# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address T.Rauchfuss ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'De Gioia, Luca' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; A.K.Justice '' G.Zampella '' _publ_contact_author_name 'T. Rauchfuss' _publ_contact_author_address ; Department of Chemistry University of Illinois 505 S Mathews Street Urbana IL 61801 UNITED STATES OF AMERICA ; _publ_contact_author_email RAUCHFUZ@UIUC.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Lewis vs Bronsted-Basicities of Diiron Dithiolates: Spectroscopic Detection of the Rotated Structure and Remarkable Effects of Ethane- vs. Propanedithiolate ; _publ_contact_author ; Scott R. Wilson University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_fax '1 217 244 8068' _publ_contact_author_phone '1 217 244 1708' _publ_contact_letter ; Please consider this CIF submission for publication as a structural paper in Acta Crystallographica E. ; # end Validation Reply Form _publ_requested_category FM _publ_requested_coeditor_name ? data_gs72has5 _database_code_depnum_ccdc_archive 'CCDC 634107' _audit_creation_method SHELXL-97 _audit_update_record ; 2006-08-23 text and data added, akj ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 Fe2 O2 P4 S2' _chemical_formula_sum 'C56 H48 Fe2 O2 P4 S2' _chemical_formula_structural ? _chemical_formula_weight 1052.64 _chemical_absolute_configuration . _chemical_formula_analytical ? _chemical_compound_source ? 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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 10.9417(7) _cell_length_b 17.3546(10) _cell_length_c 26.1713(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.901(2) _cell_angle_gamma 90.00 _cell_volume 4922.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5031 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.9 _exptl_crystal_description tabular _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_crystal_id gs72has5 _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (0 -1 -1) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7444 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details 'SHELXTL/XPREP (Bruker, 2001)' _exptl_special_details ; All crystals examined exhibited non-merohedral twinning (rotational displacement roughly along the body diagonal). Two distinct cells were identified using APEX2 (Bruker, 2004) and Cell_Now (Sheldrick, 2004). Six frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2001) then corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001) before using SAINT/TWINABS (Bruker, 2001) to sort, merge, and scale the combined data. Combined unit cell parameters were determined from both components using SAINT (Bruker, 2001). The twin law by rows was (1 .02 .02), (-.06 1 0), (-.10 0 .99). Non-overlapping reflections from the primary orientation were used for phasing. Combined data with complete or no overlap were used for refinement. