# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rainer Streubel' _publ_contact_author_email R.STREUBEL@UNI-BONN.DE _publ_section_title ; Novel Access to Azaphosphiridine Complexes and first Applications using Bronsted Acid-induced Ring Expansion Reactions ; loop_ _publ_author_name 'Rainer Streubel' 'Victoria Chu' 'Jorg Daniels' 'Stefan Fankel' 'Holger Helten' 'Christina Muller' ; G.Schnakenburg ; 'G von Frantzius' #------------------------------------------------------------------------------ data_greg324 _database_code_depnum_ccdc_archive 'CCDC 695893' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H34 N3 O5 P Si2 W' _chemical_formula_sum 'C23 H34 N3 O5 P Si2 W' _chemical_formula_weight 703.53 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8089(4) _cell_length_b 10.0809(5) _cell_length_c 16.4987(9) _cell_angle_alpha 86.801(2) _cell_angle_beta 87.041(3) _cell_angle_gamma 66.682(3) _cell_volume 1495.07(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 4.032 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.40853 _exptl_absorpt_correction_T_max 0.61286 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _diffrn_reflns_number 17963 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8457 _reflns_number_gt 6849 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 8457 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.002 _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 C1 C 1.2701(3) 0.6205(3) 0.74423(18) 0.0177(7) Uani 1 1 d . . . H1A H 1.3583 0.5776 0.7066 0.021 Uiso 1 1 calc R . . C2 C 1.2399(3) 0.5516(3) 0.88177(19) 0.0188(7) Uani 1 1 d . . . C3 C 1.2826(3) 0.3202(3) 0.71836(19) 0.0187(7) Uani 1 1 d . . . H3A H 1.2101 0.2839 0.6978 0.022 Uiso 1 1 calc R . . C4 C 1.1820(3) 0.7765(3) 0.7188(2) 0.0194(7) Uani 1 1 d . . . C5 C 1.0709(3) 0.8657(3) 0.7710(2) 0.0246(7) Uani 1 1 d . . . H5A H 1.0524 0.8280 0.8225 0.030 Uiso 1 1 calc R . . C6 C 0.9874(3) 1.0088(4) 0.7484(2) 0.0308(8) Uani 1 1 d . . . H6A H 0.9112 1.0681 0.7841 0.037 Uiso 1 1 calc R . . C7 C 1.0148(4) 1.0647(4) 0.6743(2) 0.0340(9) Uani 1 1 d . . . H7A H 0.9571 1.1625 0.6587 0.041 Uiso 1 1 calc R . . C8 C 1.1252(3) 0.9795(4) 0.6229(2) 0.0327(9) Uani 1 1 d . . . H8A H 1.1446 1.0188 0.5721 0.039 Uiso 1 1 calc R . . C9 C 1.2096(3) 0.8349(4) 0.6450(2) 0.0258(8) Uani 1 1 d . . . H9A H 1.2861 0.7766 0.6091 0.031 Uiso 1 1 calc R . . C10 C 1.2401(4) 0.6971(4) 0.9953(2) 0.0375(9) Uani 1 1 d . . . H10A H 1.1360 0.7467 1.0132 0.056 Uiso 1 1 calc R . . H10B H 1.2650 0.7563 0.9528 0.056 Uiso 1 1 calc R . . H10C H 1.3043 0.6820 1.0415 0.056 Uiso 1 1 calc R . . C11 C 1.2051(3) 0.4721(4) 1.0185(2) 0.0295(8) Uani 1 1 d . . . H11A H 1.2252 0.3784 0.9954 0.044 Uiso 1 1 calc R . . H11B H 1.0977 0.5245 1.0268 0.044 Uiso 1 1 calc R . . H11C H 1.2535 0.4567 1.0707 0.044 Uiso 1 1 calc R . . C12 C 1.4776(4) 0.0009(4) 0.7552(2) 0.0397(10) Uani 1 1 d . . . H12A H 1.5598 0.0062 0.7207 0.059 Uiso 1 1 calc R . . H12B H 1.4105 -0.0226 0.7223 0.059 Uiso 1 1 calc R . . H12C H 1.5171 -0.0743 0.7981 0.059 Uiso 1 1 calc R . . C13 C 1.5080(3) 0.2208(4) 0.8623(2) 0.0323(9) Uani 1 1 d . . . H13A H 1.4531 0.2990 0.8990 0.048 Uiso 1 1 calc R . . H13B H 1.5726 0.2509 0.8251 0.048 Uiso 1 1 calc R . . H13C H 1.5686 0.1344 0.8942 0.048 Uiso 1 1 calc R . . C14 C 1.2294(4) 0.1508(4) 0.8714(2) 0.0344(9) Uani 1 1 d . . . H14A H 1.1728 0.1100 0.8411 0.052 Uiso 1 1 calc R . . H14B H 1.1621 0.2436 0.8928 0.052 Uiso 1 1 calc R . . H14C H 1.2779 0.0839 0.9165 0.052 Uiso 1 1 calc R . . C15 C 1.5942(3) 0.2959(4) 0.6489(2) 0.0375(10) Uani 1 1 d . . . H15A H 1.6427 0.2057 0.6809 0.056 Uiso 1 1 calc R . . H15B H 1.5874 0.3779 0.6805 0.056 Uiso 1 1 calc R . . H15C H 1.6526 0.2938 0.5986 0.056 Uiso 1 1 calc R . . C16 C 1.4203(4) 0.1591(4) 0.5614(2) 0.0418(10) Uani 1 1 d . . . H16A H 1.3215 0.1703 0.5453 0.063 Uiso 1 1 calc R . . H16B H 1.4655 0.0687 0.5937 0.063 Uiso 1 1 calc R . . H16C H 1.4829 0.1568 0.5128 0.063 Uiso 1 1 calc R . . C17 C 1.3187(3) 0.4809(4) 0.5560(2) 0.0304(8) Uani 1 1 d . . . H17A H 1.2193 0.5404 0.5774 0.046 Uiso 1 1 calc R . . H17B H 1.3115 0.4523 0.5011 0.046 Uiso 1 1 calc R . . H17C H 1.3813 0.5365 0.5542 0.046 Uiso 1 1 calc R . . C18 C 1.4542(3) 0.6227(4) 0.8440(2) 0.0340(9) Uani 1 1 d . . . H18A H 1.4376 0.7252 0.8388 0.051 Uiso 1 1 calc R . . H18B H 1.5326 0.5682 0.8050 0.051 Uiso 1 1 calc R . . H18C H 1.4846 0.5859 0.8993 0.051 Uiso 1 1 calc R . . C19 C 0.6899(3) 0.6432(3) 0.66476(19) 0.0196(7) Uani 1 1 d . . . C20 C 0.8312(3) 0.7170(3) 0.7969(2) 0.0206(7) Uani 1 1 d . . . C21 C 0.8750(3) 0.4269(3) 0.76921(19) 0.0201(7) Uani 1 1 d . . . C22 C 0.9755(3) 0.4488(3) 0.6067(2) 0.0196(7) Uani 1 1 d . . . C23 C 0.8965(3) 0.7596(3) 0.6254(2) 0.0210(7) Uani 1 1 d . . . N1 N 1.3177(3) 0.6060(3) 0.82767(16) 0.0201(6) Uani 1 1 d . . . N2 N 1.1516(2) 0.4969(3) 0.85522(15) 0.0174(6) Uani 1 1 d . . . N3 N 1.2627(3) 0.5561(3) 0.96305(16) 0.0242(6) Uani 1 1 d . . . O1 O 0.5707(2) 0.6725(3) 0.64428(14) 0.0316(6) Uani 1 1 d . . . O2 O 0.7943(2) 0.7860(3) 0.85329(14) 0.0307(6) Uani 1 1 d . . . O3 O 0.8519(2) 0.3387(2) 0.80801(14) 0.0310(6) Uani 1 1 d . . . O4 O 1.0183(2) 0.3669(2) 0.55670(14) 0.0291(6) Uani 1 1 d . . . O5 O 0.8810(2) 0.8580(3) 0.58313(15) 0.0343(6) Uani 1 1 d . . . P P 1.15790(8) 0.50168(9) 0.75198(5) 0.01566(17) Uani 1 1 d . . . Si1 Si 1.37346(9) 0.17903(10) 0.80231(6) 0.0257(2) Uani 1 1 d . . . Si2 Si 1.40322(9) 0.31511(10) 0.62365(6) 0.0244(2) Uani 1 1 d . . . W W 0.898163(12) 0.587704(14) 0.699294(8) 0.01623(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0175(14) 0.0248(18) 0.0147(16) 0.0002(14) -0.0025(12) -0.0122(13) C2 0.0192(15) 0.0165(17) 0.0187(17) 0.0027(13) -0.0051(12) -0.0047(13) C3 0.0173(14) 0.0185(17) 0.0212(18) -0.0026(14) -0.0036(12) -0.0073(12) C4 0.0162(15) 0.0186(17) 0.0258(19) 0.0032(14) -0.0075(13) -0.0092(13) C5 0.0278(17) 0.0210(19) 0.029(2) -0.0013(15) -0.0014(14) -0.0134(14) C6 0.0280(18) 0.023(2) 0.042(2) -0.0086(17) -0.0015(16) -0.0089(15) C7 0.0315(19) 0.022(2) 0.049(3) 0.0052(18) -0.0116(18) -0.0115(16) C8 0.0336(19) 0.037(2) 0.035(2) 0.0177(18) -0.0136(16) -0.0237(17) C9 0.0211(16) 0.031(2) 0.028(2) 0.0015(16) -0.0023(14) -0.0133(15) C10 0.055(2) 0.044(3) 0.023(2) -0.0056(18) -0.0021(17) -0.029(2) C11 0.0349(19) 0.047(2) 0.0157(18) 0.0045(16) -0.0049(14) -0.0259(17) C12 0.038(2) 0.021(2) 0.055(3) -0.0029(19) -0.0144(19) -0.0045(16) C13 0.0278(18) 0.031(2) 0.036(2) 0.0025(17) -0.0138(16) -0.0093(15) C14 0.042(2) 0.035(2) 0.032(2) 0.0108(18) -0.0126(17) -0.0217(17) C15 0.0215(17) 0.045(2) 0.044(3) -0.001(2) -0.0001(16) -0.0114(16) C16 0.047(2) 0.040(3) 0.037(2) -0.016(2) 0.0062(18) -0.0158(19) C17 0.0316(18) 0.039(2) 0.0165(18) -0.0049(16) 0.0062(14) -0.0096(16) C18 0.0310(19) 0.051(3) 0.029(2) 0.0049(19) -0.0083(16) -0.0265(18) C19 0.0221(16) 0.0203(18) 0.0172(17) -0.0003(14) 0.0018(13) -0.0094(13) C20 0.0158(15) 0.0204(18) 0.0235(19) 0.0021(15) -0.0015(13) -0.0052(13) C21 0.0162(15) 0.0239(19) 0.0186(18) -0.0058(14) 0.0011(12) -0.0058(13) C22 0.0173(15) 0.0204(18) 0.0215(18) 0.0049(15) -0.0045(13) -0.0083(13) C23 0.0166(15) 0.0249(19) 0.0227(19) -0.0049(15) -0.0062(13) -0.0084(13) N1 0.0187(13) 0.0302(16) 0.0165(14) 0.0013(12) -0.0052(10) -0.0147(11) N2 0.0166(12) 0.0219(15) 0.0148(14) -0.0002(11) -0.0037(10) -0.0085(11) N3 0.0305(15) 0.0321(18) 0.0149(15) 0.0018(13) -0.0055(12) -0.0176(13) O1 0.0201(11) 0.0456(16) 0.0280(15) -0.0008(12) -0.0049(10) -0.0114(11) O2 0.0334(13) 0.0313(15) 0.0242(14) -0.0071(12) 0.0025(11) -0.0091(11) O3 0.0425(14) 0.0261(14) 0.0258(14) -0.0007(11) 0.0081(11) -0.0162(11) O4 0.0382(13) 0.0273(14) 0.0200(14) -0.0074(11) 0.0016(11) -0.0106(11) O5 0.0434(14) 0.0316(15) 0.0327(16) 0.0114(12) -0.0130(12) -0.0200(12) P 0.0166(4) 0.0172(4) 0.0140(4) 0.0003(3) -0.0017(3) -0.0075(3) Si1 0.0246(5) 0.0205(5) 0.0315(6) 0.0032(4) -0.0110(4) -0.0078(4) Si2 0.0194(4) 0.0273(6) 0.0246(5) -0.0069(4) 0.0016(4) -0.0067(4) W 0.01471(6) 0.01997(7) 0.01382(6) -0.00032(5) -0.00120(4) -0.00657(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 C1 N1 1.458(4) . ? C1 C4 1.511(4) . ? C1 P 1.917(3) . ? C1 H1A 1.0000 . ? C2 N2 1.300(4) . ? C2 N1 1.373(4) . ? C2 N3 1.377(4) . ? C3 P 1.850(3) . ? C3 Si2 1.901(3) . ? C3 Si1 1.908(3) . ? C3 H3A 1.0000 . ? C4 C9 1.383(4) . ? C4 C5 1.397(4) . ? C5 C6 1.387(4) . ? C5 H5A 0.9500 . ? C6 C7 1.377(5) . ? C6 H6A 0.9500 . ? C7 C8 1.371(5) . ? C7 H7A 0.9500 . ? C8 C9 1.400(4) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 N3 1.476(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.453(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.869(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.876(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.869(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si2 1.872(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.873(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.875(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N1 1.455(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O1 1.152(3) . ? C19 W 1.998(3) . ? C20 O2 1.148(4) . ? C20 W 2.042(3) . ? C21 O3 1.155(4) . ? C21 W 2.016(3) . ? C22 O4 1.142(4) . ? C22 W 2.037(3) . ? C23 O5 1.144(4) . ? C23 W 2.057(3) . ? N2 P 1.700(3) . ? P W 2.5286(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C4 111.8(3) . . ? N1 C1 P 100.1(2) . . ? C4 C1 P 114.57(19) . . ? N1 C1 H1A 110.0 . . ? C4 C1 H1A 110.0 . . ? P C1 H1A 110.0 . . ? N2 C2 N1 119.9(3) . . ? N2 C2 N3 123.1(3) . . ? N1 C2 N3 117.0(3) . . ? P C3 Si2 116.22(16) . . ? P C3 Si1 116.14(16) . . ? Si2 C3 Si1 115.98(14) . . ? P C3 H3A 101.5 . . ? Si2 C3 H3A 101.5 . . ? Si1 C3 H3A 101.5 . . ? C9 C4 C5 118.6(3) . . ? C9 C4 C1 121.7(3) . . ? C5 C4 C1 119.7(3) . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C4 C9 C8 120.3(3) . . ? C4 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 W 178.6(3) . . ? O2 C20 W 177.9(3) . . ? O3 C21 W 175.5(3) . . ? O4 C22 W 177.4(3) . . ? O5 C23 W 173.1(2) . . ? C2 N1 C18 125.6(3) . . ? C2 N1 C1 114.0(2) . . ? C18 N1 C1 119.3(3) . . ? C2 N2 P 110.1(2) . . ? C2 N3 C11 116.3(3) . . ? C2 N3 C10 117.8(3) . . ? C11 N3 C10 112.3(3) . . ? N2 P C3 108.04(13) . . ? N2 P C1 93.22(13) . . ? C3 P C1 107.32(13) . . ? N2 P W 110.05(8) . . ? C3 P W 113.64(10) . . ? C1 P W 122.17(10) . . ? C12 Si1 C14 105.14(17) . . ? C12 Si1 C13 107.65(15) . . ? C14 Si1 C13 110.43(16) . . ? C12 Si1 C3 108.66(16) . . ? C14 Si1 C3 110.68(14) . . ? C13 Si1 C3 113.84(15) . . ? C15 Si2 C16 108.43(16) . . ? C15 Si2 C17 108.50(16) . . ? C16 Si2 C17 105.83(17) . . ? C15 Si2 C3 112.06(15) . . ? C16 Si2 C3 109.80(16) . . ? C17 Si2 C3 111.98(13) . . ? C19 W C21 88.11(12) . . ? C19 W C22 90.36(12) . . ? C21 W C22 88.82(12) . . ? C19 W C20 92.62(12) . . ? C21 W C20 88.91(12) . . ? C22 W C20 176.19(12) . . ? C19 W C23 85.42(12) . . ? C21 W C23 173.48(11) . . ? C22 W C23 92.01(12) . . ? C20 W C23 90.59(13) . . ? C19 W P 174.93(9) . . ? C21 W P 86.86(8) . . ? C22 W P 90.18(8) . . ? C20 W P 86.64(8) . . ? C23 W P 99.61(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C4 C9 133.9(3) . . . . ? P C1 C4 C9 -113.2(3) . . . . ? N1 C1 C4 C5 -45.3(4) . . . . ? P C1 C4 C5 67.7(3) . . . . ? C9 C4 C5 C6 1.7(5) . . . . ? C1 C4 C5 C6 -179.2(3) . . . . ? C4 C5 C6 C7 -0.8(5) . . . . ? C5 C6 C7 C8 -0.4(5) . . . . ? C6 C7 C8 C9 0.7(5) . . . . ? C5 C4 C9 C8 -1.4(5) . . . . ? C1 C4 C9 C8 179.5(3) . . . . ? C7 C8 C9 C4 0.2(5) . . . . ? N2 C2 N1 C18 -157.0(3) . . . . ? N3 C2 N1 C18 21.8(5) . . . . ? N2 C2 N1 C1 11.0(4) . . . . ? N3 C2 N1 C1 -170.1(3) . . . . ? C4 C1 N1 C2 105.9(3) . . . . ? P C1 N1 C2 -15.8(3) . . . . ? C4 C1 N1 C18 -85.2(3) . . . . ? P C1 N1 C18 153.1(2) . . . . ? N1 C2 N2 P 1.8(3) . . . . ? N3 C2 N2 P -177.0(2) . . . . ? N2 C2 N3 C11 11.3(4) . . . . ? N1 C2 N3 C11 -167.5(3) . . . . ? N2 C2 N3 C10 -126.5(3) . . . . ? N1 C2 N3 C10 54.7(4) . . . . ? C2 N2 P C3 99.5(2) . . . . ? C2 N2 P C1 -9.9(2) . . . . ? C2 N2 P W -135.90(18) . . . . ? Si2 C3 P N2 -143.06(15) . . . . ? Si1 C3 P N2 -1.3(2) . . . . ? Si2 C3 P C1 -43.66(19) . . . . ? Si1 C3 P C1 98.13(18) . . . . ? Si2 C3 P W 94.52(15) . . . . ? Si1 C3 P W -123.69(13) . . . . ? N1 C1 P N2 14.25(19) . . . . ? C4 C1 P N2 -105.5(2) . . . . ? N1 C1 P C3 -95.8(2) . . . . ? C4 C1 P C3 144.5(2) . . . . ? N1 C1 P W 130.41(15) . . . . ? C4 C1 P W 10.6(3) . . . . ? P C3 Si1 C12 174.17(17) . . . . ? Si2 C3 Si1 C12 -43.9(2) . . . . ? P C3 Si1 C14 59.2(2) . . . . ? Si2 C3 Si1 C14 -158.92(17) . . . . ? P C3 Si1 C13 -65.9(2) . . . . ? Si2 C3 Si1 C13 76.0(2) . . . . ? P C3 Si2 C15 96.51(19) . . . . ? Si1 C3 Si2 C15 -45.3(2) . . . . ? P C3 Si2 C16 -142.93(18) . . . . ? Si1 C3 Si2 C16 75.2(2) . . . . ? P C3 Si2 C17 -25.7(2) . . . . ? Si1 C3 Si2 C17 -167.53(16) . . . . ? O1 C19 W C21 -58(12) . . . . ? O1 C19 W C22 31(12) . . . . ? O1 C19 W C20 -147(12) . . . . ? O1 C19 W C23 123(12) . . . . ? O1 C19 W P -65(12) . . . . ? O3 C21 W C19 -8(4) . . . . ? O3 C21 W C22 -98(4) . . . . ? O3 C21 W C20 85(4) . . . . ? O3 C21 W C23 -1(4) . . . . ? O3 C21 W P 172(4) . . . . ? O4 C22 W C19 -91(6) . . . . ? O4 C22 W C21 -3(6) . . . . ? O4 C22 W C20 51(6) . . . . ? O4 C22 W C23 -176(100) . . . . ? O4 C22 W P 84(6) . . . . ? O2 C20 W C19 104(7) . . . . ? O2 C20 W C21 16(7) . . . . ? O2 C20 W C22 -37(8) . . . . ? O2 C20 W C23 -170(7) . . . . ? O2 C20 W P -71(7) . . . . ? O5 C23 W C19 4(2) . . . . ? O5 C23 W C21 -3(3) . . . . ? O5 C23 W C22 94(2) . . . . ? O5 C23 W C20 -89(2) . . . . ? O5 C23 W P -175(2) . . . . ? N2 P W C19 -47.4(10) . . . . ? C3 P W C19 73.9(10) . . . . ? C1 P W C19 -154.9(10) . . . . ? N2 P W C21 -54.74(13) . . . . ? C3 P W C21 66.57(14) . . . . ? C1 