Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Leslie D. Field' _publ_contact_author_address ; School of Chemistry University of Sydney Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_phone '+61 2 9351 2060' _publ_contact_author_fax '+61 2 9351 6650' _publ_contact_author_email l.field@chem.usyd.edu.au _publ_requested_journal 'Dalton Transactions' _publ_section_title ; An Iron(II) Dihydrogen Hydrido Complex Containing the Tripodal Tetraphosphine Ligand P(CH2CH2PMe2)3 ; loop_ _publ_author_name _publ_author_address 'Leslie D. Field' ; School of Chemistry, University of Sydney, Sydney, N.S.W. 2006 ; 'Hsiu L. Li' ; School of Chemistry, University of Sydney, Sydney, N.S.W. 2006 ; 'Barbara A. Messerle' ; School of Chemistry, University of Sydney, Sydney, N.S.W. 2006 ; 'Ronald J. Smernik' ; School of Chemistry, University of Sydney, Sydney, N.S.W. 2006 ; 'Peter Turner' ; School of Chemistry, University of Sydney, Sydney, N.S.W. 2006 ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ldf131 _database_code_depnum_ccdc_archive 'CCDC 230875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H41 Cl Fe O2 P4' _chemical_formula_weight 504.69 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.502(2) _cell_length_b 9.1318(15) _cell_length_c 19.697(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.820(3) _cell_angle_gamma 90.00 _cell_volume 2532.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 963 _cell_measurement_theta_min 3.088 _cell_measurement_theta_max 26.705 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.398 _exptl_crystal_size_mid 0.294 _exptl_crystal_size_min 0.116 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 128 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 24965 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6050 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+5.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6050 _refine_ls_number_parameters 209 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2708 _refine_ls_wR_factor_gt 0.2483 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.246 _refine_ls_shift/su_max 0.007 _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 0.30239(6) 0.19663(11) 0.53377(5) 0.0681(3) Uani 1 1 d . . . Cl1 Cl 0.39396(11) 0.16266(18) 0.82023(7) 0.0714(5) Uani 1 1 d . . . P1 P 0.23303(14) 0.32879(17) 0.59915(10) 0.0776(6) Uani 1 1 d . . . P2 P 0.25565(11) 0.00505(15) 0.58769(7) 0.0559(4) Uani 1 1 d . . . P3 P 0.16694(12) 0.2242(2) 0.45270(8) 0.0666(5) Uani 1 1 d . . . P4 P 0.43534(14) 0.2592(3) 0.61309(13) 0.1029(9) Uani 1 1 d . . . O1 O 0.3890(7) 0.024(2) 0.4438(5) 0.261(9) Uani 1 1 d . . . C1 C 0.3352(7) 0.3922(15) 0.4847(6) 0.182(7) Uani 1 1 d . . . H1A H 0.3781 0.3689 0.4547 