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id gs72has5 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21096 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.08 _reflns_number_total 20391 _reflns_number_gt 11987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V1.0-27 (Bruker, 2004)' _computing_cell_refinement 'SAINT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL V6.12 (Bruker, 2001)' _computing_publication_material 'XCIF (Bruker, 2001)' _refine_special_details ; Structure was phased by direct methods. Systematic conditions suggested the unambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. Separate batch scale factors were refined for individual and overlapping components. The highest peaks in the final difference Fourier map were in the vicinity of atoms Fe1, C56, and C39; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed minimal dependence on amplitude and resolution. ; _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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20391 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 0.05665(2) 0.720234(14) 0.116935(10) 0.01930(7) Uani 1 1 d . . . Fe2 Fe 0.06990(2) 0.858038(14) 0.152996(10) 0.01935(7) Uani 1 1 d . . . S1 S 0.22116(4) 0.79918(3) 0.117276(17) 0.02170(12) Uani 1 1 d . . . S2 S -0.03368(4) 0.82354(3) 0.075836(17) 0.02082(11) Uani 1 1 d . . . P1 P 0.08248(5) 0.63413(3) 0.059082(18) 0.02268(12) Uani 1 1 d . . . P2 P -0.12311(5) 0.66656(3) 0.123170(19) 0.02277(13) Uani 1 1 d . . . P3 P 0.09132(5) 0.98216(3) 0.146136(18) 0.02217(12) Uani 1 1 d . . . P4 P 0.17896(5) 0.86820(3) 0.229652(18) 0.02381(13) Uani 1 1 d . . . O1 O -0.15534(13) 0.87399(9) 0.19899(5) 0.0511(4) Uani 1 1 d . . . O2 O 0.17991(13) 0.62426(8) 0.19922(5) 0.0444(4) Uani 1 1 d . . . C1 C -0.06528(18) 0.86581(11) 0.18049(7) 0.0275(5) Uani 1 1 d . . . C2 C 0.12947(17) 0.66390(10) 0.16688(7) 0.0247(5) Uani 1 1 d . . . C3 C 0.20345(16) 0.83459(10) 0.05077(6) 0.0254(5) Uani 1 1 d . . . H3A H 0.2574 0.8800 0.0488 0.030 Uiso 1 1 calc R . . H3B H 0.2302 0.7941 0.0281 0.030 Uiso 1 1 calc R . . C4 C 0.07055(16) 0.85684(10) 0.03158(6) 0.0239(5) Uani 1 1 d . . . H4A H 0.0454 0.8340 -0.0029 0.029 Uiso 1 1 calc R . . H4B H 0.0644 0.9136 0.0281 0.029 Uiso 1 1 calc R . . C5 C -0.03874(17) 0.56187(10) 0.05945(7) 0.0272(5) Uani 1 1 d . . . H5 H -0.0372 0.5153 0.0405 0.033 Uiso 1 1 calc R . . C6 C -0.12839(17) 0.57658(10) 0.08687(7) 0.0272(5) Uani 1 1 d . . . H6 H -0.1943 0.5411 0.0877 0.033 Uiso 1 1 calc R . . C7 C 0.05958(17) 0.65347(10) -0.01078(7) 0.0242(5) Uani 1 1 d . . . C8 C -0.04684(17) 0.69380(10) -0.03040(7) 0.0292(5) Uani 1 1 d . . . H8 H -0.0964 0.7159 -0.0072 0.035 Uiso 1 1 calc R . . C9 C -0.08177(19) 0.70226(11) -0.08298(8) 0.0376(6) Uani 1 1 d . . . H9 H -0.1552 0.7294 -0.0955 0.045 Uiso 1 1 calc R . . C10 C -0.0106(2) 0.67149(12) -0.11678(8) 0.0411(6) Uani 1 1 d . . . H10 H -0.0355 0.6763 -0.1529 0.049 Uiso 1 1 calc R . . C11 C 0.0971(2) 0.63357(11) -0.09874(8) 0.0420(6) Uani 1 1 d . . . H11 H 0.1474 0.6134 -0.1224 0.050 Uiso 1 1 calc R . . C12 C 0.13269(19) 0.62469(10) -0.04580(7) 0.0317(5) Uani 1 1 d . . . H12 H 0.2075 0.5988 -0.0336 0.038 Uiso 1 1 calc R . . C13 C 0.22300(17) 0.57622(11) 0.06723(7) 0.0264(5) Uani 1 1 d . . . C14 C 0.22261(19) 0.49735(12) 