P W C21 -162.20(14) . . . . ? N2 P W C22 -143.54(13) . . . . ? C3 P W C22 -22.24(14) . . . . ? C1 P W C22 109.00(14) . . . . ? N2 P W C20 34.36(13) . . . . ? C3 P W C20 155.66(14) . . . . ? C1 P W C20 -73.10(15) . . . . ? N2 P W C23 124.39(13) . . . . ? C3 P W C23 -114.31(14) . . . . ? C1 P W C23 16.93(15) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.501 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.141 # Attachment 'Dalton-09-SF-HH-GvF-RS.cif' data_greg177 _database_code_depnum_ccdc_archive 'CCDC 743280' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Fe N O5 P Si2 W' _chemical_formula_weight 741.36 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 14.5415(2) _cell_length_b 16.5338(2) _cell_length_c 19.5865(2) _cell_angle_alpha 109.0050(7) _cell_angle_beta 90.3535(6) _cell_angle_gamma 97.4184(6) _cell_volume 4409.30(9) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14841 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 4.572 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.48284 _exptl_absorpt_correction_T_max 0.67580 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _diffrn_reflns_number 49604 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.1728 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 29.00 _reflns_number_total 22997 _reflns_number_gt 12350 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 22997 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 0.744 _refine_ls_restrained_S_all 0.744 _refine_ls_shift/su_max 0.002 _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 C1 C 0.2760(4) -0.0498(4) 0.4597(3) 0.0184(13) Uani 1 1 d . . . H1A H 0.3239 -0.0020 0.4893 0.022 Uiso 1 1 calc R . . C2 C 0.2168(4) -0.0930(3) 0.5021(3) 0.0153(12) Uani 1 1 d . . . C3 C 0.2454(4) -0.1047(4) 0.5682(3) 0.0237(14) Uani 1 1 d . . . H3A H 0.3059 -0.0886 0.5911 0.028 Uiso 1 1 calc R . . C4 C 0.1663(5) -0.1449(4) 0.5929(3) 0.0317(17) Uani 1 1 d . . . H4A H 0.1647 -0.1598 0.6358 0.038 Uiso 1 1 calc R . . C5 C 0.0902(4) -0.1589(4) 0.5431(3) 0.0250(15) Uani 1 1 d . . . H5A H 0.0291 -0.1852 0.5464 0.030 Uiso 1 1 calc R . . C6 C 0.1215(4) -0.1266(4) 0.4874(3) 0.0222(14) Uani 1 1 d . . . H6A H 0.0847 -0.1274 0.4469 0.027 Uiso 1 1 calc R . . C7 C 0.0873(5) 0.0748(4) 0.5792(3) 0.0308(16) Uani 1 1 d . . . H7A H 0.0678 0.0828 0.5358 0.037 Uiso 1 1 calc R . . C8 C 0.0311(4) 0.0369(4) 0.6204(3) 0.0324(17) Uani 1 1 d . . . H8A H -0.0330 0.0153 0.6101 0.039 Uiso 1 1 calc R . . C9 C 0.0852(5) 0.0357(5) 0.6803(3) 0.043(2) Uani 1 1 d . . . H9A H 0.0647 0.0128 0.7171 0.051 Uiso 1 1 calc R . . C10 C 0.1770(5) 0.0758(4) 0.6746(3) 0.0408(19) Uani 1 1 d . . . H10A H 0.2284 0.0846 0.7075 0.049 Uiso 1 1 calc R . . C11 C 0.1778(5) 0.0998(4) 0.6116(3) 0.0356(18) Uani 1 1 d . . . H11A H 0.2295 0.1274 0.5944 0.043 Uiso 1 1 calc R . . C12 C 0.2383(4) 0.0621(4) 0.4069(3) 0.0281(16) Uani 1 1 d . . . H12C H 0.2029 0.0685 0.3667 0.042 Uiso 1 1 calc R . . H12B H 0.3044 0.0815 0.4041 0.042 Uiso 1 1 calc R . . H12A H 0.2162 0.0971 0.4528 0.042 Uiso 1 1 calc R . . C13 C 0.2359(4) -0.2040(3) 0.3303(3) 0.0197(14) Uani 1 1 d . . . H13A H 0.1902 -0.2008 0.3687 0.024 Uiso 1 1 calc R . . C14 C 0.0365(4) -0.2581(4) 0.2713(3) 0.0378(17) Uani 1 1 d . . . H14A H 0.0179 -0.2131 0.3134 0.057 Uiso 1 1 calc R . . H14B H 0.0365 -0.3115 0.2827 0.057 Uiso 1 1 calc R . . H14C H -0.0074 -0.2684 0.2302 0.057 Uiso 1 1 calc R . . C15 C 0.1557(4) -0.1195(4) 0.2267(3) 0.0306(16) Uani 1 1 d . . . H15A H 0.2189 -0.0988 0.2171 0.046 Uiso 1 1 calc R . . H15B H 0.1337 -0.0758 0.2680 0.046 Uiso 1 1 calc R . . H15C H 0.1145 -0.1302 0.1839 0.046 Uiso 1 1 calc R . . C16 C 0.1851(5) -0.3101(4) 0.1651(3) 0.0357(17) Uani 1 1 d . . . H16A H 0.1803 -0.3647 0.1754 0.054 Uiso 1 1 calc R . . H16B H 0.2486 -0.2950 0.1525 0.054 Uiso 1 1 calc R . . H16C H 0.1416 -0.3165 0.1247 0.054 Uiso 1 1 calc R . . C17 C 0.3794(4) -0.3344(4) 0.2622(3) 0.0330(16) Uani 1 1 d . . . H17A H 0.4273 -0.2860 0.2645 0.050 Uiso 1 1 calc R . . H17B H 0.3458 -0.3548 0.2149 0.050 Uiso 1 1 calc R . . H17C H 0.4086 -0.3815 0.2693 0.050 Uiso 1 1 calc R . . C18 C 0.2032(5) -0.3892(4) 0.3282(3) 0.0446(19) Uani 1 1 d . . . H18A H 0.1669 -0.4049 0.2823 0.067 Uiso 1 1 calc R . . H18B H 0.1624 -0.3714 0.3685 0.067 Uiso 1 1 calc R . . H18C H 0.2311 -0.4392 0.3306 0.067 Uiso 1 1 calc R . . C19 C 0.3596(4) -0.2691(4) 0.4234(3) 0.0324(16) Uani 1 1 d . . . H19A H 0.3152 -0.2574 0.4617 0.049 Uiso 1 1 calc R . . H19B H 0.4051 -0.2175 0.4307 0.049 Uiso 1 1 calc R . . H19C H 0.3917 -0.3171 0.4250 0.049 Uiso 1 1 calc R . . C20 C 0.5709(4) -0.0058(4) 0.2823(3) 0.0234(14) Uani 1 1 d . . . C21 C 0.5257(4) -0.1341(4) 0.3433(3) 0.0267(15) Uani 1 1 d . . . C22 C 0.4829(4) 0.0351(4) 0.4188(3) 0.0263(15) Uani 1 1 d . . . C23 C 0.3928(4) 0.0381(4) 0.2855(3) 0.0246(14) Uani 1 1 d . . . C24 C 0.4190(4) -0.1371(4) 0.2151(3) 0.0262(15) Uani 1 1 d . . . C25 C 0.2091(4) 0.1973(4) 1.1104(3) 0.0211(14) Uani 1 1 d . . . H25A H 0.2306 0.1499 1.1249 0.025 Uiso 1 1 calc R . . C26 C 0.1885(4) 0.2714(4) 1.1719(3) 0.0208(14) Uani 1 1 d . . . C27 C 0.2389(4) 0.3049(4) 1.2404(3) 0.0248(15) Uani 1 1 d . . . H27A H 0.2910 0.2830 1.2536 0.030 Uiso 1 1 calc R . . C28 C 0.1992(4) 0.3753(4) 1.2853(3) 0.0266(15) Uani 1 1 d . . . H28A H 0.2203 0.4094 1.3333 0.032 Uiso 1 1 calc R . . C29 C 0.1226(4) 0.3865(4) 1.2467(3) 0.0250(15) Uani 1 1 d . . . H29A H 0.0829 0.4293 1.2643 0.030 Uiso 1 1 calc R . . C30 C 0.1146(4) 0.3225(3) 1.1763(3) 0.0194(13) Uani 1 1 d . . . H30A H 0.0687 0.3152 1.1393 0.023 Uiso 1 1 calc R . . C31 C 0.0145(4) 0.1530(4) 1.2288(3) 0.0309(16) Uani 1 1 d . . . H31A H -0.0060 0.1169 1.1812 0.037 Uiso 1 1 calc R . . C32 C 0.0931(4) 0.1465(4) 1.2685(3) 0.0310(16) Uani 1 1 d . . . H32A H 0.1350 0.1054 1.2524 0.037 Uiso 1 1 calc R . . C33 C 0.0980(4) 0.2120(4) 1.3364(3) 0.0313(16) Uani 1 1 d . . . H33A H 0.1437 0.2217 1.3741 0.038 Uiso 1 1 calc R . . C34 C 0.0249(4) 0.2606(4) 1.3395(3) 0.0282(16) Uani 1 1 d . . . H34A H 0.0133 0.3093 1.3787 0.034 Uiso 1 1 calc R . . C35 C -0.0286(4) 0.2235(4) 1.2731(3) 0.0299(16) Uani 1 1 d . . . H35A H -0.0833 0.2422 1.2603 0.036 Uiso 1 1 calc R . . C36 C 0.1024(4) 0.0761(4) 1.0244(3) 0.0298(15) Uani 1 1 d . . . H36C H 0.0593 0.0636 0.9824 0.045 Uiso 1 1 calc R . . H36B H 0.0686 0.0644 1.0641 0.045 Uiso 1 1 calc R . . H36A H 0.1517 0.0395 1.0114 0.045 Uiso 1 1 calc R . . C37 C 0.2396(4) 0.3065(3) 1.0163(3) 0.0165(13) Uani 1 1 d . . . H37A H 0.1987 0.3300 1.0568 0.020 Uiso 1 1 calc R . . C38 C 0.0751(4) 0.3747(4) 0.9707(3) 0.0318(16) Uani 1 1 d . . . H38A H 0.1049 0.4336 0.9967 0.048 Uiso 1 1 calc R . . H38B H 0.0379 0.3523 1.0039 0.048 Uiso 1 1 calc R . . H38C H 0.0347 0.3753 0.9307 0.048 Uiso 1 1 calc R . . C39 C 0.2317(4) 0.3458(4) 0.8691(3) 0.0363(18) Uani 1 1 d . . . H39A H 0.2819 0.3114 0.8512 0.054 Uiso 1 1 calc R . . H39B H 0.2580 0.4062 0.8932 0.054 Uiso 1 1 calc R . . H39C H 0.1898 0.3418 0.8284 0.054 Uiso 1 1 calc R . . C40 C 0.1086(4) 0.1923(4) 0.8838(3) 0.0303(16) Uani 1 1 d . . . H40A H 0.0683 0.1708 0.9158 0.045 Uiso 1 1 calc R . . H40B H 0.1560 0.1543 0.8667 0.045 Uiso 1 1 calc R . . H40C H 0.0713 0.1933 0.8423 0.045 Uiso 1 1 calc R . . C41 C 0.4421(4) 0.3737(4) 0.9762(3) 0.0351(17) Uani 1 1 d . . . H41A H 0.4173 0.3760 0.9303 0.053 Uiso 1 1 calc R . . H41B H 0.4624 0.3173 0.9684 0.053 Uiso 1 1 calc R . . H41C H 0.4950 0.4193 0.9946 0.053 Uiso 1 1 calc R . . C42 C 0.3999(4) 0.3891(4) 1.1306(3) 0.0341(16) Uani 1 1 d . . . H42A H 0.4156 0.3315 1.1249 0.051 Uiso 1 1 calc R . . H42B H 0.3545 0.4039 1.1680 0.051 Uiso 1 1 calc R . . H42C H 0.4561 0.4315 1.1450 0.051 Uiso 1 1 calc R . . C43 C 0.3139(5) 0.4988(4) 1.0594(3) 0.0373(18) Uani 1 1 d . . . H43A H 0.2708 0.5107 1.0986 0.056 Uiso 1 1 calc R . . H43B H 0.2833 0.5001 1.0151 0.056 Uiso 1 1 calc R . . H43C H 0.3690 0.5427 1.0728 0.056 Uiso 1 1 calc R . . C44 C 0.4320(5) 0.0101(4) 0.9002(3) 0.0332(17) Uani 1 1 d . . . C45 C 0.2437(4) 0.0234(4) 0.8907(3) 0.0226(14) Uani 1 1 d . . . C46 C 0.3398(4) 0.0410(4) 1.0317(3) 0.0289(15) Uani 1 1 d . . . C47 C 0.4740(5) 0.1737(4) 1.0104(3) 0.0261(15) Uani 1 1 d . . . C48 C 0.3697(4) 0.1571(4) 0.8765(3) 0.0222(14) Uani 1 1 d . . . C49 C 0.6956(4) 0.3284(3) 0.2027(3) 0.0184(13) Uani 1 1 d . . . H49A H 0.6429 0.2870 0.1725 0.022 Uiso 1 1 calc R . . C50 C 0.7634(4) 0.3662(4) 0.1607(3) 0.0214(14) Uani 1 1 d . . . C51 C 0.7421(4) 0.3847(4) 0.0952(3) 0.0265(15) Uani 1 1 d . . . H51A H 0.6822 0.3785 0.0729 0.032 Uiso 1 1 calc R . . C52 C 0.8280(5) 0.4139(4) 0.0709(3) 0.0314(17) Uani 1 1 d . . . H52A H 0.8349 0.4306 0.0290 0.038 Uiso 1 1 calc R . . C53 C 0.9011(5) 0.4141(4) 0.1183(3) 0.0284(16) Uani 1 1 d . . . H53A H 0.9651 0.4313 0.1142 0.034 Uiso 1 1 calc R . . C54 C 0.8616(4) 0.3839(4) 0.1737(3) 0.0224(14) Uani 1 1 d . . . H54A H 0.8953 0.3769 0.2127 0.027 Uiso 1 1 calc R . . C55 C 0.7645(4) 0.1688(4) 0.0539(3) 0.0223(14) Uani 1 1 d . . . H55A H 0.7102 0.1525 0.0756 0.027 Uiso 1 1 calc R . . C56 C 0.7671(4) 0.1899(4) -0.0103(3) 0.0268(15) Uani 1 1 d . . . H56A H 0.7147 0.1896 -0.0397 0.032 Uiso 1 1 calc R . . C57 C 0.8606(5) 0.2115(4) -0.0233(3) 0.0314(17) Uani 1 1 d . . . H57A H 0.8828 0.2288 -0.0626 0.038 Uiso 1 1 calc R . . C58 C 0.9156(5) 0.2026(4) 0.0331(3) 0.0297(16) Uani 1 1 d . . . H58A H 0.9815 0.2128 0.0383 0.036 Uiso 1 1 calc R . . C59 C 0.8556(4) 0.1760(4) 0.0800(3) 0.0250(15) Uani 1 1 d . . . H59A H 0.8740 0.1649 0.1223 0.030 Uiso 1 1 calc R . . C60 C 0.7097(4) 0.2069(4) 0.2497(3) 0.0273(15) Uani 1 1 d . . . H60C H 0.7418 0.1933 0.2879 0.041 Uiso 1 1 calc R . . H60B H 0.7262 0.1701 0.2024 0.041 Uiso 1 1 calc R . . H60A H 0.6425 0.1965 0.2540 0.041 Uiso 1 1 calc R . . C61 C 0.7516(4) 0.4752(3) 0.3355(3) 0.0179(13) Uani 1 1 d . . . H61A H 0.7980 0.4686 0.2972 0.021 Uiso 1 1 calc R . . C62 C 0.8091(4) 0.3760(4) 0.4369(3) 0.0329(16) Uani 1 1 d . . . H62A H 0.8246 0.3293 0.3948 0.049 Uiso 1 1 calc R . . H62B H 0.7439 0.3635 0.4473 0.049 Uiso 1 1 calc R . . H62C H 0.8491 0.3807 0.4788 0.049 Uiso 1 1 calc R . . C63 C 0.8111(5) 0.5688(4) 0.5016(3) 0.0389(18) Uani 1 1 d . . . H63A H 0.7464 0.5621 0.5148 0.058 Uiso 1 1 calc R . . H63B H 0.8263 0.6245 0.4938 0.058 Uiso 1 1 calc R . . H63C H 0.8521 0.5667 0.5407 0.058 Uiso 1 1 calc R . . C64 C 0.9504(4) 0.4999(4) 0.3923(3) 0.0364(17) Uani 1 1 d . . . H64A H 0.9606 0.5545 0.3821 0.055 Uiso 1 1 calc R . . H64B H 0.9622 0.4525 0.3493 0.055 Uiso 1 1 calc R . . H64C H 0.9927 0.5030 0.4326 0.055 Uiso 1 1 calc R . . C65 C 0.6374(4) 0.5528(4) 0.2480(3) 0.0276(15) Uani 1 1 d . . . H65A H 0.5857 0.5068 0.2440 0.041 Uiso 1 1 calc R . . H65B H 0.6780 0.5337 0.2078 0.041 Uiso 1 1 calc R . . H65C H 0.6129 0.6047 0.2463 0.041 Uiso 1 1 calc R . . C66 C 0.6300(4) 0.6237(4) 0.4110(3) 0.0316(16) Uani 1 1 d . . . H66A H 0.6659 0.6387 0.4570 0.047 Uiso 1 1 calc R . . H66B H 0.5762 0.5808 0.4097 0.047 Uiso 1 1 calc R . . H66C H 0.6087 0.6756 0.4063 0.047 Uiso 1 1 calc R . . C67 C 0.8089(5) 0.6588(4) 0.3388(3) 0.0408(18) Uani 1 1 d . . . H67C H 0.7888 0.7129 0.3383 0.061 Uiso 1 1 calc R . . H67B H 0.8459 0.6364 0.2968 0.061 Uiso 1 1 calc R . . H67A H 0.8467 0.6694 0.3832 0.061 Uiso 1 1 calc R . . C68 C 0.3983(4) 0.3037(4) 0.3824(3) 0.0236(14) Uani 1 1 d . . . C69 C 0.4568(4) 0.4383(4) 0.3291(3) 0.0207(14) Uani 1 1 d . . . C70 C 0.5641(4) 0.4208(4) 0.4482(3) 0.0231(14) Uani 1 1 d . . . C71 C 0.5651(4) 0.2441(4) 0.3722(3) 0.0216(14) Uani 1 1 d . . . C72 C 0.4745(4) 0.2593(4) 0.2433(3) 0.0254(15) Uani 1 1 d . . . Fe1 Fe 0.13953(6) -0.03059(6) 0.58538(4) 0.0231(2) Uani 1 1 d . . . Fe2 Fe 0.10496(6) 0.26538(5) 1.25550(4) 0.0192(2) Uani 1 1 d . . . Fe3 Fe 0.82802(6) 0.29191(5) 0.07511(4) 0.0196(2) Uani 1 1 d . . . N1 N 0.2255(3) -0.0293(3) 0.4025(2) 0.0208(12) Uani 1 1 d . . . N2 N 0.1431(3) 0.1665(3) 1.0472(2) 0.0197(11) Uani 1 1 d . . . N3 N 0.7379(3) 0.2982(3) 0.2570(2) 0.0196(11) Uani 1 1 d . . . O1 O 0.6400(3) 0.0205(3) 0.26285(19) 0.0293(11) Uani 1 1 d . . . O2 O 0.5731(3) -0.1773(3) 0.3573(2) 0.0437(13) Uani 1 1 d . . . O3 O 0.4990(3) 0.0827(3) 0.4767(2) 0.0401(12) Uani 1 1 d . . . O4 O 0.3624(3) 0.0872(3) 0.2655(2) 0.0392(13) Uani 1 1 d . . . O5 O 0.4015(3) -0.1822(3) 0.1573(2) 0.0381(12) Uani 1 1 d . . . O6 O 0.4747(3) -0.0438(3) 0.8672(2) 0.0531(15) Uani 1 1 d . . . O7 O 0.1848(3) -0.0187(3) 0.8515(2) 0.0356(11) Uani 1 1 d . . . O8 O 0.3303(3) 0.0081(3) 1.0759(2) 0.0444(13) Uani 1 1 d . . . O9 O 0.5406(3) 0.2116(3) 1.0396(2) 0.0432(13) Uani 1 1 d . . . O10 O 0.3779(3) 0.1866(3) 0.8316(2) 0.0365(12) Uani 1 1 d . . . O11 O 0.3284(3) 0.2762(3) 0.4015(2) 0.0369(12) Uani 1 1 d . . . O12 O 0.4185(3) 0.4916(3) 0.3220(2) 0.0338(11) Uani 1 1 d . . . O13 O 0.5892(3) 0.4605(3) 0.5056(2) 0.0339(11) Uani 1 1 d . . . O14 O 0.5853(3) 0.1892(3) 0.3897(2) 0.0328(11) Uani 1 1 d . . . O15 O 0.4510(3) 0.2147(3) 0.1870(2) 0.0288(11) Uani 1 1 d . . . P1 P 0.30477(11) -0.09946(9) 0.36532(7) 0.0168(3) Uani 1 1 d . . . P2 P 0.25190(11) 0.20308(10) 1.02390(7) 0.0177(3) Uani 1 1 d . . . P3 P 0.67034(11) 0.37861(10) 0.29746(7) 0.0181(3) Uani 1 1 d . . . Si1 Si 0.15554(12) -0.22205(11) 0.24764(8) 0.0243(4) Uani 1 1 d . . . Si2 Si 0.29689(13) -0.29809(11) 0.33441(8) 0.0250(4) Uani 1 1 d . . . Si3 Si 0.16618(12) 0.30393(11) 0.93432(8) 0.0233(4) Uani 1 1 d . . . Si4 Si 0.34944(12) 0.38995(11) 1.04349(8) 0.0234(4) Uani 1 1 d . . . Si5 Si 0.82733(12) 0.48007(11) 0.41727(8) 0.0233(4) Uani 1 1 d . . . Si6 Si 0.70462(12) 0.57777(11) 0.33488(8) 0.0237(4) Uani 1 1 d . . . W1 W 0.452739(17) -0.050263(16) 0.316628(12) 0.02011(6) Uani 1 1 d . . . W2 W 0.355266(18) 0.099258(16) 0.954147(12) 0.02186(6) Uani 1 1 d . . . W3 W 0.517508(17) 0.341558(15) 0.346413(12) 