# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 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 ; 'Bryan E. Barton' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Luca De Gioia' '' 'Aaron K. Justice' '' 'Giuseppe Zampella' '' _publ_contact_author_name 'T Rauchfuss' _publ_contact_author_email RAUCHFUZ@UIUC.EDU _publ_section_title ; Isomerization of the Hydride Complexes [HFe2(SR)2(PR)x(CO)6-x]+ (x = 2, 3, 4) Relevant to the Active Site Models for the [FeFe]-Hydrogenases ; _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. ; _publ_requested_category FM _publ_requested_coeditor_name ? _publ_requested_journal 'Acta Crystallographica E' # Attachment 'HFe2_dppv__PMe3_edt.cif' data_g12kas _database_code_depnum_ccdc_archive 'CCDC 733498' _audit_creation_method SHELXL-97 _audit_update_record ; 2006-09-20 text and data added, akj ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Fe2 O3 P3 S2, F6 P' _chemical_formula_sum 'C34 H36 F6 Fe2 O3 P4 S2' _chemical_formula_structural ? _chemical_formula_weight 906.33 _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' 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' 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 10.818(2) _cell_length_b 11.253(2) _cell_length_c 16.208(3) _cell_angle_alpha 78.473(3) _cell_angle_beta 86.415(3) _cell_angle_gamma 81.525(3) _cell_volume 1911.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 959 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_crystal_id g12kas _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 0) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6869 _exptl_absorpt_correction_T_max 0.8572 _exptl_absorpt_process_details 'SHELXTL/XPREP (Bruker, 2001)' _exptl_special_details ; One distinct cell was identified using SMART (Bruker, 2001). 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/SADABS (Bruker, 2001) to sort, merge, and scale the combined data. A series of identical frames was collected twice during the experiment to monitor decay. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id g12kas _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Siemens Platform/CCD' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 367 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 304 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 23821 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9184 _reflns_number_gt 7101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _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 ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atoms F1, C9, and F4; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed no dependence on amplitude or 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^)+(0.0442P)^2^+0.4382P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9184 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _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 0.67396(2) 0.43483(2) 0.268570(16) 0.02345(7) Uani 1 1 d . . . Fe2 Fe 0.48688(3) 0.59410(2) 0.295306(17) 0.02694(7) Uani 1 1 d . . . H1 