Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #1. SUBMISSION DETAILS _publ_contact_author_name 'Professor Jim Simpson' _publ_contact_author_address ; Professor Jim Simpson Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_phone '+64 3 4797914' _publ_contact_author_fax '+64 3 4797906' _publ_contact_author_email jsimpson@alkali.otago.ac.nz #3. TITLE AND AUTHOR LIST _publ_section_title ; The dimerisation of carbon disulfide on Fe centres. Some new tetrathiolene complexes of iron ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Cromhout, Natalie L.' ; Department of Chemistry University College Dublin Belfield Dublin 4 IRELAND ; 'Manning, Anthony R.' ; Department of Chemistry University College Dublin Belfield Dublin 4 IRELAND ; 'McAdam, C. John' ; Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; 'Palmer, Anthony J.' ; Department of Chemistry University College Dublin Belfield Dublin 4 IRELAND ; 'Rieger, Anne L.' ; Department of Chemistry Brown University Providence RI 02912 USA ; 'Rieger, Philip H.' ; Department of Chemistry Brown University Providence RI 02912 USA ; 'Robinson, Brian H.' ; Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; 'Simpson, Jim' ; Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; _publ_section_references ; Bruker (1997) XSCANS: Area detector control and integration software, Bruker (1997) Madison Wisconsin SADABS (absorption correction for area detector data) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Hunter K.A. and Simpson J. (1999) TITAN2000 A molecular graphics program to aid structure solution and refinement with the SHELX suite of programs. University of Otago, New Zealand. Sheldrick, G.M. (1997) SHELXS-97 A program for the solution of crystal structures from diffraction data. University of G\"ottingen, Germany. Sheldrick, G.M. (1997) SHELXL-97 A program for the refinement of crystal structures. University of Gottingen, Germany. ; data_compound2c _database_code_CSD 194364 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H84 Fe2 O14 P4 S4' _chemical_formula_sum 'C40 H84 Fe2 O14 P4 S4' _chemical_formula_weight 1152.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.168(4) _cell_length_b 11.255(4) _cell_length_c 12.083(4) _cell_angle_alpha 78.93(2) _cell_angle_beta 82.73(2) _cell_angle_gamma 86.46(2) _cell_volume 1477.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 146(2) _cell_measurement_reflns_used 7182 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.62055 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Bruker 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 146(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 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7182 _diffrn_reflns_av_R_equivalents 0.1166 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5344 _reflns_number_gt 4369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL 1994' _computing_structure_solution ; SHELXS-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ; _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ; _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Molecules of the compound lie about a centre of inversion located at the midpoint of the C1-C1* bond of the C~2~S~4~ unit; refinement therefore involved only one half of the molecular unit. ; _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^)+(0.0608P)^2^+7.8708P] 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 5344 