0.01777(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(3) 0.024(4) 0.015(3) 0.004(3) -0.002(2) 0.004(3) C2 0.013(3) 0.015(3) 0.016(3) 0.002(2) -0.002(2) 0.003(3) C3 0.019(4) 0.032(4) 0.024(3) 0.010(3) 0.000(3) 0.012(3) C4 0.040(4) 0.037(4) 0.031(4) 0.026(3) 0.010(3) 0.012(4) C5 0.019(4) 0.022(4) 0.036(4) 0.014(3) 0.000(3) -0.002(3) C6 0.024(4) 0.027(4) 0.020(3) 0.013(3) 0.002(3) 0.007(3) C7 0.033(4) 0.035(4) 0.026(3) 0.007(3) 0.007(3) 0.019(4) C8 0.020(4) 0.044(5) 0.035(4) 0.012(3) 0.015(3) 0.013(3) C9 0.050(5) 0.053(5) 0.030(4) 0.014(4) 0.016(4) 0.029(4) C10 0.046(5) 0.037(5) 0.027(4) -0.011(3) -0.013(3) 0.020(4) C11 0.032(4) 0.034(4) 0.043(4) 0.014(4) 0.011(4) 0.007(4) C12 0.037(4) 0.024(4) 0.028(3) 0.012(3) 0.008(3) 0.009(3) C13 0.025(4) 0.023(4) 0.011(3) 0.007(3) 0.002(3) 0.003(3) C14 0.022(4) 0.051(5) 0.043(4) 0.023(4) -0.010(3) -0.003(4) C15 0.036(4) 0.034(4) 0.023(3) 0.010(3) -0.005(3) 0.011(3) C16 0.046(5) 0.034(4) 0.025(3) 0.004(3) -0.004(3) 0.010(4) C17 0.043(5) 0.022(4) 0.030(3) 0.004(3) -0.010(3) 0.005(3) C18 0.045(5) 0.033(5) 0.059(5) 0.023(4) -0.017(4) -0.006(4) C19 0.037(4) 0.029(4) 0.036(4) 0.017(3) -0.004(3) 0.007(3) C20 0.032(4) 0.022(4) 0.014(3) 0.002(3) -0.005(3) 0.005(3) C21 0.029(4) 0.027(4) 0.025(3) 0.013(3) 0.005(3) -0.003(3) C22 0.019(4) 0.037(4) 0.020(3) 0.008(3) -0.003(3) -0.004(3) C23 0.022(4) 0.025(4) 0.024(3) 0.009(3) 0.008(3) -0.007(3) C24 0.023(4) 0.026(4) 0.027(3) 0.006(3) -0.001(3) 0.000(3) C25 0.021(4) 0.027(4) 0.017(3) 0.011(3) 0.005(3) 0.004(3) C26 0.019(3) 0.026(4) 0.021(3) 0.011(3) 0.003(3) 0.004(3) C27 0.018(3) 0.032(4) 0.026(3) 0.013(3) 0.006(3) 0.000(3) C28 0.031(4) 0.026(4) 0.019(3) 0.006(3) 0.000(3) -0.005(3) C29 0.032(4) 0.012(3) 0.028(3) 0.004(3) 0.010(3) -0.002(3) C30 0.020(3) 0.020(3) 0.022(3) 0.014(3) 0.002(3) 0.000(3) C31 0.035(4) 0.031(4) 0.024(3) 0.009(3) 0.004(3) -0.006(3) C32 0.030(4) 0.027(4) 0.043(4) 0.019(3) 0.004(3) 0.011(3) C33 0.028(4) 0.041(4) 0.033(4) 0.027(4) -0.003(3) -0.007(3) C34 0.025(4) 0.036(4) 0.028(3) 0.015(3) 0.007(3) 0.007(3) C35 0.008(3) 0.048(5) 0.041(4) 0.028(4) 0.000(3) -0.007(3) C36 0.030(4) 0.026(4) 0.029(3) 0.006(3) 0.005(3) -0.009(3) C37 0.016(3) 0.019(3) 0.014(3) 0.007(2) 0.000(2) -0.001(3) C38 0.023(4) 0.042(4) 0.036(4) 0.021(3) 0.000(3) 0.001(3) C39 0.035(4) 0.056(5) 0.028(3) 0.025(4) 0.004(3) 0.014(4) C40 0.027(4) 0.043(4) 0.021(3) 0.012(3) -0.009(3) 0.003(3) C41 0.030(4) 0.034(4) 0.045(4) 0.020(4) 0.008(3) -0.003(3) C42 0.035(4) 0.031(4) 0.035(4) 0.012(3) -0.011(3) -0.004(3) C43 0.051(5) 0.022(4) 0.039(4) 0.010(3) 0.012(4) 0.005(4) C44 0.031(4) 0.053(5) 0.019(3) 0.016(3) -0.005(3) 0.009(4) C45 0.020(4) 0.014(3) 0.031(4) 0.005(3) 0.007(3) -0.001(3) C46 0.026(4) 0.018(4) 0.034(4) -0.003(3) -0.010(3) 0.002(3) C47 0.026(4) 0.024(4) 0.025(3) 0.004(3) 0.004(3) 0.002(3) C48 0.014(3) 0.015(3) 0.027(3) -0.009(3) 0.001(3) 0.005(3) C49 0.019(3) 0.020(3) 0.014(3) 0.001(2) 0.002(3) 0.004(3) C50 0.029(4) 0.018(3) 0.018(3) 0.005(3) 0.004(3) 0.009(3) C51 0.030(4) 0.029(4) 0.025(3) 0.011(3) 0.008(3) 0.014(3) C52 0.038(4) 0.027(4) 0.039(4) 0.022(3) 0.020(4) 0.010(3) C53 0.031(4) 0.028(4) 0.026(3) 0.007(3) 0.009(3) 0.008(3) C54 0.021(4) 0.025(4) 0.024(3) 0.010(3) 0.008(3) 0.006(3) C55 0.022(4) 0.018(3) 0.025(3) 0.006(3) 0.005(3) 0.002(3) C56 0.027(4) 0.032(4) 0.022(3) 0.008(3) -0.005(3) 0.006(3) C57 0.039(5) 0.037(4) 0.021(3) 0.010(3) 0.009(3) 0.014(4) C58 0.026(4) 0.031(4) 0.028(3) 0.004(3) 0.003(3) 0.008(3) C59 0.032(4) 0.024(4) 0.020(3) 0.007(3) 0.004(3) 0.010(3) C60 0.031(4) 0.029(4) 0.024(3) 0.009(3) 0.009(3) 0.008(3) C61 0.021(3) 0.013(3) 0.020(3) 0.004(2) 0.004(3) 0.004(3) C62 0.033(4) 0.040(4) 0.030(3) 0.018(3) -0.004(3) 0.002(3) C63 0.040(5) 0.046(5) 0.028(3) 0.007(3) -0.004(3) 0.007(4) C64 0.028(4) 0.050(5) 0.031(4) 0.011(3) 0.000(3) 0.006(4) C65 0.037(4) 0.026(4) 0.024(3) 0.014(3) -0.001(3) 0.004(3) C66 0.035(4) 0.029(4) 0.034(4) 0.013(3) -0.002(3) 0.012(3) C67 0.041(5) 0.032(4) 0.048(4) 0.015(4) -0.004(4) -0.002(4) C68 0.022(4) 0.029(4) 0.021(3) 0.007(3) -0.002(3) 0.012(3) C69 0.024(4) 0.024(4) 0.014(3) 0.006(3) 0.004(3) 0.001(3) C70 0.015(3) 0.035(4) 0.016(3) 0.003(3) 0.008(3) 0.004(3) C71 0.021(4) 0.025(4) 0.022(3) 0.013(3) 0.003(3) 0.002(3) C72 0.020(4) 0.030(4) 0.035(4) 0.019(3) 0.006(3) 0.013(3) Fe1 0.0210(5) 0.0316(6) 0.0205(4) 0.0114(4) 0.0035(4) 0.0099(4) Fe2 0.0173(5) 0.0241(5) 0.0173(4) 0.0095(4) 0.0015(4) 0.0004(4) Fe3 0.0199(5) 0.0240(5) 0.0160(4) 0.0077(4) 0.0021(4) 0.0038(4) N1 0.023(3) 0.024(3) 0.022(2) 0.015(2) 0.004(2) 0.005(2) N2 0.019(3) 0.024(3) 0.017(2) 0.007(2) 0.002(2) 0.003(2) N3 0.019(3) 0.026(3) 0.018(2) 0.013(2) 0.007(2) 0.006(2) O1 0.025(3) 0.040(3) 0.023(2) 0.012(2) 0.003(2) -0.001(2) O2 0.035(3) 0.055(4) 0.055(3) 0.033(3) 0.003(3) 0.014(3) O3 0.042(3) 0.043(3) 0.026(2) 0.006(2) 0.004(2) -0.011(3) O4 0.053(3) 0.039(3) 0.040(3) 0.029(2) 0.011(2) 0.017(3) O5 0.034(3) 0.049(3) 0.024(2) 0.003(2) -0.003(2) 0.002(3) O6 0.048(4) 0.066(4) 0.042(3) 0.004(3) 0.000(3) 0.031(3) O7 0.038(3) 0.025(3) 0.038(3) 0.005(2) -0.002(2) -0.004(2) O8 0.056(4) 0.046(3) 0.039(3) 0.026(3) -0.008(2) 0.002(3) O9 0.026(3) 0.051(4) 0.048(3) 0.014(3) -0.006(2) -0.004(3) O10 0.046(3) 0.040(3) 0.026(2) 0.014(2) 0.005(2) 0.009(2) O11 0.025(3) 0.052(3) 0.034(3) 0.015(2) 0.003(2) 0.003(2) O12 0.037(3) 0.032(3) 0.037(3) 0.014(2) 0.000(2) 0.015(2) O13 0.031(3) 0.044(3) 0.022(2) 0.003(2) -0.004(2) 0.009(2) O14 0.038(3) 0.037(3) 0.035(2) 0.024(2) 0.003(2) 0.015(2) O15 0.033(3) 0.029(3) 0.021(2) 0.003(2) 0.001(2) 0.006(2) P1 0.0189(9) 0.0175(9) 0.0143(7) 0.0054(6) 0.0005(7) 0.0027(7) P2 0.0168(9) 0.0194(9) 0.0167(7) 0.0065(7) -0.0004(7) 0.0009(7) P3 0.0178(9) 0.0232(9) 0.0156(7) 0.0090(7) 0.0014(7) 0.0042(7) Si1 0.0222(10) 0.0274(11) 0.0217(9) 0.0060(8) -0.0043(8) 0.0029(8) Si2 0.0302(11) 0.0192(10) 0.0252(9) 0.0073(8) -0.0042(8) 0.0014(8) Si3 0.0211(10) 0.0323(11) 0.0205(8) 0.0128(8) 0.0004(8) 0.0071(8) Si4 0.0235(10) 0.0239(10) 0.0231(9) 0.0097(8) -0.0018(8) -0.0004(8) Si5 0.0216(10) 0.0282(11) 0.0177(8) 0.0041(8) -0.0011(8) 0.0039(8) Si6 0.0283(11) 0.0216(10) 0.0212(9) 0.0074(8) 0.0019(8) 0.0023(8) W1 0.02004(14) 0.02330(15) 0.01704(12) 0.00771(11) 0.00213(11) 0.00036(12) W2 0.02047(15) 0.02341(15) 0.02052(13) 0.00481(11) 0.00052(11) 0.00524(12) W3 0.01710(14) 0.02154(14) 0.01672(12) 0.00825(11) 0.00217(10) 0.00485(11) _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 C1 C2 1.475(6) . ? C1 N1 1.487(6) . ? C1 P1 1.838(5) . ? C1 H1A 1.0000 . ? C2 C6 1.415(8) . ? C2 C3 1.437(7) . ? C2 Fe1 2.053(5) . ? C3 C4 1.420(8) . ? C3 Fe1 2.052(5) . ? C3 H3A 0.9500 . ? C4 C5 1.416(8) . ? C4 Fe1 2.028(5) . ? C4 H4A 0.9500 . ? C5 C6 1.415(6) . ? C5 Fe1 2.038(6) . ? C5 H5A 0.9500 . ? C6 Fe1 2.043(6) . ? C6 H6A 0.9500 . ? C7 C8 1.384(7) . ? C7 C11 1.409(9) . ? C7 Fe1 2.026(6) . ? C7 H7A 0.9500 . ? C8 C9 1.416(8) . ? C8 Fe1 2.042(5) . ? C8 H8A 0.9500 . ? C9 C10 1.433(10) . ? C9 Fe1 2.048(6) . ? C9 H9A 0.9500 . ? C10 C11 1.413(7) . ? C10 Fe1 2.045(7) . ? C10 H10A 0.9500 . ? C11 Fe1 2.045(7) . ? C11 H11A 0.9500 . ? C12 N1 1.472(6) . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 P1 1.799(6) . ? C13 Si1 1.909(5) . ? C13 Si2 1.910(5) . ? C13 H13A 1.0000 . ? C14 Si1 1.868(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.870(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si1 1.885(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.858(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Si2 1.868(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 Si2 1.850(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O1 1.159(6) . ? C20 W1 1.989(6) . ? C21 O2 1.146(6) . ? C21 W1 2.041(6) . ? C22 O3 1.152(6) . ? C22 W1 2.044(6) . ? C23 O4 1.143(6) . ? C23 W1 2.042(6) . ? C24 O5 1.140(7) . ? C24 W1 2.050(6) . ? C25 N2 1.471(7) . ? C25 C26 1.477(7) . ? C25 P2 1.836(4) . ? C25 H25A 1.0000 . ? C26 C27 1.430(8) . ? C26 C30 1.437(7) . ? C26 Fe2 2.066(5) . ? C27 C28 1.405(7) . ? C27 Fe2 2.027(6) . ? C27 H27A 0.9500 . ? C28 C29 1.407(8) . ? C28 Fe2 2.044(6) . ? C28 H28A 0.9500 . ? C29 C30 1.430(7) . ? C29 Fe2 2.049(5) . ? C29 H29A 0.9500 . ? C30 Fe2 2.059(4) . ? C30 H30A 0.9500 . ? C31 C32 1.413(8) . ? C31 C35 1.428(8) . ? C31 Fe2 2.046(6) . ? C31 H31A 0.9500 . ? C32 C33 1.409(8) . ? C32 Fe2 2.049(6) . ? C32 H32A 0.9500 . ? C33 C34 1.404(7) . ? C33 Fe2 2.047(5) . ? C33 H33A 0.9500 . ? C34 C35 1.420(8) . ? C34 Fe2 2.038(5) . ? C34 H34A 0.9500 . ? C35 Fe2 2.046(5) . ? C35 H35A 0.9500 . ? C36 N2 1.455(7) . ? C36 H36C 0.9800 . ? C36 H36B 0.9800 . ? C36 H36A 0.9800 . ? C37 P2 1.795(5) . ? C37 Si3 1.908(5) . ? C37 Si4 1.919(6) . ? C37 H37A 1.0000 . ? C38 Si3 1.871(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 Si3 1.854(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 Si3 1.868(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Si4 1.873(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 Si4 1.858(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 Si4 1.865(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 O6 1.171(7) . ? C44 W2 1.990(6) . ? C45 O7 1.139(7) . ? C45 W2 2.045(7) . ? C46 O8 1.165(6) . ? C46 W2 2.045(6) . ? C47 O9 1.122(7) . ? C47 W2 2.063(7) . ? C48 O10 1.138(5) . ? C48 W2 2.042(6) . ? C49 N3 1.475(6) . ? C49 C50 1.491(7) . ? C49 P3 1.832(5) . ? C49 H49A 1.0000 . ? C50 C54 1.424(8) . ? C50 C51 1.454(7) . ? C50 Fe3 2.044(5) . ? C51 C52 1.422(8) . ? C51 Fe3 2.044(5) . ? C51 H51A 0.9500 . ? C52 C53 1.406(8) . ? C52 Fe3 2.045(5) . ? C52 H52A 0.9500 . ? C53 C54 1.430(6) . ? C53 Fe3 2.061(6) . ? C53 H53A 0.9500 . ? C54 Fe3 2.041(6) . ? C54 H54A 0.9500 . ? C55 C59 1.393(8) . ? C55 C56 1.410(6) . ? C55 Fe3 2.031(6) . ? C55 H55A 0.9500 . ? C56 C57 1.407(8) . ? C56 Fe3 2.046(6) . ? C56 H56A 0.9500 . ? C57 C58 1.417(8) . ? C57 Fe3 2.052(5) . ? C57 H57A 0.9500 . ? C58 C59 1.404(7) . ? C58 Fe3 2.047(5) . ? C58 H58A 0.9500 . ? C59 Fe3 2.039(5) . ? C59 H59A 0.9500 . ? C60 N3 1.472(7) . ? C60 H60C 0.9800 . ? C60 H60B 0.9800 . ? C60 H60A 0.9800 . ? C61 P3 1.797(6) . ? C61 Si5 1.911(5) . ? C61 Si6 1.913(5) . ? C61 H61A 1.0000 . ? C62 Si5 1.868(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 Si5 1.858(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 Si5 1.874(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 Si6 1.855(6) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 Si6 1.863(5) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 Si6 1.873(7) . ? C67 H67C 0.9800 . ? C67 H67B 0.9800 . ? C67 H67A 0.9800 . ? C68 O11 1.173(6) . ? C68 W3 1.979(6) . ? C69 O12 1.146(6) . ? C69 W3 2.041(5) . ? C70 O13 1.132(6) . ? C70 W3 2.051(6) . ? C71 O14 1.140(5) . ? C71 W3 2.035(5) . ? C72 O15 1.132(7) . ? C72 W3 2.072(7) . ? N1 P1 1.735(4) . ? N2 P2 1.738(5) . ? N3 P3 1.738(4) . ? P1 W1 2.5059(14) . ? P2 W2 2.4973(14) . ? P3 W3 2.5081(14) . ? 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 C1 N1 114.9(5) . . ? C2 C1 P1 125.6(4) . . ? N1 C1 P1 61.9(2) . . ? C2 C1 H1A 114.5 . . ? N1 C1 H1A 114.5 . . ? P1 C1 H1A 114.5 . . ? C6 C2 C3 107.7(4) . . ? C6 C2 C1 126.8(5) . . ? C3 C2 C1 125.4(5) . . ? C6 C2 Fe1 69.4(3) . . ? C3 C2 Fe1 69.4(3) . . ? C1 C2 Fe1 124.3(4) . . ? C4 C3 C2 107.2(5) . . ? C4 C3 Fe1 68.8(3) . . ? C2 C3 Fe1 69.6(3) . . ? C4 C3 H3A 126.4 . . ? C2 C3 H3A 126.4 . . ? Fe1 C3 H3A 126.8 . . ? C5 C4 C3 108.8(4) . . ? C5 C4 Fe1 70.0(3) . . ? C3 C4 Fe1 70.5(3) . . ? C5 C4 H4A 125.6 . . ? C3 C4 H4A 125.6 . . ? Fe1 C4 H4A 125.4 . . ? C6 C5 C4 107.7(5) . . ? C6 C5 Fe1 69.9(3) . . ? C4 C5 Fe1 69.2(4) . . ? C6 C5 H5A 126.1 . . ? C4 C5 H5A 126.1 . . ? Fe1 C5 H5A 126.3 . . ? C2 C6 C5 108.6(5) . . ? C2 C6 Fe1 70.2(3) . . ? C5 C6 Fe1 69.5(3) . . ? C2 C6 H6A 125.7 . . ? C5 C6 H6A 125.7 . . ? Fe1 C6 H6A 126.2 . . ? C8 C7 C11 109.7(5) . . ? C8 C7 Fe1 70.7(3) . . ? C11 C7 Fe1 70.5(3) . . ? C8 C7 H7A 125.2 . . ? C11 C7 H7A 125.2 . . ? Fe1 C7 H7A 125.2 . . ? C7 C8 C9 108.5(6) . . ? C7 C8 Fe1 69.5(3) . . ? C9 C8 Fe1 70.0(3) . . ? C7 C8 H8A 125.7 . . ? C9 C8 H8A 125.7 . . ? Fe1 C8 H8A 126.4 . . ? C8 C9 C10 106.6(5) . . ? C8 C9 Fe1 69.5(3) . . ? C10 C9 Fe1 69.4(3) . . ? C8 C9 H9A 126.7 . . ? C10 C9 H9A 126.7 . . ? Fe1 C9 H9A 126.0 . . ? C11 C10 C9 108.4(6) . . ? C11 C10 Fe1 69.8(4) . . ? C9 C10 Fe1 69.6(4) . . ? C11 C10 H10A 125.8 . . ? C9 C10 H10A 125.8 . . ? Fe1 C10 H10A 126.3 . . ? C7 C11 C10 106.8(6) . . ? C7 C11 Fe1 69.0(4) . . ? C10 C11 Fe1 69.8(4) . . ? C7 C11 H11A 126.6 . . ? C10 C11 H11A 126.6 . . ? Fe1 C11 H11A 126.2 . . ? N1 C12 H12C 109.5 . . ? N1 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? N1 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? P1 C13 Si1 116.0(2) . . ? P1 C13 Si2 114.9(3) . . ? Si1 C13 Si2 117.9(3) . . ? P1 C13 H13A 101.3 . . ? Si1 C13 H13A 101.3 . . ? Si2 C13 H13A 101.3 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C20 W1 179.4(6) . . ? O2 C21 W1 174.4(5) . . ? O3 C22 W1 179.2(6) . . ? O4 C23 W1 176.6(4) . . ? O5 C24 W1 176.6(5) . . ? N2 C25 C26 117.3(5) . . ? N2 C25 P2 62.3(2) . . ? C26 C25 P2 125.5(4) . . ? N2 C25 H25A 113.9 . . ? C26 C25 H25A 113.9 . . ? P2 C25 H25A 113.9 . . ? C27 C26 C30 106.4(5) . . ? C27 C26 C25 125.5(5) . . ? C30 C26 C25 128.0(5) . . ? C27 C26 Fe2 68.1(3) . . ? C30 C26 Fe2 69.4(3) . . ? C25 C26 Fe2 126.2(4) . . ? C28 C27 C26 109.4(5) . . ? C28 C27 Fe2 70.5(3) . . ? C26 C27 Fe2 71.0(3) . . ? C28 C27 H27A 125.3 . . ? C26 C27 H27A 125.3 . . ? Fe2 C27 H27A 124.8 . . ? C27 C28 C29 108.0(5) . . ? C27 C28 Fe2 69.2(4) . . ? C29 C28 Fe2 70.1(4) . . ? C27 C28 H28A 126.0 . . ? C29 C28 H28A 126.0 . . ? Fe2 C28 H28A 126.3 . . ? C28 C29 C30 108.5(5) . . ? C28 C29 Fe2 69.7(3) . . ? C30 C29 Fe2 70.0(3) . . ? C28 C29 H29A 125.7 . . ? C30 C29 H29A 