0.274 Uiso 1 1 calc R . . H1B H 0.3660 0.4625 0.5206 0.274 Uiso 1 1 calc R . . H1C H 0.2765 0.4350 0.4564 0.274 Uiso 1 1 calc R . . C2 C 0.3584(6) 0.0798(18) 0.4787(5) 0.136(5) Uani 1 1 d . . . C3 C 0.1953(5) 0.2199(7) 0.6627(4) 0.0734(18) Uani 1 1 d . . . H3A H 0.2481 0.2088 0.7048 0.088 Uiso 1 1 calc R . . H3B H 0.1417 0.2683 0.6767 0.088 Uiso 1 1 calc R . . C4 C 0.1647(4) 0.0709(7) 0.6317(3) 0.0637(14) Uani 1 1 d . . . H4A H 0.1024 0.0784 0.5976 0.076 Uiso 1 1 calc R . . H4B H 0.1584 0.0017 0.6690 0.076 Uiso 1 1 calc R . . C5 C 0.3325(5) -0.0902(7) 0.6607(3) 0.082(2) Uani 1 1 d . . . H5A H 0.2984 -0.1739 0.6741 0.123 Uiso 1 1 calc R . . H5B H 0.3511 -0.0231 0.7005 0.123 Uiso 1 1 calc R . . H5C H 0.3893 -0.1249 0.6470 0.123 Uiso 1 1 calc R . . C6 C 0.2043(6) -0.1577(7) 0.5381(3) 0.0768(19) Uani 1 1 d . . . H6A H 0.2543 -0.2120 0.5232 0.115 Uiso 1 1 calc R . . H6B H 0.1555 -0.1276 0.4969 0.115 Uiso 1 1 calc R . . H6C H 0.1756 -0.2206 0.5678 0.115 Uiso 1 1 calc R . . C7 C 0.1219(7) 0.4138(10) 0.5501(4) 0.132(4) Uani 1 1 d D . . H7A H 0.0675 0.3714 0.5655 0.158 Uiso 1 1 calc R . . H7B H 0.1236 0.5203 0.5597 0.158 Uiso 1 1 calc R . . C8 C 0.1091(7) 0.3892(11) 0.4737(4) 0.125(4) Uani 1 1 d D . . H8A H 0.1347 0.4746 0.4533 0.151 Uiso 1 1 calc R . . H8B H 0.0403 0.3828 0.4517 0.151 Uiso 1 1 calc R . . C9 C 0.0676(5) 0.0995(9) 0.4358(4) 0.091(2) Uani 1 1 d . . . H9A H 0.0150 0.1419 0.4005 0.136 Uiso 1 1 calc R . . H9B H 0.0471 0.0826 0.4791 0.136 Uiso 1 1 calc R . . H9C H 0.0866 0.0063 0.4186 0.136 Uiso 1 1 calc R . . C10 C 0.1698(7) 0.2560(14) 0.3636(4) 0.121(4) Uani 1 1 d . . . H10A H 0.1906 0.1667 0.3440 0.181 Uiso 1 1 calc R . . H10B H 0.2143 0.3357 0.3614 0.181 Uiso 1 1 calc R . . H10C H 0.1062 0.2830 0.3366 0.181 Uiso 1 1 calc R . . C11 C 0.3110(6) 0.4678(8) 0.6493(5) 0.125(4) Uani 1 1 d D . . H11A H 0.3141 0.5546 0.6198 0.150 Uiso 1 1 calc R . . H11B H 0.2871 0.4992 0.6901 0.150 Uiso 1 1 calc R . . C12 C 0.4069(6) 0.3997(10) 0.6730(6) 0.139(4) Uani 1 1 d D . . H12A H 0.4117 0.3541 0.7193 0.166 Uiso 1 1 calc R . . H12B H 0.4554 0.4781 0.6791 0.166 Uiso 1 1 calc R . . C13 C 0.5093(6) 0.1352(13) 0.6735(5) 0.127(3) Uani 1 1 d . . . H13A H 0.5201 0.0462 0.6486 0.191 Uiso 1 1 calc R . . H13B H 0.4777 0.1095 0.7106 0.191 Uiso 1 1 calc R . . H13C H 0.5703 0.1823 0.6940 0.191 Uiso 1 1 calc R . . C14 C 0.5304(6) 0.3410(13) 0.5779(5) 0.127(3) Uani 1 1 d U . . H14A H 0.5865 0.3577 0.6162 0.191 Uiso 1 1 calc R . . H14B H 0.5084 0.4345 0.5554 0.191 Uiso 1 1 calc R . . H14C H 0.5467 0.2744 0.5436 0.191 Uiso 1 1 calc R . . O2A O 0.0970(8) 0.7536(13) 0.3556(5) 0.103 Uiso 0.50 1 d PG A 1 C15A C 0.0407(7) 0.7537(17) 0.2856(6) 0.125 Uiso 0.50 1 d PG A 1 H15A H -0.0050 0.8359 0.2785 0.150 Uiso 