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.1992 _refine_ls_wR_factor_gt 0.1863 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Fe1 Fe 0.11531(7) 0.22421(7) -0.15189(7) 0.0243(2) Uani 1 1 d . . . S1 S -0.06123(12) 0.18421(12) -0.05658(12) 0.0268(3) Uani 1 1 d . . . S2 S -0.17784(12) -0.03621(12) 0.08703(12) 0.0278(3) Uani 1 1 d . . . C1 C -0.0532(5) 0.0324(5) 0.0073(4) 0.0236(11) Uani 1 1 d . . . C2 C 0.0525(5) 0.3676(5) -0.2016(5) 0.0315(13) Uani 1 1 d . . . O2 O 0.0073(4) 0.4591(4) -0.2385(5) 0.0483(12) Uani 1 1 d . . . P1 P 0.18530(13) 0.20595(13) -0.32017(12) 0.0261(3) Uani 1 1 d . . . O11 O 0.2211(4) 0.3332(4) -0.3967(3) 0.0357(10) Uani 1 1 d . . . C11 C 0.2649(6) 0.3493(6) -0.5178(5) 0.0398(15) Uani 1 1 d . . . H11 H 0.2415 0.2789 -0.5487 0.048 Uiso 1 1 calc R . . C111 C 0.3995(7) 0.3547(9) -0.5321(7) 0.065(2) Uani 1 1 d . . . H11A H 0.4229 0.4204 -0.4974 0.098 Uiso 1 1 calc R . . H11B H 0.4294 0.3698 -0.6132 0.098 Uiso 1 1 calc R . . H11C H 0.4345 0.2775 -0.4952 0.098 Uiso 1 1 calc R . . C112 C 0.2026(8) 0.4625(8) -0.5738(7) 0.061(2) Uani 1 1 d . . . H11D H 0.1150 0.4527 -0.5615 0.092 Uiso 1 1 calc R . . H11E H 0.2297 0.4778 -0.6555 0.092 Uiso 1 1 calc R . . H11F H 0.2222 0.5311 -0.5410 0.092 Uiso 1 1 calc R . . O12 O 0.3022(3) 0.1255(3) -0.3500(3) 0.0286(8) Uani 1 1 d . . . C12 C 0.3047(5) -0.0054(5) -0.3448(5) 0.0295(12) Uani 1 1 d . . . H12 H 0.2280 -0.0401 -0.3026 0.035 Uiso 1 1 calc R . . C121 C 0.3185(6) -0.0261(7) -0.4652(6) 0.0510(18) Uani 1 1 d . . . H12A H 0.2491 0.0115 -0.5027 0.076 Uiso 1 1 calc R . . H12B H 0.3227 -0.1133 -0.4652 0.076 Uiso 1 1 calc R . . H12C H 0.3929 0.0101 -0.5061 0.076 Uiso 1 1 calc R . . C122 C 0.4113(6) -0.0574(6) -0.2825(6) 0.0394(15) Uani 1 1 d . . . H12D H 0.4172 -0.1455 -0.2773 0.059 Uiso 1 1 calc R . . H12E H 0.4000 -0.0385 -0.2059 0.059 Uiso 1 1 calc R . . H12F H 0.4857 -0.0219 -0.3239 0.059 Uiso 1 1 calc R . . O13 O 0.0948(4) 0.1511(4) -0.3881(3) 0.0324(9) Uani 1 1 d . . . C13 C -0.0353(5) 0.1737(6) -0.3743(6) 0.0388(15) Uani 1 1 d . . . H13 H -0.0553 0.2361 -0.3254 0.047 Uiso 1 1 calc R . . C131 C -0.0928(6) 0.0574(7) -0.3158(6) 0.0474(17) Uani 1 1 d . . . H13A H -0.1804 0.0715 -0.3014 0.071 Uiso 1 1 calc R . . H13B H -0.0600 0.0284 -0.2435 0.071 Uiso 1 1 calc R . . H13C H -0.0756 -0.0037 -0.3642 0.071 Uiso 1 1 calc R . . C132 C -0.0750(7) 0.2219(7) -0.4893(6) 0.0494(18) Uani 1 1 d . . . H13D H -0.0585 0.1601 -0.5370 0.074 Uiso 1 1 calc R . . H13E H -0.0305 0.2945 -0.5250 0.074 Uiso 1 1 calc R . . H13F H -0.1618 0.2426 -0.4810 0.074 Uiso 1 1 calc R . . P2 P 0.27868(13) 0.29493(13) -0.11915(13) 0.0268(3) Uani 1 1 d . . . O21 O 0.3190(4) 0.4273(4) -0.1818(4) 0.0369(10) Uani 1 1 d . . . C21 C 0.2624(6) 0.5393(6) -0.1513(7) 0.0455(17) Uani 1 1 d . . . H21 H 0.1818 0.5218 -0.1065 0.055 Uiso 1 1 calc R . . C211 C 0.2457(8) 0.6246(7) -0.2606(8) 0.068(3) Uani 1 1 d . . . H21A H 0.3249 0.6467 -0.3019 0.101 Uiso 1 1 calc R . . H21B H 0.2004 0.6979 -0.2441 0.101 Uiso 1 1 calc R . . H21C H 0.2009 0.5851 -0.3072 0.101 Uiso 1 1 calc R . . C212 C 0.3433(9) 0.5874(8) -0.0799(9) 0.071(3) Uani 1 1 d . . . H21D H 0.4229 0.6028 -0.1233 0.107 Uiso 1 1 calc R . . H21E H 0.3522 0.5275 -0.0106 0.107 Uiso 1 1 calc R . . H21F H 0.3073 0.6630 -0.0595 0.107 Uiso 1 1 calc R . . O22 O 0.2812(4) 0.3117(4) 0.0100(4) 0.0412(11) Uani 1 1 d . . . C22 C 0.2235(7) 0.2342(6) 0.1106(6) 0.0436(16) Uani 1 1 d . . . H22 H 0.1950 0.1602 0.0891 