0.07537(8) 0.0436(6) Uani 1 1 d . . . H14 H 0.1468 0.4715 0.0770 0.052 Uiso 1 1 calc R . . C15 C 0.3316(2) 0.45603(13) 0.08108(9) 0.0615(8) Uani 1 1 d . . . H15 H 0.3301 0.4021 0.0872 0.074 Uiso 1 1 calc R . . C16 C 0.4413(2) 0.49196(14) 0.07807(10) 0.0637(8) Uani 1 1 d . . . H16 H 0.5156 0.4630 0.0812 0.076 Uiso 1 1 calc R . . C17 C 0.4434(2) 0.57004(14) 0.07057(10) 0.0682(8) Uani 1 1 d . . . H17 H 0.5195 0.5955 0.0686 0.082 Uiso 1 1 calc R . . C18 C 0.3352(2) 0.61151(12) 0.06582(9) 0.0512(7) Uani 1 1 d . . . H18 H 0.3380 0.6658 0.0615 0.061 Uiso 1 1 calc R . . C19 C -0.26555(17) 0.71195(11) 0.09242(8) 0.0277(5) Uani 1 1 d . . . C20 C -0.30977(18) 0.69964(12) 0.04076(8) 0.0416(6) Uani 1 1 d . . . H20 H -0.2690 0.6641 0.0212 0.050 Uiso 1 1 calc R . . C21 C -0.4130(2) 0.73890(15) 0.01746(9) 0.0594(8) Uani 1 1 d . . . H21 H -0.4423 0.7303 -0.0180 0.071 Uiso 1 1 calc R . . C22 C -0.4730(2) 0.78988(15) 0.04504(11) 0.0657(9) Uani 1 1 d . . . H22 H -0.5430 0.8170 0.0287 0.079 Uiso 1 1 calc R . . C23 C -0.4321(2) 0.80201(13) 0.09657(11) 0.0571(7) Uani 1 1 d . . . H23 H -0.4749 0.8367 0.1159 0.069 Uiso 1 1 calc R . . C24 C -0.32826(18) 0.76345(11) 0.12013(8) 0.0386(6) Uani 1 1 d . . . H24 H -0.2997 0.7724 0.1556 0.046 Uiso 1 1 calc R . . C25 C -0.17166(17) 0.63178(10) 0.18356(7) 0.0240(5) Uani 1 1 d . . . C26 C -0.27720(18) 0.58645(11) 0.18237(8) 0.0367(6) Uani 1 1 d . . . H26 H -0.3264 0.5765 0.1502 0.044 Uiso 1 1 calc R . . C27 C -0.31162(19) 0.55570(11) 0.22693(8) 0.0402(6) Uani 1 1 d . . . H27 H -0.3835 0.5246 0.2252 0.048 Uiso 1 1 calc R . . C28 C -0.2419(2) 0.57009(12) 0.27369(8) 0.0447(6) Uani 1 1 d . . . H28 H -0.2645 0.5485 0.3044 0.054 Uiso 1 1 calc R . . C29 C -0.1393(2) 0.61599(13) 0.27565(8) 0.0507(7) Uani 1 1 d . . . H29 H -0.0913 0.6264 0.3080 0.061 Uiso 1 1 calc R . . C30 C -0.10467(19) 0.64756(11) 0.23101(7) 0.0380(6) Uani 1 1 d . . . H30 H -0.0344 0.6802 0.2332 0.046 Uiso 1 1 calc R . . C31 C 0.13982(17) 1.02011(11) 0.21097(7) 0.0285(5) Uani 1 1 d . . . H31 H 0.1394 1.0738 0.2179 0.034 Uiso 1 1 calc R . . C32 C 0.17536(17) 0.96984(10) 0.24766(7) 0.0310(5) Uani 1 1 d . . . H32 H 0.1984 0.9858 0.2824 0.037 Uiso 1 1 calc R . . C33 C -0.04248(17) 1.04252(11) 0.12249(7) 0.0240(5) Uani 1 1 d . . . C34 C -0.14103(17) 1.00986(11) 0.09090(7) 0.0325(5) Uani 1 1 d . . . H34 H -0.1387 0.9567 0.0826 0.039 Uiso 1 1 calc R . . C35 C -0.24294(19) 1.05348(12) 0.07128(8) 0.0396(6) Uani 1 1 d . . . H35 H -0.3081 1.0305 0.0486 0.048 Uiso 1 1 calc R . . C36 C -0.24990(19) 1.12927(12) 0.08444(8) 0.0379(6) Uani 1 1 d . . . H36 H -0.3206 1.1588 0.0716 0.046 Uiso 1 1 calc R . . C37 C -0.1551(2) 1.16260(12) 0.11617(9) 0.0473(6) Uani 1 1 d . . . H37 H -0.1603 1.2152 0.1256 0.057 Uiso 1 1 calc R . . C38 C -0.05088(19) 1.11988(11) 0.13479(8) 0.0398(6) Uani 1 1 d . . . H38 H 0.0153 1.1440 0.1562 0.048 Uiso 1 1 calc R . . C39 C 0.21067(16) 1.02043(10) 0.11004(7) 0.0211(4) Uani 1 1 d . . . C40 C 0.18460(17) 1.06520(10) 0.06593(7) 0.0266(5) Uani 1 1 d . . . H40 H 0.1022 1.0814 0.0550 0.032 Uiso 1 1 calc R . . C41 C 0.27713(18) 1.08654(11) 0.03767(7) 0.0320(5) Uani 1 1 d . . . H41 H 