H 0.620(2) 0.585(2) 0.2405(15) 0.047(7) Uiso 1 1 d . . . S1 S 0.47152(4) 0.41138(4) 0.26088(3) 0.02775(11) Uani 1 1 d . . . S2 S 0.59936(4) 0.46411(4) 0.39871(3) 0.02777(11) Uani 1 1 d . . . P1 P 0.77368(5) 0.24605(4) 0.30071(3) 0.02674(11) Uani 1 1 d . . . P2 P 0.85823(5) 0.49838(4) 0.27441(3) 0.02562(11) Uani 1 1 d . . . P3 P 0.41117(5) 0.69872(5) 0.17110(4) 0.03511(13) Uani 1 1 d . . . P4 P 0.26132(5) 0.14430(6) 0.18730(4) 0.04012(14) Uani 1 1 d . . . F1 F 0.24453(15) 0.22261(15) 0.26060(9) 0.0597(4) Uani 1 1 d . . . F2 F 0.18525(14) 0.04519(13) 0.24613(10) 0.0577(4) Uani 1 1 d . . . F3 F 0.38791(14) 0.07100(18) 0.22795(11) 0.0759(5) Uani 1 1 d . . . F4 F 0.33694(17) 0.24268(18) 0.13010(11) 0.0806(5) Uani 1 1 d . . . F5 F 0.27607(17) 0.06571(15) 0.11471(10) 0.0714(5) Uani 1 1 d . . . F6 F 0.13309(13) 0.21652(12) 0.14932(9) 0.0498(3) Uani 1 1 d . . . O1 O 0.71140(15) 0.43386(15) 0.08955(9) 0.0437(4) Uani 1 1 d . . . O2 O 0.56576(19) 0.81155(16) 0.33850(12) 0.0589(5) Uani 1 1 d . . . O3 O 0.24472(16) 0.61394(17) 0.38524(12) 0.0568(5) Uani 1 1 d . . . C1 C 0.69907(18) 0.43396(18) 0.16005(13) 0.0291(4) Uani 1 1 d . . . C2 C 0.5346(2) 0.7277(2) 0.32086(14) 0.0368(5) Uani 1 1 d . . . C3 C 0.3399(2) 0.6076(2) 0.34976(14) 0.0374(5) Uani 1 1 d . . . C4 C 0.49319(19) 0.35008(19) 0.43485(13) 0.0332(4) Uani 1 1 d . . . H4A H 0.5402 0.2755 0.4680 0.040 Uiso 1 1 calc R . . H4B H 0.4267 0.3830 0.4723 0.040 Uiso 1 1 calc R . . C5 C 0.4336(2) 0.31628(19) 0.36173(12) 0.0334(4) Uani 1 1 d . . . H5A H 0.3416 0.3257 0.3712 0.040 Uiso 1 1 calc R . . H5B H 0.4628 0.2293 0.3597 0.040 Uiso 1 1 calc R . . C6 C 0.4192(3) 0.6156(3) 0.08518(16) 0.0585(7) Uani 1 1 d . . . H6A H 0.3794 0.5415 0.1035 0.088 Uiso 1 1 calc R . . H6B H 0.5069 0.5929 0.0688 0.088 Uiso 1 1 calc R . . H6C H 0.3756 0.6677 0.0369 0.088 Uiso 1 1 calc R . . C7 C 0.4899(2) 0.8295(2) 0.12408(17) 0.0535(7) Uani 1 1 d . . . H7A H 0.4496 0.8719 0.0718 0.080 Uiso 1 1 calc R . . H7B H 0.5779 0.8012 0.1117 0.080 Uiso 1 1 calc R . . H7C H 0.4846 0.8860 0.1635 0.080 Uiso 1 1 calc R . . C8 C 0.2477(2) 0.7637(2) 0.17530(17) 0.0500(6) Uani 1 1 d . . . H8A H 0.2362 0.8231 0.2128 0.075 Uiso 1 1 calc R . . H8B H 0.1967 0.6983 0.1967 0.075 Uiso 1 1 calc R . . H8C H 0.2218 0.8049 0.1186 0.075 Uiso 1 1 calc R . . C9 C 0.93746(18) 0.25510(18) 0.31488(12) 0.0306(4) Uani 1 1 d . . . H9 H 0.9964 0.1830 0.3267 0.037 Uiso 1 1 calc R . . C10 C 0.97255(18) 0.36460(18) 0.30830(12) 0.0287(4) Uani 1 1 d . . . H10 H 1.0550 0.3730 0.3209 0.034 Uiso 1 1 calc R . . C11 C 0.74064(18) 0.14409(17) 0.40024(12) 0.0300(4) Uani 1 1 d . . . C12 C 0.6774(2) 0.04410(18) 0.40385(13) 0.0349(5) Uani 1 1 d . . . H12 H 0.6505 0.0261 0.3536 0.042 Uiso 1 1 calc R . . C13 C 0.6537(2) -0.0296(2) 0.48131(15) 0.0430(5) Uani 1 1 d . . . H13 H 0.6096 -0.0973 0.4838 0.052 Uiso 1 1 calc R . . C14 C 0.6938(2) -0.0051(2) 0.55446(15) 0.0454(6) Uani 1 1 d . . . H14 H 0.6777 -0.0562 0.6070 0.054 Uiso 1 1 calc R . . C15 C 0.7574(2) 0.0934(2) 0.55150(14) 0.0437(5) Uani 1 1 d . . . H15 H 0.7851 0.1100 0.6020 