0.052 Uiso 1 1 calc R . . C221 C 0.3164(8) 0.1988(8) 0.1890(6) 0.062(2) Uani 1 1 d . . . H22A H 0.3845 0.1564 0.1517 0.093 Uiso 1 1 calc R . . H22B H 0.2815 0.1450 0.2577 0.093 Uiso 1 1 calc R . . H22C H 0.3448 0.2714 0.2096 0.093 Uiso 1 1 calc R . . C222 C 0.1186(8) 0.3024(11) 0.1601(8) 0.084(3) Uani 1 1 d . . . H22D H 0.1464 0.3755 0.1802 0.126 Uiso 1 1 calc R . . H22E H 0.0794 0.2513 0.2283 0.126 Uiso 1 1 calc R . . H22F H 0.0608 0.3254 0.1044 0.126 Uiso 1 1 calc R . . O23 O 0.3972(3) 0.2181(4) -0.1503(4) 0.0319(9) Uani 1 1 d . . . C23 C 0.5189(5) 0.2535(6) -0.1389(6) 0.0386(15) Uani 1 1 d . . . H23 H 0.5139 0.3200 -0.0940 0.046 Uiso 1 1 calc R . . C231 C 0.5796(7) 0.2966(9) -0.2584(8) 0.078(3) Uani 1 1 d . . . H23A H 0.5819 0.2312 -0.3019 0.118 Uiso 1 1 calc R . . H23B H 0.6621 0.3193 -0.2550 0.118 Uiso 1 1 calc R . . H23C H 0.5338 0.3669 -0.2954 0.118 Uiso 1 1 calc R . . C232 C 0.5829(6) 0.1430(7) -0.0792(7) 0.0482(18) Uani 1 1 d . . . H23D H 0.5388 0.1154 -0.0040 0.072 Uiso 1 1 calc R . . H23E H 0.6650 0.1629 -0.0706 0.072 Uiso 1 1 calc R . . H23F H 0.5866 0.0786 -0.1238 0.072 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 Fe1 0.0198(4) 0.0250(4) 0.0261(4) -0.0002(3) -0.0029(3) 0.0001(3) S1 0.0217(6) 0.0253(6) 0.0306(8) -0.0016(5) -0.0004(5) 0.0031(5) S2 0.0200(6) 0.0291(7) 0.0298(8) 0.0018(5) 0.0014(5) 0.0019(5) C1 0.024(3) 0.028(3) 0.016(3) 0.002(2) -0.004(2) 0.001(2) C2 0.029(3) 0.039(3) 0.029(3) -0.008(2) -0.013(2) 0.006(2) O2 0.046(3) 0.033(2) 0.065(3) -0.002(2) -0.018(2) 0.010(2) P1 0.0236(7) 0.0277(7) 0.0261(8) -0.0005(6) -0.0061(6) -0.0008(5) O11 0.044(2) 0.031(2) 0.030(2) 0.0024(17) -0.0029(19) -0.0096(18) C11 0.054(4) 0.039(3) 0.026(3) 0.000(3) -0.007(3) -0.013(3) C111 0.053(5) 0.080(6) 0.052(5) 0.009(4) 0.003(4) -0.010(4) C112 0.065(5) 0.067(5) 0.041(4) 0.020(4) -0.010(4) -0.010(4) O12 0.0200(18) 0.032(2) 0.032(2) -0.0017(16) -0.0034(16) -0.0045(15) C12 0.024(3) 0.028(3) 0.038(3) -0.011(2) 0.000(2) -0.004(2) C121 0.038(4) 0.068(5) 0.054(5) -0.029(4) -0.006(3) -0.001(3) C122 0.030(3) 0.045(4) 0.040(4) -0.004(3) -0.002(3) 0.010(3) O13 0.026(2) 0.038(2) 0.035(2) -0.0109(18) -0.0088(17) 0.0044(17) C13 0.024(3) 0.039(3) 0.056(4) -0.016(3) -0.010(3) 0.002(2) C131 0.036(4) 0.063(5) 0.046(4) -0.012(3) -0.006(3) -0.015(3) C132 0.046(4) 0.053(4) 0.052(5) -0.006(3) -0.026(3) 0.005(3) P2 0.0270(7) 0.0252(7) 0.0277(8) -0.0008(6) -0.0076(6) -0.0020(5) O21 0.038(2) 0.028(2) 0.044(3) -0.0013(18) -0.0097(19) -0.0054(18) C21 0.042(4) 0.025(3) 0.074(5) -0.012(3) -0.018(3) 0.000(3) C211 0.060(5) 0.034(4) 0.101(7) 0.024(4) -0.030(5) -0.007(3) C212 0.072(6) 0.046(4) 0.108(8) -0.026(5) -0.033(5) -0.005(4) O22 0.054(3) 0.036(2) 0.035(3) -0.0055(19) -0.012(2) -0.004(2) C22 0.051(4) 0.047(4) 0.033(4) -0.012(3) 0.003(3) -0.005(3) C221 0.070(5) 0.080(6) 0.032(4) -0.001(4) -0.017(4) 0.014(4) C222 0.054(5) 0.140(10) 0.065(6) -0.044(6) -0.011(4) 0.030(6) O23 0.0223(19) 0.031(2) 0.043(2) -0.0051(18) -0.0101(17) -0.0002(16) C23 0.021(3) 0.037(3) 0.058(4) -0.002(3) -0.013(3) -0.004(2) C231 0.038(4) 0.092(7) 0.084(7) 0.036(5) 0.001(4) -0.016(4) C232 0.027(3) 0.050(4) 0.064(5) 0.004(3) -0.016(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.747(6) . ? Fe1 P1 2.1275(18) . ? Fe1 P2 2.1452(17) . ? Fe1 S1 2.1799(17) . ? Fe1 S2 2.2132(17) 2 ? S1 C1 1.736(5) . ? S2 C1 1.724(5) . ? S2 Fe1 2.2132(17) 2 ? C1 C1 1.365(10) 2 ? C2 O2 1.154(7) . ? P1 O12 1.585(4) . ? P1 O11 1.592(4) . ? P1 O13 1.599(4) . ? O11 C11 1.463(7) . ? C11 C111 1.495(11) . ? C11 C112 1.498(10) . ? O12 C12 1.462(7) . ? C12 C121 1.504(9) . ? C12 C122 1.516(8) . ? O13 C13 1.454(7) . ? C13 C132 1.503(10) . ? C13 C131 1.503(9) . ? P2 O23 1.581(4) . ? P2 O21 1.599(4) . ? P2 O22 1.611(5) . ? O21 C21 1.465(8) . ? C21 C211 1.502(11) . ? C21 C212 1.515(10) . ? O22 C22 1.455(8) . ? C22 C221 1.478(11) . ? C22 C222 1.486(11) . ? O23 C23 1.471(7) . ? C23 C232 1.502(9) . ? C23 C231 1.517(11) . ? 