0.2575 1.1169 0.0075 0.038 Uiso 1 1 calc R . . C42 C 0.39756(18) 1.06411(11) 0.05296(7) 0.0330(5) Uani 1 1 d . . . H42 H 0.4608 1.0786 0.0334 0.040 Uiso 1 1 calc R . . C43 C 0.42526(18) 1.02008(11) 0.09735(8) 0.0352(5) Uani 1 1 d . . . H43 H 0.5081 1.0049 0.1085 0.042 Uiso 1 1 calc R . . C44 C 0.33299(17) 0.99831(11) 0.12524(7) 0.0299(5) Uani 1 1 d . . . H44 H 0.3529 0.9677 0.1553 0.036 Uiso 1 1 calc R . . C45 C 0.12435(18) 0.82192(11) 0.28544(7) 0.0268(5) Uani 1 1 d . . . C46 C 0.17313(18) 0.75408(11) 0.30733(7) 0.0346(5) Uani 1 1 d . . . H46 H 0.2424 0.7315 0.2949 0.042 Uiso 1 1 calc R . . C47 C 0.1233(2) 0.71847(13) 0.34689(8) 0.0475(7) Uani 1 1 d . . . H47 H 0.1586 0.6720 0.3614 0.057 Uiso 1 1 calc R . . C48 C 0.0234(2) 0.74993(14) 0.36527(8) 0.0504(7) Uani 1 1 d . . . H48 H -0.0103 0.7256 0.3927 0.061 Uiso 1 1 calc R . . C49 C -0.0282(2) 0.81678(14) 0.34408(8) 0.0511(7) Uani 1 1 d . . . H49 H -0.0983 0.8383 0.3565 0.061 Uiso 1 1 calc R . . C50 C 0.0224(2) 0.85306(12) 0.30431(8) 0.0418(6) Uani 1 1 d . . . H50 H -0.0132 0.8995 0.2900 0.050 Uiso 1 1 calc R . . C51 C 0.34584(17) 0.84924(12) 0.23983(7) 0.0279(5) Uani 1 1 d . . . C52 C 0.39016(19) 0.77539(13) 0.23156(7) 0.0361(5) Uani 1 1 d . . . H52 H 0.3335 0.7352 0.2208 0.043 Uiso 1 1 calc R . . C53 C 0.5157(2) 0.76007(15) 0.23882(8) 0.0506(7) Uani 1 1 d . . . H53 H 0.5443 0.7092 0.2343 0.061 Uiso 1 1 calc R . . C54 C 0.5990(2) 0.81836(17) 0.25262(8) 0.0593(8) Uani 1 1 d . . . H54 H 0.6850 0.8078 0.2576 0.071 Uiso 1 1 calc R . . C55 C 0.5576(2) 0.89149(16) 0.25919(8) 0.0566(8) Uani 1 1 d . . . H55 H 0.6153 0.9320 0.2676 0.068 Uiso 1 1 calc R . . C56 C 0.4323(2) 0.90709(13) 0.25367(7) 0.0409(6) Uani 1 1 d . . . H56 H 0.4050 0.9579 0.2594 0.049 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 0.02189(16) 0.01690(16) 0.01871(15) 0.00072(12) 0.00138(12) -0.00099(12) Fe2 0.02168(16) 0.01734(16) 0.01902(15) -0.00025(12) 0.00272(12) -0.00217(12) S1 0.0211(3) 0.0234(3) 0.0204(3) 0.0018(2) 0.0024(2) -0.0012(2) S2 0.0217(3) 0.0191(3) 0.0210(3) 0.0009(2) 0.0008(2) -0.0004(2) P1 0.0263(3) 0.0186(3) 0.0232(3) -0.0009(2) 0.0039(2) -0.0014(2) P2 0.0245(3) 0.0210(3) 0.0228(3) -0.0004(2) 0.0034(2) -0.0025(2) P3 0.0247(3) 0.0184(3) 0.0233(3) 0.0004(2) 0.0030(2) -0.0014(2) P4 0.0296(3) 0.0211(3) 0.0200(3) 0.0012(2) 0.0009(2) -0.0035(2) O1 0.0348(10) 0.0684(12) 0.0542(10) -0.0155(9) 0.0210(8) -0.0085(9) O2 0.0532(11) 0.0382(10) 0.0383(9) 0.0154(8) -0.0064(8) 0.0073(8) C1 0.0292(13) 0.0263(12) 0.0264(12) -0.0040(10) 0.0018(10) -0.0065(10) C2 0.0243(12) 0.0232(12) 0.0271(12) -0.0014(10) 0.0052(9) -0.0057(9) C3 0.0266(12) 0.0270(12) 0.0235(11) 0.0020(9) 0.0072(9) -0.0039(9) C4 0.0299(12) 0.0218(11) 0.0201(11) 0.0027(9) 0.0034(9) -0.0017(9) C5 0.0375(13) 0.0190(12) 0.0254(12) -0.0036(9) 0.0059(10) -0.0049(10) C6 0.0306(13) 0.0219(12) 0.0298(12) -0.0042(9) 0.0069(10) -0.0089(10) C7 0.0320(13) 0.0168(11) 0.0243(11) -0.0039(9) 0.0055(9) -0.0064(9) C8 0.0318(13) 0.0307(13) 0.0255(12) -0.0024(10) 0.0048(10) -0.0052(10) C9 0.0430(15) 0.0370(14) 0.0304(13) 0.0020(11) -0.0034(11) -0.0052(11) C10 0.0663(18) 0.0335(14) 0.0222(12) -0.0015(11) 