.571(10) . ? P1B F3B 1.571(10) . ? P1B F4B 1.573(10) . ? P2A F8A 1.534(16) . ? P2A F11A 1.534(16) . ? P2A F7A 1.534(16) . ? P2A F10A 1.536(16) . ? P2A F12A 1.536(16) . ? P2A F9A 1.538(16) . ? P2B F7B 1.567(10) . ? P2B F11B 1.570(11) . ? P2B F10B 1.573(11) . ? P2B F12B 1.574(10) . ? P2B F8B 1.574(11) . ? P2B F9B 1.576(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se3 Pt Se2 91.91(6) . . ? Se3 Pt Se4 96.83(6) . . ? Se2 Pt Se4 171.11(5) . . ? Se3 Pt Se1 170.63(5) . . ? Se2 Pt Se1 89.74(5) . . ? Se4 Pt Se1 81.89(5) . . ? C15 Se1 C1 95.9(6) . . ? C15 Se1 Pt 98.9(3) . . ? C1 Se1 Pt 107.3(4) . . ? C3 Se2 C4 92.3(8) . . ? C3 Se2 Pt 100.0(6) . . ? C4 Se2 Pt 105.2(7) . . ? C6 Se3 C7 93.9(9) . . ? C6 Se3 Pt 108.7(6) . . ? C7 Se3 Pt 110.1(5) . . ? C10 Se4 C9 100.8(6) . . ? C10 Se4 Pt 102.7(4) . . ? C9 Se4 Pt 113.5(5) . . ? C2 C1 Se1 115.8(10) . . ? C2 C1 H11 108.3 . . ? Se1 C1 H11 108.3 . . ? C2 C1 H12 108.3 . . ? Se1 C1 H12 108.3 . . ? H11 C1 H12 107.4 . . ? C3 C2 C1 118.0(13) . . ? C3 C2 H21 107.8 . . ? C1 C2 H21 107.8 . . ? C3 C2 H22 107.8 . . ? C1 C2 H22 107.8 . . ? H21 C2 H22 107.1 . . ? C2 C3 Se2 114.0(11) . . ? C2 C3 H31 108.7 . . ? Se2 C3 H31 108.7 . . ? C2 C3 H32 108.7 . . ? Se2 C3 H32 108.7 . . ? H31 C3 H32 107.6 . . ? C5 C4 Se2 116.8(14) . . ? C5 C4 H41 108.1 . . ? Se2 C4 H41 108.1 . . ? C5 C4 H42 108.1 . . ? Se2 C4 H42 108.1 . . ? H41 C4 H42 107.3 . . ? C4 C5 C6 124(2) . . ? C4 C5 H51 106.3 . . ? C6 C5 H51 106.3 . . ? C4 C5 H52 106.3 . . ? C6 C5 H52 106.3 . . ? H51 C5 H52 106.4 . . ? C5 C6 Se3 112.0(14) . . ? C5 C6 H61 109.2 . . ? Se3 C6 H61 109.2 . . ? C5 C6 H62 109.2 . . ? Se3 C6 H62 109.2 . . ? H61 C6 H62 107.9 . . ? C8 C7 Se3 116.9(11) . . ? C8 C7 H71 108.1 . . ? Se3 C7 H71 108.1 . . ? C8 C7 H72 108.1 . . ? Se3 C7 H72 108.1 . . ? H71 C7 H72 107.3 . . ? C9 C8 C7 117.9(16) . . ? C9 C8 H81 107.8 . . ? C7 C8 H81 107.8 . . ? C9 C8 H82 107.8 . . ? C7 C8 H82 107.8 . . ? H81 C8 H82 107.2 . . ? C8 C9 Se4 116.5(11) . . ? C8 C9 H91 108.2 . . ? Se4 C9 H91 108.2 . . ? C8 C9 H92 108.2 . . ? Se4 C9 H92 108.2 . . ? H91 C9 H92 107.3 . . ? C13 Fe C10 68.5(6) . . ? C13 Fe C18 104.0(7) . . ? C10 Fe C18 158.9(7) . . ? C13 Fe C17 120.2(7) . . ? C10 Fe C17 159.7(7) . . ? C18 Fe C17 41.1(7) . . ? C13 Fe C11 68.6(6) . . ? C10 Fe C11 41.0(5) . . ? C18 Fe C11 156.4(7) . . ? C17 Fe C11 121.8(7) . . ? C13 Fe C14 39.9(6) . . ? C10 Fe C14 41.6(5) . . ? C18 Fe C14 120.2(7) . . ? C17 Fe C14 155.8(7) . . ? C11 Fe C14 69.2(6) . . ? C13 Fe C19 121.2(6) . . ? C10 Fe C19 125.5(6) . . ? C18 Fe C19 40.3(6) . . ? C17 Fe C19 67.9(7) . . ? C11 Fe C19 162.5(5) . . ? C14 Fe C19 108.1(6) . . ? C13 Fe C15 159.2(7) . . ? C10 Fe C15 111.0(5) . . ? C18 Fe C15 68.7(5) . . ? C17 Fe C15 67.9(5) . . ? C11 Fe C15 125.6(5) . . ? C14 Fe C15 125.7(6) . . ? C19 Fe C15 41.0(5) . . ? C13 Fe C16 157.5(7) . . ? C10 Fe C16 124.7(5) . . ? C18 Fe C16 69.6(6) . . ? C17 Fe C16 41.1(6) . . ? C11 Fe C16 108.2(6) . . ? C14 Fe C16 161.8(6) . . ? C19 Fe C16 68.6(6) . . ? C15 Fe C16 40.2(5) . . ? C13 Fe C12 40.6(6) . . ? C10 Fe C12 68.5(5) . . ? C18 Fe C12 119.4(6) . . ? C17 Fe C12 105.3(7) . . ? C11 Fe C12 40.7(5) . . ? C14 Fe C12 68.1(7) . . ? C19 Fe C12 155.9(6) . . ? C15 Fe C12 160.0(6) . . ? C16 Fe C12 122.5(7) . . ? C11 C10 C14 107.7(12) . . ? C11 C10 Se4 130.0(10) . . ? C14 C10 Se4 121.7(10) . . ? C11 C10 Fe 69.8(7) . . ? C14 C10 Fe 69.7(7) . . ? Se4 C10 Fe 118.7(6) . . ? C12 C11 C10 107.5(12) . . ? C12 C11 Fe 70.0(7) . . ? C10 C11 Fe 69.1(7) . . ? C12 C11 H111 126.3 . . ? C10 C11 H111 126.3 . . ? Fe C11 H111 126.1 . . ? C13 C12 C11 107.9(14) . . ? C13 C12 Fe 68.9(8) . . ? C11 C12 Fe 69.3(7) . . ? C13 C12 H121 126.0 . . ? C11 C12 H121 126.0 . . ? Fe C12 H121 127.3 . . ? C14 C13 C12 109.7(14) . . ? C14 C13 Fe 70.7(8) . . ? C12 C13 Fe 70.5(8) . . ? C14 C13 H131 125.2 . . ? C12 C13 H131 125.2 . . ? Fe C13 H131 125.3 . . ? C13 C14 C10 107.3(14) . . ? C13 C14 Fe 69.5(9) . . ? C10 C14 Fe 68.7(7) . . ? C13 C14 H141 126.4 . . ? C10 C14 H141 126.4 . . ? Fe C14 H141 127.0 . . ? C16 C15 C19 108.6(11) . . ? C16 C15 Se1 126.9(10) . . ? C19 C15 Se1 124.5(10) . . ? C16 C15 Fe 69.9(7) . . ? C19 C15 Fe 69.4(7) . . ? Se1 C15 Fe 126.5(6) . . ? C15 C16 C17 106.8(14) . . ? C15 C16 Fe 69.9(8) . . ? C17 C16 Fe 69.0(8) . . ? C15 C16 H161 126.6 . . ? C17 C16 H161 126.6 . . ? Fe C16 H161 126.1 . . ? C18 C17 C16 108.7(14) . . ? C18 C17 Fe 69.2(9) . . ? C16 C17 Fe 69.9(7) . . ? C18 C17 H171 125.6 . . ? C16 C17 H171 125.6 . . ? Fe C17 H171 126.9 . . ? C19 C18 C17 107.3(14) . . ? C19 C18 Fe 70.5(8) . . ? C17 C18 Fe 69.7(9) . . ? C19 C18 H181 126.4 . . ? C17 C18 H181 126.4 . . ? Fe C18 H181 125.0 . . ? C18 C19 C15 108.5(14) . . ? C18 C19 Fe 69.2(8) . . ? C15 C19 Fe 69.6(7) . . ? C18 C19 H191 125.7 . . ? C15 C19 H191 125.7 . . ? Fe C19 H191 127.0 . . ? F6A P1A F2A 90.1(4) . . ? F6A P1A F3A 90.1(4) . . ? F2A P1A F3A 90(2) . . ? F6A P1A F1A 90.1(4) . . ? F2A P1A F1A 90.1(5) . . ? F3A P1A F1A 179(2) . . ? F6A P1A F4A 90.0(4) . . ? F2A P1A F4A 179.9(8) . . ? F3A P1A F4A 90(2) . . ? F1A P1A F4A 89.9(5) . . ? F6A P1A F5A 179.9(7) . . ? F2A P1A F5A 90.0(4) . . ? F3A P1A F5A 89.9(4) . . ? F1A P1A F5A 89.9(4) . . ? F4A P1A F5A 89.9(4) . . ? F6B P1B F5B 179.8(6) . . ? F6B P1B F1B 90.1(4) . . ? F5B P1B F1B 90.1(4) . . ? F6B P1B F2B 90.2(4) . . ? F5B P1B F2B 90.0(4) . . ? F1B P1B F2B 89.9(5) . . ? F6B P1B F3B 90.1(4) . . ? F5B P1B F3B 89.7(4) . . ? F1B P1B F3B 179.3(10) . . ? F2B P1B F3B 90.7(11) . . ? F6B P1B F4B 89.9(4) . . ? F5B P1B F4B 89.9(4) . . ? F1B P1B F4B 89.7(5) . . ? F2B P1B F4B 179.6(8) . . ? F3B P1B F4B 89.6(11) . . ? F8A P2A F11A 89.9(4) . . ? F8A P2A F7A 90.2(4) . . ? F11A P2A F7A 90.0(5) . . ? F8A P2A F10A 179.9(6) . . ? F11A P2A F10A 90.1(4) . . ? F7A P2A F10A 89.9(4) . . ? F8A P2A F12A 90.1(4) . . ? F11A P2A F12A 179.9(10) . . ? F7A P2A F12A 89.9(5) . . ? F10A P2A F12A 89.9(4) . . ? F8A P2A F9A 90.1(4) . . ? F11A P2A F9A 95(2) . . ? F7A P2A F9A 175(2) . . ? F10A P2A F9A 89.8(4) . . ? F12A P2A F9A 85(2) . . ? F7B P2B F11B 90.4(5) . . ? F7B P2B F10B 90.1(4) . . ? F11B P2B F10B 90.0(4) . . ? F7B P2B F12B 90.1(5) . . ? F11B P2B F12B 179.5(8) . . ? F10B P2B F12B 89.8(4) . . ? F7B P2B F8B 90.2(4) . . ? F11B P2B F8B 90.1(4) . . ? F10B P2B F8B 179.7(5) . . ? F12B P2B F8B 90.1(4) . . ? F7B P2B F9B 179.2(14) . . ? F11B P2B F9B 88.8(13) . . ? F10B P2B F9B 89.9(4) . . ? F12B P2B F9B 90.8(13) . . ? F8B P2B F9B 89.8(4) . . ? 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 Se3 Pt Se1 C15 -4.0(5) . . . . ? Se2 Pt Se1 C15 -104.2(4) . . . . ? Se4 Pt Se1 C15 78.8(4) . . . . ? Se3 Pt Se1 C1 95.1(6) . . . . ? Se2 Pt Se1 C1 -5.1(5) . . . . ? Se4 Pt Se1 C1 178.0(5) . . . . ? Se3 Pt Se2 C3 142.3(5) . . . . ? Se4 Pt Se2 C3 -27.1(7) . . . . ? Se1 Pt Se2 C3 -46.9(5) . . . . ? Se3 Pt Se2 C4 47.1(7) . . . . ? Se4 Pt Se2 C4 -122.3(8) . . . . ? Se1 Pt Se2 C4 -142.1(7) . . . . ? Se2 Pt Se3 C6 -49.7(7) . . . . ? Se4 Pt Se3 C6 128.6(7) . . . . ? Se1 Pt Se3 C6 -149.8(8) . . . . ? Se2 Pt Se3 C7 -151.2(7) . . . . ? Se4 Pt Se3 C7 27.1(7) . . . . ? Se1 Pt Se3 C7 108.7(7) . . . . ? Se3 Pt Se4 C10 83.5(4) . . . . ? Se2 Pt Se4 C10 -107.2(5) . . . . ? Se1 Pt Se4 C10 -87.1(4) . . . . ? Se3 Pt Se4 C9 -24.4(6) . . . . ? Se2 Pt Se4 C9 144.9(7) . . . . ? Se1 Pt Se4 C9 164.9(6) . . . . ? C15 Se1 C1 C2 166.1(12) . . . . ? Pt Se1 C1 C2 64.8(13) . . . . ? Se1 C1 C2 C3 -50(2) . . . . ? C1 C2 C3 Se2 -32(2) . . . . ? C4 Se2 C3 C2 -168.4(15) . . . . ? Pt Se2 C3 C2 85.7(14) . . . . ? C3 Se2 C4 C5 -160(2) . . . . ? Pt Se2 C4 C5 -59(2) . . . . ? Se2 C4 C5 C6 73(3) . . . . ? C4 C5 C6 Se3 -71(3) . . . . ? C7 Se3 C6 C5 172.6(17) . . . . ? Pt Se3 C6 C5 59.9(18) . . . . ? C6 Se3 C7 C8 -165.0(15) . . . . ? Pt Se3 C7 C8 -53.5(16) . . . . ? Se3 C7 C8 C9 79.6(19) . . . . ? C7 C8 C9 Se4 -72.8(18) . . . . ? C10 Se4 C9 C8 -64.8(15) . . . . ? Pt Se4 C9 C8 44.3(15) . . . . ? C9 Se4 C10 C11 84.4(12) . . . . ? Pt Se4 C10 C11 -32.9(11) . . . . ? C9 Se4 C10 C14 -105.9(11) . . . . ? Pt Se4 C10 C14 136.7(9) . . . . ? C9 Se4 C10 Fe 171.3(8) . . . . ? Pt Se4 C10 Fe 54.0(7) . . . . ? C13 Fe C10 C11 -81.7(9) . . . . ? C18 Fe C10 C11 -154.3(15) . . . . ? C17 Fe C10 C11 37.7(18) . . . . ? C14 Fe C10 