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 C2 Fe1 P1 90.9(2) . . ? C2 Fe1 P2 93.5(2) . . ? P1 Fe1 P2 93.56(7) . . ? C2 Fe1 S1 86.3(2) . . ? P1 Fe1 S1 130.88(7) . . ? P2 Fe1 S1 135.56(7) . . ? C2 Fe1 S2 174.7(2) . 2 ? P1 Fe1 S2 90.37(6) . 2 ? P2 Fe1 S2 91.56(6) . 2 ? S1 Fe1 S2 88.97(6) . 2 ? C1 S1 Fe1 106.30(18) . . ? C1 S2 Fe1 105.28(19) . 2 ? C1 C1 S2 120.3(5) 2 . ? C1 C1 S1 119.1(5) 2 . ? S2 C1 S1 120.6(3) . . ? O2 C2 Fe1 175.9(5) . . ? O12 P1 O11 100.4(2) . . ? O12 P1 O13 98.2(2) . . ? O11 P1 O13 105.3(2) . . ? O12 P1 Fe1 123.76(16) . . ? O11 P1 Fe1 111.57(18) . . ? O13 P1 Fe1 115.06(17) . . ? C11 O11 P1 123.6(4) . . ? O11 C11 C111 108.8(6) . . ? O11 C11 C112 106.3(6) . . ? C111 C11 C112 113.7(6) . . ? C12 O12 P1 125.0(3) . . ? O12 C12 C121 107.1(5) . . ? O12 C12 C122 106.4(5) . . ? C121 C12 C122 112.5(5) . . ? C13 O13 P1 123.6(4) . . ? O13 C13 C132 108.4(6) . . ? O13 C13 C131 108.0(5) . . ? C132 C13 C131 113.4(6) . . ? O23 P2 O21 100.0(2) . . ? O23 P2 O22 106.3(2) . . ? O21 P2 O22 98.3(2) . . ? O23 P2 Fe1 114.39(16) . . ? O21 P2 Fe1 120.55(17) . . ? O22 P2 Fe1 114.92(19) . . ? C21 O21 P2 123.6(4) . . ? O21 C21 C211 106.8(7) . . ? O21 C21 C212 108.3(6) . . ? C211 C21 C212 113.1(6) . . ? C22 O22 P2 125.6(4) . . ? O22 C22 C221 106.8(6) . . ? O22 C22 C222 108.8(7) . . ? C221 C22 C222 112.7(7) . . ? C23 O23 P2 123.1(4) . . ? O23 C23 C232 107.0(5) . . ? O23 C23 C231 106.6(6) . . ? C232 C23 C231 111.9(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 S1 C1 C1 S2 0.7(9) . . 2 2 ? S1 C1 C1 S1 180.0 . . 2 2 ? S2 C1 C1 S2 180.0 . . 2 2 ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 1.025 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.121 data_compound2a _database_code_CSD 194365 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H60 Fe2 O14 P4 S4' _chemical_formula_sum 'C76 H60 Fe2 O14 P4 S4' _chemical_formula_weight 1561.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.609(6) _cell_length_b 11.223(6) _cell_length_c 16.205(9) _cell_angle_alpha 91.665(7) _cell_angle_beta 92.351(8) _cell_angle_gamma 113.701(7) _cell_volume 1763.1(17) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 3849 _cell_measurement_theta_min 2.386 _cell_measurement_theta_max 23.839 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5076 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Bruker 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22761 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.44 _reflns_number_total 7083 _reflns_number_gt 3923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL 1994' _computing_structure_solution ; SHELXS-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ; _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) & TITAN2000 (Hunter & Simpson 1999) ; _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Molecules of the compound lie on a centre of symmetry, located at the midpoint of the C1-C1* bond of the C~2~S~4~ unit; refinement