0.0020(12) -0.0111(12) C11 0.0699(18) 0.0298(14) 0.0313(14) -0.0047(11) 0.0245(12) -0.0023(13) C12 0.0436(14) 0.0199(12) 0.0338(13) 0.0013(10) 0.0125(11) -0.0007(10) C13 0.0315(13) 0.0223(12) 0.0251(11) -0.0024(9) 0.0028(9) 0.0022(10) C14 0.0337(14) 0.0283(14) 0.0662(17) 0.0012(12) -0.0022(12) 0.0010(11) C15 0.0522(18) 0.0281(15) 0.099(2) 0.0001(14) -0.0088(16) 0.0113(13) C16 0.0419(17) 0.0475(18) 0.100(2) 0.0099(16) 0.0017(15) 0.0211(14) C17 0.0291(16) 0.0551(19) 0.120(2) 0.0303(17) 0.0084(15) 0.0042(13) C18 0.0312(15) 0.0285(14) 0.092(2) 0.0142(13) 0.0021(14) 0.0004(11) C19 0.0203(12) 0.0270(13) 0.0360(13) 0.0054(10) 0.0048(10) -0.0072(10) C20 0.0259(13) 0.0610(17) 0.0379(14) 0.0113(12) 0.0040(11) -0.0070(11) C21 0.0283(15) 0.102(2) 0.0456(16) 0.0337(16) -0.0016(12) -0.0068(15) C22 0.0251(15) 0.087(2) 0.086(2) 0.0566(19) 0.0117(15) 0.0087(14) C23 0.0343(16) 0.0474(17) 0.093(2) 0.0218(16) 0.0222(15) 0.0099(12) C24 0.0293(14) 0.0354(14) 0.0523(15) 0.0028(12) 0.0094(11) -0.0013(11) C25 0.0279(12) 0.0194(11) 0.0256(11) -0.0009(9) 0.0071(9) -0.0011(9) C26 0.0365(14) 0.0413(14) 0.0324(13) -0.0004(11) 0.0050(11) -0.0123(11) C27 0.0432(15) 0.0342(14) 0.0468(15) 0.0001(12) 0.0185(12) -0.0157(11) C28 0.0614(17) 0.0443(16) 0.0331(14) 0.0011(12) 0.0236(12) -0.0093(13) C29 0.0640(18) 0.0655(18) 0.0229(13) -0.0028(12) 0.0065(12) -0.0242(14) C30 0.0429(14) 0.0433(15) 0.0294(13) -0.0052(11) 0.0109(11) -0.0184(11) C31 0.0382(13) 0.0182(12) 0.0296(12) -0.0045(10) 0.0063(10) -0.0048(10) C32 0.0445(14) 0.0260(13) 0.0216(11) -0.0055(10) 0.0013(10) -0.0086(10) C33 0.0234(12) 0.0216(12) 0.0284(12) 0.0035(9) 0.0083(9) 0.0034(9) C34 0.0337(13) 0.0285(13) 0.0342(13) -0.0057(10) 0.0009(10) 0.0078(10) C35 0.0328(14) 0.0459(15) 0.0386(14) -0.0041(12) -0.0009(11) 0.0129(11) C36 0.0320(14) 0.0376(15) 0.0464(15) 0.0115(12) 0.0134(11) 0.0158(11) C37 0.0430(16) 0.0201(13) 0.0811(19) 0.0037(12) 0.0161(14) 0.0083(11) C38 0.0307(14) 0.0238(13) 0.0643(16) -0.0019(12) 0.0037(12) -0.0007(10) C39 0.0222(11) 0.0153(11) 0.0250(11) 0.0000(9) 0.0011(9) -0.0030(9) C40 0.0211(12) 0.0272(12) 0.0305(12) 0.0039(10) 0.0007(9) 0.0007(9) C41 0.0376(14) 0.0330(13) 0.0251(12) 0.0050(10) 0.0029(10) -0.0051(11) C42 0.0316(13) 0.0360(14) 0.0331(13) -0.0006(11) 0.0101(10) -0.0072(10) C43 0.0217(13) 0.0372(14) 0.0464(14) 0.0061(11) 0.0033(10) 0.0007(10) C44 0.0278(13) 0.0275(13) 0.0338(12) 0.0094(10) 0.0019(10) -0.0018(10) C45 0.0335(13) 0.0254(12) 0.0209(11) -0.0008(9) 0.0010(9) -0.0068(10) C46 0.0331(13) 0.0386(14) 0.0310(13) 0.0110(11) 0.0003(10) -0.0056(11) C47 0.0526(17) 0.0473(16) 0.0398(15) 0.0209(12) -0.0041(12) -0.0171(13) C48 0.0653(19) 0.0633(19) 0.0227(13) 0.0042(13) 0.0060(12) -0.0312(15) C49 0.0580(18) 0.0593(18) 0.0406(15) -0.0112(14) 0.0236(13) -0.0074(14) C50 0.0575(17) 0.0365(14) 0.0336(13) 0.0019(11) 0.0138(12) 0.0008(12) C51 0.0293(12) 0.0381(14) 0.0152(11) 0.0073(10) -0.0011(9) -0.0062(11) C52 0.0320(14) 0.0498(16) 0.0251(12) 0.0019(11) -0.0006(10) 0.0023(12) C53 0.0389(16) 0.081(2) 0.0317(14) 0.0040(13) 0.0050(12) 0.0158(14) C54 0.0280(15) 0.117(3) 0.0333(15) 0.0215(17) 