C11 -118.7(11) . . . . ? C19 Fe C10 C11 164.6(8) . . . . ? C15 Fe C10 C11 120.7(8) . . . . ? C16 Fe C10 C11 77.5(9) . . . . ? C12 Fe C10 C11 -37.9(8) . . . . ? C13 Fe C10 C14 37.0(9) . . . . ? C18 Fe C10 C14 -35.6(19) . . . . ? C17 Fe C10 C14 156.4(16) . . . . ? C11 Fe C10 C14 118.7(11) . . . . ? C19 Fe C10 C14 -76.7(10) . . . . ? C15 Fe C10 C14 -120.6(8) . . . . ? C16 Fe C10 C14 -163.8(9) . . . . ? C12 Fe C10 C14 80.8(9) . . . . ? C13 Fe C10 Se4 153.0(10) . . . . ? C18 Fe C10 Se4 80.3(17) . . . . ? C17 Fe C10 Se4 -87.6(17) . . . . ? C11 Fe C10 Se4 -125.4(11) . . . . ? C14 Fe C10 Se4 115.9(11) . . . . ? C19 Fe C10 Se4 39.2(10) . . . . ? C15 Fe C10 Se4 -4.7(9) . . . . ? C16 Fe C10 Se4 -47.9(10) . . . . ? C12 Fe C10 Se4 -163.3(10) . . . . ? C14 C10 C11 C12 0.1(14) . . . . ? Se4 C10 C11 C12 170.9(9) . . . . ? Fe C10 C11 C12 59.8(9) . . . . ? C14 C10 C11 Fe -59.7(8) . . . . ? Se4 C10 C11 Fe 111.0(10) . . . . ? C13 Fe C11 C12 -37.3(10) . . . . ? C10 Fe C11 C12 -118.7(12) . . . . ? C18 Fe C11 C12 38(2) . . . . ? C17 Fe C11 C12 75.8(11) . . . . ? C14 Fe C11 C12 -80.2(10) . . . . ? C19 Fe C11 C12 -164.5(19) . . . . ? C15 Fe C11 C12 160.1(9) . . . . ? C16 Fe C11 C12 119.0(10) . . . . ? C13 Fe C11 C10 81.4(9) . . . . ? C18 Fe C11 C10 157.0(15) . . . . ? C17 Fe C11 C10 -165.5(8) . . . . ? C14 Fe C11 C10 38.5(7) . . . . ? C19 Fe C11 C10 -46(2) . . . . ? C15 Fe C11 C10 -81.2(9) . . . . ? C16 Fe C11 C10 -122.3(8) . . . . ? C12 Fe C11 C10 118.7(12) . . . . ? C10 C11 C12 C13 -1.0(15) . . . . ? Fe C11 C12 C13 58.3(10) . . . . ? C10 C11 C12 Fe -59.2(8) . . . . ? C10 Fe C12 C13 -81.6(10) . . . . ? C18 Fe C12 C13 76.6(12) . . . . ? C17 Fe C12 C13 118.7(11) . . . . ? C11 Fe C12 C13 -119.9(14) . . . . ? C14 Fe C12 C13 -36.7(9) . . . . ? C19 Fe C12 C13 49(2) . . . . ? C15 Fe C12 C13 -174.0(14) . . . . ? C16 Fe C12 C13 160.0(9) . . . . ? C13 Fe C12 C11 119.9(14) . . . . ? C10 Fe C12 C11 38.3(8) . . . . ? C18 Fe C12 C11 -163.5(10) . . . . ? C17 Fe C12 C11 -121.4(10) . . . . ? C14 Fe C12 C11 83.2(9) . . . . ? C19 Fe C12 C11 168.7(14) . . . . ? C15 Fe C12 C11 -54(2) . . . . ? C16 Fe C12 C11 -80.1(10) . . . . ? C11 C12 C13 C14 1.5(16) . . . . ? Fe C12 C13 C14 60.0(10) . . . . ? C11 C12 C13 Fe -58.5(10) . . . . ? C10 Fe C13 C14 -38.6(9) . . . . ? C18 Fe C13 C14 120.7(11) . . . . ? C17 Fe C13 C14 161.9(10) . . . . ? C11 Fe C13 C14 -82.8(10) . . . . ? C19 Fe C13 C14 80.9(11) . . . . ? C15 Fe C13 C14 54(2) . . . . ? C16 Fe C13 C14 -168.9(14) . . . . ? C12 Fe C13 C14 -120.2(13) . . . . ? C10 Fe C13 C12 81.6(9) . . . . ? C18 Fe C13 C12 -119.1(10) . . . . ? C17 Fe C13 C12 -77.9(12) . . . . ? C11 Fe C13 C12 37.4(9) . . . . ? C14 Fe C13 C12 120.2(13) . . . . ? C19 Fe C13 C12 -158.9(9) . . . . ? C15 Fe C13 C12 174.2(13) . . . . ? C16 Fe C13 C12 -49(2) . . . . ? C12 C13 C14 C10 -1.5(16) . . . . ? Fe C13 C14 C10 58.5(9) . . . . ? C12 C13 C14 Fe -59.9(10) . . . . ? C11 C10 C14 C13 0.8(14) . . . . ? Se4 C10 C14 C13 -170.8(9) . . . . ? Fe C10 C14 C13 -58.9(10) . . . . ? C11 C10 C14 Fe 59.8(8) . . . . ? Se4 C10 C14 Fe -111.9(8) . . . . ? C10 Fe C14 C13 119.1(13) . . . . ? C18 Fe C14 C13 -74.9(12) . . . . ? C17 Fe C14 C13 -41(2) . . . . ? C11 Fe C14 C13 81.1(10) . . . . ? C19 Fe C14 C13 -117.3(10) . . . . ? C15 Fe C14 C13 -159.3(9) . . . . ? C16 Fe C14 C13 166.4(18) . . . . ? C12 Fe C14 C13 37.3(9) . . . . ? C13 Fe C14 C10 -119.1(13) . . . . ? C18 Fe C14 C10 166.0(8) . . . . ? C17 Fe C14 C10 -160.2(16) . . . . ? C11 Fe C14 C10 -38.0(7) . . . . ? C19 Fe C14 C10 123.6(8) . . . . ? C15 Fe C14 C10 81.6(9) . . . . ? C16 Fe C14 C10 47(2) . . . . ? C12 Fe C14 C10 -81.8(8) . . . . ? C1 Se1 C15 C16 -64.6(12) . . . . ? Pt Se1 C15 C16 44.0(11) . . . . ? C1 Se1 C15 C19 115.4(11) . . . . ? Pt Se1 C15 C19 -136.0(10) . . . . ? C1 Se1 C15 Fe -155.8(8) . . . . ? Pt Se1 C15 Fe -47.2(7) . . . . ? C13 Fe C15 C16 156.1(16) . . . . ? C10 Fe C15 C16 -119.5(8) . . . . ? C18 Fe C15 C16 83.2(9) . . . . ? C17 Fe C15 C16 38.8(9) . . . . ? C11 Fe C15 C16 -75.4(9) . . . . ? C14 Fe C15 C16 -164.1(8) . . . . ? C19 Fe C15 C16 120.0(11) . . . . ? C12 Fe C15 C16 -35.0(18) . . . . ? C13 Fe C15 C19 36.2(19) . . . . ? C10 Fe C15 C19 120.5(9) . . . . ? C18 Fe C15 C19 -36.8(9) . . . . ? C17 Fe C15 C19 -81.2(10) . . . . ? C11 Fe C15 C19 164.6(9) . . . . ? C14 Fe C15 C19 75.9(10) . . . . ? C16 Fe C15 C19 -120.0(11) . . . . ? C12 Fe C15 C19 -155.0(15) . . . . ? C13 Fe C15 Se1 -82.3(18) . . . . ? C10 Fe C15 Se1 2.1(9) . . . . ? C18 Fe C15 Se1 -155.2(10) . . . . ? C17 Fe C15 Se1 160.4(11) . . . . ? C11 Fe C15 Se1 46.2(10) . . . . ? C14 Fe C15 Se1 -42.5(10) . . . . ? C19 Fe C15 Se1 -118.4(12) . . . . ? C16 Fe C15 Se1 121.6(11) . . . . ? C12 Fe C15 Se1 86.6(17) . . . . ? C19 C15 C16 C17 -0.5(14) . . . . ? Se1 C15 C16 C17 179.5(9) . . . . ? Fe C15 C16 C17 -59.4(9) . . . . ? C19 C15 C16 Fe 58.8(8) . . . . ? Se1 C15 C16 Fe -121.2(9) . . . . ? C13 Fe C16 C15 -158.0(14) . . . . ? C10 Fe C16 C15 81.6(9) . . . . ? C18 Fe C16 C15 -80.8(9) . . . . ? C17 Fe C16 C15 -118.1(13) . . . . ? C11 Fe C16 C15 124.1(8) . . . . ? C14 Fe C16 C15 45(2) . . . . ? C19 Fe C16 C15 -37.6(7) . . . . ? C12 Fe C16 C15 166.6(7) . . . . ? C13 Fe C16 C17 -40(2) . . . . ? C10 Fe C16 C17 -160.3(10) . . . . ? C18 Fe C16 C17 37.3(10) . . . . ? C11 Fe C16 C17 -117.8(11) . . . . ? C14 Fe C16 C17 163.3(19) . . . . ? C19 Fe C16 C17 80.5(11) . . . . ? C15 Fe C16 C17 118.1(13) . . . . ? C12 Fe C16 C17 -75.3(12) . . . . ? C15 C16 C17 C18 1.6(16) . . . . ? Fe C16 C17 C18 -58.4(10) . . . . ? C15 C16 C17 Fe 59.9(9) . . . . ? C13 Fe C17 C18 -76.2(12) . . . . ? C10 Fe C17 C18 173.4(14) . . . . ? C11 Fe C17 C18 -158.3(9) . . . . ? C14 Fe C17 C18 -47(2) . . . . ? C19 Fe C17 C18 38.1(9) . . . . ? C15 Fe C17 C18 82.5(10) . . . . ? C16 Fe C17 C18 120.4(14) . . . . ? C12 Fe C17 C18 -117.4(10) . . . . ? C13 Fe C17 C16 163.5(10) . . . . ? C10 Fe C17 C16 53(2) . . . . ? C18 Fe C17 C16 -120.4(14) . . . . ? C11 Fe C17 C16 81.3(10) . . . . ? C14 Fe C17 C16 -167.3(14) . . . . ? C19 Fe C17 C16 -82.3(10) . . . . ? C15 Fe C17 C16 -37.9(8) . . . . ? C12 Fe C17 C16 122.2(10) . . . . ? C16 C17 C18 C19 -2.0(17) . . . . ? Fe C17 C18 C19 -60.8(10) . . . . ? C16 C17 C18 Fe 58.8(10) . . . . ? C13 Fe C18 C19 -122.1(11) . . . . ? C10 Fe C18 C19 -55.8(19) . . . . ? C17 Fe C18 C19 117.8(13) . . . . ? C11 Fe C18 C19 169.6(13) . . . . ? C14 Fe C18 C19 -82.4(11) . . . . ? C15 Fe C18 C19 37.4(9) . . . . ? C16 Fe C18 C19 80.6(10) . . . . ? C12 Fe C18 C19 -162.8(9) . . . . ? C13 Fe C18 C17 120.1(10) . . . . ? C10 Fe C18 C17 -173.7(13) . . . . ? C11 Fe C18 C17 51.7(19) . . . . ? C14 Fe C18 C17 159.7(9) . . . . ? C19 Fe C18 C17 -117.8(13) . . . . ? C15 Fe C18 C17 -80.4(9) . . . . ? C16 Fe C18 C17 -37.3(9) . . . . ? C12 Fe C18 C17 79.4(11) . . . . ? C17 C18 C19 C15 1.6(16) . . . . ? Fe C18 C19 C15 -58.6(9) . . . . ? C17 C18 C19 Fe 60.3(10) . . . . ? C16 C15 C19 C18 -0.7(15) . . . . ? Se1 C15 C19 C18 179.3(9) . . . . ? Fe C15 C19 C18 58.4(9) . . . . ? C16 C15 C19 Fe -59.1(9) . . . . ? Se1 C15 C19 Fe 120.9(9) . . . . ? C13 Fe C19 C18 73.9(12) . . . . ? C10 Fe C19 C18 158.5(10) . . . . ? C17 Fe C19 C18 -38.9(9) . . . . ? C11 Fe C19 C18 -166.1(18) . . . . ? C14 Fe C19 C18 115.7(11) . . . . ? C15 Fe C19 C18 -120.2(13) . . . . ? C16 Fe C19 C18 -83.3(10) . . . . ? C12 Fe C19 C18 39(2) . . . . ? C13 Fe C19 C15 -165.8(9) . . . . ? C10 Fe C19 C15 -81.3(9) . . . . ? C18 Fe C19 C15 120.2(13) . . . . ? C17 Fe C19 C15 81.3(9) . . . . ? C11 Fe C19 C15 -46(2) . . . . ? C14 Fe C19 C15 -124.1(8) . . . . ? C16 Fe C19 C15 36.9(7) . . . . ? C12 Fe C19 C15 159.3(14) . . . . ? ######################################################## # END of CIF ######################################################## ######################################################## # END of CIF ######################################################## # Attachment '- Pd.cif' #========================================================================= data_js140 _database_code_depnum_ccdc_archive 'CCDC 770361' #TrackingRef '- Pd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 Fe Pd Se4 2+, 2(P F6) 2-' _chemical_formula_sum 'C19 H26 F12 Fe P2 Pd Se4' _chemical_formula_weight 1022.43 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 10.0072(3) _cell_length_b 18.4143(4) _cell_length_c 15.9982(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.850(3) _cell_angle_gamma 90.00 _cell_volume 2821.51(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16912 _cell_measurement_theta_min 3.93 _cell_measurement_theta_max 29.59 _exptl_crystal_description 'irregular bloc' _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 6.