0.50 1 calc PR A 1 H15B H 0.0048 0.6609 0.2755 0.150 Uiso 0.50 1 calc PR A 1 C16A C 0.1944(7) 0.743(2) 0.3541(7) 0.135(8) Uiso 0.50 1 d PG A 1 H16A H 0.2259 0.6643 0.3860 0.162 Uiso 0.50 1 calc PR A 1 H16B H 0.2275 0.8364 0.3692 0.162 Uiso 0.50 1 calc PR A 1 C17A C 0.1975(10) 0.709(2) 0.2814(8) 0.147(9) Uiso 0.50 1 d PG A 1 H17A H 0.2013 0.6022 0.2742 0.177 Uiso 0.50 1 calc PR A 1 H17B H 0.2525 0.7571 0.2690 0.177 Uiso 0.50 1 calc PR A 1 C18A C 0.1064(12) 0.770(2) 0.2392(5) 0.117(6) Uiso 0.50 1 d PG A 1 H18A H 0.1135 0.8739 0.2275 0.140 Uiso 0.50 1 calc PR A 1 H18B H 0.0837 0.7135 0.1954 0.140 Uiso 0.50 1 calc PR A 1 O2B O 0.0474(6) 0.8141(11) 0.2818(6) 0.100 Uiso 0.50 1 d PG B 2 C15B C 0.1246(9) 0.8868(12) 0.2632(7) 0.114(6) Uiso 0.50 1 d PG B 2 H15C H 0.1262 0.9912 0.2770 0.137 Uiso 0.50 1 calc PR B 2 H15D H 0.1179 0.8813 0.2120 0.137 Uiso 0.50 1 calc PR B 2 C16B C 0.0816(8) 0.6835(12) 0.3188(7) 0.103(5) Uiso 0.50 1 d PG B 2 H16C H 0.0414 0.5992 0.2986 0.124 Uiso 0.50 1 calc PR B 2 H16D H 0.0805 0.6931 0.3686 0.124 Uiso 0.50 1 calc PR B 2 C17B C 0.1799(9) 0.6615(13) 0.3119(9) 0.127 Uiso 0.50 1 d PG B 2 H17C H 0.1813 0.5972 0.2717 0.152 Uiso 0.50 1 calc PR B 2 H17D H 0.2199 0.6178 0.3550 0.152 Uiso 0.50 1 calc PR B 2 C18B C 0.2124(6) 0.8121(16) 0.3005(8) 0.115(6) Uiso 0.50 1 d PG B 2 H18C H 0.2405 0.8611 0.3456 0.138 Uiso 0.50 1 calc PR B 2 H18D H 0.2600 0.8102 0.2719 0.138 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0547(5) 0.0819(7) 0.0614(5) 0.0273(4) 0.0013(4) -0.0099(4) Cl1 0.0712(9) 0.0732(9) 0.0534(7) -0.0159(6) -0.0174(6) 0.0196(7) P1 0.0809(11) 0.0416(8) 0.0846(11) -0.0051(7) -0.0312(9) 0.0018(7) P2 0.0739(9) 0.0393(7) 0.0478(7) 0.0021(5) 0.0011(6) 0.0002(6) P3 0.0635(9) 0.0745(10) 0.0541(8) 0.0194(7) -0.0009(7) -0.0108(8) P4 0.0602(11) 0.133(2) 0.0985(15) 0.0495(14) -0.0149(10) -0.0351(12) O1 0.147(8) 0.54(3) 0.106(6) -0.037(10) 0.042(6) 0.081(12) C1 0.107(7) 0.217(14) 0.174(10) 0.121(10) -0.064(7) -0.087(8) C2 0.063(5) 0.283(16) 0.061(4) 0.014(7) 0.013(4) 0.007(7) C3 0.062(4) 0.072(4) 0.075(4) -0.023(3) -0.006(3) 0.005(3) C4 0.069(4) 0.062(3) 0.059(3) -0.001(3) 0.012(3) -0.012(3) C5 0.103(5) 0.056(4) 0.071(4) 0.013(3) -0.012(4) 0.008(3) C6 0.109(5) 0.049(3) 0.059(3) -0.011(3) -0.004(3) 0.000(3) C7 0.139(8) 0.085(6) 0.122(7) -0.035(5) -0.065(6) 0.060(5) C8 0.105(6) 0.106(7) 0.126(7) -0.003(6) -0.052(6) 0.019(5) C9 0.078(4) 0.098(5) 0.078(4) 0.030(4) -0.019(3) -0.029(4) C10 0.103(6) 0.191(10) 0.059(4) 0.047(6) -0.001(4) -0.021(7) C11 0.143(8) 0.054(4) 0.130(7) 0.007(4) -0.064(6) -0.032(5) C12 0.131(8) 0.097(7) 0.140(8) 0.015(6) -0.061(6) -0.049(6) C13 0.067(3) 0.194(7) 0.106(4) 0.060(5) -0.007(3) -0.034(4) C14 0.067(3) 0.194(7) 0.106(4) 