125.7 . . ? Fe2 C29 H29A 126.1 . . ? C29 C30 C26 107.6(5) . . ? C29 C30 Fe2 69.2(3) . . ? C26 C30 Fe2 69.8(3) . . ? C29 C30 H30A 126.2 . . ? C26 C30 H30A 126.2 . . ? Fe2 C30 H30A 126.3 . . ? C32 C31 C35 107.8(6) . . ? C32 C31 Fe2 69.9(4) . . ? C35 C31 Fe2 69.6(4) . . ? C32 C31 H31A 126.1 . . ? C35 C31 H31A 126.1 . . ? Fe2 C31 H31A 126.0 . . ? C33 C32 C31 107.6(5) . . ? C33 C32 Fe2 69.8(3) . . ? C31 C32 Fe2 69.7(3) . . ? C33 C32 H32A 126.2 . . ? C31 C32 H32A 126.2 . . ? Fe2 C32 H32A 125.9 . . ? C34 C33 C32 109.3(6) . . ? C34 C33 Fe2 69.5(3) . . ? C32 C33 Fe2 69.9(3) . . ? C34 C33 H33A 125.3 . . ? C32 C33 H33A 125.3 . . ? Fe2 C33 H33A 126.8 . . ? C33 C34 C35 107.4(5) . . ? C33 C34 Fe2 70.3(3) . . ? C35 C34 Fe2 70.0(3) . . ? C33 C34 H34A 126.3 . . ? C35 C34 H34A 126.3 . . ? Fe2 C34 H34A 125.1 . . ? C34 C35 C31 107.8(5) . . ? C34 C35 Fe2 69.3(3) . . ? C31 C35 Fe2 69.6(3) . . ? C34 C35 H35A 126.1 . . ? C31 C35 H35A 126.1 . . ? Fe2 C35 H35A 126.6 . . ? N2 C36 H36C 109.5 . . ? N2 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? N2 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? P2 C37 Si3 115.6(3) . . ? P2 C37 Si4 114.8(3) . . ? Si3 C37 Si4 117.2(2) . . ? P2 C37 H37A 101.9 . . ? Si3 C37 H37A 101.9 . . ? Si4 C37 H37A 101.9 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si3 C40 H40A 109.5 . . ? Si3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O6 C44 W2 177.9(7) . . ? O7 C45 W2 175.4(5) . . ? O8 C46 W2 179.5(5) . . ? O9 C47 W2 177.1(6) . . ? O10 C48 W2 177.7(5) . . ? N3 C49 C50 114.7(5) . . ? N3 C49 P3 62.3(2) . . ? C50 C49 P3 126.2(4) . . ? N3 C49 H49A 114.3 . . ? C50 C49 H49A 114.3 . . ? P3 C49 H49A 114.3 . . ? C54 C50 C51 107.3(5) . . ? C54 C50 C49 126.5(5) . . ? C51 C50 C49 126.0(6) . . ? C54 C50 Fe3 69.5(3) . . ? C51 C50 Fe3 69.2(3) . . ? C49 C50 Fe3 122.7(4) . . ? C52 C51 C50 106.9(6) . . ? C52 C51 Fe3 69.7(3) . . ? C50 C51 Fe3 69.2(3) . . ? C52 C51 H51A 126.6 . . ? C50 C51 H51A 126.6 . . ? Fe3 C51 H51A 126.1 . . ? C53 C52 C51 109.6(5) . . ? C53 C52 Fe3 70.6(3) . . ? C51 C52 Fe3 69.6(3) . . ? C53 C52 H52A 125.2 . . ? C51 C52 H52A 125.2 . . ? Fe3 C52 H52A 126.2 . . ? C52 C53 C54 107.7(5) . . ? C52 C53 Fe3 69.4(4) . . ? C54 C53 Fe3 68.9(3) . . ? C52 C53 H53A 126.1 . . ? C54 C53 H53A 126.1 . . ? Fe3 C53 H53A 127.2 . . ? C50 C54 C53 108.5(5) . . ? C50 C54 Fe3 69.7(3) . . ? C53 C54 Fe3 70.3(3) . . ? C50 C54 H54A 125.8 . . ? C53 C54 H54A 125.8 . . ? Fe3 C54 H54A 125.8 . . ? C59 C55 C56 108.1(5) . . ? C59 C55 Fe3 70.3(3) . . ? C56 C55 Fe3 70.4(3) . . ? C59 C55 H55A 125.9 . . ? C56 C55 H55A 125.9 . . ? Fe3 C55 H55A 125.0 . . ? C57 C56 C55 108.1(5) . . ? C57 C56 Fe3 70.2(4) . . ? C55 C56 Fe3 69.2(3) . . ? C57 C56 H56A 125.9 . . ? C55 C56 H56A 125.9 . . ? Fe3 C56 H56A 126.3 . . ? C56 C57 C58 107.4(5) . . ? C56 C57 Fe3 69.7(3) . . ? C58 C57 Fe3 69.6(3) . . ? C56 C57 H57A 126.3 . . ? C58 C57 H57A 126.3 . . ? Fe3 C57 H57A 126.0 . . ? C59 C58 C57 107.9(6) . . ? C59 C58 Fe3 69.6(3) . . ? C57 C58 Fe3 70.0(3) . . ? C59 C58 H58A 126.0 . . ? C57 C58 H58A 126.0 . . ? Fe3 C58 H58A 125.9 . . ? C55 C59 C58 108.4(5) . . ? C55 C59 Fe3 69.7(3) . . ? C58 C59 Fe3 70.2(3) . . ? C55 C59 H59A 125.8 . . ? C58 C59 H59A 125.8 . . ? Fe3 C59 H59A 125.9 . . ? N3 C60 H60C 109.5 . . ? N3 C60 H60B 109.5 . . ? H60C C60 H60B 109.5 . . ? N3 C60 H60A 109.5 . . ? H60C C60 H60A 109.5 . . ? H60B C60 H60A 109.5 . . ? P3 C61 Si5 116.2(2) . . ? P3 C61 Si6 113.5(3) . . ? Si5 C61 Si6 118.5(3) . . ? P3 C61 H61A 101.6 . . ? Si5 C61 H61A 101.6 . . ? Si6 C61 H61A 101.6 . . ? Si5 C62 H62A 109.5 . . ? Si5 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si5 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si5 C63 H63A 109.5 . . ? Si5 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? Si5 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si5 C64 H64A 109.5 . . ? Si5 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? Si5 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si6 C65 H65A 109.5 . . ? Si6 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si6 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si6 C66 H66A 109.5 . . ? Si6 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? Si6 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? Si6 C67 H67C 109.5 . . ? Si6 C67 H67B 109.5 . . ? H67C C67 H67B 109.5 . . ? Si6 C67 H67A 109.5 . . ? H67C C67 H67A 109.5 . . ? H67B C67 H67A 109.5 . . ? O11 C68 W3 176.0(5) . . ? O12 C69 W3 175.9(4) . . ? O13 C70 W3 176.1(5) . . ? O14 C71 W3 174.4(5) . . ? O15 C72 W3 179.7(5) . . ? C7 Fe1 C4 169.1(3) . . ? C7 Fe1 C5 131.1(3) . . ? C4 Fe1 C5 40.8(2) . . ? C7 Fe1 C8 39.8(2) . . ? C4 Fe1 C8 130.6(2) . . ? C5 Fe1 C8 109.1(3) . . ? C7 Fe1 C6 110.0(2) . . ? C4 Fe1 C6 68.3(2) . . ? C5 Fe1 C6 40.58(18) . . ? C8 Fe1 C6 117.5(3) . . ? C7 Fe1 C10 67.6(3) . . ? C4 Fe1 C10 116.1(3) . . ? C5 Fe1 C10 148.8(2) . . ? C8 Fe1 C10 68.0(3) . . ? C6 Fe1 C10 169.3(3) . . ? C7 Fe1 C11 40.5(2) . . ? C4 Fe1 C11 148.6(3) . . ? C5 Fe1 C11 169.7(2) . . ? C8 Fe1 C11 67.9(3) . . ? C6 Fe1 C11 131.1(2) . . ? C10 Fe1 C11 40.4(2) . . ? C7 Fe1 C9 67.8(2) . . ? C4 Fe1 C9 107.7(2) . . ? C5 Fe1 C9 116.0(3) . . ? C8 Fe1 C9 40.5(2) . . ? C6 Fe1 C9 149.0(3) . . ? C10 Fe1 C9 41.0(3) . . ? C11 Fe1 C9 68.6(3) . . ? C7 Fe1 C3 149.7(2) . . ? C4 Fe1 C3 40.7(2) . . ? C5 Fe1 C3 68.6(2) . . ? C8 Fe1 C3 168.8(2) . . ? C6 Fe1 C3 68.5(2) . . ? C10 Fe1 C3 108.0(3) . . ? C11 Fe1 C3 116.3(3) . . ? C9 Fe1 C3 129.7(2) . . ? C7 Fe1 C2 117.7(2) . . ? C4 Fe1 C2 68.6(2) . . ? C5 Fe1 C2 68.4(2) . . ? C8 Fe1 C2 149.4(2) . . ? C6 Fe1 C2 40.4(2) . . ? C10 Fe1 C2 130.4(3) . . ? C11 Fe1 C2 108.8(2) . . ? C9 Fe1 C2 169.1(3) . . ? C3 Fe1 C2 41.00(18) . . ? C27 Fe2 C34 137.9(3) . . ? C27 Fe2 C28 40.4(2) . . ? C34 Fe2 C28 110.5(2) . . ? C27 Fe2 C35 178.0(2) . . ? C34 Fe2 C35 40.7(2) . . ? C28 Fe2 C35 140.1(2) . . ? C27 Fe2 C31 138.5(2) . . ? C34 Fe2 C31 68.6(2) . . ? C28 Fe2 C31 177.1(2) . . ? C35 Fe2 C31 40.8(2) . . ? C27 Fe2 C33 110.5(2) . . ? C34 Fe2 C33 40.2(2) . . ? C28 Fe2 C33 109.9(2) . . ? C35 Fe2 C33 67.6(2) . . ? C31 Fe2 C33 67.6(2) . . ? C27 Fe2 C32 110.2(2) . . ? C34 Fe2 C32 68.3(2) . . ? C28 Fe2 C32 136.8(3) . . ? C35 Fe2 C32 68.2(2) . . ? C31 Fe2 C32 40.4(2) . . ? C33 Fe2 C32 40.2(2) . . ? C27 Fe2 C29 67.8(2) . . ? C34 Fe2 C29 111.4(2) . . ? C28 Fe2 C29 40.2(2) . . ? C35 Fe2 C29 113.7(2) . . ? C31 Fe2 C29 142.6(3) . . ? C33 Fe2 C29 137.6(2) . . ? C32 Fe2 C29 176.9(3) . . ? C27 Fe2 C30 68.4(2) . . ? C34 Fe2 C30 139.8(2) . . ? C28 Fe2 C30 68.3(2) . . ? C35 Fe2 C30 113.6(2) . . ? C31 Fe2 C30 114.2(2) . . ? C33 Fe2 C30 178.2(3) . . ? C32 Fe2 C30 141.3(2) . . ? C29 Fe2 C30 40.8(2) . . ? C27 Fe2 C26 40.9(2) . . ? C34 Fe2 C26 178.8(3) . . ? C28 Fe2 C26 68.5(2) . . ? C35 Fe2 C26 140.5(2) . . ? C31 Fe2 C26 112.3(2) . . ? C33 Fe2 C26 139.2(2) . . ? C32 Fe2 C26 111.8(2) . . ? C29 Fe2 C26 68.5(2) . . ? C30 Fe2 C26 40.78(19) . . ? C55 Fe3 C59 40.0(2) . . ? C55 Fe3 C54 127.8(2) . . ? C59 Fe3 C54 108.8(2) . . ? C55 Fe3 C50 106.0(2) . . ? C59 Fe3 C50 116.51(19) . . ? C54 Fe3 C50 40.8(2) . . ? C55 Fe3 C51 115.9(2) . . ? C59 Fe3 C51 149.6(2) . . ? C54 Fe3 C51 69.1(2) . . ? C50 Fe3 C51 41.66(19) . . ? C55 Fe3 C52 150.4(3) . . ? C59 Fe3 C52 168.8(3) . . ? C54 Fe3 C52 68.2(2) . . ? C50 Fe3 C52 68.8(2) . . ? C51 Fe3 C52 40.7(2) . . ? C55 Fe3 C56 40.45(19) . . ? C59 Fe3 C56 67.5(2) . . ? C54 Fe3 C56 165.6(2) . . ? C50 Fe3 C56 127.0(2) . . ? C51 Fe3 C56 106.6(2) . . ? C52 Fe3 C56 118.2(2) . . ? C55 Fe3 C58 67.6(2) . . ? C59 Fe3 C58 40.19(19) . . ? C54 Fe3 C58 119.3(2) . . ? C50 Fe3 C58 150.8(2) . . ? C51 Fe3 C58 167.3(2) . . ? C52 Fe3 C58 130.9(2) . . ? C56 Fe3 C58 67.6(2) . . ? C55 Fe3 C57 67.9(2) . . ? C59 Fe3 C57 67.8(2) . . ? C54 Fe3 C57 153.0(3) . . ? C50 Fe3 C57 165.7(3) . . ? C51 Fe3 C57 128.0(2) . . ? C52 Fe3 C57 109.7(2) . . ? C56 Fe3 C57 40.1(2) . . ? C58 Fe3 C57 40.5(2) . . ? C55 Fe3 C53 167.2(2) . . ? C59 Fe3 C53 130.8(3) . . ? C54 Fe3 C53 40.78(18) . . ? C50 Fe3 C53 68.7(2) . . ? C51 Fe3 C53 68.5(2) . . ? C52 Fe3 C53 40.0(2) . . ? C56 Fe3 C53 151.9(2) . . ? C58 Fe3 C53 111.0(3) . . ? C57 Fe3 C53 119.9(2) . . ? C12 N1 C1 116.0(5) . . ? C12 N1 P1 123.4(3) . . ? C1 N1 P1 69.1(3) . . ? C36 N2 C25 117.0(4) . . ? C36 N2 P2 124.1(3) . . ? C25 N2 P2 69.2(3) . . ? C60 N3 C49 115.8(5) . . ? C60 N3 P3 122.8(3) . . ? C49 N3 P3 69.0(3) . . ? N1 P1 C13 104.7(2) . . ? N1 P1 C1 49.08(19) . . ? C13 P1 C1 108.0(2) . . ? N1 P1 W1 121.65(16) . . ? C13 P1 W1 126.37(17) . . ? C1 P1 W1 122.0(2) . . ? N2 P2 C37 104.2(2) . . ? N2 P2 C25 48.5(2) . . ? C37 P2 C25 109.8(2) . . ? N2 P2 W2 120.90(17) . . ? C37 P2 W2 126.94(16) . . ? C25 P2 W2 120.42(17) . . ? N3 P3 C61 105.1(2) . . ? N3 P3 C49 48.74(19) . . ? C61 P3 C49 108.5(2) . . ? N3 P3 W3 120.19(16) . . ? C61 P3 W3 126.58(17) . . ? C49 P3 W3 122.0(2) . . ? C14 Si1 C15 109.5(3) . . ? C14 Si1 C16 107.0(3) . . ? C15 Si1 C16 109.9(2) . . ? C14 Si1 C13 106.5(2) . . ? C15 Si1 C13 110.7(3) . . ? C16 Si1 C13 113.1(3) . . ? C19 Si2 C17 108.7(3) . . ? C19 Si2 C18 107.2(3) . . ? C17 Si2 C18 109.5(3) . . ? C19 Si2 C13 109.7(3) . . ? C17 Si2 C13 115.0(2) . . ? C18 Si2 C13 106.3(3) . . ? C39 Si3 C40 107.7(3) . . ? C39 Si3 C38 108.1(2) . . ? C40 Si3 C38 109.1(3) . . ? C39 Si3 C37 114.2(3) . . ? C40 Si3 C37 111.5(2) . . ? C38 Si3 C37 106.0(2) . . ? C42 Si4 C43 107.4(3) . . ? C42 Si4 C41 108.4(3) . . ? C43 Si4 C41 108.8(2) . . ? C42 Si4 C37 108.8(2) . . ? C43 Si4 C37 107.7(3) . . ? C41 Si4 C37 115.4(3) . . ? C63 Si5 C62 108.2(3) . . ? C63 Si5 C64 107.3(3) . . ? C62 Si5 C64 109.0(3) . . ? C63 Si5 C61 114.6(3) . . ? C62 Si5 C61 111.6(3) . . ? C64 Si5 C61 105.8(2) . . ? C65 Si6 C66 109.1(3) . . ? C65 Si6 C67 109.3(3) . . ? C66 Si6 C67 109.4(3) . . ? C65 Si6 C61 108.0(3) . . ? C66 Si6 C61 114.9(2) . . ? C67 Si6 C61 105.9(3) . . ? C20 W1 C21 86.7(2) . . ? C20 W1 C23 87.0(2) . . ? C21 W1 C23 173.7(2) . . ? C20 W1 C22 91.4(2) . . ? C21 W1 C22 88.8(2) . . ? C23 W1 C22 91.7(2) . . ? C20 W1 C24 90.2(2) . . ? C21 W1 C24 91.3(2) . . ? C23 W1 C24 88.3(2) . . ? C22 W1 C24 178.3(2) . . ? C20 W1 P1 177.12(17) . . ? C21 W1 P1 94.06(15) . . ? C23 W1 P1 92.22(15) . . ? C22 W1 P1 85.83(16) . . ? C24 W1 P1 92.52(17) . . ? C44 W2 C48 90.8(2) . . ? C44 W2 C46 89.4(2) . . ? C48 W2 C46 179.6(3) . . ? C44 W2 C45 87.3(3) . . ? C48 W2 C45 85.4(2) . . ? C46 W2 C45 94.2(2) . . ? C44 W2 C47 89.2(3) . . ? C48 W2 C47 91.4(2) . . ? C46 W2 C47 89.0(2) . . ? C45 W2 C47 175.2(2) . . ? C44 W2 P2 176.03(19) . . ? C48 W2 P2 92.31(14) . . ? C46 W2 P2 87.54(16) . . ? C45 W2 P2 90.45(15) . . ? C47 W2 P2 93.21(16) . . ? C68 W3 C71 85.2(2) . . ? C68 W3 C69 88.0(2) . . ? C71 W3 C69 172.80(19) . . ? C68 W3 C70 91.6(2) . . ? C71 W3 C70 87.1(2) . . ? C69 W3 C70 90.7(2) . . ? C68 W3 C72 89.4(2) . . ? C71 W3 C72 91.3(2) . . ? C69 W3 C72 91.0(2) . . ? C70 W3 C72 178.0(2) . . ? C68 W3 P3 175.96(17) . . ? C71 W3 P3 91.50(15) . . ? C69 W3 P3 95.39(15) . . ? C70 W3 P3 90.52(15) . . ? C72 W3 P3 88.30(16) . . ? 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 N1 C1 C2 C6 9.3(8) . . . . ? P1 C1 C2 C6 -62.8(7) . . . . ? N1 C1 C2 C3 -167.5(5) . . . . ? P1 C1 C2 C3 120.4(5) . . . . ? N1 C1 C2 Fe1 -79.5(6) . . . . ? P1 C1 C2 Fe1 -151.6(3) . . . . ? C6 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 176.9(5) . . . . ? Fe1 C2 C3 C4 58.7(4) . . . . ? C6 C2 C3 Fe1 -59.1(4) . . . . ? C1 C2 C3 Fe1 118.2(5) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? Fe1 C3 C4 C5 59.8(4) . . . . ? C2 C3 C4 Fe1 -59.2(4) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? Fe1 C4 C5 C6 59.5(4) . . . . ? C3 C4 C5 Fe1 -60.1(4) . . . . ? C3 C2 C6 C5 0.0(6) . . . . ? C1 C2 C6 C5 -177.2(5) . . . . ? Fe1 C2 C6 C5 -59.1(4) . . . . ? C3 C2 C6 Fe1 59.1(4) . . . . ? C1 C2 C6 Fe1 -118.2(5) . . . . ? C4 C5 C6 C2 0.3(6) . . . . ? Fe1 C5 C6 C2 59.4(4) . . . . ? C4 C5 C6 Fe1 -59.1(4) . . . . ? C11 C7 C8 C9 -0.7(7) . . . . ? Fe1 C7 C8 C9 59.3(4) . . . . ? C11 C7 C8 Fe1 -60.0(4) . . . . ? C7 C8 C9 C10 0.8(7) . . . . ? Fe1 C8 C9 C10 59.8(4) . . . . ? C7 C8 C9 Fe1 -59.0(4) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? Fe1 C9 C10 C11 59.3(4) . . . . ? C8 C9 C10 Fe1 -59.9(4) . . . . ? C8 C7 C11 C10 0.3(7) . . . . ? Fe1 C7 C11 C10 -59.8(4) . . . . ? C8 C7 C11 Fe1 60.1(4) . . . . ? C9 C10 C11 C7 0.2(7) . . . . ? Fe1 C10 C11 C7 59.3(4) . . . . ? C9 C10 C11 Fe1 -59.2(5) . . . . ? N2 C25 C26 C27 173.4(5) . . . . ? P2 C25 C26 C27 -112.5(6) . . . . ? N2 C25 C26 C30 -5.0(8) . . . . ? P2 C25 C26 C30 69.0(8) . . . . ? N2 C25 C26 Fe2 86.0(5) . . . . ? P2 C25 C26 Fe2 160.0(3) . . . . ? C30 C26 C27 C28 -1.2(6) . . . . ? C25 C26 C27 C28 -179.9(5) . . . . ? Fe2 C26 C27 C28 -60.2(4) . . . . ? C30 C26 C27 Fe2 59.1(3) . . . . ? C25 C26 C27 Fe2 -119.7(5) . . . . ? C26 C27 C28 C29 1.0(6) . . . . ? Fe2 C27 C28 C29 -59.6(4) . . . . ? C26 C27 C28 Fe2 60.6(4) . . . . ? C27 C28 C29 C30 -0.5(6) . . . . ? Fe2 C28 C29 C30 -59.4(4) . . . . ? C27 C28 C29 Fe2 59.0(4) . . . . ? C28 C29 C30 C26 -0.3(6) . . . . ? Fe2 C29 C30 C26 -59.5(3) . . . . ? C28 C29 C30 Fe2 59.2(4) . . . . ? C27 C26 C30 C29 0.9(6) . . . . ? C25 C26 C30 C29 179.6(5) . . . . ? Fe2 C26 C30 C29 59.1(3) . . . . ? C27 C26 C30 Fe2 -58.3(3) . . . . ? C25 C26 C30 Fe2 120.4(6) . . . . ? C35 C31 C32 C33 0.2(6) . . . . ? Fe2 C31 C32 C33 59.8(4) . . . . ? C35 C31 C32 Fe2 -59.5(4) . . . . ? C31 C32 C33 C34 -1.2(6) . . . . ? Fe2 C32 C33 C34 58.5(4) . . . . ? C31 C32 C33 Fe2 -59.7(4) . . . . ? C32 C33 C34 C35 1.6(6) . . . . ? Fe2 C33 C34 C35 60.4(4) . . . . ? C32 C33 C34 Fe2 -58.8(4) . . . . ? C33 C34 C35 C31 -1.5(6) . . . . ? Fe2 C34 C35 C31 59.1(4) . . . . ? C33 C34 C35 Fe2 -60.6(4) . . . . ? C32 C31 C35 C34 0.7(6) . . . . ? Fe2 C31 C35 C34 -59.0(4) . . . . ? C32 