0.0047(12) -0.0003(17) C55 0.0408(17) 0.089(2) 0.0376(15) 0.0223(15) -0.0044(12) -0.0288(15) C56 0.0387(15) 0.0492(16) 0.0325(13) 0.0138(11) -0.0037(11) -0.0137(12) _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 1.7357(19) . ? Fe1 P1 2.1732(6) . ? Fe1 P2 2.2026(6) . ? Fe1 S2 2.2485(5) . ? Fe1 S1 2.2611(5) . ? Fe1 Fe2 2.5678(4) . ? Fe2 C1 1.737(2) . ? Fe2 P3 2.1769(6) . ? Fe2 P4 2.1958(5) . ? Fe2 S1 2.2542(5) . ? Fe2 S2 2.2565(5) . ? S1 C3 1.8309(17) . ? S2 C4 1.8273(17) . ? P1 C13 1.8246(19) . ? P1 C5 1.8264(18) . ? P1 C7 1.8419(18) . ? P2 C6 1.8246(18) . ? P2 C19 1.8309(19) . ? P2 C25 1.8372(18) . ? P3 C31 1.8295(18) . ? P3 C33 1.8369(18) . ? P3 C39 1.8380(18) . ? P4 C32 1.8276(18) . ? P4 C45 1.8367(19) . ? P4 C51 1.838(2) . ? O1 C1 1.165(2) . ? O2 C2 1.1687(19) . ? C3 C4 1.522(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.318(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.389(2) . ? C7 C8 1.395(2) . ? C8 C9 1.384(2) . ? C8 H8 0.9500 . ? C9 C10 1.365(3) . ? C9 H9 0.9500 . ? C10 C11 1.375(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.377(2) . ? C13 C14 1.385(2) . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.364(3) . ? C15 H15 0.9500 . ? C16 C17 1.370(3) . ? C16 H16 0.9500 . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(2) . ? C19 C24 1.390(2) . ? C20 C21 1.387(3) . ? C20 H20 0.9500 . ? C21 C22 1.365(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.380(2) . ? C25 C26 1.394(2) . ? C26 C27 1.381(2) . ? C26 H26 0.9500 . ? C27 C28 1.373(3) . ? C27 H27 0.9500 . ? C28 C29 1.371(3) . ? C28 H28 0.9500 . ? C29 C30 1.389(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.316(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.387(2) . ? C33 C34 1.387(2) . ? C34 C35 1.387(2) . ? C34 H34 0.9500 . ? C35 C36 1.364(2) . ? C35 H35 0.9500 . ? C36 C37 1.365(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.388(2) . ? C39 C44 1.397(2) . ? C40 C41 1.384(2) . ? C40 H40 0.9500 . ? C41 C42 1.380(2) . ? C41 H41 0.9500 . ? C42 C43 1.389(2) . ? C42 H42 0.9500 . ? C43 C44 1.377(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.384(2) . ? C45 C50 1.390(3) . ? C46 C47 1.381(3) . ? C46 H46 0.9500 . ? C47 C48 1.367(3) . ? C47 H47 0.9500 . ? C48 C49 1.374(3) . ? C48 H48 0.9500 . ? C49 C50 1.394(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.393(2) . ? C51 C52 1.398(2) . ? C52 C53 1.387(3) . ? C52 H52 0.9500 . ? C53 C54 1.376(3) . ? C53 H53 0.9500 . ? C54 C55 1.366(3) . ? C54 H54 0.9500 . ? C55 C56 1.386(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 P1 92.70(6) . . ? C2 Fe1 P2 91.61(6) . . ? P1 Fe1 P2 87.93(2) . . ? C2 Fe1 S2 159.30(6) . . ? P1 Fe1 S2 107.80(2) . . ? P2 Fe1 S2 91.97(2) . . ? C2 Fe1 S1 93.18(6) . . ? P1 Fe1 S1 103.87(2) . . ? P2 Fe1 S1 167.03(2) . . ? S2 Fe1 S1 79.404(19) . . ? C2 Fe1 Fe2 104.53(6) . . ? P1 Fe1 Fe2 152.906(19) . . ? P2 Fe1 Fe2 111.874(18) . . ? S2 Fe1 Fe2 55.396(14) . . ? S1 Fe1 Fe2 55.216(15) . . ? C1 Fe2 P3 93.71(6) . . ? C1 Fe2 P4 90.12(6) . . ? P3 Fe2 P4 86.83(2) . . ? C1 Fe2 S1 157.31(6) . . ? P3 Fe2 S1 108.71(2) . . ? P4 Fe2 S1 94.45(2) . . ? C1 Fe2 S2 92.28(6) . . ? P3 Fe2 S2 103.61(2) . . ? P4 