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1986)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.4547 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25189 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 5703 _reflns_number_gt 4613 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Oxford Diffraction software, CrysAlisPro 171.29.2' _computing_cell_refinement 'Oxford Diffraction software, CrysAlisPro, Version 171.33.41' _computing_data_reduction 'Oxford Diffraction software, CrysAlisPro 171.29.2' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+5.7815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00070(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5703 _refine_ls_number_parameters 481 _refine_ls_number_restraints 480 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.084 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.122 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 Pd Pd 0.82557(3) 0.042146(15) 0.248478(17) 0.01473(8) Uani 1 1 d . . . Se1 Se 0.73559(4) -0.037100(19) 0.34506(2) 0.01539(9) Uani 1 1 d . . . Se2 Se 0.65750(4) -0.01035(2) 0.12218(2) 0.02502(10) Uani 1 1 d . . . Se3 Se 0.88262(4) 0.13779(2) 0.16291(3) 0.02410(10) Uani 1 1 d . . . Se4 Se 0.99633(4) 0.07596(2) 0.38577(2) 0.01842(9) Uani 1 1 d . . . C1 C 0.5678(4) -0.0855(2) 0.2711(3) 0.0224(8) Uani 1 1 d . . . H11 H 0.5202 -0.1109 0.3090 0.027 Uiso 1 1 calc R . . H12 H 0.5028 -0.0482 0.2375 0.027 Uiso 1 1 calc R . . C2 C 0.5993(5) -0.1397(2) 0.2079(3) 0.0299(10) Uani 1 1 d . . . H21 H 0.6431 -0.1831 0.2415 0.036 Uiso 1 1 calc R . . H22 H 0.5097 -0.1555 0.1666 0.036 Uiso 1 1 calc R . . C3 C 0.6931(5) -0.1130(2) 0.1557(3) 0.0293(9) Uani 1 1 d . . . H31 H 0.6778 -0.1430 0.1023 0.035 Uiso 1 1 calc R . . H32 H 0.7918 -0.1188 0.1907 0.035 Uiso 1 1 calc R . . C4 C 0.7495(6) -0.0140(3) 0.0295(3) 0.0410(12) Uani 1 1 d . . . H41 H 0.8377 -0.0416 0.0509 0.049 Uiso 1 1 calc R . . H42 H 0.6887 -0.0408 -0.0210 0.049 Uiso 1 1 calc R . . C5 C 0.7811(6) 0.0592(3) -0.0006(3) 0.0500(14) Uani 1 1 d . . . H51 H 0.7003 0.0914 -0.0048 0.060 Uiso 1 1 calc R . . H52 H 0.7916 0.0543 -0.0600 0.060 Uiso 1 1 calc R . . C6 C 0.9105(5) 0.0950(3) 0.0573(3) 0.0366(11) Uani 1 1 d . . . H61 H 0.9410 0.1335 0.0237 0.044 Uiso 1 1 calc R . . H62 H 0.9862 0.0585 0.0744 0.044 Uiso 1 1 calc R . . C7 C 1.0782(5) 0.1686(2) 0.2093(3) 0.0351(11) Uani 1 1 d . . . H71 H 1.1391 0.1279 0.2032 0.042 Uiso 1 1 calc R . . H72 H 1.0951 0.2093 0.1732 0.042 Uiso 1 1 calc R . . C8 C 1.1202(4) 0.1925(2) 0.3042(3) 0.0306(10) Uani 1 1 d . . . H81 H 1.2027 0.2247 0.3148 0.037 Uiso 1 1 calc R . . H82 H 1.0431 0.2213 0.3147 0.037 Uiso 1 1 calc R . . C9 C 1.1547(4) 0.1304(2) 0.3689(3) 0.0282(9) Uani 1 1 d . . . H91 H 1.2092 0.1502 0.4262 0.034 Uiso 1 1 calc R . . H92 H 1.2158 0.0960 0.3497 0.034 Uiso 1 1 calc R . . Fe Fe 0.70807(5) 0.13426(3) 0.43525(3) 0.01572(12) Uani 1 1 d . . . C10 C 0.9039(4) 0.1504(2) 0.4292(2) 0.0193(8) Uani 1 1 d . . . C11 C 0.8144(4) 0.2056(2) 0.3815(3) 0.0237(9) Uani 1 1 d . . . H111 H 0.7963 0.2162 0.3211 0.028 Uiso 1 1 calc R . . C12 C 0.7574(4) 0.2418(2) 0.4415(3) 0.0285(9) Uani 1 1 d . . . H121 H 0.6942 0.2815 0.4280 0.034 Uiso 1 1 calc R . . C13 C 0.8097(4) 0.2093(2) 0.5244(3) 0.0284(9) Uani 1 1 d . . . H131 H 0.7871 0.2232 0.5759 0.034 Uiso 1 1 calc R . . C14 C 0.9009(4) 0.1529(2) 0.5179(3) 0.0239(9) Uani 1 1 d . . . H141 H 0.9513 0.1221 0.5639 0.029 Uiso 1 1 calc R . . C15 C 0.6366(4) 0.03585(19) 0.3875(2) 0.0170(7) Uani 1 1 d . . . C16 C 0.5520(4) 0.0914(2) 0.3357(3) 0.0206(8) Uani 1 1 d . . . H161 H 0.5363 0.0994 0.2750 0.025 Uiso 1 1 calc R . . C17 C 0.4958(4) 0.1322(2) 0.3930(3) 0.0268(9) Uani 1 1 d . . . H171 H 0.4353 0.1728 0.3769 0.032 Uiso 1 1 calc R . . C18 C 0.5451(4) 0.1022(2) 0.4784(3) 0.0257(9) Uani 1 1 d . . . H181 H 0.5234 0.1195 0.5289 0.031 Uiso 1 1 calc R . . C19 C 0.6320(4) 0.0419(2) 0.4754(2) 0.0216(8) Uani 1 1 d . . . H191 H 0.6784 0.0115 0.5229 0.026 Uiso 1 1 calc R . . P1A P 0.4095(17) 0.2103(9) 0.0928(9) 0.031(3) Uani 0.25(3) 1 d PDU A 1 F1A F 0.474(3) 0.1325(12) 0.1059(15) 0.064(7) Uani 0.25(3) 1 d PDU A 1 F2A F 0.547(2) 0.2422(17) 0.1552(14) 0.042(5) Uani 0.25(3) 1 d PDU A 1 F3A F 0.354(4) 0.2900(12) 0.0834(16) 0.054(6) Uani 0.25(3) 1 d PDU A 1 F4A F 0.272(2) 0.1789(18) 0.0299(16) 0.042(5) Uani 0.25(3) 1 d PDU A 1 F5A F 0.351(3) 0.1986(13) 0.1719(17) 0.063(9) Uani 0.25(3) 1 d PDU A 1 F6A F 0.468(3) 0.2218(15) 0.0134(14) 0.047(5) Uani 0.25(3) 1 d PDU A 1 P1B P 0.3902(9) 0.2185(3) 0.0896(3) 0.0290(10) Uani 0.75(3) 1 d PDU A 2 F1B F 0.4783(8) 0.1465(5) 0.0881(8) 0.064(2) Uani 0.75(3) 1 d PDU A 2 F2B F 0.5299(11) 0.2627(6) 0.1325(8) 0.054(2) Uani 0.75(3) 1 d PDU A 2 F3B F 0.2988(16) 0.2901(4) 0.0888(5) 0.062(3) Uani 0.75(3) 1 d PDU A 2 F4B F 0.2481(10) 0.1750(6) 0.0461(7) 0.045(2) Uani 0.75(3) 1 d PDU A 2 F5B F 0.3788(12) 0.1990(3) 0.1848(6) 0.0394(19) Uani 0.75(3) 1 d PDU A 2 F6B F 0.399(2) 0.2386(5) -0.0066(6) 0.067(4) Uani 0.75(3) 1 d PDU A 2 P2A P 1.1592(12) -0.0913(6) 0.2413(8) 0.036(4) Uani 0.256(18) 1 d PDU B 1 F7A F 1.215(3) -0.0144(8) 0.2232(13) 0.073(6) Uani 0.256(18) 1 d PDU B 1 F8A F 1.063(2) -0.0542(12) 0.2919(12) 0.064(6) Uani 0.256(18) 1 d PDU B 1 F9A F 1.109(2) -0.1687(10) 0.2635(14) 0.045(5) Uani 0.256(18) 1 d PDU B 1 F10A F 1.2550(18) -0.1289(8) 0.1913(9) 0.018(3) Uani 0.256(18) 1 d PDU B 1 F11A F 1.2806(17) -0.0966(11) 0.3297(9) 0.043(5) Uani 0.256(18) 1 d PDU B 1 F12A F 1.0374(15) -0.0852(17) 0.1530(10) 0.072(6) Uani 0.256(18) 1 d PDU B 1 P2B P 1.1434(5) -0.09802(19) 0.2377(2) 0.0256(10) Uani 0.744(18) 1 d PDU B 2 F7B F 1.1305(12) -0.0176(3) 0.2005(4) 0.063(2) Uani 0.744(18) 1 d PDU B 2 F8B F 1.0233(7) -0.0817(4) 0.2826(4) 0.0495(17) Uani 0.744(18) 1 d PDU B 2 F9B F 1.1517(9) -0.1793(3) 0.2728(5) 0.0565(19) Uani 0.744(18) 1 d PDU B 2 F10B F 1.2622(7) -0.1148(5) 0.1928(5) 0.057(2) Uani 0.744(18) 1 d PDU B 2 F11B F 1.2564(8) -0.0735(5) 0.3237(4) 0.063(2) Uani 0.744(18) 1 d PDU B 2 F12B F 1.0289(5) -0.1232(4) 0.1505(3) 0.0454(16) Uani 0.744(18) 1 d PDU B 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 Pd 0.01723(14) 0.01151(14) 0.01655(14) 0.00139(11) 0.00662(11) 0.00057(11) Se1 0.01803(18) 0.01074(17) 0.01773(18) 0.00010(14) 0.00572(14) -0.00167(14) Se2 0.0320(2) 0.0225(2) 0.01774(19) 0.00041(16) 0.00288(16) -0.00154(17) Se3 0.0296(2) 0.0169(2) 0.0288(2) 0.00867(17) 0.01323(17) 0.00192(16) Se4 0.01381(17) 0.01605(19) 0.0242(2) 0.00179(16) 0.00357(15) -0.00132(15) C1 0.0221(19) 0.018(2) 0.027(2) -0.0050(17) 0.0057(16) -0.0082(16) C2 0.040(2) 0.017(2) 0.032(2) -0.0069(18) 0.0085(19) -0.0063(18) C3 0.043(3) 0.019(2) 0.028(2) -0.0047(18) 0.0129(19) 0.0037(18) C4 0.066(3) 0.042(3) 0.020(2) -0.003(2) 0.019(2) 0.000(2) C5 0.085(4) 0.044(3) 0.024(2) 0.010(2) 0.021(3) 0.002(3) C6 0.047(3) 0.041(3) 0.029(2) 0.010(2) 0.022(2) 0.002(2) C7 0.032(2) 0.032(2) 0.047(3) 0.013(2) 0.020(2) -0.008(2) C8 0.022(2) 0.022(2) 0.048(3) 0.005(2) 0.0122(19) -0.0044(17) C9 0.0116(18) 0.029(2) 0.045(3) 0.001(2) 0.0096(17) -0.0046(17) Fe 0.0173(3) 0.0112(3) 0.0198(3) -0.0014(2) 0.0071(2) -0.0016(2) C10 0.0154(18) 0.0158(19) 0.027(2) -0.0016(16) 0.0063(15) -0.0036(15) C11 0.026(2) 0.015(2) 0.032(2) 0.0023(17) 0.0125(18) -0.0056(16) C12 0.035(2) 0.0109(19) 0.042(3) -0.0047(18) 0.016(2) -0.0050(17) C13 0.033(2) 0.025(2) 0.028(2) -0.0117(18) 0.0123(18) -0.0112(18) C14 0.024(2) 0.024(2) 0.021(2) -0.0056(17) 0.0025(16) -0.0078(17) C15 0.0167(18) 0.0139(18) 0.0225(19) -0.0013(15) 0.0090(15) -0.0032(15) C16 0.0162(18) 0.0155(19) 0.029(2) -0.0031(16) 0.0043(16) -0.0025(15) C17 0.0150(19) 0.023(2) 0.044(3) -0.0044(19) 0.0107(18) 0.0010(16) C18 0.026(2) 0.023(2) 0.035(2) -0.0099(18) 