C31 C35 Fe2 59.7(4) . . . . ? N3 C49 C50 C54 -7.4(8) . . . . ? P3 C49 C50 C54 65.3(7) . . . . ? N3 C49 C50 C51 166.9(5) . . . . ? P3 C49 C50 C51 -120.4(6) . . . . ? N3 C49 C50 Fe3 80.1(6) . . . . ? P3 C49 C50 Fe3 152.8(3) . . . . ? C54 C50 C51 C52 -0.5(6) . . . . ? C49 C50 C51 C52 -175.7(5) . . . . ? Fe3 C50 C51 C52 -59.8(4) . . . . ? C54 C50 C51 Fe3 59.3(4) . . . . ? C49 C50 C51 Fe3 -116.0(5) . . . . ? C50 C51 C52 C53 0.0(7) . . . . ? Fe3 C51 C52 C53 -59.4(4) . . . . ? C50 C51 C52 Fe3 59.4(4) . . . . ? C51 C52 C53 C54 0.5(7) . . . . ? Fe3 C52 C53 C54 -58.3(4) . . . . ? C51 C52 C53 Fe3 58.8(4) . . . . ? C51 C50 C54 C53 0.8(6) . . . . ? C49 C50 C54 C53 176.0(5) . . . . ? Fe3 C50 C54 C53 59.9(4) . . . . ? C51 C50 C54 Fe3 -59.1(4) . . . . ? C49 C50 C54 Fe3 116.1(5) . . . . ? C52 C53 C54 C50 -0.8(6) . . . . ? Fe3 C53 C54 C50 -59.4(4) . . . . ? C52 C53 C54 Fe3 58.7(4) . . . . ? C59 C55 C56 C57 -0.9(7) . . . . ? Fe3 C55 C56 C57 59.6(4) . . . . ? C59 C55 C56 Fe3 -60.4(4) . . . . ? C55 C56 C57 C58 0.6(7) . . . . ? Fe3 C56 C57 C58 59.6(4) . . . . ? C55 C56 C57 Fe3 -59.0(4) . . . . ? C56 C57 C58 C59 -0.2(7) . . . . ? Fe3 C57 C58 C59 59.5(4) . . . . ? C56 C57 C58 Fe3 -59.7(4) . . . . ? C56 C55 C59 C58 0.7(7) . . . . ? Fe3 C55 C59 C58 -59.7(4) . . . . ? C56 C55 C59 Fe3 60.5(4) . . . . ? C57 C58 C59 C55 -0.3(7) . . . . ? Fe3 C58 C59 C55 59.4(4) . . . . ? C57 C58 C59 Fe3 -59.7(4) . . . . ? C8 C7 Fe1 C4 30.1(14) . . . . ? C11 C7 Fe1 C4 150.2(12) . . . . ? C8 C7 Fe1 C5 68.3(4) . . . . ? C11 C7 Fe1 C5 -171.6(3) . . . . ? C11 C7 Fe1 C8 120.1(5) . . . . ? C8 C7 Fe1 C6 109.3(4) . . . . ? C11 C7 Fe1 C6 -130.6(3) . . . . ? C8 C7 Fe1 C10 -81.9(4) . . . . ? C11 C7 Fe1 C10 38.2(3) . . . . ? C8 C7 Fe1 C11 -120.1(5) . . . . ? C8 C7 Fe1 C9 -37.5(4) . . . . ? C11 C7 Fe1 C9 82.6(4) . . . . ? C8 C7 Fe1 C3 -169.5(5) . . . . ? C11 C7 Fe1 C3 -49.3(6) . . . . ? C8 C7 Fe1 C2 152.9(4) . . . . ? C11 C7 Fe1 C2 -87.0(4) . . . . ? C5 C4 Fe1 C7 45.5(14) . . . . ? C3 C4 Fe1 C7 165.0(12) . . . . ? C3 C4 Fe1 C5 119.4(5) . . . . ? C5 C4 Fe1 C8 70.5(4) . . . . ? C3 C4 Fe1 C8 -170.0(4) . . . . ? C5 C4 Fe1 C6 -37.7(3) . . . . ? C3 C4 Fe1 C6 81.7(4) . . . . ? C5 C4 Fe1 C10 153.0(3) . . . . ? C3 C4 Fe1 C10 -87.6(4) . . . . ? C5 C4 Fe1 C11 -172.7(4) . . . . ? C3 C4 Fe1 C11 -53.2(5) . . . . ? C5 C4 Fe1 C9 109.5(4) . . . . ? C3 C4 Fe1 C9 -131.0(4) . . . . ? C5 C4 Fe1 C3 -119.4(5) . . . . ? C5 C4 Fe1 C2 -81.3(3) . . . . ? C3 C4 Fe1 C2 38.1(3) . . . . ? C6 C5 Fe1 C7 71.3(4) . . . . ? C4 C5 Fe1 C7 -169.7(3) . . . . ? C6 C5 Fe1 C4 -119.1(5) . . . . ? C6 C5 Fe1 C8 110.2(3) . . . . ? C4 C5 Fe1 C8 -130.7(3) . . . . ? C4 C5 Fe1 C6 119.1(5) . . . . ? C6 C5 Fe1 C10 -171.0(5) . . . . ? C4 C5 Fe1 C10 -52.0(6) . . . . ? C6 C5 Fe1 C11 39.0(14) . . . . ? C4 C5 Fe1 C11 158.1(12) . . . . ? C6 C5 Fe1 C9 153.6(3) . . . . ? C4 C5 Fe1 C9 -87.3(4) . . . . ? C6 C5 Fe1 C3 -81.5(3) . . . . ? C4 C5 Fe1 C3 37.6(3) . . . . ? C6 C5 Fe1 C2 -37.2(3) . . . . ? C4 C5 Fe1 C2 81.8(3) . . . . ? C9 C8 Fe1 C7 -119.8(6) . . . . ? C7 C8 Fe1 C4 -172.8(4) . . . . ? C9 C8 Fe1 C4 67.3(5) . . . . ? C7 C8 Fe1 C5 -132.2(4) . . . . ? C9 C8 Fe1 C5 108.0(4) . . . . ? C7 C8 Fe1 C6 -88.7(4) . . . . ? C9 C8 Fe1 C6 151.4(4) . . . . ? C7 C8 Fe1 C10 81.1(4) . . . . ? C9 C8 Fe1 C10 -38.7(4) . . . . ? C7 C8 Fe1 C11 37.3(4) . . . . ? C9 C8 Fe1 C11 -82.5(5) . . . . ? C7 C8 Fe1 C9 119.8(6) . . . . ? C7 C8 Fe1 C3 151.6(13) . . . . ? C9 C8 Fe1 C3 31.8(16) . . . . ? C7 C8 Fe1 C2 -52.6(7) . . . . ? C9 C8 Fe1 C2 -172.4(5) . . . . ? C2 C6 Fe1 C7 109.6(3) . . . . ? C5 C6 Fe1 C7 -130.6(3) . . . . ? C2 C6 Fe1 C4 -82.0(3) . . . . ? C5 C6 Fe1 C4 37.9(3) . . . . ? C2 C6 Fe1 C5 -119.8(4) . . . . ? C2 C6 Fe1 C8 152.4(3) . . . . ? C5 C6 Fe1 C8 -87.7(4) . . . . ? C2 C6 Fe1 C10 34.3(14) . . . . ? C5 C6 Fe1 C10 154.2(12) . . . . ? C2 C6 Fe1 C11 68.7(4) . . . . ? C5 C6 Fe1 C11 -171.4(4) . . . . ? C2 C6 Fe1 C9 -170.6(4) . . . . ? C5 C6 Fe1 C9 -50.7(5) . . . . ? C2 C6 Fe1 C3 -38.0(3) . . . . ? C5 C6 Fe1 C3 81.8(3) . . . . ? C5 C6 Fe1 C2 119.8(4) . . . . ? C11 C10 Fe1 C7 -38.2(3) . . . . ? C9 C10 Fe1 C7 81.4(4) . . . . ? C11 C10 Fe1 C4 153.0(4) . . . . ? C9 C10 Fe1 C4 -87.4(4) . . . . ? C11 C10 Fe1 C5 -172.1(4) . . . . ? C9 C10 Fe1 C5 -52.5(6) . . . . ? C11 C10 Fe1 C8 -81.3(4) . . . . ? C9 C10 Fe1 C8 38.3(3) . . . . ? C11 C10 Fe1 C6 41.0(14) . . . . ? C9 C10 Fe1 C6 160.7(11) . . . . ? C9 C10 Fe1 C11 119.6(6) . . . . ? C11 C10 Fe1 C9 -119.6(6) . . . . ? C11 C10 Fe1 C3 109.8(4) . . . . ? C9 C10 Fe1 C3 -130.6(4) . . . . ? C11 C10 Fe1 C2 69.8(4) . . . . ? C9 C10 Fe1 C2 -170.6(3) . . . . ? C10 C11 Fe1 C7 118.2(5) . . . . ? C7 C11 Fe1 C4 -169.6(4) . . . . ? C10 C11 Fe1 C4 -51.5(6) . . . . ? C7 C11 Fe1 C5 38.3(14) . . . . ? C10 C11 Fe1 C5 156.4(12) . . . . ? C7 C11 Fe1 C8 -36.7(3) . . . . ? C10 C11 Fe1 C8 81.5(4) . . . . ? C7 C11 Fe1 C6 71.2(4) . . . . ? C10 C11 Fe1 C6 -170.7(4) . . . . ? C7 C11 Fe1 C10 -118.2(5) . . . . ? C7 C11 Fe1 C9 -80.4(4) . . . . ? C10 C11 Fe1 C9 37.7(4) . . . . ? C7 C11 Fe1 C3 154.7(3) . . . . ? C10 C11 Fe1 C3 -87.1(4) . . . . ? C7 C11 Fe1 C2 110.8(3) . . . . ? C10 C11 Fe1 C2 -131.0(4) . . . . ? C8 C9 Fe1 C7 36.8(4) . . . . ? C10 C9 Fe1 C7 -81.0(4) . . . . ? C8 C9 Fe1 C4 -132.6(4) . . . . ? C10 C9 Fe1 C4 109.6(4) . . . . ? C8 C9 Fe1 C5 -89.4(4) . . . . ? C10 C9 Fe1 C5 152.8(4) . . . . ? C10 C9 Fe1 C8 -117.8(6) . . . . ? C8 C9 Fe1 C6 -55.3(6) . . . . ? C10 C9 Fe1 C6 -173.1(4) . . . . ? C8 C9 Fe1 C10 117.8(6) . . . . ? C8 C9 Fe1 C11 80.6(4) . . . . ? C10 C9 Fe1 C11 -37.3(4) . . . . ? C8 C9 Fe1 C3 -172.4(4) . . . . ? C10 C9 Fe1 C3 69.8(5) . . . . ? C8 C9 Fe1 C2 159.1(11) . . . . ? C10 C9 Fe1 C2 41.2(14) . . . . ? C4 C3 Fe1 C7 -174.4(5) . . . . ? C2 C3 Fe1 C7 -55.6(6) . . . . ? C2 C3 Fe1 C4 118.9(5) . . . . ? C4 C3 Fe1 C5 -37.6(3) . . . . ? C2 C3 Fe1 C5 81.2(4) . . . . ? C4 C3 Fe1 C8 42.6(15) . . . . ? C2 C3 Fe1 C8 161.5(13) . . . . ? C4 C3 Fe1 C6 -81.4(4) . . . . ? C2 C3 Fe1 C6 37.5(3) . . . . ? C4 C3 Fe1 C10 109.3(4) . . . . ? C2 C3 Fe1 C10 -131.8(4) . . . . ? C4 C3 Fe1 C11 152.3(4) . . . . ? C2 C3 Fe1 C11 -88.9(4) . . . . ? C4 C3 Fe1 C9 69.0(5) . . . . ? C2 C3 Fe1 C9 -172.1(4) . . . . ? C4 C3 Fe1 C2 -118.9(5) . . . . ? C6 C2 Fe1 C7 -88.8(4) . . . . ? C3 C2 Fe1 C7 152.0(4) . . . . ? C1 C2 Fe1 C7 32.4(6) . . . . ? C6 C2 Fe1 C4 81.3(4) . . . . ? C3 C2 Fe1 C4 -37.9(4) . . . . ? C1 C2 Fe1 C4 -157.5(5) . . . . ? C6 C2 Fe1 C5 37.4(3) . . . . ? C3 C2 Fe1 C5 -81.8(4) . . . . ? C1 C2 Fe1 C5 158.6(5) . . . . ? C6 C2 Fe1 C8 -53.9(6) . . . . ? C3 C2 Fe1 C8 -173.0(5) . . . . ? C1 C2 Fe1 C8 67.4(7) . . . . ? C3 C2 Fe1 C6 -119.2(5) . . . . ? C1 C2 Fe1 C6 121.2(6) . . . . ? C6 C2 Fe1 C10 -172.1(3) . . . . ? C3 C2 Fe1 C10 68.7(4) . . . . ? C1 C2 Fe1 C10 -50.9(5) . . . . ? C6 C2 Fe1 C11 -132.1(3) . . . . ? C3 C2 Fe1 C11 108.7(4) . . . . ? C1 C2 Fe1 C11 -10.9(5) . . . . ? C6 C2 Fe1 C9 153.3(12) . . . . ? C3 C2 Fe1 C9 34.1(14) . . . . ? C1 C2 Fe1 C9 -85.5(13) . . . . ? C6 C2 Fe1 C3 119.2(5) . . . . ? C1 C2 Fe1 C3 -119.6(6) . . . . ? C28 C27 Fe2 C34 -60.3(5) . . . . ? C26 C27 Fe2 C34 180.0(3) . . . . ? C26 C27 Fe2 C28 -119.7(5) . . . . ? C28 C27 Fe2 C35 -105(8) . . . . ? C26 C27 Fe2 C35 135(8) . . . . ? C28 C27 Fe2 C31 -175.9(3) . . . . ? C26 C27 Fe2 C31 64.4(5) . . . . ? C28 C27 Fe2 C33 -96.9(4) . . . . ? C26 C27 Fe2 C33 143.4(3) . . . . ? C28 C27 Fe2 C32 -140.0(3) . . . . ? C26 C27 Fe2 C32 100.4(3) . . . . ? C28 C27 Fe2 C29 37.4(3) . . . . ? C26 C27 Fe2 C29 -82.2(3) . . . . ? C28 C27 Fe2 C30 81.5(3) . . . . ? C26 C27 Fe2 C30 -38.1(3) . . . . ? C28 C27 Fe2 C26 119.7(5) . . . . ? C33 C34 Fe2 C27 -59.9(5) . . . . ? C35 C34 Fe2 C27 -177.9(4) . . . . ? C33 C34 Fe2 C28 -96.8(4) . . . . ? C35 C34 Fe2 C28 145.2(4) . . . . ? C33 C34 Fe2 C35 118.0(6) . . . . ? C33 C34 Fe2 C31 80.2(4) . . . . ? C35 C34 Fe2 C31 -37.8(4) . . . . ? C35 C34 Fe2 C33 -118.0(6) . . . . ? C33 C34 Fe2 C32 36.7(4) . . . . ? C35 C34 Fe2 C32 -81.3(4) . . . . ? C33 C34 Fe2 C29 -140.0(4) . . . . ? C35 C34 Fe2 C29 102.0(4) . . . . ? C33 C34 Fe2 C30 -177.2(4) . . . . ? C35 C34 Fe2 C30 64.9(5) . . . . ? C33 C34 Fe2 C26 -60(11) . . . . ? C35 C34 Fe2 C26 -178(100) . . . . ? C29 C28 Fe2 C27 119.3(5) . . . . ? C27 C28 Fe2 C34 141.6(3) . . . . ? C29 C28 Fe2 C34 -99.2(3) . . . . ? C27 C28 Fe2 C35 177.1(3) . . . . ? C29 C28 Fe2 C35 -63.7(4) . . . . ? C27 C28 Fe2 C31 69(4) . . . . ? C29 C28 Fe2 C31 -171(4) . . . . ? C27 C28 Fe2 C33 98.6(4) . . . . ? C29 C28 Fe2 C33 -142.1(3) . . . . ? C27 C28 Fe2 C32 61.8(4) . . . . ? C29 C28 Fe2 C32 -178.9(3) . . . . ? C27 C28 Fe2 C29 -119.3(5) . . . . ? C27 C28 Fe2 C30 -81.7(3) . . . . ? C29 C28 Fe2 C30 37.6(3) . . . . ? C27 C28 Fe2 C26 -37.7(3) . . . . ? C29 C28 Fe2 C26 81.6(3) . . . . ? C34 C35 Fe2 C27 47(8) . . . . ? C31 C35 Fe2 C27 -73(8) . . . . ? C31 C35 Fe2 C34 -119.3(5) . . . . ? C34 C35 Fe2 C28 -56.5(5) . . . . ? C31 C35 Fe2 C28 -175.8(3) . . . . ? C34 C35 Fe2 C31 119.3(5) . . . . ? C34 C35 Fe2 C33 38.1(3) . . . . ? C31 C35 Fe2 C33 -81.2(4) . . . . ? C34 C35 Fe2 C32 81.7(4) . . . . ? C31 C35 Fe2 C32 -37.7(3) . . . . ? C34 C35 Fe2 C29 -95.7(4) . . . . ? C31 C35 Fe2 C29 145.0(3) . . . . ? C34 C35 Fe2 C30 -140.4(3) . . . . ? C31 C35 Fe2 C30 100.3(4) . . . . ? C34 C35 Fe2 C26 179.9(3) . . . . ? C31 C35 Fe2 C26 60.6(5) . . . . ? C32 C31 Fe2 C27 58.3(5) . . . . ? C35 C31 Fe2 C27 177.2(3) . . . . ? C32 C31 Fe2 C34 -81.3(3) . . . . ? C35 C31 Fe2 C34 37.6(3) . . . . ? C32 C31 Fe2 C28 -8(5) . . . . ? C35 C31 Fe2 C28 111(4) . . . . ? C32 C31 Fe2 C35 -118.9(5) . . . . ? C32 C31 Fe2 C33 -37.8(3) . . . . ? C35 C31 Fe2 C33 81.1(3) . . . . ? C35 C31 Fe2 C32 118.9(5) . . . . ? C32 C31 Fe2 C29 -178.8(3) . . . . ? C35 C31 Fe2 C29 -59.9(5) . . . . ? C32 C31 Fe2 C30 142.4(3) . . . . ? C35 C31 Fe2 C30 -98.7(3) . . . . ? C32 C31 Fe2 C26 97.9(3) . . . . ? C35 C31 Fe2 C26 -143.2(3) . . . . ? C34 C33 Fe2 C27 141.8(4) . . . . ? C32 C33 Fe2 C27 -97.4(4) . . . . ? C32 C33 Fe2 C34 120.8(6) . . . . ? C34 C33 Fe2 C28 98.6(4) . . . . ? C32 C33 Fe2 C28 -140.6(4) . . . . ? C34 C33 Fe2 C35 -38.5(4) . . . . ? C32 C33 Fe2 C35 82.3(4) . . . . ? C34 C33 Fe2 C31 -82.9(4) . . . . ? C32 C33 Fe2 C31 37.9(4) . . . . ? C34 C33 Fe2 C32 -120.8(6) . . . . ? C34 C33 Fe2 C29 62.6(5) . . . . ? C32 C33 Fe2 C29 -176.6(4) . . . . ? C34 C33 Fe2 C30 91(7) . . . . ? C32 C33 Fe2 C30 -148(7) . . . . ? C34 C33 Fe2 C26 178.4(4) . . . . ? C32 C33 Fe2 C26 -60.8(6) . . . . ? C33 C32 Fe2 C27 98.2(4) . . . . ? C31 C32 Fe2 C27 -143.1(3) . . . . ? C33 C32 Fe2 C34 -36.6(4) . . . . ? C31 C32 Fe2 C34 82.1(4) . . . . ? C33 C32 Fe2 C28 60.7(5) . . . . ? C31 C32 Fe2 C28 179.4(3) . . . . ? C33 C32 Fe2 C35 -80.6(4) . . . . ? C31 C32 Fe2 C35 38.1(3) . . . . ? C33 C32 Fe2 C31 -118.7(5) . . . . ? C31 C32 Fe2 C33 118.7(5) . . . . ? C33 C32 Fe2 C29 48(4) . . . . ? C31 C32 Fe2 C29 167(4) . . . . ? C33 C32 Fe2 C30 178.5(4) . . . . ? C31 C32 Fe2 C30 -62.8(5) . . . . ? C33 C32 Fe2 C26 142.1(4) . . . . ? C31 C32 Fe2 C26 -99.2(4) . . . . ? C28 C29 Fe2 C27 -37.6(3) . . . . ? C30 C29 Fe2 C27 82.1(3) . . . . ? C28 C29 Fe2 C34 97.0(4) . . . . ? C30 C29 Fe2 C34 -143.3(3) . . . . ? C30 C29 Fe2 C28 119.7(5) . . . . ? C28 C29 Fe2 C35 141.1(3) . . . . ? C30 C29 Fe2 C35 -99.2(4) . . . . ? C28 C29 Fe2 C31 179.3(3) . . . . ? C30 C29 Fe2 C31 -61.0(5) . . . . ? C28 C29 Fe2 C33 59.0(5) . . . . ? C30 C29 Fe2 C33 178.7(4) . . . . ? C28 C29 Fe2 C32 14(4) . . . . ? C30 C29 Fe2 C32 133(4) . . . . ? C28 C29 Fe2 C30 -119.7(5) . . . . ? C28 C29 Fe2 C26 -81.8(3) . . . . ? C30 C29 Fe2 C26 37.9(3) . . . . ? C29 C30 Fe2 C27 -80.7(4) . . . . ? C26 C30 Fe2 C27 38.2(4) . . . . ? C29 C30 Fe2 C34 59.4(5) . . . . ? C26 C30 Fe2 C34 178.4(4) . . . . ? C29 C30 Fe2 C28 -37.1(3) . . . . ? C26 C30 Fe2 C28 81.8(4) . . . . ? C29 C30 Fe2 C35 99.5(4) . . . . ? C26 C30 Fe2 C35 -141.5(4) . . . . ? C29 C30 Fe2 C31 144.4(4) . . . . ? C26 C30 Fe2 C31 -96.6(4) . . . . ? C29 C30 Fe2 C33 -29(7) . . . . ? C26 C30 Fe2 C33 90(7) . . . . ? C29 C30 Fe2 C32 -176.4(4) . . . . ? C26 C30 Fe2 C32 -57.5(5) . . . . ? C26 C30 Fe2 C29 119.0(5) . . . . ? C29 C30 Fe2 C26 -119.0(5) . . . . ? C30 C26 Fe2 C27 -118.5(5) . . . . ? C25 C26 Fe2 C27 118.8(6) . . . . ? C27 C26 Fe2 C34 0(11) . . . . ? C30 C26 Fe2 C34 -119(11) . . . . ? C25 C26 Fe2 C34 119(11) . . . . ? C27 C26 Fe2 C28 37.2(3) . . . . ? C30 C26 Fe2 C28 -81.3(4) . . . . ? C25 C26 Fe2 C28 156.0(6) . . . . ? C27 C26 Fe2 C35 -177.8(4) . . . . ? C30 C26 Fe2 C35 63.7(5) . . . . ? C25 C26 Fe2 C35 -59.0(6) . . . . ? C27 C26 Fe2 C31 -139.8(3) . . . . ? C30 C26 Fe2 C31 101.7(4) . . . . ? C25 C26 Fe2 C31 -21.0(6) . . . . ? C27 C26 Fe2 C33 -58.7(5) . . . . ? C30 C26 Fe2 C33 -177.2(4) . . . . ? C25 C26 Fe2 C33 60.1(7) . . . . ? C27 C26 Fe2 C32 -96.1(4) . . . . ? C30 C26 Fe2 C32 145.4(4) . . . . ? C25 C26 Fe2 C32 22.7(6) . . . . ? C27 C26 Fe2 C29 80.6(4) . . . . ? C30 C26 Fe2 C29 -37.9(4) . . . . ? C25 C26 Fe2 C29 -160.6(6) . . . . ? C27 C26 Fe2 C30 118.5(5) . . . . ? C25 C26 Fe2 C30 -122.7(7) . . . . ? C56 C55 Fe3 C59 -118.6(4) . . . . ? C59 C55 Fe3 C54 -73.1(4) . . . . ? C56 C55 Fe3 C54 168.3(3) . . . . ? C59 C55 Fe3 C50 -112.4(3) . . . . ? C56 C55 Fe3 C50 129.0(3) . . . . ? C59 C55 Fe3 C51 -155.9(3) . . . . ? C56 C55 Fe3 C51 85.4(4) . . . . ? C59 C55 Fe3 C52 172.5(4) . . . . ? C56 C55 Fe3 C52 53.9(5) . . . . ? C59 C55 Fe3 C56 118.6(4) . . . . ? C59 C55 Fe3 C58 37.4(3) . . . . ? C56 C55 Fe3 C58 -81.2(3) . . . . ? C59 C55 Fe3 C57 81.3(3) . . . . ? C56 C55 Fe3 C57 -37.3(3) . . . . ? C59 C55 Fe3 C53 -48.8(11) . . . . ? C56 C55 Fe3 C53 -167.4(9) . . . . ? C58 C59 Fe3 C55 119.4(5) . . . . ? C55 C59 Fe3 C54 127.0(3) . . . . ? C58 C59 Fe3 C54 -113.5(4) . . . . ? C55 C59 Fe3 C50 83.4(4) . . . . ? C58 C59 Fe3 C50 -157.2(4) . . . . ? C55 C59 