0.060(5) -0.007(3) -0.034(4) _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 1.843(13) . ? Fe1 C1 2.138(10) . ? Fe1 P1 2.178(2) . ? Fe1 P3 2.2299(17) . ? Fe1 P2 2.2342(17) . ? Fe1 P4 2.246(2) . ? P1 C3 1.784(8) . ? P1 C11 1.826(7) . ? P1 C7 1.841(7) . ? P2 C5 1.817(6) . ? P2 C6 1.836(6) . ? P2 C4 1.843(6) . ? P3 C10 1.789(7) . ? P3 C9 1.804(7) . ? P3 C8 1.820(9) . ? P4 C13 1.800(9) . ? P4 C14 1.842(8) . ? P4 C12 1.855(11) . ? O1 C2 1.038(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C3 C4 1.513(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.487(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.493(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O2A C16A 1.4233 . ? O2A C15A 1.4234 . ? C15A C18A 1.4765 . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.4766 . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A C18A 1.4889 . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? O2B C15B 1.4233 . ? O2B C16B 1.4233 . ? C15B C18B 1.4766 . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17B 1.4766 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B C18B 1.4889 . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? 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 C1 92.3(6) . . ? C2 Fe1 P1 178.1(4) . . ? C1 Fe1 P1 89.3(5) . . ? C2 Fe1 P3 94.6(3) . . ? C1 Fe1 P3 80.5(2) . . ? P1 Fe1 P3 84.76(7) . . ? C2 Fe1 P2 93.0(4) . . ? C1 Fe1 P2 174.1(4) . . ? P1 Fe1 P2 85.27(7) . . ? P3 Fe1 P2 96.51(6) . . ? C2 Fe1 P4 97.5(3) . . ? C1 Fe1 P4 81.7(2) . . ? P1 Fe1 P4 83.61(10) . . ? P3 Fe1 P4 158.77(10) . . ? P2 Fe1 P4 100.14(7) . . ? C3 P1 C11 105.2(4) . . ? C3 P1 C7 103.1(4) . . ? C11 P1 C7 110.0(4) . . ? C3 P1 Fe1 111.6(2) . . ? C11 P1 Fe1 113.0(4) . . ? C7 P1 Fe1 113.1(3) . . ? C5 P2 C6 97.3(3) . . ? C5 P2 C4 99.0(3) . . ? C6 P2 C4 105.6(3) . . ? C5 P2 Fe1 123.6(3) . . ? C6 P2 Fe1 120.8(2) . . ? C4 P2 Fe1 107.5(2) . . ? C10 P3 C9 97.2(4) . . ? C10 P3 C8 102.1(5) . . ? C9 P3 C8 100.0(5) . . ? C10 P3 Fe1 119.8(3) . . ? C9 P3 Fe1 126.1(2) . . ? C8 P3 Fe1 107.8(2) . . ? C13 P4 C14 97.0(4) . . ? C13 P4 C12 101.7(5) . . ? C14 P4 C12 105.0(5) . . ? C13 P4 Fe1 125.2(4) . . ? C14 P4 Fe1 115.9(3) . . ? C12 P4 Fe1 109.5(3) . . ? Fe1 C1 H1A 109.5 . . ? Fe1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Fe1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 Fe1 173.6(15) . . ? C4 C3 P1 109.1(4) . . ? C4 C3 H3A 109.9 . . ? P1 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? P1 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 P2 108.0(4) . . ? C3 C4 H4A 110.1 . . ? P2 C4 H4A 110.1 . . ? C3 C4 H4B 110.1 . . ? P2 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P1 110.5(6) . . ? C8 C7 H7A 109.6 . . ? P1 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? P1 