0.0202(18) -0.0104(17) C19 0.026(2) 0.0179(19) 0.024(2) 0.0011(17) 0.0116(16) -0.0078(17) P1A 0.043(5) 0.024(6) 0.031(5) 0.003(4) 0.019(4) 0.001(4) F1A 0.093(16) 0.020(9) 0.073(12) -0.022(8) 0.017(10) 0.005(9) F2A 0.043(8) 0.046(12) 0.036(9) 0.002(8) 0.009(7) -0.026(8) F3A 0.069(16) 0.021(8) 0.065(10) -0.001(7) 0.009(10) 0.021(8) F4A 0.030(8) 0.063(11) 0.040(10) -0.014(8) 0.021(7) -0.001(7) F5A 0.043(12) 0.12(2) 0.025(10) 0.002(10) 0.016(9) -0.039(11) F6A 0.047(11) 0.069(11) 0.027(8) -0.003(7) 0.013(7) -0.007(9) P1B 0.047(2) 0.0125(14) 0.0310(17) -0.0035(11) 0.0162(13) -0.0015(13) F1B 0.045(4) 0.031(3) 0.122(6) -0.012(4) 0.033(4) 0.007(3) F2B 0.072(4) 0.035(4) 0.060(4) -0.009(3) 0.030(4) -0.028(3) F3B 0.083(7) 0.039(3) 0.045(3) -0.014(2) -0.012(3) 0.038(4) F4B 0.044(4) 0.049(3) 0.044(4) -0.019(3) 0.015(3) -0.008(3) F5B 0.045(4) 0.039(4) 0.029(3) 0.007(2) 0.004(3) -0.003(2) F6B 0.125(10) 0.047(4) 0.035(3) -0.008(3) 0.033(5) -0.034(5) P2A 0.022(4) 0.055(7) 0.034(6) -0.005(5) 0.012(4) 0.016(4) F7A 0.089(13) 0.047(8) 0.097(11) 0.011(8) 0.046(10) -0.001(9) F8A 0.077(12) 0.059(11) 0.071(10) 0.028(8) 0.045(9) 0.051(9) F9A 0.051(7) 0.044(7) 0.049(7) 0.002(6) 0.029(6) -0.031(6) F10A 0.032(6) 0.017(5) 0.010(5) 0.003(4) 0.014(5) 0.005(4) F11A 0.038(7) 0.065(11) 0.029(7) 0.022(7) 0.015(6) 0.005(7) F12A 0.043(8) 0.124(16) 0.042(8) 0.031(10) 0.003(6) 0.000(10) P2B 0.0314(16) 0.0257(16) 0.0187(17) 0.0018(12) 0.0057(12) 0.0097(12) F7B 0.115(6) 0.031(2) 0.054(3) 0.013(2) 0.042(4) 0.013(3) F8B 0.055(3) 0.060(4) 0.044(3) 0.010(2) 0.031(2) 0.027(3) F9B 0.083(5) 0.036(3) 0.051(3) 0.006(2) 0.021(3) 0.030(3) F10B 0.037(3) 0.083(5) 0.054(4) -0.020(3) 0.015(3) -0.001(3) F11B 0.067(4) 0.079(5) 0.032(3) -0.028(3) -0.005(3) -0.006(3) F12B 0.033(2) 0.069(4) 0.030(2) -0.004(2) 0.0020(18) 0.000(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Se3 2.3990(5) . ? Pd Se2 2.4240(5) . ? Pd Se4 2.4406(5) . ? Pd Se1 2.4767(4) . ? Se1 C15 1.907(4) . ? Se1 C1 1.965(4) . ? Se2 C4 1.960(4) . ? Se2 C3 1.969(4) . ? Se3 C6 1.956(4) . ? Se3 C7 1.965(4) . ? Se4 C10 1.895(4) . ? Se4 C9 1.959(4) . ? C1 C2 1.519(5) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 C3 1.510(6) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 C5 1.496(7) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C5 C6 1.508(7) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? C7 C8 1.517(6) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 C9 1.514(6) . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? Fe C10 2.012(4) . ? Fe C15 2.016(4) . ? Fe C14 2.028(4) . ? Fe C11 2.032(4) . ? Fe C13 2.034(4) . ? Fe C17 2.034(4) . ? Fe C18 2.035(4) . ? Fe C12 2.036(4) . ? Fe C16 2.039(4) . ? Fe C19 2.041(4) . ? C10 C11 1.421(5) . ? C10 C14 1.428(5) . ? C11 C12 1.416(6) . ? C11 H111 0.9500 . ? C12 C13 1.410(6) . ? C12 H121 0.9500 . ? C13 C14 1.407(6) . ? C13 H131 0.9500 . ? C14 H141 0.9500 . ? C15 C19 1.425(5) . ? C15 C16 1.429(5) . ? C16 C17 1.421(5) . ? C16 H161 0.9500 . ? C17 C18 1.423(6) . ? C17 H171 0.9500 . ? C18 C19 1.420(6) . ? C18 H181 0.9500 . ? C19 H191 0.9500 . ? P1A F2A 1.558(15) . ? P1A F5A 1.559(14) . ? P1A F1A 1.560(15) . ? P1A F3A 1.561(15) . ? P1A F4A 1.562(15) . ? P1A F6A 1.563(14) . ? P1B F2B 1.591(6) . ? P1B F1B 1.597(6) . ? P1B F5B 1.600(6) . ? P1B F3B 1.602(6) . ? P1B F4B 1.605(6) . ? P1B F6B 1.610(6) . ? P2A F10A 1.575(10) . ? P2A F11A 1.577(11) . ? P2A F7A 1.579(10) . ? P2A F12A 1.580(10) . ? P2A F8A 1.581(11) . ? P2A F9A 1.586(10) . ? P2B F11B 1.573(5) . ? P2B F7B 1.587(4) . ? P2B F10B 1.588(5) . ? P2B F9B 1.593(5) . ? P2B F12B 1.595(5) . ? P2B F8B 1.598(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se3 Pd Se2 92.264(17) . . ? Se3 Pd Se4 96.079(16) . . ? Se2 Pd Se4 170.958(18) . . ? Se3 Pd Se1 168.030(17) . . ? Se2 Pd Se1 89.725(15) . . ? Se4 Pd Se1 82.830(14) . . ? C15 Se1 C1 95.28(16) . . ? C15 Se1 Pd 97.31(11) . . ? C1 Se1 Pd 107.05(12) . . ? C4 Se2 C3 94.87(19) . . ? C4 Se2 Pd 106.27(15) . . ? C3 Se2 Pd 97.41(13) . . ? C6 Se3 C7 93.8(2) . . ? C6 Se3 Pd 108.31(14) . . ? C7 Se3 Pd 111.85(13) . . ? C10 Se4 C9 100.39(17) . . ? C10 Se4 Pd 103.03(11) . . ? C9 Se4 Pd 112.94(13) . . ? C2 C1 Se1 113.1(3) . . ? C2 C1 H11 109.0 . . ? Se1 C1 H11 109.0 . . ? C2 C1 H12 109.0 . . ? Se1 C1 H12 109.0 . . ? H11 C1 H12 107.8 . . ? C3 C2 C1 115.9(3) . . ? C3 C2 H21 108.3 . . ? C1 C2 H21 108.3 . . ? C3 C2 H22 108.3 . . ? C1 C2 H22 108.3 . . ? H21 C2 H22 107.4 . . ? C2 C3 Se2 111.8(3) . . ? C2 C3 H31 109.3 . . ? Se2 C3 H31 109.3 . . ? C2 C3 H32 109.3 . . ? Se2 C3 H32 109.3 . . ? H31 C3 H32 107.9 . . ? C5 C4 Se2 113.7(3) . . ? C5 C4 H41 108.8 . . ? Se2 C4 H41 108.8 . . ? C5 C4 H42 108.8 . . ? Se2 C4 H42 108.8 . . ? H41 C4 H42 107.7 . . ? C4 C5 C6 114.9(4) . . ? C4 C5 H51 108.5 . . ? C6 C5 H51 108.5 . . ? C4 C5 H52 108.5 . . ? C6 C5 H52 108.5 . . ? H51 C5 H52 107.5 . . ? C5 C6 Se3 113.2(3) . . ? C5 C6 H61 108.9 . . ? Se3 C6 H61 108.9 . . ? C5 C6 H62 108.9 . . ? Se3 C6 H62 108.9 . . ? H61 C6 H62 107.7 . . ? C8 C7 Se3 114.8(3) . . ? C8 C7 H71 108.6 . . ? Se3 C7 H71 108.6 . . ? C8 C7 H72 108.6 . . ? Se3 C7 H72 108.6 . . ? H71 C7 H72 107.5 . . ? C9 C8 C7 114.0(4) . . ? C9 C8 H81 108.7 . . ? C7 C8 H81 108.7 . . ? C9 C8 H82 108.7 . . ? C7 C8 H82 108.7 . . ? H81 C8 H82 107.6 . . ? C8 C9 Se4 116.6(3) . . ? C8 C9 H91 108.1 . . ? Se4 C9 H91 108.1 . . ? C8 C9 H92 108.1 . . ? Se4 C9 H92 108.1 . . ? H91 C9 H92 107.3 . . ? C10 Fe C15 110.99(15) . . ? C10 Fe C14 41.40(15) . . ? C15 Fe C14 124.43(16) . . ? C10 Fe C11 41.15(15) . . ? C15 Fe C11 126.35(15) . . ? C14 Fe C11 69.51(16) . . ? C10 Fe C13 68.73(16) . . ? C15 Fe C13 157.98(16) . . ? C14 Fe C13 40.53(16) . . ? C11 Fe C13 68.93(16) . . ? C10 Fe C17 157.60(17) . . ? C15 Fe C17 68.63(15) . . ? C14 Fe C17 157.64(16) . . ? C11 Fe C17 119.74(17) . . ? C13 Fe C17 120.49(17) . . ? C10 Fe C18 161.30(17) . . ? C15 Fe C18 68.68(15) . . ? C14 Fe C18 122.23(17) . . ? C11 Fe C18 154.31(16) . . ? C13 Fe C18 104.27(16) . . ? C17 Fe C18 40.94(17) . . ? C10 Fe C12 68.43(16) . . ? C15 Fe C12 161.30(16) . . ? C14 Fe C12 68.41(17) . . ? C11 Fe C12 40.75(16) . . ? C13 Fe C12 40.55(17) . . ? C17 Fe C12 104.46(17) . . ? C18 Fe C12 118.22(17) . . ? C10 Fe C16 123.79(15) . . ? C15 Fe C16 41.28(15) . . ? C14 Fe C16 160.68(16) . . ? C11 Fe C16 107.25(16) . . ? C13 Fe C16 157.64(16) . . ? C17 Fe C16 40.83(15) . . ? C18 Fe C16 69.17(16) . . ? C12 Fe C16 122.32(17) . . ? C10 Fe C19 126.56(15) . . ? C15 Fe C19 41.11(14) . . ? C14 Fe C19 107.89(16) . . ? C11 Fe C19 163.86(16) . . ? C13 Fe C19 120.11(16) . . ? C17 Fe C19 68.92(16) . . ? C18 Fe C19 40.77(16) . . ? C12 Fe C19 154.44(16) . . ? C16 Fe C19 69.64(16) . . ? C11 C10 C14 108.6(3) . . ? C11 C10 Se4 128.3(3) . . ? C14 C10 Se4 122.7(3) . . ? C11 C10 Fe 70.2(2) . . ? C14 C10 Fe 69.9(2) . . ? Se4 C10 Fe 119.75(18) . . ? C12 C11 C10 106.7(3) . . ? C12 C11 Fe 69.8(2) . . ? C10 C11 Fe 68.7(2) . . ? C12 C11 H111 126.7 . . ? C10 C11 H111 126.7 . . ? Fe C11 H111 126.5 . . ? C13 C12 C11 109.0(4) . . ? C13 C12 Fe 69.6(2) . . ? C11 C12 Fe 69.5(2) . . ? C13 C12 H121 125.5 . . ? C11 C12 H121 125.5 . . ? Fe C12 H121 127.0 . . ? C14 C13 C12 108.4(4) . . ? C14 C13 Fe 69.5(2) . . ? C12 C13 Fe 69.8(2) . . ? C14 C13 H131 125.8 . . ? C12 C13 H131 125.8 . . ? Fe C13 H131 126.5 . . ? C13 C14 C10 107.3(4) . . ? C13 C14 Fe 70.0(2) . . ? C10 C14 Fe 68.7(2) . . ? C13 C14 H141 126.3 . . ? C10 C14 H141 126.3 . . ? Fe C14 H141 126.5 . . ? C19 C15 C16 109.4(3) . . ? C19 C15 Se1 125.1(3) . . ? C16 C15 Se1 125.4(3) . . ? C19 C15 Fe 70.4(2) . . ? C16 C15 Fe 70.2(2) . . ? Se1 C15 Fe 127.20(18) . . ? C17 C16 C15 106.5(3) . . ? C17 C16 Fe 69.4(2) . . ? C15 C16 Fe 68.5(2) . . ? C17 C16 H161 126.8 . . ? C15 C16 H161 126.8 . . ? Fe C16 H161 126.9 . . ? C16 C17 C18 108.8(3) . . ? C16 C17 Fe 69.8(2) . . ? C18 C17 Fe 69.6(2) . . ? C16 C17 H171 125.6 . . ? C18 C17 H171 125.6 . . ? Fe C17 H171 126.7 . . ? C19 C18 C17 108.4(3) . . ? C19 C18 Fe 69.8(2) . . ? C17 C18 Fe 69.5(2) . . ? C19 C18 H181 125.8 . . ? C17 C18 H181 125.8 . . ? Fe C18 H181 126.4 . . ? C18 C19 C15 106.9(3) . . ? C18 C19 Fe 69.4(2) . . ? C15 C19 Fe 68.5(2) . . ? C18 C19 H191 126.5 . . ? C15 C19 H191 126.5 . . ? Fe C19 H191 