therefore involved only one half of the molecular unit. A difference map following the location of all non-hydrogen atoms revealed several high peaks consistent with positional disorder of the C41-C46 phenyl ring. This was resolved by refining two unique positions for the atoms C42, C43, C45 and C46 with occupancy factors f and f' refined such that f' = 1-f. The final value of f refined to 0.524(5). ; _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^)+(0.0575P)^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_number_reflns 7083 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 Fe1 Fe 0.17165(6) 0.18242(5) 0.14787(3) 0.02653(17) Uani 1 1 d . . . S1 S 0.04750(11) 0.19890(9) 0.03859(6) 0.0286(3) Uani 1 1 d . . . S2 S -0.13087(11) 0.01618(9) -0.10128(6) 0.0291(3) Uani 1 1 d . . . C1 C -0.0195(4) 0.0481(3) -0.0141(2) 0.0248(9) Uani 1 1 d . . . C2 C 0.2497(4) 0.3549(4) 0.1560(2) 0.0342(10) Uani 1 1 d . . . O2 O 0.3045(3) 0.4668(3) 0.15911(18) 0.0461(8) Uani 1 1 d . . . P1 P 0.04043(11) 0.16075(10) 0.24745(6) 0.0298(3) Uani 1 1 d . . . O11 O 0.1173(3) 0.2055(3) 0.33807(15) 0.0379(7) Uani 1 1 d . B . C11 C 0.0564(5) 0.1940(4) 0.4155(2) 0.0327(10) Uani 1 1 d . . . C14 C -0.0417(6) 0.1759(6) 0.5727(3) 0.0616(15) Uani 1 1 d . . . H14 H -0.0740 0.1757 0.6265 0.074 Uiso 1 1 calc R A 1 C12 C -0.0529(8) 0.2151(7) 0.4281(4) 0.032(2) Uani 0.524(5) 1 d P B 1 H12 H -0.0989 0.2401 0.3848 0.039 Uiso 0.524(5) 1 calc PR B 1 C13 C -0.1007(9) 0.1995(9) 0.5083(5) 0.036(2) Uani 0.524(5) 1 d P B 1 H13 H -0.1855 0.2074 0.5157 0.043 Uiso 0.524(5) 1 calc PR B 1 C15 C 0.0887(9) 0.1472(8) 0.5552(5) 0.045(2) Uani 0.524(5) 1 d P B 1 H15 H 0.1321 0.1170 0.5972 0.054 Uiso 0.524(5) 1 calc PR B 1 C16 C 0.1384(8) 0.1673(7) 0.4764(4) 0.034(2) Uani 0.524(5) 1 d P B 1 H16 H 0.2235 0.1632 0.4644 0.040 Uiso 0.524(5) 1 calc PR B 1 C12A C 0.1136(10) 0.2876(9) 0.4741(6) 0.043(3) Uani 0.476(5) 1 d P B 2 H12A H 0.1946 0.3596 0.4610 0.051 Uiso 0.476(5) 1 calc PR B 2 C13A C 0.0668(11) 0.2911(9) 0.5532(6) 0.051(3) Uani 0.476(5) 1 d P B 2 H13A H 0.1054 0.3653 0.5904 0.061 Uiso 0.476(5) 1 calc PR B 2 C15A C -0.1201(11) 0.0896(13) 0.5198(6) 0.052(3) Uani 0.476(5) 1 d P B 2 H15A H -0.2074 0.0279 0.5341 0.062 Uiso 0.476(5) 1 calc PR B 2 C16A C -0.0749(10) 0.0872(10) 0.4397(5) 0.045(3) Uani 0.476(5) 1 d P B 2 H16A H -0.1273 0.0182 0.4008 0.054 Uiso 0.476(5) 1 calc PR B 2 O12 O -0.0663(3) 0.2324(3) 0.24254(16) 0.0389(7) Uani 1 1 d . . . C21 C -0.0210(5) 0.3657(4) 0.2282(3) 0.0379(11) Uani 1 1 d . . . C22 C -0.0707(5) 0.3997(5) 0.1564(3) 0.0453(12) Uani 1 1 d . . . H22 H -0.1297 0.3349 0.1171 0.054 Uiso 1 1 calc R . . C23 C -0.0326(5) 0.5292(5) 0.1437(3) 0.0548(14) Uani 1 1 d . . . H23 H -0.0655 0.5543 0.0946 0.066 Uiso 1 1 calc R . . C24 C 0.0532(5) 0.6248(5) 0.2011(3) 0.0560(14) Uani 1 1 d . . . H24 H 0.0776 0.7143 0.1915 0.067 Uiso 1 1 calc R . . C25 C 0.1029(6) 0.5892(5) 0.2724(3) 0.0581(14) Uani 1 1 d . . . H25 H 0.1631 0.6542 0.3112 0.070 Uiso 1 1 calc R . . C26 C 0.0650(5) 0.4600(4) 0.2868(3) 0.0498(13) Uani 1 1 d . . . H26 H 0.0970 0.4348 0.3361 0.060 Uiso 1 1 calc R . . O31 O -0.0687(3) 0.0191(3) 0.26801(15) 0.0343(7) Uani 1 1 d . . . C31 C -0.1585(4) -0.0792(4) 0.2114(2) 0.0332(10) Uani 1 1 d . . . C32 C -0.2299(4) -0.0543(5) 0.1467(3) 0.0419(11) Uani 1 1 d . . . H32 H -0.2176 0.0326 0.1367 0.050 Uiso 1 1 calc R . . C33 C -0.3205(4) -0.1575(5) 0.0959(3) 0.0477(12) Uani 1 1 d . . . H33 H -0.3697 -0.1409 