Fe2 S2 169.11(2) . . ? S1 Fe2 S2 79.382(19) . . ? C1 Fe2 Fe1 102.49(6) . . ? P3 Fe2 Fe1 153.200(18) . . ? P4 Fe2 Fe1 114.002(18) . . ? S1 Fe2 Fe1 55.468(15) . . ? S2 Fe2 Fe1 55.106(14) . . ? C3 S1 Fe2 104.74(6) . . ? C3 S1 Fe1 102.68(6) . . ? Fe2 S1 Fe1 69.316(17) . . ? C4 S2 Fe1 106.49(6) . . ? C4 S2 Fe2 101.70(6) . . ? Fe1 S2 Fe2 69.498(16) . . ? C13 P1 C5 102.83(9) . . ? C13 P1 C7 102.34(9) . . ? C5 P1 C7 97.50(8) . . ? C13 P1 Fe1 119.05(6) . . ? C5 P1 Fe1 107.72(6) . . ? C7 P1 Fe1 123.60(6) . . ? C6 P2 C19 100.09(9) . . ? C6 P2 C25 100.05(8) . . ? C19 P2 C25 100.96(9) . . ? C6 P2 Fe1 106.74(7) . . ? C19 P2 Fe1 120.02(6) . . ? C25 P2 Fe1 124.71(6) . . ? C31 P3 C33 102.91(8) . . ? C31 P3 C39 102.16(8) . . ? C33 P3 C39 102.15(8) . . ? C31 P3 Fe2 107.49(6) . . ? C33 P3 Fe2 120.15(6) . . ? C39 P3 Fe2 119.48(6) . . ? C32 P4 C45 101.32(9) . . ? C32 P4 C51 101.05(9) . . ? C45 P4 C51 103.39(8) . . ? C32 P4 Fe2 106.55(6) . . ? C45 P4 Fe2 119.72(6) . . ? C51 P4 Fe2 121.48(6) . . ? O1 C1 Fe2 177.44(18) . . ? O2 C2 Fe1 177.61(17) . . ? C4 C3 S1 111.74(12) . . ? C4 C3 H3A 109.3 . . ? S1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? S1 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 S2 111.22(12) . . ? C3 C4 H4A 109.4 . . ? S2 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? S2 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 P1 117.73(15) . . ? C6 C5 H5 121.1 . . ? P1 C5 H5 121.1 . . ? C5 C6 P2 118.48(15) . . ? C5 C6 H6 120.8 . . ? P2 C6 H6 120.8 . . ? C12 C7 C8 117.70(18) . . ? C12 C7 P1 125.25(15) . . ? C8 C7 P1 116.72(14) . . ? C9 C8 C7 121.44(19) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.53(19) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C18 C13 C14 117.72(19) . . ? C18 C13 P1 119.47(16) . . ? C14 C13 P1 122.81(16) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.5(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 121.6(2) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C20 C19 C24 118.42(19) . . ? C20 C19 P2 121.56(16) . . ? C24 C19 P2 119.92(15) . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.8(2) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C19 120.7(2) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C30 C25 C26 117.90(18) . . ? C30 C25 P2 121.90(15) . . ? C26 C25 P2 120.18(14) . . ? C27 C26 C25 121.36(19) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 120.0(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 119.4(2) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 120.9(2) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C25 C30 C29 120.38(19) . . ? C25 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 P3 117.20(15) . . ? C32 C31 H31 121.4 . . ? P3 C31 H31 121.4 . . ? C31 C32 P4 117.80(15) . . ? C31 C32 H32 121.1 . . ? P4 C32 H32 121.1 . . ? C38 C33 C34 117.59(18) . . ? C38 C33 P3 123.31(15) . . ? C34 C33 P3 119.10(15) . . ? C33 C34 C35 121.17(19) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 120.2(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 119.86(19) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.3(2) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 