127.1 . . ? F2A P1A F5A 90.1(4) . . ? F2A P1A F1A 90.3(5) . . ? F5A P1A F1A 90.2(4) . . ? F2A P1A F3A 86.0(16) . . ? F5A P1A F3A 90.0(4) . . ? F1A P1A F3A 176.3(16) . . ? F2A P1A F4A 179.6(8) . . ? F5A P1A F4A 90.1(4) . . ? F1A P1A F4A 90.0(5) . . ? F3A P1A F4A 93.6(17) . . ? F2A P1A F6A 90.0(4) . . ? F5A P1A F6A 179.8(6) . . ? F1A P1A F6A 89.7(4) . . ? F3A P1A F6A 90.1(4) . . ? F4A P1A F6A 89.8(4) . . ? F2B P1B F1B 90.7(3) . . ? F2B P1B F5B 90.1(3) . . ? F1B P1B F5B 91.1(3) . . ? F2B P1B F3B 90.6(5) . . ? F1B P1B F3B 178.4(5) . . ? F5B P1B F3B 89.7(3) . . ? F2B P1B F4B 179.2(4) . . ? F1B P1B F4B 90.1(3) . . ? F5B P1B F4B 90.1(3) . . ? F3B P1B F4B 88.6(6) . . ? F2B P1B F6B 90.6(3) . . ? F1B P1B F6B 89.6(3) . . ? F5B P1B F6B 179.0(4) . . ? F3B P1B F6B 89.6(3) . . ? F4B P1B F6B 89.2(3) . . ? F10A P2A F11A 90.3(4) . . ? F10A P2A F7A 90.1(4) . . ? F11A P2A F7A 89.9(5) . . ? F10A P2A F12A 90.2(4) . . ? F11A P2A F12A 179.4(6) . . ? F7A P2A F12A 89.6(5) . . ? F10A P2A F8A 179.5(5) . . ? F11A P2A F8A 89.5(4) . . ? F7A P2A F8A 90.3(4) . . ? F12A P2A F8A 90.1(4) . . ? F10A P2A F9A 89.9(4) . . ? F11A P2A F9A 87.5(11) . . ? F7A P2A F9A 177.4(11) . . ? F12A P2A F9A 92.9(11) . . ? F8A P2A F9A 89.6(4) . . ? F11B P2B F7B 91.2(3) . . ? F11B P2B F10B 90.5(3) . . ? F7B P2B F10B 90.1(3) . . ? F11B P2B F9B 90.6(4) . . ? F7B P2B F9B 178.2(4) . . ? F10B P2B F9B 90.5(3) . . ? F11B P2B F12B 179.8(4) . . ? F7B P2B F12B 89.1(3) . . ? F10B P2B F12B 89.5(2) . . ? F9B P2B F12B 89.2(4) . . ? F11B P2B F8B 89.8(3) . . ? F7B P2B F8B 90.2(2) . . ? F10B P2B F8B 179.6(4) . . ? F9B P2B F8B 89.2(3) . . ? F12B P2B F8B 90.3(2) . . ? 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 Se3 Pd Se1 C15 -6.24(14) . . . . ? Se2 Pd Se1 C15 -105.90(11) . . . . ? Se4 Pd Se1 C15 79.24(11) . . . . ? Se3 Pd Se1 C1 91.59(15) . . . . ? Se2 Pd Se1 C1 -8.07(12) . . . . ? Se4 Pd Se1 C1 177.08(12) . . . . ? Se3 Pd Se2 C4 46.61(15) . . . . ? Se4 Pd Se2 C4 -110.72(19) . . . . ? Se1 Pd Se2 C4 -145.19(15) . . . . ? Se3 Pd Se2 C3 143.91(12) . . . . ? Se4 Pd Se2 C3 -13.42(17) . . . . ? Se1 Pd Se2 C3 -47.90(12) . . . . ? Se2 Pd Se3 C6 -46.36(15) . . . . ? Se4 Pd Se3 C6 130.15(15) . . . . ? Se1 Pd Se3 C6 -145.76(17) . . . . ? Se2 Pd Se3 C7 -148.40(15) . . . . ? Se4 Pd Se3 C7 28.11(15) . . . . ? Se1 Pd Se3 C7 112.20(17) . . . . ? Se3 Pd Se4 C10 82.66(11) . . . . ? Se2 Pd Se4 C10 -120.13(16) . . . . ? Se1 Pd Se4 C10 -85.34(11) . . . . ? Se3 Pd Se4 C9 -24.74(13) . . . . ? Se2 Pd Se4 C9 132.48(17) . . . . ? Se1 Pd Se4 C9 167.26(13) . . . . ? C15 Se1 C1 C2 167.6(3) . . . . ? Pd Se1 C1 C2 68.2(3) . . . . ? Se1 C1 C2 C3 -48.7(5) . . . . ? C1 C2 C3 Se2 -36.8(5) . . . . ? C4 Se2 C3 C2 -162.0(3) . . . . ? Pd Se2 C3 C2 90.8(3) . . . . ? C3 Se2 C4 C5 -164.7(4) . . . . ? Pd Se2 C4 C5 -65.5(4) . . . . ? Se2 C4 C5 C6 80.2(5) . . . . ? C4 C5 C6 Se3 -77.7(5) . . . . ? C7 Se3 C6 C5 177.3(3) . . . . ? Pd Se3 C6 C5 62.8(3) . . . . ? C6 Se3 C7 C8 -167.5(3) . . . . ? Pd Se3 C7 C8 -56.1(3) . . . . ? Se3 C7 C8 C9 81.3(4) . . . . ? C7 C8 C9 Se4 -76.2(4) . . . . ? C10 Se4 C9 C8 -61.8(3) . . . . ? Pd Se4 C9 C8 47.2(3) . . . . ? C9 Se4 C10 C11 79.3(3) . . . . ? Pd Se4 C10 C11 -37.4(3) . . . . ? C9 Se4 C10 C14 -109.3(3) . . . . ? Pd Se4 C10 C14 134.0(3) . . . . ? C9 Se4 C10 Fe 166.7(2) . . . . ? Pd Se4 C10 Fe 50.0(2) . . . . ? C15 Fe C10 C11 121.7(2) . . . . ? C14 Fe C10 C11 -119.6(3) . . . . ? C13 Fe C10 C11 -81.9(2) . . . . ? C17 Fe C10 C11 37.1(5) . . . . ? C18 Fe C10 C11 -152.9(5) . . . . ? C12 Fe C10 C11 -38.2(2) . . . . ? C16 Fe C10 C11 77.1(3) . . . . ? C19 Fe C10 C11 165.7(2) . . . . ? C15 Fe C10 C14 -118.7(2) . . . . ? C11 Fe C10 C14 119.6(3) . . . . ? C13 Fe C10 C14 37.7(2) . . . . ? C17 Fe C10 C14 156.6(4) . . . . ? C18 Fe C10 C14 -33.4(6) . . . . ? C12 Fe C10 C14 81.4(3) . . . . ? C16 Fe C10 C14 -163.3(2) . . . . ? C19 Fe C10 C14 -74.8(3) . . . . ? C15 Fe C10 Se4 -1.8(3) . . . . ? C14 Fe C10 Se4 116.9(3) . . . . ? C11 Fe C10 Se4 -123.5(3) . . . . ? C13 Fe C10 Se4 154.6(3) . . . . ? C17 Fe C10 Se4 -86.5(5) . . . . ? C18 Fe C10 Se4 83.6(5) . . . . ? C12 Fe C10 Se4 -161.7(3) . . . . ? C16 Fe C10 Se4 -46.4(3) . . . . ? C19 Fe C10 Se4 42.1(3) . . . . ? C14 C10 C11 C12 0.2(4) . . . . ? Se4 C10 C11 C12 172.5(3) . . . . ? Fe C10 C11 C12 59.7(3) . . . . ? C14 C10 C11 Fe -59.5(3) . . . . ? Se4 C10 C11 Fe 112.8(3) . . . . ? C10 Fe C11 C12 -118.2(3) . . . . ? C15 Fe C11 C12 161.4(2) . . . . ? C14 Fe C11 C12 -80.3(3) . . . . ? C13 Fe C11 C12 -36.8(3) . . . . ? C17 Fe C11 C12 77.1(3) . . . . ? C18 Fe C11 C12 42.1(5) . . . . ? C16 Fe C11 C12 119.8(3) . . . . ? C19 Fe C11 C12 -163.9(5) . . . . ? C15 Fe C11 C10 -80.4(3) . . . . ? C14 Fe C11 C10 37.9(2) . . . . ? C13 Fe C11 C10 81.4(2) . . . . ? C17 Fe C11 C10 -164.7(2) . . . . ? C18 Fe C11 C10 160.3(3) . . . . ? C12 Fe C11 C10 118.2(3) . . . . ? C16 Fe C11 C10 -122.0(2) . . . . ? C19 Fe C11 C10 -45.7(7) . . . . ? C10 C11 C12 C13 -0.4(4) . . . . ? Fe C11 C12 C13 58.6(3) . . . . ? C10 C11 C12 Fe -59.0(2) . . . . ? C10 Fe C12 C13 -82.1(3) . . . . ? C15 Fe C12 C13 -174.0(4) . . . . ? C14 Fe C12 C13 -37.4(2) . . . . ? C11 Fe C12 C13 -120.6(4) . . . . ? C17 Fe C12 C13 120.3(3) . . . . ? C18 Fe C12 C13 78.6(3) . . . . ? C16 Fe C12 C13 160.7(2) . . . . ? C19 Fe C12 C13 49.1(5) . . . . ? C10 Fe C12 C11 38.6(2) . . . . ? C15 Fe C12 C11 -53.4(6) . . . . ? C14 Fe C12 C11 83.3(3) . . . . ? C13 Fe C12 C11 120.6(4) . . . . ? C17 Fe C12 C11 -119.0(3) . . . . ? C18 Fe C12 C11 -160.7(2) . . . . ? C16 Fe C12 C11 -78.6(3) . . . . ? C19 Fe C12 C11 169.7(3) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? Fe C12 C13 C14 59.0(3) . . . . ? C11 C12 C13 Fe -58.5(3) . . . . ? C10 Fe C13 C14 -38.4(2) . . . . ? C15 Fe C13 C14 55.1(5) . . . . ? C11 Fe C13 C14 -82.7(3) . . . . ? C17 Fe C13 C14 164.3(2) . . . . ? C18 Fe C13 C14 123.3(3) . . . . ? C12 Fe C13 C14 -119.7(4) . . . . ? C16 Fe C13 C14 -166.9(4) . . . . ? C19 Fe C13 C14 82.4(3) . . . . ? C10 Fe C13 C12 81.3(3) . . . . ? C15 Fe C13 C12 174.9(4) . . . . ? C14 Fe C13 C12 119.7(4) . . . . ? C11 Fe C13 C12 37.0(2) . . . . ? C17 Fe C13 C12 -76.0(3) . . . . ? C18 Fe C13 C12 -117.0(3) . . . . ? C16 Fe C13 C12 -47.2(5) . . . . ? C19 Fe C13 C12 -157.9(2) . . . . ? C12 C13 C14 C10 -0.4(4) . . . . ? Fe C13 C14 C10 58.8(3) . . . . ? C12 C13 C14 Fe -59.2(3) . . . . ? C11 C10 C14 C13 0.1(4) . . . . ? Se4 C10 C14 C13 -172.7(3) . . . . ? Fe C10 C14 C13 -59.6(3) . . . . ? C11 C10 C14 Fe 59.7(3) . . . . ? Se4 C10 C14 Fe -113.1(3) . . . . ? C10 Fe C14 C13 118.8(3) . . . . ? C15 Fe C14 C13 -158.1(2) . . . . ? C11 Fe C14 C13 81.2(3) . . . . ? C17 Fe C14 C13 -37.8(5) . . . . ? C18 Fe C14 C13 -73.2(3) . . . . ? C12 Fe C14 C13 37.4(2) . . . . ? C16 Fe C14 C13 164.9(4) . . . . ? C19 Fe C14 C13 -115.7(2) . . . . ? C15 Fe C14 C10 83.1(3) . . . . ? C11 Fe C14 C10 -37.7(2) . . . . ? C13 Fe C14 C10 -118.8(3) . . . . ? C17 Fe C14 C10 -156.6(4) . . . . ? C18 Fe C14 C10 168.0(2) . . . . ? C12 Fe C14 C10 -81.4(2) . . . . ? C16 Fe C14 C10 46.1(6) . . . . ? C19 Fe C14 C10 125.5(2) . . . . ? C1 Se1 C15 C19 112.4(3) . . . . ? Pd Se1 C15 C19 -139.6(3) . . . . ? C1 Se1 C15 C16 -65.4(3) . . . . ? Pd Se1 C15 C16 42.6(3) . . . . ? C1 Se1 C15 Fe -156.5(2) . . . . ? Pd Se1 C15 Fe -48.5(2) . . . . ? C10 Fe C15 C19 122.0(2) . . . . ? C14 Fe C15 C19 77.4(3) . . . . ? C11 Fe C15 C19 166.1(2) . . . . ? C13 Fe C15 C19 37.1(5) . . . . ? C17 Fe C15 C19 -82.0(2) . . . . ? C18 Fe C15 C19 -37.9(2) . . . . ? C12 Fe C15 C19 -153.4(5) . . . . ? C16 Fe C15 C19 -120.2(3) . . . . ? C10 Fe C15 C16 -117.8(2) . . . . ? C14 Fe C15 C16 -162.4(2) . . . . ? C11 Fe C15 C16 -73.7(3) . . . . ? C13 Fe C15 C16 157.3(4) . . . . ? C17 Fe C15 C16 38.2(2) . . . . ? C18 Fe C15 C16 82.3(2) . . . . ? C12 Fe C15 C16 -33.2(6) . . . . ? C19 Fe C15 C16 120.2(3) . . . . ? C10 Fe C15 Se1 2.3(3) . . . . ? C14 Fe C15 Se1 -42.4(3) . . . . ? C11 Fe C15 Se1 46.3(3) . . . . ? C13 Fe C15 Se1 -82.7(5) . . . . ? C17 Fe C15 Se1 158.2(3) . . . . ? C18 Fe C15 Se1 -157.7(3) . . . . ? C12 Fe C15 Se1 86.9(5) . . . . ? C16 Fe C15 Se1 120.0(3) . . . . ? C19 Fe C15 Se1 -119.8(3) . . . . ? C19 C15 C16 C17 0.4(4) . . . . ? Se1 C15 C16 C17 178.5(3) . . . . ? Fe C15 