Fe3 C51 46.5(6) . . . . ? C58 C59 Fe3 C51 165.9(5) . . . . ? C55 C59 Fe3 C52 -160.8(11) . . . . ? C58 C59 Fe3 C52 -41.4(13) . . . . ? C55 C59 Fe3 C56 -38.1(3) . . . . ? C58 C59 Fe3 C56 81.4(4) . . . . ? C55 C59 Fe3 C58 -119.4(5) . . . . ? C55 C59 Fe3 C57 -81.6(4) . . . . ? C58 C59 Fe3 C57 37.8(4) . . . . ? C55 C59 Fe3 C53 167.3(3) . . . . ? C58 C59 Fe3 C53 -73.3(4) . . . . ? C50 C54 Fe3 C55 -68.6(4) . . . . ? C53 C54 Fe3 C55 172.0(3) . . . . ? C50 C54 Fe3 C59 -109.1(3) . . . . ? C53 C54 Fe3 C59 131.4(3) . . . . ? C53 C54 Fe3 C50 -119.4(4) . . . . ? C50 C54 Fe3 C51 38.6(3) . . . . ? C53 C54 Fe3 C51 -80.9(3) . . . . ? C50 C54 Fe3 C52 82.4(3) . . . . ? C53 C54 Fe3 C52 -37.0(3) . . . . ? C50 C54 Fe3 C56 -36.7(10) . . . . ? C53 C54 Fe3 C56 -156.1(8) . . . . ? C50 C54 Fe3 C58 -151.9(3) . . . . ? C53 C54 Fe3 C58 88.7(4) . . . . ? C50 C54 Fe3 C57 173.2(4) . . . . ? C53 C54 Fe3 C57 53.7(6) . . . . ? C50 C54 Fe3 C53 119.4(4) . . . . ? C54 C50 Fe3 C55 130.1(3) . . . . ? C51 C50 Fe3 C55 -111.1(4) . . . . ? C49 C50 Fe3 C55 9.1(5) . . . . ? C54 C50 Fe3 C59 88.4(4) . . . . ? C51 C50 Fe3 C59 -152.8(4) . . . . ? C49 C50 Fe3 C59 -32.5(6) . . . . ? C51 C50 Fe3 C54 118.8(5) . . . . ? C49 C50 Fe3 C54 -121.0(6) . . . . ? C54 C50 Fe3 C51 -118.8(5) . . . . ? C49 C50 Fe3 C51 120.2(7) . . . . ? C54 C50 Fe3 C52 -80.7(4) . . . . ? C51 C50 Fe3 C52 38.1(4) . . . . ? C49 C50 Fe3 C52 158.3(5) . . . . ? C54 C50 Fe3 C56 169.3(3) . . . . ? C51 C50 Fe3 C56 -72.0(4) . . . . ? C49 C50 Fe3 C56 48.3(5) . . . . ? C54 C50 Fe3 C58 57.5(6) . . . . ? C51 C50 Fe3 C58 176.3(5) . . . . ? C49 C50 Fe3 C58 -63.5(8) . . . . ? C54 C50 Fe3 C57 -167.3(8) . . . . ? C51 C50 Fe3 C57 -48.5(10) . . . . ? C49 C50 Fe3 C57 71.7(10) . . . . ? C54 C50 Fe3 C53 -37.6(3) . . . . ? C51 C50 Fe3 C53 81.2(4) . . . . ? C49 C50 Fe3 C53 -158.6(5) . . . . ? C52 C51 Fe3 C55 -156.7(4) . . . . ? C50 C51 Fe3 C55 85.2(4) . . . . ? C52 C51 Fe3 C59 172.1(5) . . . . ? C50 C51 Fe3 C59 54.0(7) . . . . ? C52 C51 Fe3 C54 80.4(4) . . . . ? C50 C51 Fe3 C54 -37.8(3) . . . . ? C52 C51 Fe3 C50 118.2(6) . . . . ? C50 C51 Fe3 C52 -118.2(6) . . . . ? C52 C51 Fe3 C56 -114.2(4) . . . . ? C50 C51 Fe3 C56 127.6(4) . . . . ? C52 C51 Fe3 C58 -53.6(14) . . . . ? C50 C51 Fe3 C58 -171.8(11) . . . . ? C52 C51 Fe3 C57 -75.4(5) . . . . ? C50 C51 Fe3 C57 166.4(4) . . . . ? C52 C51 Fe3 C53 36.5(3) . . . . ? C50 C51 Fe3 C53 -81.7(4) . . . . ? C53 C52 Fe3 C55 166.9(4) . . . . ? C51 C52 Fe3 C55 46.2(6) . . . . ? C53 C52 Fe3 C59 -38.5(13) . . . . ? C51 C52 Fe3 C59 -159.2(10) . . . . ? C53 C52 Fe3 C54 37.7(3) . . . . ? C51 C52 Fe3 C54 -83.0(4) . . . . ? C53 C52 Fe3 C50 81.7(3) . . . . ? C51 C52 Fe3 C50 -38.9(4) . . . . ? C53 C52 Fe3 C51 120.7(5) . . . . ? C53 C52 Fe3 C56 -156.6(3) . . . . ? C51 C52 Fe3 C56 82.7(4) . . . . ? C53 C52 Fe3 C58 -72.8(4) . . . . ? C51 C52 Fe3 C58 166.5(4) . . . . ? C53 C52 Fe3 C57 -113.4(3) . . . . ? C51 C52 Fe3 C57 125.9(4) . . . . ? C51 C52 Fe3 C53 -120.7(5) . . . . ? C57 C56 Fe3 C55 -119.4(5) . . . . ? C57 C56 Fe3 C59 -81.7(4) . . . . ? C55 C56 Fe3 C59 37.7(3) . . . . ? C57 C56 Fe3 C54 -159.5(8) . . . . ? C55 C56 Fe3 C54 -40.1(10) . . . . ? C57 C56 Fe3 C50 171.2(3) . . . . ? C55 C56 Fe3 C50 -69.3(4) . . . . ? C57 C56 Fe3 C51 130.0(3) . . . . ? C55 C56 Fe3 C51 -110.6(3) . . . . ? C57 C56 Fe3 C52 87.5(4) . . . . ? C55 C56 Fe3 C52 -153.0(3) . . . . ? C57 C56 Fe3 C58 -38.1(3) . . . . ? C55 C56 Fe3 C58 81.3(3) . . . . ? C55 C56 Fe3 C57 119.4(5) . . . . ? C57 C56 Fe3 C53 54.7(6) . . . . ? C55 C56 Fe3 C53 174.1(4) . . . . ? C59 C58 Fe3 C55 -37.3(3) . . . . ? C57 C58 Fe3 C55 81.7(4) . . . . ? C57 C58 Fe3 C59 119.0(6) . . . . ? C59 C58 Fe3 C54 84.7(4) . . . . ? C57 C58 Fe3 C54 -156.3(4) . . . . ? C59 C58 Fe3 C50 45.4(7) . . . . ? C57 C58 Fe3 C50 164.4(5) . . . . ? C59 C58 Fe3 C51 -145.8(11) . . . . ? C57 C58 Fe3 C51 -26.8(14) . . . . ? C59 C58 Fe3 C52 170.2(4) . . . . ? C57 C58 Fe3 C52 -70.8(5) . . . . ? C59 C58 Fe3 C56 -81.2(4) . . . . ? C57 C58 Fe3 C56 37.8(4) . . . . ? C59 C58 Fe3 C57 -119.0(6) . . . . ? C59 C58 Fe3 C53 129.0(4) . . . . ? C57 C58 Fe3 C53 -112.0(4) . . . . ? C56 C57 Fe3 C55 37.6(3) . . . . ? C58 C57 Fe3 C55 -80.9(4) . . . . ? C56 C57 Fe3 C59 81.0(4) . . . . ? C58 C57 Fe3 C59 -37.6(4) . . . . ? C56 C57 Fe3 C54 168.9(4) . . . . ? C58 C57 Fe3 C54 50.4(6) . . . . ? C56 C57 Fe3 C50 -29.5(10) . . . . ? C58 C57 Fe3 C50 -148.0(8) . . . . ? C56 C57 Fe3 C51 -68.7(4) . . . . ? C58 C57 Fe3 C51 172.8(4) . . . . ? C56 C57 Fe3 C52 -110.8(4) . . . . ? C58 C57 Fe3 C52 130.7(4) . . . . ? C58 C57 Fe3 C56 -118.5(5) . . . . ? C56 C57 Fe3 C58 118.5(5) . . . . ? C56 C57 Fe3 C53 -153.7(3) . . . . ? C58 C57 Fe3 C53 87.8(4) . . . . ? C52 C53 Fe3 C55 -149.5(9) . . . . ? C54 C53 Fe3 C55 -29.9(11) . . . . ? C52 C53 Fe3 C59 170.8(3) . . . . ? C54 C53 Fe3 C59 -69.6(4) . . . . ? C52 C53 Fe3 C54 -119.6(5) . . . . ? C52 C53 Fe3 C50 -82.0(3) . . . . ? C54 C53 Fe3 C50 37.7(3) . . . . ? C52 C53 Fe3 C51 -37.1(3) . . . . ? C54 C53 Fe3 C51 82.6(3) . . . . ? C54 C53 Fe3 C52 119.6(5) . . . . ? C52 C53 Fe3 C56 48.0(6) . . . . ? C54 C53 Fe3 C56 167.6(4) . . . . ? C52 C53 Fe3 C58 129.4(3) . . . . ? C54 C53 Fe3 C58 -111.0(3) . . . . ? C52 C53 Fe3 C57 85.4(4) . . . . ? C54 C53 Fe3 C57 -155.0(3) . . . . ? C2 C1 N1 C12 123.3(5) . . . . ? P1 C1 N1 C12 -118.0(4) . . . . ? C2 C1 N1 P1 -118.7(4) . . . . ? C26 C25 N2 C36 -123.5(5) . . . . ? P2 C25 N2 C36 118.6(4) . . . . ? C26 C25 N2 P2 117.8(5) . . . . ? C50 C49 N3 C60 -123.1(5) . . . . ? P3 C49 N3 C60 117.3(4) . . . . ? C50 C49 N3 P3 119.5(4) . . . . ? C12 N1 P1 C13 -150.7(4) . . . . ? C1 N1 P1 C13 101.3(3) . . . . ? C12 N1 P1 C1 108.0(5) . . . . ? C12 N1 P1 W1 1.2(5) . . . . ? C1 N1 P1 W1 -106.8(3) . . . . ? Si1 C13 P1 N1 69.8(3) . . . . ? Si2 C13 P1 N1 -147.1(2) . . . . ? Si1 C13 P1 C1 121.0(3) . . . . ? Si2 C13 P1 C1 -95.9(3) . . . . ? Si1 C13 P1 W1 -80.3(3) . . . . ? Si2 C13 P1 W1 62.8(3) . . . . ? C2 C1 P1 N1 101.8(5) . . . . ? C2 C1 P1 C13 7.7(5) . . . . ? N1 C1 P1 C13 -94.0(3) . . . . ? C2 C1 P1 W1 -152.1(4) . . . . ? N1 C1 P1 W1 106.1(3) . . . . ? C36 N2 P2 C37 146.7(4) . . . . ? C25 N2 P2 C37 -104.0(3) . . . . ? C36 N2 P2 C25 -109.3(5) . . . . ? C36 N2 P2 W2 -4.3(5) . . . . ? C25 N2 P2 W2 105.0(3) . . . . ? Si3 C37 P2 N2 -71.4(3) . . . . ? Si4 C37 P2 N2 147.3(3) . . . . ? Si3 C37 P2 C25 -122.0(3) . . . . ? Si4 C37 P2 C25 96.7(3) . . . . ? Si3 C37 P2 W2 77.2(3) . . . . ? Si4 C37 P2 W2 -64.1(3) . . . . ? C26 C25 P2 N2 -105.2(6) . . . . ? N2 C25 P2 C37 91.7(3) . . . . ? C26 C25 P2 C37 -13.4(6) . . . . ? N2 C25 P2 W2 -106.0(3) . . . . ? C26 C25 P2 W2 148.8(4) . . . . ? C60 N3 P3 C61 150.5(4) . . . . ? C49 N3 P3 C61 -101.6(3) . . . . ? C60 N3 P3 C49 -107.9(5) . . . . ? C60 N3 P3 W3 -0.1(5) . . . . ? C49 N3 P3 W3 107.8(3) . . . . ? Si5 C61 P3 N3 -70.2(3) . . . . ? Si6 C61 P3 N3 147.2(2) . . . . ? Si5 C61 P3 C49 -121.1(3) . . . . ? Si6 C61 P3 C49 96.3(3) . . . . ? Si5 C61 P3 W3 78.0(3) . . . . ? Si6 C61 P3 W3 -64.6(3) . . . . ? C50 C49 P3 N3 -101.5(5) . . . . ? N3 C49 P3 C61 94.1(3) . . . . ? C50 C49 P3 C61 -7.4(5) . . . . ? N3 C49 P3 W3 -103.9(3) . . . . ? C50 C49 P3 W3 154.5(4) . . . . ? P1 C13 Si1 C14 -125.6(3) . . . . ? Si2 C13 Si1 C14 92.4(3) . . . . ? P1 C13 Si1 C15 -6.7(4) . . . . ? Si2 C13 Si1 C15 -148.6(3) . . . . ? P1 C13 Si1 C16 117.1(3) . . . . ? Si2 C13 Si1 C16 -24.8(4) . . . . ? P1 C13 Si2 C19 44.1(3) . . . . ? Si1 C13 Si2 C19 -173.6(3) . . . . ? P1 C13 Si2 C17 -78.9(3) . . . . ? Si1 C13 Si2 C17 63.5(4) . . . . ? P1 C13 Si2 C18 159.7(3) . . . . ? Si1 C13 Si2 C18 -57.9(4) . . . . ? P2 C37 Si3 C39 -115.1(3) . . . . ? Si4 C37 Si3 C39 25.2(4) . . . . ? P2 C37 Si3 C40 7.3(4) . . . . ? Si4 C37 Si3 C40 147.6(3) . . . . ? P2 C37 Si3 C38 125.9(3) . . . . ? Si4 C37 Si3 C38 -93.7(3) . . . . ? P2 C37 Si4 C42 -46.5(3) . . . . ? Si3 C37 Si4 C42 172.8(3) . . . . ? P2 C37 Si4 C43 -162.7(3) . . . . ? Si3 C37 Si4 C43 56.6(3) . . . . ? P2 C37 Si4 C41 75.5(3) . . . . ? Si3 C37 Si4 C41 -65.2(4) . . . . ? P3 C61 Si5 C63 -118.0(3) . . . . ? Si6 C61 Si5 C63 22.6(4) . . . . ? P3 C61 Si5 C62 5.5(4) . . . . ? Si6 C61 Si5 C62 146.1(3) . . . . ? P3 C61 Si5 C64 123.9(3) . . . . ? Si6 C61 Si5 C64 -95.5(3) . . . . ? P3 C61 Si6 C65 -39.9(3) . . . . ? Si5 C61 Si6 C65 178.4(3) . . . . ? P3 C61 Si6 C66 82.2(4) . . . . ? Si5 C61 Si6 C66 -59.5(4) . . . . ? P3 C61 Si6 C67 -156.9(3) . . . . ? Si5 C61 Si6 C67 61.4(3) . . . . ? O1 C20 W1 C21 -88(56) . . . . ? O1 C20 W1 C23 92(56) . . . . ? O1 C20 W1 C22 0(56) . . . . ? O1 C20 W1 C24 -180(100) . . . . ? O1 C20 W1 P1 18(58) . . . . ? O2 C21 W1 C20 11(5) . . . . ? O2 C21 W1 C23 14(7) . . . . ? O2 C21 W1 C22 -80(5) . . . . ? O2 C21 W1 C24 101(5) . . . . ? O2 C21 W1 P1 -166(5) . . . . ? O4 C23 W1 C20 28(10) . . . . ? O4 C23 W1 C21 25(11) . . . . ? O4 C23 W1 C22 120(10) . . . . ? O4 C23 W1 C24 -62(10) . . . . ? O4 C23 W1 P1 -154(10) . . . . ? O3 C22 W1 C20 -170(100) . . . . ? O3 C22 W1 C21 -83(46) . . . . ? O3 C22 W1 C23 103(46) . . . . ? O3 C22 W1 C24 12(51) . . . . ? O3 C22 W1 P1 11(46) . . . . ? O5 C24 W1 C20 -45(9) . . . . ? O5 C24 W1 C21 -132(9) . . . . ? O5 C24 W1 C23 42(9) . . . . ? O5 C24 W1 C22 133(9) . . . . ? O5 C24 W1 P1 134(9) . . . . ? N1 P1 W1 C20 42(3) . . . . ? C13 P1 W1 C20 -172(3) . . . . ? C1 P1 W1 C20 -16(3) . . . . ? N1 P1 W1 C21 148.1(3) . . . . ? C13 P1 W1 C21 -66.4(3) . . . . ? C1 P1 W1 C21 89.6(3) . . . . ? N1 P1 W1 C23 -31.9(3) . . . . ? C13 P1 W1 C23 113.5(3) . . . . ? C1 P1 W1 C23 -90.4(2) . . . . ? N1 P1 W1 C22 59.6(2) . . . . ? C13 P1 W1 C22 -154.9(3) . . . . ? C1 P1 W1 C22 1.1(2) . . . . ? N1 P1 W1 C24 -120.3(2) . . . . ? C13 P1 W1 C24 25.1(3) . . . . ? C1 P1 W1 C24 -178.9(2) . . . . ? O6 C44 W2 C48 -85(14) . . . . ? O6 C44 W2 C46 95(14) . . . . ? O6 C44 W2 C45 1(14) . . . . ? O6 C44 W2 C47 -176(100) . . . . ? O6 C44 W2 P2 56(15) . . . . ? O10 C48 W2 C44 32(13) . . . . ? O10 C48 W2 C46 -76(34) . . . . ? O10 C48 W2 C45 -55(13) . . . . ? O10 C48 W2 C47 121(13) . . . . ? O10 C48 W2 P2 -145(13) . . . . ? O8 C46 W2 C44 -151(82) . . . . ? O8 C46 W2 C48 -43(100) . . . . ? O8 C46 W2 C45 -64(82) . . . . ? O8 C46 W2 C47 120(82) . . . . ? O8 C46 W2 P2 26(82) . . . . ? O7 C45 W2 C44 -55(7) . . . . ? O7 C45 W2 C48 36(7) . . . . ? O7 C45 W2 C46 -145(7) . . . . ? O7 C45 W2 C47 -12(9) . . . . ? O7 C45 W2 P2 128(7) . . . . ? O9 C47 W2 C44 -4(11) . . . . ? O9 C47 W2 C48 -95(11) . . . . ? O9 C47 W2 C46 85(11) . . . . ? O9 C47 W2 C45 -48(12) . . . . ? O9 C47 W2 P2 172(11) . . . . ? N2 P2 W2 C44 -15(3) . . . . ? C37 P2 W2 C44 -159(3) . . . . ? C25 P2 W2 C44 42(3) . . . . ? N2 P2 W2 C48 125.7(2) . . . . ? C37 P2 W2 C48 -18.3(3) . . . . ? C25 P2 W2 C48 -177.2(3) . . . . ? N2 P2 W2 C46 -53.9(3) . . . . ? C37 P2 W2 C46 162.1(3) . . . . ? C25 P2 W2 C46 3.2(3) . . . . ? N2 P2 W2 C45 40.3(2) . . . . ? C37 P2 W2 C45 -103.7(3) . . . . ? C25 P2 W2 C45 97.3(3) . . . . ? N2 P2 W2 C47 -142.8(2) . . . . ? C37 P2 W2 C47 73.2(3) . . . . ? C25 P2 W2 C47 -85.7(3) . . . . ? O11 C68 W3 C71 -44(7) . . . . ? O11 C68 W3 C69 139(7) . . . . ? O11 C68 W3 C70 -131(7) . . . . ? O11 C68 W3 C72 48(7) . . . . ? O11 C68 W3 P3 -8(9) . . . . ? O14 C71 W3 C68 -14(6) . . . . ? O14 C71 W3 C69 6(7) . . . . ? O14 C71 W3 C70 78(6) . . . . ? O14 C71 W3 C72 -103(6) . . . . ? O14 C71 W3 P3 169(6) . . . . ? O12 C69 W3 C68 16(8) . . . . ? O12 C69 W3 C71 -4(9) . . . . ? O12 C69 W3 C70 -76(8) . . . . ? O12 C69 W3 C72 105(8) . . . . ? O12 C69 W3 P3 -167(8) . . . . ? O13 C70 W3 C68 59(7) . . . . ? O13 C70 W3 C71 -26(7) . . . . ? O13 C70 W3 C69 147(7) . . . . ? O13 C70 W3 C72 -64(11) . . . . ? O13 C70 W3 P3 -117(7) . . . . ? O15 C72 W3 C68 111(100) . . . . ? O15 C72 W3 C71 -164(100) . . . . ? O15 C72 W3 C69 23(100) . . . . ? O15 C72 W3 C70 -126(100) . . . . ? O15 C72 W3 P3 -72(100) . . . . ? N3 P3 W3 C68 -3(2) . . . . ? C61 P3 W3 C68 -147(2) . . . . ? C49 P3 W3 C68 54(2) . . . . ? N3 P3 W3 C71 31.9(2) . . . . ? C61 P3 W3 C71 -111.9(3) . . . . ? C49 P3 W3 C71 89.5(2) . . . . ? N3 P3 W3 C69 -150.2(2) . . . . ? C61 P3 W3 C69 66.0(3) . . . . ? C49 P3 W3 C69 -92.6(2) . . . . ? N3 P3 W3 C70 119.1(2) . . . . ? C61 P3 W3 C70 -24.8(3) . . . . ? C49 P3 W3 C70 176.7(2) . . . . ? N3 P3 W3 C72 -59.3(2) . . . . ? C61 P3 W3 C72 156.8(2) . . . . ? C49 P3 W3 C72 -1.