0.0505 0.057 Uiso 1 1 calc R . . C34 C -0.3395(5) -0.2831(5) 0.1107(3) 0.0512(13) Uani 1 1 d . . . H34 H -0.4022 -0.3537 0.0762 0.061 Uiso 1 1 calc R . . C35 C -0.2662(6) -0.3052(5) 0.1763(3) 0.0674(17) Uani 1 1 d . . . H35 H -0.2791 -0.3921 0.1869 0.081 Uiso 1 1 calc R . . C36 C -0.1740(5) -0.2034(5) 0.2274(3) 0.0523(14) Uani 1 1 d . . . H36 H -0.1230 -0.2194 0.2721 0.063 Uiso 1 1 calc R . . P2 P 0.34335(11) 0.17966(10) 0.22427(7) 0.0307(3) Uani 1 1 d . . . O22 O 0.4696(3) 0.1610(3) 0.18131(17) 0.0405(7) Uani 1 1 d . . . C51 C 0.5387(4) 0.2168(4) 0.1119(2) 0.0315(10) Uani 1 1 d . . . C56 C 0.5876(4) 0.1401(4) 0.0658(3) 0.0353(10) Uani 1 1 d . . . H56 H 0.5687 0.0533 0.0803 0.042 Uiso 1 1 calc R . . C55 C 0.6649(4) 0.1917(4) -0.0019(3) 0.0403(11) Uani 1 1 d . . . H55 H 0.6992 0.1396 -0.0333 0.048 Uiso 1 1 calc R . . C54 C 0.6923(4) 0.3169(4) -0.0240(2) 0.0389(11) Uani 1 1 d . . . H54 H 0.7445 0.3512 -0.0705 0.047 Uiso 1 1 calc R . . C53 C 0.6417(4) 0.3924(4) 0.0233(2) 0.0372(10) Uani 1 1 d . . . H53 H 0.6604 0.4790 0.0088 0.045 Uiso 1 1 calc R . . C52 C 0.5647(4) 0.3427(4) 0.0912(2) 0.0317(10) Uani 1 1 d . . . H52 H 0.5304 0.3946 0.1229 0.038 Uiso 1 1 calc R . . O23 O 0.4193(3) 0.3114(3) 0.28084(17) 0.0454(8) Uani 1 1 d . . . C61 C 0.5225(5) 0.3393(4) 0.3446(3) 0.0414(11) Uani 1 1 d . . . C62 C 0.6501(7) 0.3599(13) 0.3279(4) 0.244(7) Uani 1 1 d . . . H62 H 0.6730 0.3508 0.2727 0.293 Uiso 1 1 calc R . . C63 C 0.7487(9) 0.3946(18) 0.3914(6) 0.386(13) Uani 1 1 d . . . H63 H 0.8416 0.4148 0.3790 0.464 Uiso 1 1 calc R . . C64 C 0.7186(9) 0.4013(11) 0.4718(5) 0.200(6) Uani 1 1 d . . . H64 H 0.7885 0.4229 0.5151 0.240 Uiso 1 1 calc R . . C65 C 0.5925(6) 0.3776(5) 0.4880(3) 0.0585(15) Uani 1 1 d . . . H65 H 0.5682 0.3802 0.5436 0.070 Uiso 1 1 calc R . . C66 C 0.4931(5) 0.3483(4) 0.4233(3) 0.0493(13) Uani 1 1 d . . . H66 H 0.4015 0.3343 0.4354 0.059 Uiso 1 1 calc R . . O21 O 0.3122(3) 0.0666(3) 0.28778(16) 0.0351(7) Uani 1 1 d . . . C41 C 0.3912(4) -0.0077(4) 0.3038(2) 0.0314(10) Uani 1 1 d . . . C42 C 0.3813(6) -0.1062(5) 0.2508(3) 0.0583(14) Uani 1 1 d . . . H42 H 0.3250 -0.1229 0.2011 0.070 Uiso 1 1 calc R . . C43 C 0.4517(7) -0.1824(5) 0.2679(4) 0.0730(18) Uani 1 1 d . . . H43 H 0.4402 -0.2545 0.2316 0.088 Uiso 1 1 calc R . . C44 C 0.5372(6) -0.1549(6) 0.3362(5) 0.079(2) Uani 1 1 d . . . H44 H 0.5912 -0.2036 0.3461 0.095 Uiso 1 1 calc R . . C45 C 0.5460(9) -0.0579(7) 0.3909(5) 0.155(4) Uani 1 1 d . . . H45 H 0.6019 -0.0417 0.4407 0.186 Uiso 1 1 calc R . . C46 C 0.4721(8) 0.0187(6) 0.3735(4) 0.114(3) Uani 1 1 d . . . H46 H 0.4793 0.0885 0.4107 0.137 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 Fe1 0.0341(4) 0.0262(3) 0.0227(3) -0.0026(2) -0.0015(3) 0.0162(3) S1 0.0414(7) 0.0276(6) 0.0221(5) -0.0030(4) -0.0022(5) 0.0200(5) S2 0.0395(7) 0.0304(6) 0.0231(5) -0.0031(4) -0.0030(5) 0.0208(5) C1 0.028(2) 0.033(2) 0.019(2) 0.0010(17) 0.0022(17) 0.0169(19) C2 0.040(3) 0.045(3) 0.024(2) 0.001(2) 0.000(2) 0.024(2) O2 0.060(2) 0.0252(18) 0.051(2) 0.0031(15) -0.0029(16) 0.0149(16) P1 0.0376(7) 0.0349(6) 0.0222(6) -0.0065(5) -0.0032(5) 0.0211(6) O11 0.0444(19) 0.059(2) 0.0206(15) -0.0117(13) -0.0068(13) 0.0336(16) C11 0.051(3) 0.031(2) 0.020(2) -0.0040(18) -0.004(2) 0.022(2) C14 0.056(4) 0.084(4) 0.024(3) 0.007(3) 0.004(3) 0.006(3) C12 0.041(5) 0.039(5) 0.025(4) 0.004(4) 0.000(4) 0.024(4) C13 0.040(6) 0.043(6) 0.031(5) 0.002(4) 0.011(4) 0.022(5) C15 0.049(6) 0.061(6) 0.028(5) 