0.052 Uiso 1 1 calc R . . C16 C 0.7808(2) 0.1684(2) 0.47476(13) 0.0374(5) Uani 1 1 d . . . H16 H 0.8242 0.2365 0.4729 0.045 Uiso 1 1 calc R . . C17 C 0.77260(19) 0.15376(17) 0.21986(12) 0.0294(4) Uani 1 1 d . . . C18 C 0.8815(2) 0.08819(19) 0.19199(14) 0.0396(5) Uani 1 1 d . . . H18 H 0.9589 0.0868 0.2170 0.048 Uiso 1 1 calc R . . C19 C 0.8758(2) 0.0248(2) 0.12711(16) 0.0497(6) Uani 1 1 d . . . H19 H 0.9497 -0.0203 0.1081 0.060 Uiso 1 1 calc R . . C20 C 0.7637(3) 0.0268(2) 0.09012(15) 0.0474(6) Uani 1 1 d . . . H20 H 0.7612 -0.0156 0.0452 0.057 Uiso 1 1 calc R . . C21 C 0.6556(2) 0.0900(2) 0.11805(14) 0.0418(5) Uani 1 1 d . . . H21 H 0.5783 0.0899 0.0933 0.050 Uiso 1 1 calc R . . C22 C 0.6602(2) 0.15378(19) 0.18253(14) 0.0371(5) Uani 1 1 d . . . H22 H 0.5857 0.1980 0.2014 0.044 Uiso 1 1 calc R . . C23 C 0.87975(18) 0.60207(18) 0.34441(13) 0.0306(4) Uani 1 1 d . . . C24 C 0.8647(2) 0.5614(2) 0.43100(13) 0.0375(5) Uani 1 1 d . . . H24 H 0.8449 0.4812 0.4521 0.045 Uiso 1 1 calc R . . C25 C 0.8784(2) 0.6373(3) 0.48642(16) 0.0477(6) Uani 1 1 d . . . H25 H 0.8677 0.6088 0.5453 0.057 Uiso 1 1 calc R . . C26 C 0.9076(2) 0.7536(3) 0.45674(18) 0.0540(7) Uani 1 1 d . . . H26 H 0.9168 0.8054 0.4950 0.065 Uiso 1 1 calc R . . C27 C 0.9234(3) 0.7945(2) 0.37159(18) 0.0570(7) Uani 1 1 d . . . H27 H 0.9440 0.8745 0.3510 0.068 Uiso 1 1 calc R . . C28 C 0.9093(2) 0.7193(2) 0.31511(15) 0.0450(5) Uani 1 1 d . . . H28 H 0.9200 0.7485 0.2563 0.054 Uiso 1 1 calc R . . C29 C 0.92613(18) 0.56661(17) 0.17339(12) 0.0276(4) Uani 1 1 d . . . C30 C 0.8617(2) 0.6701(2) 0.12441(13) 0.0396(5) Uani 1 1 d . . . H30 H 0.7838 0.7065 0.1447 0.048 Uiso 1 1 calc R . . C31 C 0.9103(2) 0.7209(2) 0.04586(14) 0.0456(6) Uani 1 1 d . . . H31 H 0.8659 0.7917 0.0128 0.055 Uiso 1 1 calc R . . C32 C 1.0234(2) 0.6679(2) 0.01623(14) 0.0425(5) Uani 1 1 d . . . H32 H 1.0576 0.7032 -0.0369 0.051 Uiso 1 1 calc R . . C33 C 1.0864(2) 0.5640(2) 0.06357(14) 0.0417(5) Uani 1 1 d . . . H33 H 1.1630 0.5267 0.0422 0.050 Uiso 1 1 calc R . . C34 C 1.03902(19) 0.51301(19) 0.14257(13) 0.0338(4) Uani 1 1 d . . . H34 H 1.0837 0.4419 0.1752 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02478(14) 0.02620(14) 0.01996(14) -0.00654(10) 0.00153(10) -0.00354(10) Fe2 0.02723(15) 0.02747(14) 0.02753(15) -0.01001(11) -0.00021(11) -0.00224(11) S1 0.0282(2) 0.0307(2) 0.0269(2) -0.01018(19) 0.00042(18) -0.00669(18) S2 0.0293(2) 0.0335(2) 0.0221(2) -0.00892(18) 0.00133(18) -0.00527(19) P1 0.0290(3) 0.0261(2) 0.0251(2) -0.00591(19) 0.00117(19) -0.00318(19) P2 0.0252(2) 0.0288(2) 0.0232(2) -0.00617(18) 0.00146(18) -0.00403(18) P3 0.0349(3) 0.0339(3) 0.0357(3) -0.0066(2) -0.0069(2) 0.0003(2) P4 0.0352(3) 0.0473(3) 0.0380(3) -0.0119(3) -0.0043(2) 0.0005(2) F1 0.0649(10) 0.0698(10) 0.0521(9) -0.0299(8) -0.0106(7) -0.0055(8) F2 0.0603(9) 0.0512(8) 0.0573(9) 0.0042(7) -0.0109(7) -0.0096(7) F3 0.0412(9) 0.1132(14) 0.0652(11) -0.0183(10) -0.0113(7) 0.0213(9) F4 0.0723(12) 0.0972(14) 0.0716(12) -0.0009(10) 0.0107(9) -0.0357(10) F5 0.0921(13) 0.0690(10) 0.0533(9) -0.0325(8) -0.0132(8) 