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.989 _refine_diff_density_min -1.823 _refine_diff_density_rms 0.170 #------------------------------------------------------------------------------ data_greg588 _database_code_depnum_ccdc_archive 'CCDC 743281' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 N O6 P Si2 W' _chemical_formula_sum 'C18 H26 N O6 P Si2 W' _chemical_formula_weight 623.40 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2166(3) _cell_length_b 9.7609(5) _cell_length_c 15.0733(4) _cell_angle_alpha 73.292(2) _cell_angle_beta 74.587(2) _cell_angle_gamma 78.755(2) _cell_volume 1241.70(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4133 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 4.843 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.18752 _exptl_absorpt_correction_T_max 0.28702 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _diffrn_reflns_number 14037 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5794 _reflns_number_gt 5181 _reflns_threshold_expression >2sigma(I) _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^)+(0.0238P)^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 5794 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.002 _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 C1 C 0.3877(4) 0.7419(4) 0.7377(2) 0.0161(8) Uani 1 1 d . . . H1A H 0.3379 0.7426 0.6861 0.019 Uiso 1 1 calc R . . C2 C 0.2993(4) 0.8276(4) 0.8040(2) 0.0178(8) Uani 1 1 d . . . C3 C 0.2813(4) 0.8114(5) 0.8988(3) 0.0240(9) Uani 1 1 d . . . H3A H 0.3248 0.7330 0.9420 0.029 Uiso 1 1 calc R . . C4 C 0.1836(4) 0.9361(5) 0.9204(3) 0.0293(10) Uani 1 1 d . . . H4A H 0.1498 0.9574 0.9808 0.035 Uiso 1 1 calc R . . C5 C 0.1487(4) 1.0176(5) 0.8384(3) 0.0292(10) Uani 1 1 d . . . H5A H 0.0850 1.1074 0.8317 0.035 Uiso 1 1 calc R . . C6 C 0.4315(4) 0.4742(5) 0.7574(3) 0.0228(9) Uani 1 1 d . . . H6C H 0.5053 0.3909 0.7765 0.034 Uiso 1 1 calc R . . H6B H 0.4392 0.4947 0.6889 0.034 Uiso 1 1 calc R . . H6A H 0.3288 0.4528 0.7917 0.034 Uiso 1 1 calc R . . C7 C 0.6673(4) 0.7694(4) 0.7889(2) 0.0141(7) Uani 1 1 d . . . H7A H 0.5733 0.7788 0.8396 0.017 Uiso 1 1 calc R . . C8 C 0.7891(5) 0.4406(5) 0.8460(3) 0.0284(9) Uani 1 1 d . . . H8A H 0.8331 0.4364 0.7799 0.043 Uiso 1 1 calc R . . H8B H 0.6837 0.4204 0.8637 0.043 Uiso 1 1 calc R . . H8C H 0.8478 0.3687 0.8877 0.043 Uiso 1 1 calc R . . C9 C 0.9964(5) 0.6576(6) 0.8238(3) 0.0395(12) Uani 1 1 d . . . H9A H 1.0027 0.7520 0.8323 0.059 Uiso 1 1 calc R . . H9B H 1.0378 0.6561 0.7571 0.059 Uiso 1 1 calc R . . H9C H 1.0549 0.5822 0.8639 0.059 Uiso 1 1 calc R . . C10 C 0.7176(5) 0.6245(6) 0.9869(3) 0.0352(11) Uani 1 1 d . . . H10A H 0.6120 0.6047 1.0062 0.053 Uiso 1 1 calc R . . H10B H 0.7222 0.7191 0.9957 0.053 Uiso 1 1 calc R . . H10C H 0.7785 0.5500 1.0259 0.053 Uiso 1 1 calc R . . C11 C 0.7319(5) 1.0139(5) 0.8535(3) 0.0318(10) Uani 1 1 d . . . H11A H 0.8175 0.9529 0.8781 0.048 Uiso 1 1 calc R . . H11B H 0.6382 1.0008 0.9027 0.048 Uiso 1 1 calc R . . H11C H 0.7490 1.1152 0.8356 0.048 Uiso 1 1 calc R . . C12 C 0.5508(4) 1.0809(5) 0.7037(3) 0.0246(9) Uani 1 1 d . . . H12A H 0.4610 1.0765 0.7562 0.037 Uiso 1 1 calc R . . H12B H 0.5307 1.0485 0.6528 0.037 Uiso 1 1 calc R . . H12C H 0.5744 1.1804 0.6792 0.037 Uiso 1 1 calc R . . C13 C 0.8943(4) 0.9886(5) 0.6537(3) 0.0232(9) Uani 1 1 d . . . H13C H 0.9180 1.0866 0.6424 0.035 Uiso 1 1 calc R . . H13B H 0.8814 0.9744 0.5945 0.035 Uiso 1 1 calc R . . H13A H 0.9775 0.9186 0.6752 0.035 Uiso 1 1 calc R . . C14 C 0.8295(4) 0.6679(5) 0.4120(3) 0.0249(9) Uani 1 1 d . . . C15 C 0.7690(4) 0.4679(5) 0.5975(2) 0.0177(8) Uani 1 1 d . . . C16 C 0.9418(4) 0.6936(5) 0.5659(2) 0.0206(8) Uani 1 1 d . . . C17 C 0.7009(4) 0.9068(5) 0.4929(2) 0.0180(8) Uani 1 1 d . . . C18 C 0.5316(4) 0.6702(4) 0.5200(2) 0.0188(8) Uani 1 1 d . . . N1 N 0.4633(3) 0.6002(4) 0.7802(2) 0.0183(7) Uani 1 1 d . . . O1 O 0.2185(3) 0.9525(3) 0.76576(17) 0.0227(6) Uani 1 1 d . . . O2 O 0.8809(3) 0.6570(4) 0.33549(18) 0.0366(8) Uani 1 1 d . . . O3 O 0.7908(3) 0.3475(3) 0.62780(19) 0.0260(6) Uani 1 1 d . . . O4 O 1.0605(3) 0.6935(4) 0.5758(2) 0.0319(7) Uani 1 1 d . . . O5 O 0.6837(3) 1.0274(3) 0.46335(19) 0.0303(7) Uani 1 1 d . . . O6 O 0.4203(3) 0.6568(3) 0.50484(19) 0.0272(7) Uani 1 1 d . . . P P 0.59622(10) 0.71066(11) 0.70707(6) 0.01326(19) Uani 1 1 d . . . Si1 Si 0.79416(11) 0.62421(13) 0.85852(7) 0.0195(2) Uani 1 1 d . . . Si2 Si 0.71473(11) 0.96207(12) 0.74690(7) 0.0178(2) Uani 1 1 d . . . W W 0.733587(14) 0.686241(16) 0.544747(8) 0.01409(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0139(16) 0.019(2) 0.0177(16) -0.0054(15) -0.0038(13) -0.0054(16) C2 0.0112(16) 0.021(2) 0.0224(17) -0.0071(16) -0.0037(14) -0.0024(16) C3 0.0183(18) 0.034(3) 0.0214(18) -0.0115(18) -0.0023(15) -0.0033(18) C4 0.022(2) 0.042(3) 0.028(2) -0.021(2) -0.0009(16) -0.002(2) C5 0.0197(19) 0.032(3) 0.037(2) -0.022(2) 0.0018(17) 0.0015(19) C6 0.0244(19) 0.019(2) 0.0263(18) -0.0058(17) -0.0002(15) -0.0127(18) C7 0.0129(16) 0.016(2) 0.0151(15) -0.0050(15) -0.0029(13) -0.0040(15) C8 0.035(2) 0.021(2) 0.027(2) -0.0036(18) -0.0110(17) 0.002(2) C9 0.027(2) 0.043(3) 0.045(3) 0.004(2) -0.0180(19) -0.007(2) C10 0.047(3) 0.037(3) 0.0202(19) -0.0036(19) -0.0128(18) 0.000(2) C11 0.037(2) 0.033(3) 0.035(2) -0.019(2) -0.0088(19) -0.008(2) C12 0.0230(19) 0.017(2) 0.035(2) -0.0079(18) -0.0073(17) -0.0043(18) C13 0.0212(19) 0.019(2) 0.0293(19) -0.0065(18) -0.0042(16) -0.0045(17) C14 0.0226(19) 0.024(3) 0.030(2) -0.0109(19) -0.0045(16) -0.0019(18) C15 0.0162(17) 0.017(2) 0.0198(17) -0.0053(16) -0.0032(14) -0.0029(16) C16 0.023(2) 0.018(2) 0.0207(17) -0.0104(16) 0.0005(15) -0.0026(17) C17 0.0187(18) 0.018(2) 0.0166(16) -0.0045(16) -0.0023(14) -0.0031(17) C18 0.025(2) 0.017(2) 0.0154(16) -0.0066(16) -0.0038(14) -0.0002(17) N1 0.0190(15) 0.0166(19) 0.0205(14) -0.0064(13) -0.0009(12) -0.0072(14) O1 0.0189(13) 0.0260(18) 0.0234(13) -0.0100(12) -0.0038(10) 0.0012(12) O2 0.0424(17) 0.045(2) 0.0210(14) -0.0167(15) 0.0010(13) -0.0008(17) O3 0.0286(15) 0.0175(17) 0.0327(14) -0.0068(13) -0.0085(12) -0.0019(13) O4 0.0191(15) 0.039(2) 0.0434(17) -0.0206(16) -0.0052(12) -0.0040(14) O5 0.0435(17) 0.0181(18) 0.0273(14) -0.0023(13) -0.0095(13) -0.0024(15) O6 0.0264(15) 0.0267(19) 0.0338(15) -0.0091(14) -0.0113(12) -0.0067(14) P 0.0141(4) 0.0123(5) 0.0143(4) -0.0039(4) -0.0023(3) -0.0040(4) Si1 0.0199(5) 0.0209(6) 0.0182(5) -0.0020(4) -0.0075(4) -0.0036(5) Si2 0.0191(5) 0.0156(6) 0.0222(5) -0.0078(4) -0.0050(4) -0.0052(4) W 0.01541(8) 0.01294(9) 0.01448(8) -0.00576(6) -0.00179(5) -0.00170(6) _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 C1 C2 1.465(5) . ? C1 N1 1.470(5) . ? C1 P 1.838(3) . ? C1 H1A 1.0000 . ? C2 O1 1.358(5) . ? C2 C3 1.360(5) . ? C3 C4 1.429(6) . ? C3 H3A 0.9500 . ? C4 C5 1.345(6) . ? C4 H4A 0.9500 . ? C5 O1 1.372(4) . ? C5 H5A 0.9500 . ? C6 N1 1.468(5) . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C6 H6A 0.9800 . ? C7 P 1.806(3) . ? C7 Si2 1.902(4) . ? C7 Si1 1.904(4) . ? C7 H7A 1.0000 . ? C8 Si1 1.866(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si1 1.864(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si1 1.876(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si2 1.870(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.859(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si2 1.872(4) . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 O2 1.151(4) . ? C14 W 2.006(4) . ? C15 O3 1.131(5) . ? C15 W 2.043(4) . ? C16 O4 1.142(5) . ? C16 W 2.045(4) . ? C17 O5 1.128(5) . ? C17 W 2.059(4) . ? C18 O6 1.147(4) . ? C18 W 2.036(4) . ? N1 P 1.730(3) . ? P W 2.4935(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 C1 N1 116.1(3) . . ? C2 C1 P 124.1(3) . . ? N1 C1 P 61.87(18) . . ? C2 C1 H1A 114.7 . . ? N1 C1 H1A 114.7 . . ? P C1 H1A 114.7 . . ? O1 C2 C3 110.3(3) . . ? O1 C2 C1 116.0(3) . . ? C3 C2 C1 133.7(4) . . ? C2 C3 C4 106.1(4) . . ? C2 C3 H3A 127.0 . . ? C4 C3 H3A 127.0 . . ? C5 C4 C3 106.6(3) . . ? C5 C4 H4A 126.7 . . ? C3 C4 H4A 126.7 . . ? C4 C5 O1 110.2(4) . . ? C4 C5 H5A 124.9 . . ? O1 C5 H5A 124.9 . . ? N1 C6 H6C 109.5 . . ? N1 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? N1 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? P C7 Si2 115.30(18) . . ? P C7 Si1 114.6(2) . . ? Si2 C7 Si1 119.08(17) . . ? P C7 H7A 101.2 . . ? Si2 C7 H7A 101.2 . . ? Si1 C7 H7A 101.2 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13C 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? Si2 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? O2 C14 W 178.2(3) . . ? O3 C15 W 178.5(3) . . ? O4 C16 W 177.2(3) . . ? O5 C17 W 179.1(3) . . ? O6 C18 W 177.5(3) . . ? C6 N1 C1 117.2(3) . . ? C6 N1 P 123.6(2) . . ? C1 N1 P 69.58(19) . . ? C2 O1 C5 106.8(3) . . ? N1 P C7 103.80(15) . . ? N1 P C1 48.55(16) . . ? C7 P C1 108.56(16) . . ? N1 P W 123.02(11) . . ? C7 P W 127.04(11) . . ? C1 P W 120.27(11) . . ? C9 Si1 C8 107.8(2) . . ? C9 Si1 C10 108.9(2) . . ? C8 Si1 C10 107.9(2) . . ? C9 Si1 C7 113.17(19) . . ? C8 Si1 C7 112.42(17) . . ? C10 Si1 C7 106.48(18) . . ? C12 Si2 C11 107.5(2) . . ? C12 Si2 C13 110.62(18) . . ? C11 Si2 C13 108.86(18) . . ? C12 Si2 C7 108.02(17) . . ? C11 Si2 C7 107.02(18) . . ? C13 Si2 C7 114.57(18) . . ? C14 W C18 87.49(14) . . ? C14 W C15 91.44(16) . . ? C18 W C15 90.57(15) . . ? C14 W C16 90.19(14) . . ? C18 W C16 176.87(14) . . ? C15 W C16 87.40(16) . . ? C14 W C17 89.00(16) . . ? C18 W C17 90.49(15) . . ? C15 W C17 178.87(13) . . ? C16 W C17 91.56(16) . . ? C14 W P 175.88(11) . . ? C18 W P 88.45(9) . . ? C15 W P 89.24(10) . . ? C16 W P 93.90(9) . . ? C17 W P 90.39(10) . . ? 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 N1 C1 C2 O1 -174.3(3) . . . . ? P C1 C2 O1 113.4(3) . . . . ? N1 C1 C2 C3 7.4(6) . . . . ? P C1 C2 C3 -65.0(6) . . . . ? O1 C2 C3 C4 -0.7(4) . . . . ? C1 C2 C3 C4 177.8(4) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 O1 -0.1(5) . . . . ? C2 C1 N1 C6 125.4(3) . . . . ? P C1 N1 C6 -118.2(3) . . . . ? C2 C1 N1 P -116.5(3) . . . . ? C3 C2 O1 C5 0.6(4) . . . . ? C1 C2 O1 C5 -178.1(3) . . . . ? C4 C5 O1 C2 -0.3(4) . . . . ? C6 N1 P C7 -147.5(3) . . . . ? C1 N1 P C7 102.7(2) . . . . ? C6 N1 P C1 109.7(4) . . . . ? C6 N1 P W 6.5(4) . . . . ? C1 N1 P W -103.18(18) . . . . ? Si2 C7 P N1 -144.11(19) . . . . ? Si1 C7 P N1 72.0(2) . . . . ? Si2 C7 P C1 -93.6(2) . . . . ? Si1 C7 P C1 122.45(19) . . . . ? Si2 C7 P W 63.2(2) . . . . ? Si1 C7 P W -80.7(2) . . . . ? C2 C1 P N1 103.9(4) . . . . ? C2 C1 P C7 11.6(4) . . . . ? N1 C1 P C7 -92.3(2) . . . . ? C2 C1 P W -147.1(3) . . . . ? N1 C1 P W 109.05(17) . . . . ? P C7 Si1 C9 111.0(2) . . . . ? Si2 C7 Si1 C9 -31.4(3) . . . . ? P C7 Si1 C8 -11.4(2) . . . . ? Si2 C7 Si1 C8 -153.82(19) . . . . ? P C7 Si1 C10 -129.4(2) . . . . ? Si2 C7 Si1 C10 88.2(2) . . . . ? P C7 Si2 C12 48.9(2) . . . . ? Si1 C7 Si2 C12 -168.88(19) . . . . ? P C7 Si2 C11 164.4(2) . . . . ? Si1 C7 Si2 C11 -53.4(2) . . . . ? P C7 Si2 C13 -74.9(2) . . . . ? Si1 C7 Si2 C13 67.3(2) . . . . ? O2 C14 W C18 -2(13) . . . . ? O2 C14 W C15 88(13) . . . . ? O2 C14 W C16 176(100) . . . . ? O2 C14 W C17 -93(13) . . . . ? O2 C14 W P -11(15) . . . . ? O6 C18 W C14 50(7) . . . . ? O6 C18 W C15 -41(7) . . . . ? O6 C18 W C16 8(9) . . . . ? O6 C18 W C17 139(7) . . . . ? O6 C18 W P -130(7) . . . . ? O3 C15 W C14 114(13) . . . . ? O3 C15 W C18 -159(13) . . . . ? O3 C15 W C16 24(13) . . . . ? O3 C15 W C17 1(17) . . . . ? O3 C15 W P -70(13) . . . . ? O4 C16 W C14 -40(8) . . . . ? O4 C16 W C18 2(9) . . . . ? O4 C16 W C15 52(8) . . . . ? O4 C16 W C17 -129(8) . . . . ? O4 C16 W P 141(8) . . . . ? O5 C17 W C14 4(22) . . . . ? O5 C17 W C18 -83(22) . . . . ? O5 C17 W C15 117(22) . . . . ? O5 C17 W C16 94(22) . . . . ? O5 C17 W P -172(100) . . . . ? N1 P W C14 54.9(19) . . . . ? C7 P W C14 -157.2(18) . . . . ? C1 P W C14 -2.8(19) . . . . ? N1 P W C18 45.85(18) . . . . ? C7 P W C18 -166.3(2) . . . . ? C1 P W C18 -11.82(19) . . . . ? N1 P W C15 -44.73(17) . . . . ? C7 P W C15 103.16(19) . . . . ? C1 P W C15 -102.41(18) . . . . ? N1 P W C16 -132.08(18) . . . . ? C7 P W C16 15.8(2) . . . . ? C1 P W C16 170.25(19) . . . . ? N1 P W C17 136.33(17) . . . . ? C7 P W C17 -75.78(19) . . . . ? C1 P W C17 78.66(18) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.305 _refine_diff_density_min -3.531 _refine_diff_density_rms 0.159 #------------------------------------------------------------------------------ data_greg607 _database_code_depnum_ccdc_archive 'CCDC 743282' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 N O5 P S Si2 W' _chemical_formula_sum 'C18 H26 N O5 P S Si2 W' _chemical_formula_weight 639.46 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3006(4) _cell_length_b 9.8061(4) _cell_length_c 15.3241(6) _cell_angle_alpha 72.925(3) _cell_angle_beta 75.155(3) _cell_angle_gamma 77.227(3) _cell_volume 1275.21(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10736 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.58 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 4.794 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4876 _exptl_absorpt_correction_T_max 0.6961 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 1 0.1030 0 0 -1 0.0060 0 -1 -1 0.0500 -1 0 0 0.0700 1 0 0 0.0700 1 1 1 0.1100 0 0 1 0.0700 _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 170 frames, detector distance = 100 mm ; _diffrn_reflns_number 10310 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5790 _reflns_number_gt 5162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0596P)^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 SHELXL _refine_ls_extinction_coef 0.0099(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5790 _refine_ls_number_parameters 289 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.016 _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 C1 C 0.3938(5) 0.7472(5) 0.7374(3) 0.0248(8) Uani 1 1 d . A . H1A H 0.3434 0.7452 0.6875 0.030 Uiso 1 1 calc R . . C2 C 0.3038(5) 0.8386(5) 0.7997(3) 0.0264(9) Uani 1 1 d D . . C3 C 0.2203(18) 0.972(2) 0.7759(14) 0.027(3) Uani 0.849(7) 1 d P A 1 H3 H 0.2117 1.0217 0.7137 0.033 Uiso 0.849(7) 1 calc PR A 1 C3S C 0.285(4) 0.831(3) 0.8913(8) 0.0382(16) Uani 0.151(7) 1 d PDU A 2 H3S H 0.3403 0.7516 0.9283 0.046 Uiso 0.151(7) 1 calc PR A 2 C4 C 0.1463(6) 1.0275(6) 0.8563(4) 0.0425(12) Uani 1 1 d . . . H4A H 0.0789 1.1161 0.8539 0.051 Uiso 1 1 calc R A 1 C5 C 0.1851(6) 0.9374(7) 0.9354(4) 0.0468(13) Uani 1 1 d D A . H5A H 0.1514 0.9579 0.9948 0.056 Uiso 1 1 calc R B 1 C6 C 0.4413(5) 0.4767(5) 0.7628(4) 0.0322(10) Uani 1 1 d . A . H6C H 0.5171 0.3933 0.7817 0.048 Uiso 1 1 calc R . . H6B H 0.4441 0.4945 0.6960 0.048 Uiso 1 1 calc R . . H6A H 0.3411 0.4571 0.7984 0.048 Uiso 1 1 calc R . . C7 C 0.6789(5) 0.7708(5) 0.7835(3) 0.0250(8) Uani 1 1 d . . . H7A H 0.5880 0.7842 0.8337 0.030 Uiso 1 1 calc R . . C8 C 0.7404(8) 0.6283(7) 0.9771(4) 0.0474(14) Uani 1 1 d . . . H8A H 0.6359 0.6106 0.9979 0.071 Uiso 1 1 calc R . . H8B H 0.7460 0.7232 0.9839 0.071 Uiso 1 1 calc R . . H8C H 0.8038 0.5533 1.0151 0.071 Uiso 1 1 calc R . . C9 C 1.0096(6) 