0.014(4) 0.000(4) 0.024(5) C16 0.037(5) 0.041(5) 0.023(4) 0.003(4) 0.003(4) 0.015(4) C12A 0.041(6) 0.035(6) 0.041(6) -0.002(5) 0.002(5) 0.005(5) C13A 0.075(8) 0.040(6) 0.032(6) -0.018(5) -0.004(5) 0.020(6) C15A 0.037(6) 0.090(10) 0.026(6) -0.010(6) 0.004(5) 0.025(6) C16A 0.042(6) 0.063(7) 0.028(5) -0.015(5) -0.009(4) 0.020(6) O12 0.0464(19) 0.0489(19) 0.0340(17) -0.0109(14) -0.0078(14) 0.0341(16) C21 0.045(3) 0.049(3) 0.034(3) -0.006(2) 0.002(2) 0.035(2) C22 0.039(3) 0.068(4) 0.040(3) 0.000(2) 0.002(2) 0.033(3) C23 0.054(3) 0.078(4) 0.051(3) 0.020(3) 0.006(3) 0.045(3) C24 0.070(4) 0.054(3) 0.065(4) 0.008(3) 0.013(3) 0.046(3) C25 0.083(4) 0.055(3) 0.050(3) -0.009(3) 0.001(3) 0.044(3) C26 0.084(4) 0.046(3) 0.034(3) -0.006(2) -0.002(3) 0.042(3) O31 0.0365(17) 0.0432(18) 0.0229(15) 0.0010(13) 0.0008(13) 0.0159(15) C31 0.031(3) 0.045(3) 0.026(2) -0.002(2) 0.0033(19) 0.018(2) C32 0.031(3) 0.050(3) 0.040(3) 0.013(2) -0.001(2) 0.010(2) C33 0.029(3) 0.070(4) 0.038(3) 0.010(3) -0.002(2) 0.013(3) C34 0.051(3) 0.061(4) 0.046(3) -0.023(3) -0.013(2) 0.030(3) C35 0.083(4) 0.053(3) 0.077(4) -0.027(3) -0.043(3) 0.045(3) C36 0.074(4) 0.053(3) 0.045(3) -0.014(2) -0.025(3) 0.045(3) P2 0.0313(7) 0.0298(6) 0.0307(6) 0.0032(5) -0.0004(5) 0.0121(5) O22 0.0307(17) 0.055(2) 0.0416(18) 0.0221(15) 0.0154(14) 0.0201(15) C51 0.020(2) 0.036(3) 0.032(2) 0.0097(19) -0.0033(19) 0.004(2) C56 0.031(3) 0.035(3) 0.041(3) 0.006(2) -0.002(2) 0.015(2) C55 0.034(3) 0.055(3) 0.036(3) 0.000(2) 0.000(2) 0.024(2) C54 0.032(3) 0.057(3) 0.024(2) 0.010(2) 0.003(2) 0.013(2) C53 0.032(3) 0.036(3) 0.036(3) 0.008(2) -0.001(2) 0.007(2) C52 0.026(2) 0.039(3) 0.028(2) 0.0039(19) 0.0019(19) 0.010(2) O23 0.052(2) 0.0325(17) 0.0427(18) -0.0049(14) -0.0190(15) 0.0105(15) C61 0.033(3) 0.053(3) 0.032(3) -0.004(2) -0.006(2) 0.012(2) C62 0.037(4) 0.55(2) 0.068(5) -0.135(8) -0.008(4) 0.048(8) C63 0.068(6) 0.92(3) 0.143(9) -0.290(15) -0.064(6) 0.197(12) C64 0.115(7) 0.439(17) 0.102(6) -0.160(8) -0.078(5) 0.190(9) C65 0.090(4) 0.052(3) 0.032(3) -0.005(2) -0.004(3) 0.028(3) C66 0.036(3) 0.054(3) 0.047(3) -0.017(2) 0.006(2) 0.008(2) O21 0.0329(17) 0.0424(18) 0.0370(17) 0.0130(13) 0.0081(13) 0.0213(14) C41 0.032(2) 0.030(2) 0.033(2) 0.0076(19) 0.003(2) 0.013(2) C42 0.094(4) 0.052(3) 0.040(3) 0.000(2) -0.007(3) 0.043(3) C43 0.115(5) 0.071(4) 0.066(4) 0.028(3) 0.038(4) 0.067(4) C44 0.040(4) 0.061(4) 0.146(6) 0.045(4) 0.019(4) 0.029(3) C45 0.193(9) 0.066(5) 0.207(9) -0.036(5) -0.161(7) 0.071(5) C46 0.198(8) 0.066(4) 0.095(5) -0.038(4) -0.101(5) 0.083(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 Fe1 C2 1.771(5) . ? Fe1 P1 2.1298(15) . ? Fe1 P2 2.1714(15) . ? Fe1 S2 2.1967(15) 2 ? Fe1 S1 2.2201(14) . ? S1 C1 1.732(4) . ? S2 C1 1.736(4) . ? S2 Fe1 2.1967(15) 2 ? C1 C1 1.384(7) 2 ? C2 O2 1.152(5) . ? P1 O31 1.601(3) . ? P1 O11 1.613(3) . ? P1 O12 1.631(3) . ? O11 C11 1.421(4) . ? C11 C12 1.296(8) . ? C11 C12A 1.324(9) . ? C11 C16 1.406(8) . ? C11 C16A 1.504(11) . ? C14 C15A 1.268(11) . ? C14 C13 1.283(9) . ? C14 C13A 1.398(11) . ? C14 C15 1.575(10) . ? C12 C13 1.404(10) . ? C15 C16 1.392(10) . ? C12A C13A 1.399(12) . ? C15A C16A 1.406(12) . ? O12 C21 1.405(5) . ? C21 C22 1.384(6) . ? C21 C26 1.395(6) . ? C22 C23 1.367(6) . ? C23 C24 1.391(7) . ? C24 C25 1.385(6) . ? C25 C26 1.371(6) . ? O31 C31 1.412(5) . ? C31 C32 1.369(5) . ? C31 C36 1.370(6) . ? C32 C33 1.388(6) . ? C33 C34 1.371(6) . ? C34 C35 1.379(6) . ? C35 C36 1.388(6) . ? P2 