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 P3 113.7(6) . . ? C7 C8 H8A 108.8 . . ? P3 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? P3 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? P3 C9 H9A 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P3 C10 H10A 109.5 . . ? P3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 106.9(5) . . ? C12 C11 H11A 110.3 . . ? P1 C11 H11A 110.3 . . ? C12 C11 H11B 110.3 . . ? P1 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? C11 C12 P4 114.9(6) . . ? C11 C12 H12A 108.5 . . ? P4 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? P4 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? P4 C13 H13A 109.5 . . ? P4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P4 C14 H14A 109.5 . . ? P4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16A O2A C15A 108.8 . . ? O2A C15A C18A 107.1 . . ? O2A C15A H15A 110.3 . . ? C18A C15A H15A 110.3 . . ? O2A C15A H15B 110.3 . . ? C18A C15A H15B 110.3 . . ? H15A C15A H15B 108.6 . . ? O2A C16A C17A 107.1 . . ? O2A C16A H16A 110.3 . . ? C17A C16A H16A 110.3 . . ? O2A C16A H16B 110.3 . . ? C17A C16A H16B 110.3 . . ? H16A C16A H16B 108.5 . . ? C16A C17A C18A 103.6 . . ? C16A C17A H17A 111.0 . . ? C18A C17A H17A 111.0 . . ? C16A C17A H17B 111.0 . . ? C18A C17A H17B 111.0 . . ? H17A C17A H17B 109.0 . . ? C15A C18A C17A 103.6 . . ? C15A C18A H18A 111.0 . . ? C17A C18A H18A 111.0 . . ? C15A C18A H18B 111.0 . . ? C17A C18A H18B 111.0 . . ? H18A C18A H18B 109.0 . . ? C15B O2B C16B 108.8 . . ? O2B C15B C18B 107.1 . . ? O2B C15B H15C 110.3 . . ? C18B C15B H15C 110.3 . . ? O2B C15B H15D 110.3 . . ? C18B C15B H15D 110.3 . . ? H15C C15B H15D 108.6 . . ? O2B C16B C17B 107.1 . . ? O2B C16B H16C 110.3 . . ? C17B C16B H16C 110.3 . . ? O2B C16B H16D 110.3 . . ? C17B C16B H16D 110.3 . . ? H16C C16B H16D 108.6 . . ? C16B C17B C18B 103.6 . . ? C16B C17B H17C 111.0 . . ? C18B C17B H17C 111.0 . . ? C16B C17B H17D 111.0 . . ? C18B C17B H17D 111.0 . . ? H17C C17B H17D 109.0 . . ? C15B C18B C17B 103.6 . . ? C15B C18B H18C 111.0 . . ? C17B C18B H18C 111.0 . . ? C15B C18B H18D 111.0 . . ? C17B C18B H18D 111.0 . . ? H18C C18B H18D 109.0 . . ? 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 C2 Fe1 P1 C3 34(9) . . . . ? C1 Fe1 P1 C3 -174.8(3) . . . . ? P3 Fe1 P1 C3 104.6(2) . . . . ? P2 Fe1 P1 C3 7.6(2) . . . . ? P4 Fe1 P1 C3 -93.2(2) . . . . ? C2 Fe1 P1 C11 152(9) . . . . ? C1 Fe1 P1 C11 -56.5(4) . . . . ? P3 Fe1 P1 C11 -137.0(3) . . . . ? P2 Fe1 P1 C11 126.0(3) . . . . ? P4 Fe1 P1 C11 25.2(3) . . . . ? C2 Fe1 P1 C7 -82(9) . . . . ? C1 Fe1 P1 C7 69.4(5) . . . . ? P3 Fe1 P1 C7 -11.2(4) . . . . ? P2 Fe1 P1 C7 -108.2(4) . . . . ? P4 Fe1 P1 C7 151.1(4) . . . . ? C2 Fe1 P2 C5 