120.8(2) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C44 118.04(17) . . ? C40 C39 P3 123.39(14) . . ? C44 C39 P3 118.36(14) . . ? C41 C40 C39 120.83(18) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C42 C41 C40 120.61(18) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 119.20(19) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.18(19) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C39 121.14(18) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? C46 C45 C50 117.80(19) . . ? C46 C45 P4 123.51(16) . . ? C50 C45 P4 118.49(15) . . ? C47 C46 C45 121.5(2) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C48 C47 C46 120.1(2) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C49 120.0(2) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 120.0(2) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C45 C50 C49 120.6(2) . . ? C45 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C56 C51 C52 117.62(19) . . ? C56 C51 P4 122.28(17) . . ? C52 C51 P4 120.04(15) . . ? C53 C52 C51 120.9(2) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C54 C53 C52 120.2(2) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.8(2) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.6(2) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C55 C56 C51 120.9(2) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.463 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.098 _vrf_REFLT03_gs72has5 ; PROBLEM: Reflection count > 15% excess reflns - sys abs data present? RESPONSE: All crystals examined were non-merohedrally twinned. Two distinct cells were identified for the data crystal. Non-overlapping reflections from the primary orientation were used for phasing. Unmerged combined data with complete or no overlap were used for refinement generating this apparent excess. ; _vrf_PLAT021_gs72has5 ; PROBLEM: Ratio Unique / Expected Reflections too High ... 2.09 RESPONSE: All crystals examined were non-merohedrally twinned. Two distinct cells were identified for the data crystal. Non-overlapping reflections from the primary orientation were used for phasing. Unmerged combined data with complete or no overlap were used for refinement generating this apparent excess. ; _publ_section_references ; Bruker (2001). SAINT, SHELXTL, XCIF. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2004). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2004). Cell_Now. Program to isolate multiple orientations for crystals suffering from non-merohedral twinning. Institute fur anorg chemie, G\"ottingen, Germany. ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2001) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ; _publ_section_exptl_prep ; Crystals were grown by liquid diffusion of hexane into methylenechloride solution. ; _publ_section_exptl_refinement ; H atoms were included as riding idealized contributors. H atom U's were assigned as 1.2 times carrier U~eq~. ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 1.00 0.0150 0.00 -1.00 -1.00 0.0150 0.00 -1.00 1.00 0.0450 0.00 1.00 -1.00 0.0450 -1.00 0.00 0.00 0.1800 1.00 0.00 0.00 0.1800