O21 1.596(3) . ? P2 O23 1.606(3) . ? P2 O22 1.617(3) . ? O22 C51 1.390(4) . ? C51 C52 1.381(5) . ? C51 C56 1.387(5) . ? C56 C55 1.393(5) . ? C55 C54 1.377(6) . ? C54 C53 1.397(5) . ? C53 C52 1.391(5) . ? O23 C61 1.406(5) . ? C61 C62 1.320(7) . ? C61 C66 1.337(6) . ? C62 C63 1.366(10) . ? C63 C64 1.362(11) . ? C64 C65 1.294(8) . ? C65 C66 1.389(6) . ? O21 C41 1.421(4) . ? C41 C46 1.341(6) . ? C41 C42 1.347(6) . ? C42 C43 1.369(6) . ? C43 C44 1.349(8) . ? C44 C45 1.354(9) . ? C45 C46 1.404(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 P1 95.86(13) . . ? C2 Fe1 P2 88.77(13) . . ? P1 Fe1 P2 95.08(6) . . ? C2 Fe1 S2 158.26(13) . 2 ? P1 Fe1 S2 105.86(5) . 2 ? P2 Fe1 S2 88.43(5) . 2 ? C2 Fe1 S1 87.60(13) . . ? P1 Fe1 S1 103.82(6) . . ? P2 Fe1 S1 161.02(5) . . ? S2 Fe1 S1 88.07(5) 2 . ? C1 S1 Fe1 106.80(12) . . ? C1 S2 Fe1 106.66(12) . 2 ? C1 C1 S1 118.4(4) 2 . ? C1 C1 S2 119.8(4) 2 . ? S1 C1 S2 121.8(2) . . ? O2 C2 Fe1 177.2(4) . . ? O31 P1 O11 98.38(15) . . ? O31 P1 O12 97.54(16) . . ? O11 P1 O12 103.95(14) . . ? O31 P1 Fe1 120.03(10) . . ? O11 P1 Fe1 115.68(12) . . ? O12 P1 Fe1 117.85(11) . . ? C11 O11 P1 127.9(3) . . ? C12 C11 C12A 83.4(6) . . ? C12 C11 C16 125.8(5) . . ? C12A C11 C16 65.4(5) . . ? C12 C11 O11 124.2(5) . . ? C12A C11 O11 119.5(5) . . ? C16 C11 O11 109.8(4) . . ? C12 C11 C16A 58.4(5) . . ? C12A C11 C16A 113.3(6) . . ? C16 C11 C16A 93.7(5) . . ? O11 C11 C16A 127.1(4) . . ? C15A C14 C13 55.5(6) . . ? C15A C14 C13A 124.6(7) . . ? C13 C14 C13A 82.4(6) . . ? C15A C14 C15 94.1(7) . . ? C13 C14 C15 114.6(6) . . ? C13A C14 C15 70.5(6) . . ? C11 C12 C13 117.4(7) . . ? C14 C13 C12 126.7(8) . . ? C16 C15 C14 118.0(7) . . ? C15 C16 C11 116.6(7) . . ? C11 C12A C13A 126.5(8) . . ? C14 C13A C12A 114.2(7) . . ? C14 C15A C16A 118.6(9) . . ? C15A C16A C11 119.9(8) . . ? C21 O12 P1 121.6(3) . . ? C22 C21 C26 121.4(4) . . ? C22 C21 O12 117.7(4) . . ? C26 C21 O12 120.8(4) . . ? C23 C22 C21 118.2(5) . . ? C22 C23 C24 121.3(5) . . ? C25 C24 C23 119.8(5) . . ? C26 C25 C24 119.9(5) . . ? C25 C26 C21 119.4(4) . . ? C31 O31 P1 127.2(2) . . ? C32 C31 C36 121.8(4) . . ? C32 C31 O31 122.9(4) . . ? C36 C31 O31 115.2(4) . . ? C31 C32 C33 119.2(4) . . ? C34 C33 C32 120.6(4) . . ? C33 C34 C35 118.9(4) . . ? C34 C35 C36 121.5(5) . . ? C31 C36 C35 118.0(4) . . ? O21 P2 O23 104.09(15) . . ? O21 P2 O22 97.18(14) . . ? O23 P2 O22 103.12(16) . . ? O21 P2 Fe1 117.95(11) . . ? O23 P2 Fe1 112.28(12) . . ? O22 P2 Fe1 119.80(12) . . ? C51 O22 P2 130.0(2) . . ? C52 C51 C56 120.9(4) . . ? C52 C51 O22 123.3(4) . . ? C56 C51 O22 115.7(4) . . ? C51 C56 C55 119.2(4) . . ? C54 C55 C56 121.1(4) . . ? C55 C54 C53 118.7(4) . . ? C52 C53 C54 121.1(4) . . ? C51 C52 C53 119.0(4) . . ? C61 O23 P2 128.7(3) . . ? C62 C61 C66 118.9(5) . . ? C62 C61 O23 120.9(5) . . ? C66 C61 O23 120.2(4) . . ? C61 C62 C63 118.8(6) . . ? C64 C63 C62 122.4(7) . . ? C65 C64 C63 118.4(6) . . ? C64 C65 C66 119.4(5) . . ? C61 C66 C65 122.0(5) . . ? C41 O21 P2 127.1(2) . . ? C46 C41 C42 120.4(4) . . ? C46 C41 O21 119.2(4) . . ? C42 C41 O21 120.3(4) . . ? C41 C42 C43 120.7(5) . . ? C44 C43 C42 119.8(6) . . ? C43 C44 C45 120.0(5) . . ? C44 C45 C46 119.6(6) . . ? C41 C46 C45 119.2(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 S1 C1 C1 S2 1.1(6) . . 2 2 ? S1 C1 C1 S1 180.0 . . 2 2 ? S2 C1 C1 S2 180.0 2 . 2 . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.950 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.076