82.2(4) . . . . ? C1 Fe1 P2 C5 -123(3) . . . . ? P1 Fe1 P2 C5 -98.7(3) . . . . ? P3 Fe1 P2 C5 177.2(3) . . . . ? P4 Fe1 P2 C5 -16.0(3) . . . . ? C2 Fe1 P2 C6 -42.8(4) . . . . ? C1 Fe1 P2 C6 112(3) . . . . ? P1 Fe1 P2 C6 136.3(3) . . . . ? P3 Fe1 P2 C6 52.2(3) . . . . ? P4 Fe1 P2 C6 -141.0(3) . . . . ? C2 Fe1 P2 C4 -163.9(3) . . . . ? C1 Fe1 P2 C4 -9(3) . . . . ? P1 Fe1 P2 C4 15.3(2) . . . . ? P3 Fe1 P2 C4 -68.9(2) . . . . ? P4 Fe1 P2 C4 97.9(2) . . . . ? C2 Fe1 P3 C10 -42.2(7) . . . . ? C1 Fe1 P3 C10 49.4(7) . . . . ? P1 Fe1 P3 C10 139.6(5) . . . . ? P2 Fe1 P3 C10 -135.8(5) . . . . ? P4 Fe1 P3 C10 82.6(5) . . . . ? C2 Fe1 P3 C9 84.5(6) . . . . ? C1 Fe1 P3 C9 176.1(6) . . . . ? P1 Fe1 P3 C9 -93.7(4) . . . . ? P2 Fe1 P3 C9 -9.1(4) . . . . ? P4 Fe1 P3 C9 -150.6(4) . . . . ? C2 Fe1 P3 C8 -158.1(6) . . . . ? C1 Fe1 P3 C8 -66.5(6) . . . . ? P1 Fe1 P3 C8 23.7(4) . . . . ? P2 Fe1 P3 C8 108.3(4) . . . . ? P4 Fe1 P3 C8 -33.3(5) . . . . ? C2 Fe1 P4 C13 -66.1(6) . . . . ? C1 Fe1 P4 C13 -157.4(6) . . . . ? P1 Fe1 P4 C13 112.3(5) . . . . ? P3 Fe1 P4 C13 169.5(5) . . . . ? P2 Fe1 P4 C13 28.3(5) . . . . ? C2 Fe1 P4 C14 54.4(6) . . . . ? C1 Fe1 P4 C14 -36.8(7) . . . . ? P1 Fe1 P4 C14 -127.1(5) . . . . ? P3 Fe1 P4 C14 -69.9(6) . . . . ? P2 Fe1 P4 C14 148.9(5) . . . . ? C2 Fe1 P4 C12 173.0(5) . . . . ? C1 Fe1 P4 C12 81.7(6) . . . . ? P1 Fe1 P4 C12 -8.6(4) . . . . ? P3 Fe1 P4 C12 48.6(4) . . . . ? P2 Fe1 P4 C12 -92.6(4) . . . . ? C1 Fe1 C2 O1 -21(11) . . . . ? P1 Fe1 C2 O1 130(12) . . . . ? P3 Fe1 C2 O1 60(11) . . . . ? P2 Fe1 C2 O1 157(10) . . . . ? P4 Fe1 C2 O1 -103(10) . . . . ? C11 P1 C3 C4 -157.4(5) . . . . ? C7 P1 C3 C4 87.3(5) . . . . ? Fe1 P1 C3 C4 -34.4(5) . . . . ? P1 C3 C4 P2 46.1(5) . . . . ? C5 P2 C4 C3 89.8(5) . . . . ? C6 P2 C4 C3 -169.9(4) . . . . ? Fe1 P2 C4 C3 -39.7(5) . . . . ? C3 P1 C7 C8 -127.9(7) . . . . ? C11 P1 C7 C8 120.3(8) . . . . ? Fe1 P1 C7 C8 -7.1(9) . . . . ? P1 C7 C8 P3 27.1(10) . . . . ? C10 P3 C8 C7 -163.0(8) . . . . ? C9 P3 C8 C7 97.3(8) . . . . ? Fe1 P3 C8 C7 -35.9(8) . . . . ? C3 P1 C11 C12 83.2(8) . . . . ? C7 P1 C11 C12 -166.3(7) . . . . ? Fe1 P1 C11 C12 -38.8(8) . . . . ? P1 C11 C12 P4 31.0(9) . . . . ? C13 P4 C12 C11 -147.3(7) . . . . ? C14 P4 C12 C11 112.1(7) . . . . ? Fe1 P4 C12 C11 -13.0(8) . . . . ? C16A O2A C15A C18A -10.1 . . . . ? C15A O2A C16A C17A -10.1 . . . . ? O2A C16A C17A C18A 25.8 . . . . ? O2A C15A C18A C17A 25.8 . . . . ? C16A C17A C18A C15A -31.1 . . . . ? C16B O2B C15B C18B -10.1 . . . . ? C15B O2B C16B C17B -10.1 . . . . ? O2B C16B C17B C18B 25.8 . . . . ? O2B C15B C18B C17B 25.8 . . . . ? C16B C17B C18B C15B -31.1 . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.255 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.126