C16 C17 -59.3(3) . . . . ? C19 C15 C16 Fe 59.7(3) . . . . ? Se1 C15 C16 Fe -122.2(3) . . . . ? C10 Fe C16 C17 -158.0(2) . . . . ? C15 Fe C16 C17 118.3(3) . . . . ? C14 Fe C16 C17 167.0(4) . . . . ? C11 Fe C16 C17 -115.8(2) . . . . ? C13 Fe C16 C17 -39.3(5) . . . . ? C18 Fe C16 C17 37.3(2) . . . . ? C12 Fe C16 C17 -73.7(3) . . . . ? C19 Fe C16 C17 81.0(3) . . . . ? C10 Fe C16 C15 83.8(2) . . . . ? C14 Fe C16 C15 48.8(6) . . . . ? C11 Fe C16 C15 125.9(2) . . . . ? C13 Fe C16 C15 -157.6(4) . . . . ? C17 Fe C16 C15 -118.3(3) . . . . ? C18 Fe C16 C15 -81.0(2) . . . . ? C12 Fe C16 C15 168.0(2) . . . . ? C19 Fe C16 C15 -37.3(2) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? Fe C16 C17 C18 -58.7(3) . . . . ? C15 C16 C17 Fe 58.7(2) . . . . ? C10 Fe C17 C16 54.9(5) . . . . ? C15 Fe C17 C16 -38.6(2) . . . . ? C14 Fe C17 C16 -168.7(4) . . . . ? C11 Fe C17 C16 82.0(3) . . . . ? C13 Fe C17 C16 163.7(2) . . . . ? C18 Fe C17 C16 -120.3(3) . . . . ? C12 Fe C17 C16 123.1(2) . . . . ? C19 Fe C17 C16 -82.9(2) . . . . ? C10 Fe C17 C18 175.1(4) . . . . ? C15 Fe C17 C18 81.7(2) . . . . ? C14 Fe C17 C18 -48.5(5) . . . . ? C11 Fe C17 C18 -157.7(2) . . . . ? C13 Fe C17 C18 -76.0(3) . . . . ? C12 Fe C17 C18 -116.6(2) . . . . ? C16 Fe C17 C18 120.3(3) . . . . ? C19 Fe C17 C18 37.4(2) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? Fe C17 C18 C19 -59.2(3) . . . . ? C16 C17 C18 Fe 58.9(3) . . . . ? C10 Fe C18 C19 -54.5(6) . . . . ? C15 Fe C18 C19 38.2(2) . . . . ? C14 Fe C18 C19 -79.9(3) . . . . ? C11 Fe C18 C19 169.2(3) . . . . ? C13 Fe C18 C19 -119.9(2) . . . . ? C17 Fe C18 C19 119.8(3) . . . . ? C12 Fe C18 C19 -161.0(2) . . . . ? C16 Fe C18 C19 82.6(2) . . . . ? C10 Fe C18 C17 -174.2(4) . . . . ? C15 Fe C18 C17 -81.6(2) . . . . ? C14 Fe C18 C17 160.3(2) . . . . ? C11 Fe C18 C17 49.5(5) . . . . ? C13 Fe C18 C17 120.4(2) . . . . ? C12 Fe C18 C17 79.3(3) . . . . ? C16 Fe C18 C17 -37.2(2) . . . . ? C19 Fe C18 C17 -119.8(3) . . . . ? C17 C18 C19 C15 0.6(4) . . . . ? Fe C18 C19 C15 -58.4(2) . . . . ? C17 C18 C19 Fe 59.0(3) . . . . ? C16 C15 C19 C18 -0.6(4) . . . . ? Se1 C15 C19 C18 -178.7(3) . . . . ? Fe C15 C19 C18 59.0(3) . . . . ? C16 C15 C19 Fe -59.6(3) . . . . ? Se1 C15 C19 Fe 122.3(3) . . . . ? C10 Fe C19 C18 161.0(2) . . . . ? C15 Fe C19 C18 -118.8(3) . . . . ? C14 Fe C19 C18 118.9(2) . . . . ? C11 Fe C19 C18 -163.0(5) . . . . ? C13 Fe C19 C18 76.3(3) . . . . ? C17 Fe C19 C18 -37.6(2) . . . . ? C12 Fe C19 C18 41.7(5) . . . . ? C16 Fe C19 C18 -81.4(2) . . . . ? C10 Fe C19 C15 -80.1(3) . . . . ? C14 Fe C19 C15 -122.2(2) . . . . ? C11 Fe C19 C15 -44.2(7) . . . . ? C13 Fe C19 C15 -164.9(2) . . . . ? C17 Fe C19 C15 81.2(2) . . . . ? C18 Fe C19 C15 118.8(3) . . . . ? C12 Fe C19 C15 160.5(4) . . . . ? C16 Fe C19 C15 37.5(2) . . . . ? # Attachment '- L.cif' data_jsl28 _database_code_depnum_ccdc_archive 'CCDC 770362' #TrackingRef '- L.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H26 Fe Se4' _chemical_formula_sum 'C19 H26 Fe Se4' _chemical_formula_weight 626.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.9573(3) _cell_length_b 16.2170(2) _cell_length_c 6.1917(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2104.34(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7006 _cell_measurement_theta_min 5.02 _cell_measurement_theta_max 72.07 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 13.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.107 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSPACK routine of Oxford Diffraction software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Oxford Diffraction, Enhance ULTRA assembly' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur PX Ultra CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.1241 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8844 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 72.27 _diffrn_reflns_theta_full 72.27 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 3193 _reflns_number_gt 3042 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Oxford Diffraction software, CrysAlisPro, Version 171.33.41' _computing_cell_refinement 'Oxford Diffraction software, CrysAlisPro, Version 171.33.41' _computing_data_reduction 'Oxford Diffraction software, CrysAlisPro, Version 171.33.41' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+2.5734P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00132(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(10) _refine_ls_number_reflns 3193 _refine_ls_number_parameters 239 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.265 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.137 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 Se1 Se 0.42004(5) 0.86000(6) 0.9501(2) 0.0592(3) Uani 1 1 d D A . Se2 Se 0.29409(7) 1.04828(8) 0.4202(3) 0.0841(5) Uani 1 1 d D . . Se3 Se 0.20553(5) 0.77370(7) 0.0898(2) 0.0650(3) Uani 1 1 d D . . Se4 Se 0.38261(4) 0.60201(5) 0.46780(19) 0.0510(3) Uani 1 1 d D . . Fe Fe 0.51340(5) 0.70788(7) 0.7129(2) 0.0376(3) Uani 1 1 d . A . C1 C 0.4259(5) 0.9806(4) 0.917(2) 0.066(3) Uani 1 1 d D . . H11A H 0.4028 1.0070 1.0342 0.079 Uiso 0.57(3) 1 calc PR A 1 H12A H 0.4702 0.9974 0.9272 0.079 Uiso 0.57(3) 1 calc PR A 1 H11B H 0.4286 1.0052 1.0600 0.079 Uiso 0.43(3) 1 calc PR A 2 H12B H 0.4651 0.9936 0.8416 0.079 Uiso 0.43(3) 1 calc PR A 2 C2A C 0.3984(8) 1.0089(10) 0.701(3) 0.065(6) Uani 0.57(3) 1 d PD A 1 H21A H 0.4078 1.0669 0.6813 0.078 Uiso 0.57(3) 1 calc PR A 1 H22A H 0.4190 0.9786 0.5857 0.078 Uiso 0.57(3) 1 calc PR A 1 C3A C 0.3263(8) 0.9961(12) 0.686(2) 0.064(6) Uani 0.57(3) 1 d PD A 1 H31A H 0.3056 1.0203 0.8111 0.077 Uiso 0.57(3) 1 calc PR A 1 H32A H 0.3168 0.9375 0.6842 0.077 Uiso 0.57(3) 1 calc PR A 1 C2B C 0.3698(10) 1.0204(13) 0.796(3) 0.059(7) Uani 0.43(3) 1 d PD A 2 H21B H 0.3302 1.0047 0.8654 0.071 Uiso 0.43(3) 1 calc PR A 2 H22B H 0.3736 1.0799 0.8048 0.071 Uiso 0.43(3) 1 calc PR A 2 C3B C 0.3668(8) 0.9953(13) 0.557(3) 0.053(6) Uani 0.43(3) 1 d PD A 2 H31B H 0.3627 0.9359 0.5458 0.064 Uiso 0.43(3) 1 calc PR A 2 H32B H 0.4058 1.0117 0.4848 0.064 Uiso 0.43(3) 1 calc PR A 2 C4 C 0.2120(5) 0.9952(7) 0.472(4) 0.096(4) Uani 1 1 d D A . H41 H 0.2017 1.0018 0.6232 0.115 Uiso 1 1 calc R . . H42 H 0.1799 1.0249 0.3898 0.115 Uiso 1 1 calc R . . C5 C 0.2059(8) 0.9046(8) 0.416(4) 0.101(6) Uani 1 1 d . . . H51 H 0.1642 0.8849 0.4608 0.122 Uiso 1 1 calc R A . H52 H 0.2378 0.8736 0.4955 0.122 Uiso 1 1 calc R . . C6 C 0.2144(8) 0.8898(6) 0.176(3) 0.083(4) Uani 1 1 d D A . H61 H 0.2564 0.9091 0.1339 0.100 Uiso 1 1 calc R . . H62 H 0.1831 0.9223 0.0985 0.100 Uiso 1 1 calc R . . C7 C 0.2815(4) 0.7346(6) 0.2392(17) 0.056(2) Uani 1 1 d D . . H71 H 0.3019 0.6928 0.1511 0.068 Uiso 1 1 calc R . . H72 H 0.3111 0.7801 0.2545 0.068 Uiso 1 1 calc R . . C8 C 0.2681(3) 0.6985(5) 0.4622(19) 0.0502(19) Uani 1 1 d . . . H81 H 0.2461 0.6463 0.4443 0.060 Uiso 1 1 calc R . . H82 H 0.2396 0.7354 0.5388 0.060 Uiso 1 1 calc R . . C9 C 0.3273(4) 0.6842(5) 0.6009(17) 0.0504(18) Uani 1 1 d D . . H91 H 0.3146 0.6655 0.7433 0.060 Uiso 1 1 calc R . . H92 H 0.3505 0.7356 0.6173 0.060 Uiso 1 1 calc R . . C10 C 0.4525(4) 0.6105(4) 0.6604(14) 0.0410(17) Uani 1 1 d . . . C11 C 0.4521(5) 0.6344(5) 0.8798(15) 0.050(2) Uani 1 1 d . . . H111 H 0.4168 0.6528 0.9571 0.060 Uiso 1 1 calc R . . C12 C 0.5150(5) 0.6254(6) 0.962(2) 0.060(2) Uani 1 1 d . . . H121 H 0.5280 0.6360 1.1024 0.072 Uiso 1 1 calc R . . C13 C 0.5546(4) 0.5972(5) 0.7900(19) 0.056(2) Uani 1 1 d . . . H13 H 0.5981 0.5862 0.7996 0.067 Uiso 1 1 calc R . . C14 C 0.5169(4) 0.5888(5) 0.6039(19) 0.049(2) Uani 1 1 d . . . H14 H 0.5311 0.5722 0.4683 0.059 Uiso 1 1 calc R . . C15 C 0.4871(4) 0.8275(4) 0.7651(14) 0.0404(16) Uani 1 1 d . . . C16 C 0.5520(4) 0.8153(5) 0.8259(18) 0.0486(19) Uani 1 1 d . A . H16 H 0.5690 0.8238 0.9628 0.058 Uiso 1 1 calc R . . C17 C 0.5863(4) 0.7880(6) 0.641(2) 0.058(3) Uani 1 1 d . . . H17 H 0.6296 0.7755 0.6365 0.070 Uiso 1 1 calc R A . C18 C 0.5440(5) 0.7831(5) 0.4660(18) 0.055(2) Uani 1 1 d . A . H18 H 0.5545 0.7673 0.3261 0.066 Uiso 1 1 calc R . . C19 C 0.4818(4) 0.8067(5) 0.5397(16) 0.0478(18) Uani 1 1 d . A . H19 H 0.4448 0.8082 0.4570 