0.0211(9) F6 0.0488(8) 0.0488(8) 0.0474(8) -0.0068(6) -0.0128(6) 0.0086(6) O1 0.0494(10) 0.0585(10) 0.0247(8) -0.0116(7) 0.0055(7) -0.0106(8) O2 0.0733(13) 0.0426(10) 0.0700(13) -0.0250(9) -0.0105(10) -0.0152(9) O3 0.0387(10) 0.0700(12) 0.0569(11) -0.0120(9) 0.0135(8) 0.0017(8) C1 0.0274(10) 0.0307(10) 0.0301(11) -0.0080(8) 0.0003(8) -0.0046(8) C2 0.0403(12) 0.0357(11) 0.0354(12) -0.0115(9) -0.0013(9) -0.0020(9) C3 0.0375(12) 0.0379(11) 0.0360(12) -0.0096(9) -0.0011(9) 0.0002(9) C4 0.0336(11) 0.0356(11) 0.0301(11) -0.0065(8) 0.0080(8) -0.0079(8) C5 0.0342(11) 0.0355(11) 0.0316(11) -0.0077(8) 0.0079(8) -0.0107(8) C6 0.0755(19) 0.0598(16) 0.0384(14) -0.0166(12) -0.0221(13) 0.0145(14) C7 0.0518(15) 0.0487(14) 0.0521(15) 0.0105(12) -0.0073(12) -0.0068(11) C8 0.0397(13) 0.0488(14) 0.0588(16) -0.0074(12) -0.0115(11) 0.0027(10) C9 0.0302(10) 0.0334(10) 0.0263(10) -0.0054(8) -0.0005(8) 0.0020(8) C10 0.0277(10) 0.0352(10) 0.0235(10) -0.0066(8) -0.0016(7) -0.0035(8) C11 0.0313(10) 0.0267(9) 0.0301(10) -0.0035(8) 0.0016(8) -0.0016(8) C12 0.0426(12) 0.0300(10) 0.0323(11) -0.0074(8) 0.0014(9) -0.0048(9) C13 0.0519(14) 0.0344(11) 0.0425(13) -0.0034(10) 0.0048(10) -0.0131(10) C14 0.0553(15) 0.0415(12) 0.0341(12) 0.0043(10) 0.0025(10) -0.0077(11) C15 0.0557(15) 0.0458(13) 0.0278(11) -0.0025(9) -0.0044(10) -0.0061(11) C16 0.0442(12) 0.0358(11) 0.0322(11) -0.0046(9) -0.0017(9) -0.0078(9) C17 0.0376(11) 0.0249(9) 0.0262(10) -0.0066(7) 0.0022(8) -0.0049(8) C18 0.0381(12) 0.0372(12) 0.0438(13) -0.0126(10) 0.0038(10) -0.0013(9) C19 0.0522(15) 0.0437(13) 0.0554(15) -0.0241(11) 0.0121(12) 0.0008(11) C20 0.0665(17) 0.0400(13) 0.0406(13) -0.0212(10) 0.0041(11) -0.0073(11) C21 0.0530(14) 0.0379(12) 0.0386(12) -0.0146(10) -0.0051(10) -0.0083(10) C22 0.0387(12) 0.0364(11) 0.0381(12) -0.0138(9) 0.0001(9) -0.0030(9) C23 0.0259(10) 0.0359(11) 0.0323(11) -0.0135(8) -0.0020(8) -0.0017(8) C24 0.0329(11) 0.0493(13) 0.0333(11) -0.0127(9) -0.0020(9) -0.0088(9) C25 0.0383(13) 0.0709(17) 0.0395(13) -0.0248(12) -0.0061(10) -0.0047(11) C26 0.0510(15) 0.0578(16) 0.0622(17) -0.0387(14) -0.0162(13) 0.0059(12) C27 0.0738(19) 0.0376(13) 0.0660(18) -0.0215(12) -0.0159(14) -0.0065(12) C28 0.0589(15) 0.0367(12) 0.0412(13) -0.0109(10) -0.0061(11) -0.0064(10) C29 0.0304(10) 0.0297(10) 0.0243(10) -0.0059(7) 0.0020(7) -0.0095(8) C30 0.0416(12) 0.0400(12) 0.0330(12) -0.0055(9) 0.0044(9) 0.0032(9) C31 0.0649(16) 0.0375(12) 0.0304(12) -0.0009(9) 0.0026(10) -0.0034(11) C32 0.0550(14) 0.0454(13) 0.0299(11) -0.0085(10) 0.0087(10) -0.0187(11) C33 0.0376(12) 0.0523(14) 0.0357(12) -0.0104(10) 0.0106(9) -0.0098(10) C34 0.0332(11) 0.0364(11) 0.0316(11) -0.0073(8) 0.0049(8) -0.0057(8) _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 C1 1.765(2) . ? Fe1 P1 2.2137(6) . ? Fe1 P2 2.2282(6) . ? Fe1 S1 2.2581(7) . ? Fe1 S2 2.2794(6) . ? Fe1 Fe2 2.5744(5) . ? Fe1 H1 1.69(2) . ? Fe2 C3 1.771(2) . ? Fe2 C2 1.790(2) . ? Fe2 P3 2.2549(7) . ? Fe2 S1 2.2668(7) . ? Fe2 S2 2.2760(6) . ? Fe2 H1 1.64(2) . ? S1 C5 1.826(2) . ? S2 C4 1.833(2) . ? P1 C9 1.821(2) . ? P1 C17 1.829(2) . ? P1 C11 1.8318(19) . ? P2 C10 1.818(2) . ? P2 C29 1.8231(19) . ? P2 C23 1.829(2) . ? P3 C8 1.814(2) . ? P3 C6 1.817(3) . ? P3 C7 1.820(2) . ? P4 F4 1.5863(17) . ? P4 F6 1.5933(14) . ? P4 F5 1.5947(16) . ? P4 F3 1.5976(16) . ? P4 F1 1.6017(15) . ? P4 F2 1.6055(15) . ? O1 C1 1.142(2) . ? O2 C2 1.140(3) . ? O3 C3 1.148(3) . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.324(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.390(3) . ? C11 C16 1.398(3) . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C15 1.380(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.391(3) . ? C17 C18 1.396(3) . ? C18 C19 1.393(3) . ? C18 H18 0.9500 . ? C19 C20 1.381(4) . ? C19 H19 0.9500 . ? C20 C21 1.377(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.387(3) . ? C23 C24 1.394(3) . ? C24 C25 1.385(3) . ? C24 H24 0.9500 . ? C25 C26 1.377(4) . ? C25 H25 0.9500 . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.393(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.390(3) . ? C29 C30 1.390(3) . ? C30 C31 1.392(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 H31 0.9500 . ? C32 C33 1.375(3) . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 P1 90.78(6) . . ? C1 Fe1 P2 91.10(6) . . ? P1 Fe1 P2 86.80(2) . . ? C1 Fe1 S1 90.70(6) . . ? P1 Fe1 S1 104.80(2) . . ? P2 Fe1 S1 168.23(2) . . ? C1 Fe1 S2 166.64(7) . . ? P1 Fe1 S2 100.41(2) . . ? P2 Fe1 S2 96.73(2) . . ? S1 Fe1 S2 79.47(2) . . ? C1 Fe1 Fe2 111.37(6) . . ? P1 Fe1 Fe2 148.911(18) . . ? P2 Fe1 Fe2 113.20(2) . . ? S1 Fe1 Fe2 55.482(18) . . ? S2 Fe1 Fe2 55.525(15) . . ? C1 Fe1 H1 87.0(8) . . ? P1 Fe1 H1 171.3(8) . . ? P2 Fe1 H1 84.8(8) . . ? S1 Fe1 H1 83.6(8) . . ? S2 Fe1 H1 83.0(8) . . ? Fe2 Fe1 H1 38.7(8) . . ? C3 Fe2 C2 95.45(10) . . ? C3 Fe2 P3 94.15(7) . . ? C2 Fe2 P3 92.44(7) . . ? C3 Fe2 S1 95.67(7) . . ? C2 Fe2 S1 167.60(7) . . ? P3 Fe2 S1 92.20(2) . . ? C3 Fe2 S2 98.76(7) . . ? C2 Fe2 S2 93.53(7) . . ? P3 Fe2 S2 165.19(2) . . ? S1 Fe2 S2 79.37(2) . . ? C3 Fe2 Fe1 141.78(7) . . ? C2 Fe2 Fe1 112.44(7) . . ? P3 Fe2 Fe1 109.54(2) . . ? S1 Fe2 Fe1 55.164(17) . . ? S2 Fe2 Fe1 55.652(17) . . ? C3 Fe2 H1 177.1(8) . . ? C2 Fe2 H1 84.8(8) . . ? P3 Fe2 H1 83.0(8) . . ? S1 Fe2 H1 84.4(8) . . ? S2 Fe2 H1 84.1(8) . . ? Fe1 Fe2 H1 40.0(8) . . ? C5 S1 Fe1 104.89(7) . . ? C5 S1 Fe2 103.30(7) . . ? Fe1 S1 Fe2 69.355(17) . . ? C4 S2 Fe2 101.09(7) . . ? C4 S2 Fe1 106.02(7) . . ? Fe2 S2 Fe1 68.82(2) . . ? C9 P1 C17 106.01(9) . . ? C9 P1 C11 99.16(9) . . ? C17 P1 C11 105.01(9) . . ? C9 P1 Fe1 108.25(7) . . ? C17 P1 Fe1 114.96(7) . . ? C11 P1 Fe1 121.43(6) . . ? C10 P2 C29 102.10(9) . . ? C10 P2 C23 103.96(9) . . ? C29 P2 C23 104.19(9) . . ? C10 P2 Fe1 108.04(7) . . ? C29 P2 Fe1 115.40(7) . . ? C23 P2 Fe1 121.02(6) . . ? C8 P3 C6 102.98(13) . . ? C8 P3 C7 103.60(12) . . ? C6 P3 C7 101.97(14) . . ? C8 P3 Fe2 114.84(9) . . ? C6 P3 Fe2 117.13(9) . . ? C7 P3 Fe2 114.47(9) . . ? F4 P4 F6 90.69(10) . . ? F4 P4 F5 90.09(11) . . ? F6 P4 F5 90.05(8) . . ? F4 P4 F3 90.61(11) . . ? F6 P4 F3 178.36(9) . . ? F5 P4 F3 90.94(9) . . ? F4 