0.057 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 Se1 0.0624(5) 0.0568(5) 0.0585(7) 0.0093(5) 0.0138(5) 0.0102(4) Se2 0.0850(8) 0.0681(7) 0.0992(12) -0.0022(7) -0.0253(8) 0.0135(5) Se3 0.0646(6) 0.0713(6) 0.0590(7) -0.0105(6) -0.0157(5) 0.0064(5) Se4 0.0469(4) 0.0520(5) 0.0541(6) -0.0142(4) -0.0007(4) -0.0009(3) Fe 0.0398(5) 0.0365(5) 0.0366(7) 0.0059(5) -0.0008(5) -0.0007(4) C1 0.067(5) 0.047(4) 0.083(8) -0.015(5) -0.005(5) 0.004(4) C2A 0.081(13) 0.030(7) 0.083(16) 0.010(9) -0.004(12) -0.003(8) C3A 0.066(11) 0.077(11) 0.050(10) 0.012(10) -0.004(8) 0.027(8) C2B 0.061(14) 0.045(11) 0.072(18) -0.013(11) -0.008(13) 0.009(9) C3B 0.048(10) 0.062(12) 0.049(13) 0.007(10) -0.003(9) 0.014(8) C4 0.108(9) 0.064(6) 0.115(13) -0.007(9) -0.006(10) 0.009(6) C5 0.118(12) 0.070(7) 0.117(16) -0.006(9) 0.021(10) 0.010(7) C6 0.108(10) 0.071(7) 0.070(9) -0.004(6) -0.024(7) 0.019(6) C7 0.047(4) 0.075(6) 0.047(5) 0.005(5) 0.002(4) 0.007(4) C8 0.038(3) 0.055(4) 0.057(5) 0.001(5) 0.013(4) -0.004(3) C9 0.050(4) 0.053(4) 0.048(5) -0.009(4) 0.007(4) 0.004(3) C10 0.046(4) 0.031(3) 0.046(5) 0.004(3) 0.008(3) -0.005(3) C11 0.066(5) 0.041(4) 0.041(5) 0.006(3) 0.007(4) -0.008(3) C12 0.088(6) 0.053(4) 0.039(5) 0.014(4) -0.006(5) -0.009(4) C13 0.056(4) 0.046(4) 0.066(7) 0.013(4) -0.002(4) 0.009(3) C14 0.048(4) 0.040(4) 0.060(6) 0.002(4) -0.005(4) 0.007(3) C15 0.046(4) 0.035(3) 0.040(4) 0.006(3) 0.003(3) -0.001(3) C16 0.039(3) 0.044(4) 0.062(6) 0.002(4) -0.003(4) -0.004(3) C17 0.043(4) 0.055(5) 0.077(8) 0.002(5) 0.014(4) -0.006(3) C18 0.077(6) 0.048(4) 0.041(5) 0.008(4) 0.018(5) -0.006(4) C19 0.055(4) 0.045(4) 0.044(5) 0.008(4) -0.005(3) -0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 C15 1.888(8) . ? Se1 C1 1.970(7) . ? Se2 C3B 1.944(10) . ? Se2 C4 1.949(9) . ? Se2 C3A 1.971(10) . ? Se3 C7 1.947(7) . ? Se3 C6 1.966(9) . ? Se4 C10 1.894(8) . ? Se4 C9 1.949(7) . ? Fe C11 2.034(8) . ? Fe C19 2.039(9) . ? Fe C12 2.040(10) . ? Fe C15 2.042(7) . ? Fe C16 2.044(8) . ? Fe C14 2.047(8) . ? Fe C13 2.048(8) . ? Fe C17 2.055(8) . ? Fe C10 2.056(7) . ? Fe C18 2.058(9) . ? C1 C2A 1.528(15) . ? C1 C2B 1.539(14) . ? C1 H11A 0.9700 . ? C1 H12A 0.9700 . ? C1 H11B 0.9700 . ? C1 H12B 0.9700 . ? C2A C3A 1.527(14) . ? C2A H21A 0.9700 . ? C2A H22A 0.9700 . ? C3A H31A 0.9700 . ? C3A H32A 0.9700 . ? C2B C3B 1.531(15) . ? C2B H21B 0.9700 . ? C2B H22B 0.9700 . ? C3B H31B 0.9700 . ? C3B H32B 0.9700 . ? C4 C5 1.514(18) . ? C4 H41 0.9700 . ? C4 H42 0.9700 . ? C5 C6 1.52(3) . ? C5 H51 0.9700 . ? C5 H52 0.9700 . ? C6 H61 0.9700 . ? C6 H62 0.9700 . ? C7 C8 1.525(15) . ? C7 H71 0.9700 . ? C7 H72 0.9700 . ? C8 C9 1.527(13) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? C10 C11 1.412(13) . ? C10 C14 1.439(11) . ? C11 C12 1.420(14) . ? C11 H111 0.9300 . ? C12 C13 1.424(16) . ? C12 H121 0.9300 . ? C13 C14 1.403(15) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.426(11) . ? C15 C19 1.440(14) . ? C16 C17 1.423(15) . ? C16 H16 0.9300 . ? C17 C18 1.401(16) . ? C17 H17 0.9300 . ? C18 C19 1.433(13) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? 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 C15 Se1 C1 99.7(4) . . ? C3B Se2 C4 115.2(9) . . ? C3B Se2 C3A 34.6(8) . . ? C4 Se2 C3A 88.7(8) . . ? C7 Se3 C6 96.0(5) . . ? C10 Se4 C9 98.2(4) . . ? C11 Fe C19 121.5(4) . . ? C11 Fe C12 40.8(4) . . ? C19 Fe C12 156.6(4) . . ? C11 Fe C15 107.8(3) . . ? C19 Fe C15 41.3(4) . . ? C12 Fe C15 120.5(4) . . ? C11 Fe C16 125.1(4) . . ? C19 Fe C16 68.8(4) . . ? C12 Fe C16 107.1(4) . . ? C15 Fe C16 40.9(3) . . ? C11 Fe C14 68.8(4) . . ? C19 Fe C14 125.4(4) . . ? C12 Fe C14 68.3(5) . . ? C15 Fe C14 163.3(3) . . ? C16 Fe C14 154.5(3) . . ? C11 Fe C13 68.6(4) . . ? C19 Fe C13 161.5(4) . . ? C12 Fe C13 40.8(4) . . ? C15 Fe C13 155.4(4) . . ? C16 Fe C13 120.0(4) . . ? C14 Fe C13 40.1(4) . . ? C11 Fe C17 161.9(5) . . ? C19 Fe C17 68.3(4) . . ? C12 Fe C17 124.5(4) . . ? C15 Fe C17 68.6(3) . . ? C16 Fe C17 40.6(4) . . ? C14 Fe C17 119.9(4) . . ? C13 Fe C17 107.0(4) . . ? C11 Fe C10 40.4(4) . . ? C19 Fe C10 108.6(3) . . ? C12 Fe C10 68.0(4) . . ? C15 Fe C10 125.9(3) . . ? C16 Fe C10 162.6(3) . . ? C14 Fe C10 41.1(3) . . ? C13 Fe C10 68.0(3) . . ? C17 Fe C10 155.9(4) . . ? C11 Fe C18 157.1(4) . . ? C19 Fe C18 40.9(4) . . ? C12 Fe C18 160.8(4) . . ? C15 Fe C18 68.8(3) . . ? C16 Fe C18 68.0(4) . . ? C14 Fe C18 107.6(4) . . ? C13 Fe C18 124.1(4) . . ? C17 Fe C18 39.8(5) . . ? C10 Fe C18 122.1(4) . . ? C2A C1 C2B 32.4(11) . . ? C2A C1 Se1 111.4(8) . . ? C2B C1 Se1 114.8(10) . . ? C2A C1 H11A 109.4 . . ? C2B C1 H11A 78.4 . . ? Se1 C1 H11A 109.4 . . ? C2A C1 H12A 109.4 . . ? C2B C1 H12A 130.1 . . ? Se1 C1 H12A 109.4 . . ? H11A C1 H12A 108.0 . . ? C2A C1 H11B 134.1 . . ? C2B C1 H11B 108.6 . . ? Se1 C1 H11B 108.6 . . ? H11A C1 H11B 33.9 . . ? H12A C1 H11B 76.9 . . ? C2A C1 H12B 80.2 . . ? C2B C1 H12B 108.6 . . ? Se1 C1 H12B 108.6 . . ? H11A C1 H12B 133.5 . . ? H12A C1 H12B 32.6 . . ? H11B C1 H12B 107.5 . . ? C3A C2A C1 112.7(12) . . ? C3A C2A H21A 109.1 . . ? C1 C2A H21A 109.1 . . ? C3A C2A H22A 109.1 . . ? C1 C2A H22A 109.1 . . ? H21A C2A H22A 107.8 . . ? C2A C3A Se2 109.4(10) . . ? C2A C3A H31A 109.8 . . ? Se2 C3A H31A 109.8 . . ? C2A C3A H32A 109.8 . . ? Se2 C3A H32A 109.8 . . ? H31A C3A H32A 108.2 . . ? C3B C2B C1 113.1(13) . . ? C3B C2B H21B 109.0 . . ? C1 C2B H21B 109.0 . . ? C3B C2B H22B 109.0 . . ? C1 C2B H22B 109.0 . . ? H21B C2B H22B 107.8 . . ? C2B C3B Se2 109.6(10) . . ? C2B C3B H31B 109.7 . . ? Se2 C3B H31B 109.7 . . ? C2B C3B H32B 109.7 . . ? Se2 C3B H32B 109.7 . . ? H31B C3B H32B 108.2 . . ? C5 C4 Se2 117.8(10) . . ? C5 C4 H41 107.9 . . ? Se2 C4 H41 107.9 . . ? C5 C4 H42 107.9 . . ? Se2 C4 H42 107.9 . . ? H41 C4 H42 107.2 . . ? C4 C5 C6 111.4(15) . . ? C4 C5 H51 109.4 . . ? C6 C5 H51 109.4 . . ? C4 C5 H52 109.4 . . ? C6 C5 H52 109.4 . . ? H51 C5 H52 108.0 . . ? C5 C6 Se3 114.0(10) . . ? C5 C6 H61 108.7 . . ? Se3 C6 H61 108.7 . . ? C5 C6 H62 108.7 . . ? Se3 C6 H62 108.7 . . ? H61 C6 H62 107.6 . . ? C8 C7 Se3 113.9(6) . . ? C8 C7 H71 108.8 . . ? Se3 C7 H71 108.8 . . ? C8 C7 H72 108.8 . . ? Se3 C7 H72 108.8 . . ? H71 C7 H72 107.7 . . ? C7 C8 C9 114.7(6) . . ? C7 C8 H81 108.6 . . ? C9 C8 H81 108.6 . . ? C7 C8 H82 108.6 . . ? C9 C8 H82 108.6 . . ? H81 C8 H82 107.6 . . ? C8 C9 Se4 110.4(6) . . ? C8 C9 H91 109.6 . . ? Se4 C9 H91 109.6 . . ? C8 C9 H92 109.6 . . ? Se4 C9 H92 109.6 . . ? H91 C9 H92 108.1 . . ? C11 C10 C14 107.9(8) . . ? C11 C10 Se4 128.4(6) . . ? C14 C10 Se4 123.7(7) . . ? C11 C10 Fe 69.0(4) . . ? C14 C10 Fe 69.1(4) . . ? Se4 C10 Fe 129.5(4) . . ? C10 C11 C12 108.0(9) . . ? C10 C11 Fe 70.6(5) . . ? C12 C11 Fe 69.8(5) . . ? C10 C11 H111 126.0 . . ? C12 C11 H111 126.0 . . ? Fe C11 H111 125.1 . . ? C11 C12 C13 108.0(10) . . ? C11 C12 Fe 69.4(5) . . ? C13 C12 Fe 69.9(6) . . ? C11 C12 H121 126.0 . . ? C13 C12 H121 126.0 . . ? Fe C12 H121 126.2 . . ? C14 C13 C12 108.4(8) . . ? C14 C13 Fe 69.9(5) . . ? C12 C13 Fe 69.3(5) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Fe C13 H13 126.5 . . ? C13 C14 C10 107.7(9) . . ? C13 C14 Fe 70.0(5) . . ? C10 C14 Fe 69.8(4) . . ? C13 C14 H14 126.1 . . ? C10 C14 H14 126.1 . . ? Fe C14 H14 125.6 . . ? C16 C15 C19 107.3(7) . . ? C16 C15 Se1 126.1(7) . . ? C19 C15 Se1 126.6(6) . . ? C16 C15 Fe 69.7(4) . . ? C19 C15 Fe 69.2(5) . . ? Se1 C15 Fe 124.2(4) . . ? C17 C16 C15 108.2(9) . . ? C17 C16 Fe 70.1(5) . . ? C15 C16 Fe 69.5(4) . . ? C17 C16 H16 125.9 . . ? C15 C16 H16 125.9 . . ? Fe C16 H16 126.1 . . ? C18 C17 C16 108.7(8) . . ? C18 C17 Fe 70.2(5) . . ? C16 C17 Fe 69.3(5) . . ? C18 C17 H17 125.7 . . ? C16 C17 H17 125.7 . . ? Fe C17 H17 126.4 . . ? C17 C18 C19 108.4(9) . . ? C17 C18 Fe 70.0(6) . . ? C19 C18 Fe 68.8(5) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? Fe C18 H18 127.0 . . ? C18 C19 C15 107.5(8) . . ? C18 C19 Fe 70.3(5) . . ? C15 C19 Fe 69.5(5) . . ? C18 C19 H19 126.2 . . ? C15 C19 H19 126.2 . . ? Fe C19 H19 125.6 . . ? 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 C15 Se1 C1 C2A 75.6(10) . . . . ? C15 Se1 C1 C2B 110.7(12) . . . . ? C2B C1 C2A C3A -36(2) . . . . ? Se1 C1 C2A C3A 67.3(16) . . . . ? C1 C2A C3A Se2 172.2(10) . . . . ? C3B Se2 C3A C2A 29.0(14) . . . . ? C4 Se2 C3A C2A 170.5(14) . . . . ? C2A C1 C2B C3B 24.7(15) . . . . ? Se1 C1 C2B C3B -67(2) . . . . ? C1 C2B C3B Se2 179.6(13) . . . . ? C4 Se2 C3B C2B -80.1(18) . . . . ? C3A Se2 C3B C2B -36.7(15) . . . . ? C3B Se2 C4 C5 -54.7(19) . . . . ? C3A Se2 C4 C5 -77.7(17) . . . . ? Se2 C4 C5 C6 -64(2) . . . . ? C4 C5 C6 Se3 -178.9(9) . . . . ? C7 Se3 C6 C5 -66.6(12) . . . . ? C6 Se3 C7 C8 96.0(9) . . . . ? Se3 C7 C8 C9 -167.8(6) . . . . ? C7 C8 C9 Se4 -63.8(9) . . . . ? C10 Se4 C9 C8 173.6(6) . . . . ? C9 Se4 C10 C11 27.7(7) . . . . ? C9 Se4 C10 C14 -155.4(6) . . . . ? C9 Se4 C10 Fe -65.7(6) . . . . ? C19 Fe C10 C11 -117.1(6) . . . . ? C12 Fe C10 C11 38.2(6) . . . . ? C15 Fe C10 C11 -74.4(6) . . . . ? C16 Fe C10 C11 -38.7(14) . . . . ? C14 Fe C10 C11 119.9(8) . . . . ? C13 Fe C10 C11 82.4(6) . . . . ? C17 Fe C10 C11 164.7(9) . . . . ? C18 Fe C10 C11 -160.2(5) . . . . ? C11 Fe C10 C14 -119.9(8) . . . . ? C19 Fe C10 C14 123.0(6) . . . . ? C12 Fe C10 C14 -81.7(6) . . . . ? C15 Fe C10 C14 165.7(6) . . . . ? C16 Fe C10 C14 -158.6(11) . . . . ? C13 Fe C10 C14 -37.6(6) . . . . ? C17 Fe C10 C14 44.8(11) . . . . ? C18 Fe C10 C14 79.9(7) . . . . ? C11 Fe C10 Se4 123.0(8) . . . . ? C19 Fe C10 Se4 6.0(6) . . . . ? C12 Fe C10 Se4 161.3(7) . . . . ? C15 Fe C10 Se4 48.7(7) . . . . ? C16 Fe C10 Se4 84.3(14) . . . . ? C14 Fe C10 Se4 -117.1(8) . . . . ? C13 Fe C10 Se4 -154.6(7) . . . . ? C17 Fe C10 Se4 -72.2(10) . . . . ? C18 Fe C10 Se4 -37.2(7) . . . . ? C14 C10 C11 C12 -1.8(8) . . . . ? Se4 C10 C11 C12 175.6(6) . . . . ? Fe C10 C11 C12 -60.1(6) . . . . ? C14 C10 C11 Fe 58.3(5) . . . . ? Se4 C10 C11 Fe -124.4(6) . . . . ? C19 Fe C11 C10 81.8(6) . . . . ? C12 Fe C11 C10 -118.5(8) . . . . ? C15 Fe C11 C10 125.0(5) . . . . ? C16 Fe C11 C10 166.8(5) . . . . ? C14 Fe C11 C10 -37.6(5) . . . . ? C13 Fe C11 C10 -80.8(6) . . . . ? C17 Fe C11 C10 -159.7(10) . . . . ? C18 Fe C11 C10 47.5(11) . . . . ? C19 Fe C11 C12 -159.7(6) . . . . ? C15 Fe C11 C12 -116.5(6) . . . . ? C16 Fe C11 C12 -74.7(7) . . . . ? C14 Fe C11 C12 80.9(6) . . . . ? C13 Fe C11 C12 37.7(7) . . . . ? C17 Fe C11 C12 -41.2(14) . . . . ? C10 Fe C11 C12 118.5(8) . . . . ? C18 Fe C11 C12 166.1(9) . . . . ? C10 C11 C12 C13 1.1(9) . . . . ? Fe C11 C12 C13 -59.5(6) . . . . ? C10 C11 C12 Fe 60.6(5) . . . . ? C19 Fe C12 C11 48.2(13) . . . . ? C15 Fe C12 C11 81.9(6) . . . . ? C16 Fe C12 C11 124.4(6) . . . . ? C14 Fe C12 C11 -82.3(6) . . . . ? C13 Fe C12 C11 -119.2(9) . . . . ? C17 Fe C12 C11 165.6(5) . . . . ? C10 Fe C12 C11 -37.9(5) . . . . ? C18 Fe C12 C11 -163.4(11) . . . . ? C11 Fe C12 C13 119.2(9) . . . . ? C19 Fe C12 C13 167.4(9) . . . . ? C15 Fe C12 C13 -158.9(5) . . . . ? C16 Fe C12 C13 -116.4(6) . . . . ? C14 Fe C12 C13 37.0(6) . . . . ? C17 Fe C12 C13 -75.1(7) . . . . ? C10 Fe C12 C13 81.4(6) . . . . ? C18 Fe C12 C13 -44.2(16) . . . . ? C11 C12 C13 C14 0.0(10) . . . . ? Fe C12 C13 C14 -59.2(6) . . . . ? C11 C12 C13 Fe 59.2(6) . . . . ? C11 Fe C13 C14 82.1(6) . . . . ? C19 Fe C13 C14 -44.4(14) . . . . ? C12 Fe C13 C14 119.8(8) . . . . ? C15 Fe C13 C14 168.1(7) . . . . ? C16 Fe C13 C14 -158.8(6) . . . . ? C17 Fe C13 C14 -116.5(6) . . . . ? C10 Fe C13 C14 38.4(6) . . . . ? C18 Fe C13 C14 -76.3(7) . . . . ? C11 Fe C13 C12 -37.8(6) . . . . ? C19 Fe C13 C12 -164.2(10) . . . . ? C15 Fe C13 C12 48.2(11) . . . . ? C16 Fe C13 C12 81.4(7) . . . . ? C14 Fe C13 C12 -119.8(8) . . . . ? C17 Fe C13 C12 123.7(6) . . . . ? C10 Fe C13 C12 -81.4(6) . . . . ? C18 Fe C13 C12 163.9(6) . . . . ? C12 C13 C14 C10 -1.1(9) . . . . ? Fe C13 C14 C10 -59.9(5) . . . . ? C12 C13 C14 Fe 58.8(6) . . . . ? C11 C10 C14 C13 1.7(9) . . . . ? Se4 C10 C14 C13 -175.7(6) . . . . ? Fe C10 C14 C13 60.0(6) . . . . ? C11 C10 C14 Fe -58.2(5) . . . . ? Se4 C10 C14 Fe 124.3(5) . . . . ? C11 Fe C14 C13 -81.6(7) . . . . ? C19 Fe C14 C13 164.2(6) . . . . ? C12 Fe C14 C13 -37.6(6) . . . . ? C15 Fe C14 C13 -162.6(11) . . . . ? C16 Fe C14 C13 46.7(13) . . . . ? C17 Fe C14 C13 80.8(8) . . . . ? C10 Fe C14 C13 -118.6(9) . . . . ? C18 Fe C14 C13 122.5(6) . . . . ? C11 Fe C14 C10 37.1(6) . . . . ? C19 Fe C14 C10 -77.2(7) . . . . ? C12 Fe C14 C10 81.0(6) . . . . ? C15 Fe C14 C10 -44.0(16) . . . . ? C16 Fe C14 C10 165.3(9) . . . . ? C13 Fe C14 C10 118.6(9) . . . . ? C17 Fe C14 C10 -160.6(6) . . . . ? C18 Fe C14 C10 -118.9(6) . . . . ? C1 Se1 C15 C16 90.4(7) . . . . ? C1 Se1 C15 C19 -92.7(8) . . . . ? C1 Se1 C15 Fe 179.0(5) . . . . ? C11 Fe C15 C16 123.6(6) . . . . ? C19 Fe C15 C16 -118.6(7) . . . . ? C12 Fe C15 C16 80.8(6) . . . . ? C14 Fe C15 C16 -161.2(13) . . . . ? C13 Fe C15 C16 46.4(10) . . . . ? C17 Fe C15 C16 -37.6(6) . . . . ? C10 Fe C15 C16 164.5(6) . . . . ? C18 Fe C15 C16 -80.5(6) . . . . ? C11 Fe C15 C19 -117.8(5) . . . . ? C12 Fe C15 C19 -160.5(5) . . . . ? C16 Fe C15 C19 118.6(7) . . . . ? C14 Fe C15 C19 -42.5(15) . . . . ? C13 Fe C15 C19 165.0(8) . . . . ? C17 Fe C15 C19 81.1(6) . . . . ? C10 Fe C15 C19 -76.8(6) . . . . ? C18 Fe C15 C19 38.2(5) . . . . ? C11 Fe C15 Se1 3.1(6) . . . . ? C19 Fe C15 Se1 120.9(7) . . . . ? C12 Fe C15 Se1 -39.6(6) . . . . ? C16 Fe C15 Se1 -120.5(8) . . . . ? C14 Fe C15 Se1 78.3(15) . . . . ? C13 Fe C15 Se1 -74.1(10) . . . . ? C17 Fe C15 Se1 -158.0(7) . . . . ? C10 Fe C15 Se1 44.1(7) . . . . ? C18 Fe C15 Se1 159.1(6) . . . . ? C19 C15 C16 C17 0.4(9) . . . . ? Se1 C15 C16 C17 177.8(6) . . . . ? Fe C15 C16 C17 59.6(6) . . . . ? C19 C15 C16 Fe -59.2(5) . . . . ? Se1 C15 C16 Fe 118.2(6) . . . . ? C11 Fe C16 C17 164.7(6) . . . . ? C19 Fe C16 C17 -80.9(6) . . . . ? C12 Fe C16 C17 123.5(6) . . . . ? C15 Fe C16 C17 -119.3(8) . . . . ? C14 Fe C16 C17 48.2(12) . . . . ? C13 Fe C16 C17 81.0(7) . . . . ? C10 Fe C16 C17 -165.6(11) . . . . ? C18 Fe C16 C17 -36.8(6) . . . . ? C11 Fe C16 C15 -75.9(7) . . . . ? C19 Fe C16 C15 38.4(5) . . . . ? C12 Fe C16 C15 -117.2(6) . . . . ? C14 Fe C16 C15 167.6(9) . . . . ? C13 Fe C16 C15 -159.7(5) . . . . ? C17 Fe C16 C15 119.3(8) . . . . ? C10 Fe C16 C15 -46.2(15) . . . . ? C18 Fe C16 C15 82.6(6) . . . . ? C15 C16 C17 C18 0.1(10) . . . . ? Fe C16 C17 C18 59.3(6) . . . . ? C15 C16 C17 Fe -59.2(5) . . . . ? C11 Fe C17 C18 -163.8(10) . . . . ? C19 Fe C17 C18 -37.6(6) . . . . ? C12 Fe C17 C18 164.7(6) . . . . ? C15 Fe C17 C18 -82.2(6) . . . . ? C16 Fe C17 C18 -120.0(8) . . . . ? C14 Fe C17 C18 81.8(6) . . . . ? C13 Fe C17 C18 123.4(6) . . . . ? C10 Fe C17 C18 49.5(11) . . . . ? C11 Fe C17 C16 -43.8(14) . . . . ? C19 Fe C17 C16 82.4(6) . . . . ? C12 Fe C17 C16 -75.3(7) . . . . ? C15 Fe C17 C16 37.8(5) . . . . ? C14 Fe C17 C16 -158.3(5) . . . . ? C13 Fe C17 C16 -116.6(6) . . . . ? C10 Fe C17 C16 169.5(7) . . . . ? C18 Fe C17 C16 120.0(8) . . . . ? C16 C17 C18 C19 -0.6(10) . . . . ? Fe C17 C18 C19 58.2(6) . . . . ? C16 C17 C18 Fe -58.8(6) . . . . ? C11 Fe C18 C17 167.2(8) . . . . ? C19 Fe C18 C17 120.1(8) . . . . ? C12 Fe C18 C17 -41.4(15) . . . . ? C15 Fe C18 C17 81.5(6) . . . . ? C16 Fe C18 C17 37.5(5) . . . . ? C14 Fe C18 C17 -115.8(6) . . . . ? C13 Fe C18 C17 -74.8(7) . . . . ? C10 Fe C18 C17 -158.5(5) . . . . ? C11 Fe C18 C19 47.1(12) . . . . ? C12 Fe C18 C19 -161.5(12) . . . . ? C15 Fe C18 C19 -38.5(5) . . . . ? C16 Fe C18 C19 -82.6(6) . . . . ? C14 Fe C18 C19 124.1(6) . . . . ? C13 Fe C18 C19 165.2(6) . . . . ? C17 Fe C18 C19 -120.1(8) . . . . ? C10 Fe C18 C19 81.4(6) . . . . ? C17 C18 C19 C15 0.8(9) . . . . ? Fe C18 C19 C15 59.7(6) . . . . ? C17 C18 C19 Fe -58.9(6) . . . . ? C16 C15 C19 C18 -0.7(9) . . . . ? Se1 C15 C19 C18 -178.1(6) . . . . ? Fe C15 C19 C18 -60.2(6) . . . . ? C16 C15 C19 Fe 59.5(5) . . . . ? Se1 C15 C19 Fe -117.9(6) . . . . ? C11 Fe C19 C18 -160.5(6) . . . . ? C12 Fe C19 C18 164.7(9) . . . . ? C15 Fe C19 C18 118.4(7) . . . . ? C16 Fe C19 C18 80.4(6) . . . . ? C14 Fe C19 C18 -75.4(7) . . . . ? C13 Fe C19 C18 -41.8(14) . . . . ? C17 Fe C19 C18 36.6(6) . . . . ? C10 Fe C19 C18 -117.9(6) . . . . ? C11 Fe C19 C15 81.1(5) . . . . ? C12 Fe C19 C15 46.3(11) . . . . ? C16 Fe C19 C15 -38.0(5) . . . . ? C14 Fe C19 C15 166.2(4) . . . . ? C13 Fe C19 C15 -160.3(10) . . . . ? C17 Fe C19 C15 -81.8(5) . . . . ? C10 Fe C19 C15 123.7(5) . . . . ? C18 Fe C19 C15 -118.4(7) . . . . ?