P4 F1 90.61(10) . . ? F6 P4 F1 89.47(8) . . ? F5 P4 F1 179.16(10) . . ? F3 P4 F1 89.52(9) . . ? F4 P4 F2 179.35(10) . . ? F6 P4 F2 89.59(8) . . ? F5 P4 F2 90.50(10) . . ? F3 P4 F2 89.11(9) . . ? F1 P4 F2 88.81(9) . . ? O1 C1 Fe1 177.88(18) . . ? O2 C2 Fe2 178.7(2) . . ? O3 C3 Fe2 178.6(2) . . ? C5 C4 S2 111.95(13) . . ? C5 C4 H4A 109.2 . . ? S2 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? S2 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 S1 112.15(14) . . ? C4 C5 H5A 109.2 . . ? S1 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? S1 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? P3 C6 H6A 109.5 . . ? P3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 118.46(15) . . ? C10 C9 H9 120.8 . . ? P1 C9 H9 120.8 . . ? C9 C10 P2 118.04(16) . . ? C9 C10 H10 121.0 . . ? P2 C10 H10 121.0 . . ? C12 C11 C16 119.35(18) . . ? C12 C11 P1 122.23(16) . . ? C16 C11 P1 118.41(15) . . ? C11 C12 C13 119.8(2) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.2(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C22 C17 C18 119.23(19) . . ? C22 C17 P1 118.61(15) . . ? C18 C17 P1 122.09(17) . . ? C19 C18 C17 119.4(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 120.6(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C17 120.8(2) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C28 C23 C24 118.7(2) . . ? C28 C23 P2 122.95(17) . . ? C24 C23 P2 118.34(16) . . ? C25 C24 C23 120.4(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 119.7(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.5(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 120.3(2) . . ? C23 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C34 C29 C30 119.29(18) . . ? C34 C29 P2 120.80(15) . . ? C30 C29 P2 119.84(15) . . ? C29 C30 C31 120.5(2) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.0(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.6(2) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C29 C34 C33 119.7(2) . . ? C29 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.392 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.062 _publ_section_references ; Bruker (2001). SAINT, SHELXTL, SMART, XCIF. Bruker AXS, Inc., Madison, Wisconsin, USA. ; _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 at room temperature by liquid diffusion of hexane into methylenechloride solution. ; _publ_section_exptl_refinement ; The metal hydride surfaced in a late difference Fourier map. The position and isotropic displacement parameter for this H atom were independently refined without restraint. Methyl H atom positions, R-CH~3~, were optimized by rotation about R-C bonds with idealized C-H, R--H and H--H distances. Remaining H atoms were included as riding idealized contributors. Methyl H atom U's were assigned as 1.5 times U~eq~ of the carrier atom; remaining 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 0.00 0.1200 0.00 -1.00 0.00 0.1200 -1.00 0.00 -1.00 0.0800 1.00 0.00 1.00 0.0800 0.00 0.00 1.00 0.2000 1.00 0.00 -1.00 0.1900 -1.00 0.00 1.00 0.1900 1.00 -1.00 -1.00 0.1800