0.6497(7) 0.8143(5) 0.0481(14) Uani 1 1 d . . . H9A H 1.0187 0.7438 0.8207 0.072 Uiso 1 1 calc R . . H9B H 1.0460 0.6460 0.7490 0.072 Uiso 1 1 calc R . . H9C H 1.0698 0.5730 0.8534 0.072 Uiso 1 1 calc R . . C10 C 0.8009(6) 0.4401(5) 0.8421(4) 0.0375(11) Uani 1 1 d . . . H10A H 0.8351 0.4362 0.7767 0.056 Uiso 1 1 calc R . . H10B H 0.6971 0.4203 0.8644 0.056 Uiso 1 1 calc R . . H10C H 0.8665 0.3676 0.8798 0.056 Uiso 1 1 calc R . . C11 C 0.7527(6) 1.0144(6) 0.8403(4) 0.0399(11) Uani 1 1 d . . . H11A H 0.8387 0.9505 0.8643 0.060 Uiso 1 1 calc R . . H11B H 0.6614 1.0056 0.8894 0.060 Uiso 1 1 calc R . . H11C H 0.7713 1.1146 0.8209 0.060 Uiso 1 1 calc R . . C12 C 0.9013(5) 0.9820(5) 0.6449(4) 0.0312(9) Uani 1 1 d . . . H12A H 0.8829 0.9711 0.5873 0.047 Uiso 1 1 calc R . . H12B H 0.9843 0.9076 0.6647 0.047 Uiso 1 1 calc R . . H12C H 0.9280 1.0778 0.6338 0.047 Uiso 1 1 calc R . . C13 C 0.5622(5) 1.0867(5) 0.6956(4) 0.0342(10) Uani 1 1 d . . . H13C H 0.5880 1.1841 0.6677 0.051 Uiso 1 1 calc R . . H13B H 0.4762 1.0893 0.7480 0.051 Uiso 1 1 calc R . . H13A H 0.5360 1.0522 0.6486 0.051 Uiso 1 1 calc R . . C14 C 0.8196(5) 0.6606(5) 0.4162(3) 0.0307(9) Uani 1 1 d . A . C15 C 0.6938(5) 0.9016(5) 0.4962(3) 0.0279(9) Uani 1 1 d . A . C16 C 0.9400(5) 0.6887(5) 0.5646(3) 0.0277(9) Uani 1 1 d . A . C17 C 0.7718(5) 0.4620(5) 0.5997(3) 0.0286(9) Uani 1 1 d . A . C18 C 0.5250(5) 0.6661(5) 0.5258(3) 0.0287(9) Uani 1 1 d . A . N N 0.4736(4) 0.6045(4) 0.7810(3) 0.0256(7) Uani 1 1 d . . . O1 O 0.8683(5) 0.6489(4) 0.3434(3) 0.0451(9) Uani 1 1 d . . . O2 O 0.6760(4) 1.0231(4) 0.4646(3) 0.0364(8) Uani 1 1 d . . . O3 O 1.0572(4) 0.6884(4) 0.5717(3) 0.0392(8) Uani 1 1 d . . . O4 O 0.7975(4) 0.3424(4) 0.6298(3) 0.0369(8) Uani 1 1 d . . . O5 O 0.4160(4) 0.6541(4) 0.5126(3) 0.0380(8) Uani 1 1 d . . . P P 0.60146(12) 0.71197(11) 0.70657(8) 0.0219(2) Uani 1 1 d . A . S1 S 0.29978(18) 0.78500(19) 0.91694(11) 0.0374(5) Uani 0.849(7) 1 d PU A 1 S1S S 0.193(3) 0.993(3) 0.763(2) 0.023(3) Uani 0.151(7) 1 d P A 2 Si1 Si 0.72739(13) 0.96193(13) 0.73828(9) 0.0260(2) Uani 1 1 d . . . Si2 Si 0.80834(14) 0.62389(14) 0.85205(9) 0.0297(3) Uani 1 1 d . . . W W 0.729636(17) 0.682068(16) 0.547480(12) 0.02243(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0201(18) 0.027(2) 0.026(2) -0.0074(17) -0.0035(16) -0.0025(15) C2 0.0213(18) 0.033(2) 0.025(2) -0.0101(17) -0.0011(16) -0.0058(16) C3 0.012(7) 0.040(7) 0.031(6) -0.013(5) -0.005(4) -0.001(5) C3S 0.031(2) 0.052(2) 0.027(2) -0.010(2) -0.003(2) 0.000(2) C4 0.026(2) 0.046(3) 0.056(4) -0.023(3) -0.001(2) 0.000(2) C5 0.036(3) 0.070(4) 0.041(3) -0.034(3) 0.001(2) -0.006(3) C6 0.032(2) 0.029(2) 0.037(3) -0.0108(19) -0.004(2) -0.0080(17) C7 0.0232(19) 0.030(2) 0.022(2) -0.0077(16) -0.0032(16) -0.0047(15) C8 0.067(4) 0.048(3) 0.030(3) -0.007(2) -0.023(3) -0.004(3) C9 0.035(3) 0.050(3) 0.055(4) 0.004(3) -0.020(3) -0.009(2) C10 0.045(3) 0.032(2) 0.033(3) -0.007(2) -0.011(2) 0.002(2) C11 0.047(3) 0.042(3) 0.038(3) -0.017(2) -0.009(2) -0.012(2) C12 0.030(2) 0.031(2) 0.034(3) -0.0118(19) -0.0029(19) -0.0064(17) C13 0.030(2) 0.027(2) 0.046(3) -0.009(2) -0.010(2) -0.0019(17) C14 0.034(2) 0.031(2) 0.026(2) -0.0120(18) -0.0033(19) 0.0009(18) C15 0.031(2) 0.026(2) 0.026(2) -0.0071(17) -0.0055(18) -0.0024(16) C16 0.0219(19) 0.028(2) 0.035(2) -0.0125(18) -0.0054(17) -0.0012(15) C17 0.027(2) 0.0202(19) 0.035(3) -0.0046(17) -0.0076(19) 0.0001(15) C18 0.029(2) 0.029(2) 0.033(2) -0.0110(18) -0.0110(19) -0.0031(16) N 0.0235(16) 0.0238(17) 0.0277(19) -0.0052(14) -0.0022(14) -0.0051(13) O1 0.054(2) 0.046(2) 0.030(2) -0.0124(17) -0.0039(17) 0.0009(17) O2 0.045(2) 0.0266(16) 0.035(2) -0.0054(14) -0.0102(16) -0.0016(14) O3 0.0277(17) 0.0404(19) 0.054(2) -0.0209(17) -0.0095(16) 0.0000(14) O4 0.0380(18) 0.0293(17) 0.042(2) -0.0111(15) -0.0065(16) -0.0015(14) O5 0.0379(19) 0.0369(18) 0.045(2) -0.0133(16) -0.0168(17) -0.0034(14) P 0.0219(5) 0.0215(5) 0.0222(5) -0.0052(4) -0.0043(4) -0.0038(4) S1 0.0309(8) 0.0516(10) 0.0259(8) -0.0108(7) -0.0030(6) -0.0006(7) S1S 0.008(7) 0.029(6) 0.036(8) -0.015(5) -0.013(4) 0.008(4) Si1 0.0257(5) 0.0260(5) 0.0289(6) -0.0092(5) -0.0064(5) -0.0051(4) Si2 0.0296(6) 0.0319(6) 0.0278(6) -0.0031(5) -0.0105(5) -0.0054(5) W 0.02287(10) 0.02156(10) 0.02258(11) -0.00752(6) -0.00371(6) -0.00137(6) _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 C1 C2 1.476(6) . ? C1 N 1.484(5) . ? C1 P 1.845(4) . ? C1 H1A 1.0000 . ? C2 C3S 1.350(2) . ? C2 C3 1.362(15) . ? C2 S1S 1.67(2) . ? C2 S1 1.710(5) . ? C3 C4 1.44(2) . ? C3 H3 0.9500 . ? C3S C5 1.440(2) . ? C3S H3S 0.9500 . ? C4 C5 1.355(9) . ? C4 S1S 1.49(3) . ? C4 H4A 0.9500 . ? C5 S1 1.685(6) . ? C5 H5A 0.9500 . ? C6 N 1.467(6) . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C6 H6A 0.9800 . ? C7 P 1.805(4) . ? C7 Si2 1.903(4) . ? C7 Si1 1.910(4) . ? C7 H7A 1.0000 . ? C8 Si2 1.868(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.863(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.870(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.865(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.869(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.871(5) . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 O1 1.121(6) . ? C14 W 2.024(5) . ? C15 O2 1.138(6) . ? C15 W 2.046(4) . ? C16 O3 1.122(5) . ? C16 W 2.057(4) . ? C17 O4 1.123(6) . ? C17 W 2.055(4) . ? C18 O5 1.120(6) . ? C18 W 2.060(4) . ? N P 1.726(4) . ? P W 2.4953(12) . ? 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 C1 N 117.4(4) . . ? C2 C1 P 125.4(3) . . ? N C1 P 61.3(2) . . ? C2 C1 H1A 114.1 . . ? N C1 H1A 114.1 . . ? P C1 H1A 114.1 . . ? C3S C2 C3 97.2(10) . . ? C3S C2 C1 134.7(5) . . ? C3 C2 C1 127.8(10) . . ? C3S C2 S1S 102.0(12) . . ? C3 C2 S1S 6.8(16) . . ? C1 C2 S1S 123.3(11) . . ? C3S C2 S1 14.3(7) . . ? C3 C2 S1 111.2(9) . . ? C1 C2 S1 120.9(3) . . ? S1S C2 S1 115.7(11) . . ? C2 C3 C4 112.1(13) . . ? C2 C3 H3 124.0 . . ? C4 C3 H3 124.0 . . ? C2 C3S C5 122.9(7) . . ? C2 C3S H3S 118.5 . . ? C5 C3S H3S 118.5 . . ? C5 C4 C3 111.4(7) . . ? C5 C4 S1S 124.0(9) . . ? C3 C4 S1S 13.7(9) . . ? C5 C4 H4A 124.3 . . ? C3 C4 H4A 124.3 . . ? S1S C4 H4A 111.5 . . ? C4 C5 C3S 96.0(6) . . ? C4 C5 S1 112.7(5) . . ? C3S C5 S1 17.0(5) . . ? C4 C5 H5A 123.6 . . ? C3S C5 H5A 140.2 . . ? S1 C5 H5A 123.6 . . ? N C6 H6C 109.5 . . ? N C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? N C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? P C7 Si2 114.7(2) . . ? P C7 Si1 115.5(2) . . ? Si2 C7 Si1 118.8(2) . . ? P C7 H7A 101.2 . . ? Si2 C7 H7A 101.2 . . ? Si1 C7 H7A 101.2 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13C 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? Si1 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? O1 C14 W 179.5(4) . . ? O2 C15 W 177.7(4) . . ? O3 C16 W 177.1(4) . . ? O4 C17 W 177.9(4) . . ? O5 C18 W 177.8(4) . . ? C6 N C1 117.2(4) . . ? C6 N P 124.2(3) . . ? C1 N P 69.7(2) . . ? N P C7 104.1(2) . . ? N P C1 48.96(18) . . ? C7 P C1 109.7(2) . . ? N P W 122.93(14) . . ? C7 P W 126.57(15) . . ? C1 P W 119.61(15) . . ? C5 S1 C2 92.5(3) . . ? C4 S1S C2 94.7(13) . . ? C11 Si1 C12 108.8(2) . . ? C11 Si1 C13 107.7(3) . . ? C12 Si1 C13 110.0(2) . . ? C11 Si1 C7 106.8(2) . . ? C12 Si1 C7 114.9(2) . . ? C13 Si1 C7 108.4(2) . . ? C9 Si2 C8 109.3(3) . . ? C9 Si2 C10 107.0(3) . . ? C8 Si2 C10 108.4(3) . . ? C9 Si2 C7 113.3(2) . . ? C8 Si2 C7 106.8(2) . . ? C10 Si2 C7 112.1(2) . . ? C14 W C15 89.39(19) . . ? C14 W C17 90.68(19) . . ? C15 W C17 178.27(17) . . ? C14 W C16 89.89(19) . . ? C15 W C16 90.79(18) . . ? C17 W C16 87.49(17) . . ? C14 W C18 87.4(2) . . ? C15 W C18 91.34(18) . . ? C17 W C18 90.39(18) . . ? C16 W C18 176.52(18) . . ? C14 W P 176.08(13) . . ? C15 W P 89.69(14) . . ? C17 W P 90.34(14) . . ? C16 W P 93.93(14) . . ? C18 W P 88.84(14) . . ? 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 N C1 C2 C3S 8(3) . . . . ? P C1 C2 C3S -65(3) . . . . ? N C1 C2 C3 -179.2(11) . . . . ? P C1 C2 C3 108.0(11) . . . . ? N C1 C2 S1S -173.0(12) . . . . ? P C1 C2 S1S 114.2(12) . . . . ? N C1 C2 S1 3.1(5) . . . . ? P C1 C2 S1 -69.7(5) . . . . ? C3S C2 C3 C4 -6(2) . . . . ? C1 C2 C3 C4 179.5(7) . . . . ? S1S C2 C3 C4 130(18) . . . . ? S1 C2 C3 C4 -2.6(15) . . . . ? C3 C2 C3S C5 7(4) . . . . ? C1 C2 C3S C5 -178.9(16) . . . . ? S1S C2 C3S C5 2(4) . . . . ? S1 C2 C3S C5 -162(11) . . . . ? C2 C3 C4 C5 3.6(15) . . . . ? C2 C3 C4 S1S -155(9) . . . . ? C3 C4 C5 C3S 0(2) . . . . ? S1S C4 C5 C3S 6(2) . . . . ? C3 C4 C5 S1 -3.0(10) . . . . ? S1S C4 C5 S1 3.1(15) . . . . ? C2 C3S C5 C4 -5(4) . . . . ? C2 C3S C5 S1 165(10) . . . . ? C2 C1 N C6 123.7(4) . . . . ? P C1 N C6 -119.0(4) . . . . ? C2 C1 N P -117.4(4) . . . . ? C6 N P C7 -146.2(4) . . . . ? C1 N P C7 104.0(3) . . . . ? C6 N P C1 109.8(4) . . . . ? C6 N P W 7.3(4) . . . . ? C1 N P W -102.5(2) . . . . ? Si2 C7 P N 71.0(3) . . . . ? Si1 C7 P N -145.2(2) . . . . ? Si2 C7 P C1 122.0(2) . . . . ? Si1 C7 P C1 -94.2(3) . . . . ? Si2 C7 P W -81.2(3) . . . . ? Si1 C7 P W 62.6(3) . . . . ? C2 C1 P N 104.8(5) . . . . ? C2 C1 P C7 13.0(4) . . . . ? N C1 P C7 -91.8(3) . . . . ? C2 C1 P W -145.7(3) . . . . ? N C1 P W 109.5(2) . . . . ? C4 C5 S1 C2 1.3(5) . . . . ? C3S C5 S1 C2 -10(6) . . . . ? C3S C2 S1 C5 12(8) . . . . ? C3 C2 S1 C5 0.8(9) . . . . ? C1 C2 S1 C5 178.9(4) . . . . ? S1S C2 S1 C5 -4.7(11) . . . . ? C5 C4 S1S C2 -5.6(19) . . . . ? C3 C4 S1S C2 19(7) . . . . ? C3S C2 S1S C4 2(3) . . . . ? C3 C2 S1S C4 -44(16) . . . . ? C1 C2 S1S C4 -177.6(7) . . . . ? S1 C2 S1S C4 6.1(17) . . . . ? P C7 Si1 C11 164.6(3) . . . . ? Si2 C7 Si1 C11 -53.2(3) . . . . ? P C7 Si1 C12 -74.6(3) . . . . ? Si2 C7 Si1 C12 67.6(3) . . . . ? P C7 Si1 C13 48.8(3) . . . . ? Si2 C7 Si1 C13 -168.9(3) . . . . ? P C7 Si2 C9 110.5(3) . . . . ? Si1 C7 Si2 C9 -32.0(4) . . . . ? P C7 Si2 C8 -129.1(3) . . . . ? Si1 C7 Si2 C8 88.4(3) . . . . ? P C7 Si2 C10 -10.6(3) . . . . ? Si1 C7 Si2 C10 -153.1(3) . . . . ? O1 C14 W C15 -75(48) . . . . ? O1 C14 W C17 107(48) . . . . ? O1 C14 W C16 -166(100) . . . . ? O1 C14 W C18 16(48) . . . . ? O1 C14 W P 2(50) . . . . ? O2 C15 W C14 1(10) . . . . ? O2 C15 W C17 93(12) . . . . ? O2 C15 W C16 90(10) . . . . ? O2 C15 W C18 -87(10) . . . . ? O2 C15 W P -176(10) . . . . ? O4 C17 W C14 120(13) . . . . ? O4 C17 W C15 28(17) . . . . ? O4 C17 W C16 31(13) . . . . ? O4 C17 W C18 -152(13) . . . . ? O4 C17 W P -63(13) . . . . ? O3 C16 W C14 -34(9) . . . . ? O3 C16 W C15 -123(9) . . . . ? O3 C16 W C17 57(9) . . . . ? O3 C16 W C18 4(11) . . . . ? O3 C16 W P 147(9) . . . . ? O5 C18 W C14 40(12) . . . . ? O5 C18 W C15 129(12) . . . . ? O5 C18 W C17 -51(12) . . . . ? O5 C18 W C16 1(14) . . . . ? O5 C18 W P -141(12) . . . . ? N P W C14 60(2) . . . . ? C7 P W C14 -152(2) . . . . ? C1 P W C14 2(2) . . . . ? N P W C15 136.85(19) . . . . ? C7 P W C15 -75.8(2) . . . . ? C1 P W C15 79.0(2) . . . . ? N P W C17 -44.88(19) . . . . ? C7 P W C17 102.5(2) . . . . ? C1 P W C17 -102.8(2) . . . . ? N P W C16 -132.38(19) . . . . ? C7 P W C16 15.0(2) . . . . ? C1 P W C16 169.7(2) . . . . ? N P W C18 45.5(2) . . . . ? C7 P W C18 -167.1(2) . . . . ? C1 P W C18 -12.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.197 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.152 #------------------------------------------------------------------------------ data_joerg34 _database_code_depnum_ccdc_archive 'CCDC 743283' _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Fe N3 O5 P Si2 W' _chemical_formula_sum 'C27 H38 Fe N3 O5 P Si2 W' _chemical_formula_weight 811.45 _chemical_absolute_configuration ad 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.6420(10) _cell_length_b 13.2433(8) _cell_length_c 11.7490(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.678(3) _cell_angle_gamma 90.00 _cell_volume 1655.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 26248 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 4.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5996 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10273 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5726 _reflns_number_gt 4789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(8) _refine_ls_number_reflns 5726 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _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 W1 W 0.09249(3) 0.24486(3) 0.28989(2) 0.02605(8) Uani 1 1 d . . . Fe1 Fe -0.30656(12) 0.55698(8) 0.26085(10) 0.0307(3) Uani 1 1 d . . . P1 P -0.1243(2) 0.22252(13) 0.19969(16) 0.0225(6) Uani 1 1 d . . . Si1 Si -0.1701(3) -0.00890(19) 0.1475(2) 0.0258(7) Uani 1 1 d . . . Si2 Si -0.2798(2) 0.08611(16) 0.37665(18) 0.0295(5) Uani 1 1 d . . . N1 N -0.3108(6) 0.3162(4) 0.0953(5) 0.0262(16) Uani 1 1 d . . . N2 N -0.1233(6) 0.2297(5) 0.0560(4) 0.0217(15) Uani 1 1 d . . . N3 N -0.2622(7) 0.2772(4) -0.0929(5) 0.0306(18) Uani 1 1 d . . . C1 C -0.2500(8) 0.3239(6) 0.2090(6) 0.0257(19) Uani 1 1 d . . . H1 H -0.3116 0.3032 0.2672 0.031 Uiso 1 1 calc R . . C2 C -0.2266(8) 0.2722(5) 0.0180(6) 0.025(2) Uani 1 1 d . . . C3 C -0.2150(10) 0.1075(6) 0.2304(8) 0.033(2) Uani 1 1 d . . . H3 H -0.2950 0.1249 0.1882 0.039 Uiso 1 1 calc R . . C4 C -0.2053(9) 0.4272(6) 0.2359(7) 0.024(2) Uani 1 1 d . . . C5 C -0.1780(9) 0.4695(6) 0.3457(7) 0.036(2) Uani 1 1 d . . . H5 H -0.1900 0.4367 0.4165 0.044 Uiso 1 1 calc R . . C6 C -0.1302(9) 0.5680(6) 0.3317(7) 0.039(2) Uani 1 1 d . . . H6 H -0.1033 0.6123 0.3911 0.046 Uiso 1 1 calc R . . C7 C -0.1295(10) 0.5893(7) 0.2119(9) 0.039(3) Uani 1 1 d . . . H7 H -0.1039 0.6509 0.1781 0.046 Uiso 1 1 calc R . . C8 C -0.1746(10) 0.5008(7) 0.1519(9) 0.023(3) Uani 1 1 d . . . H8 H -0.1825 0.4928 0.0717 0.028 Uiso 1 1 calc R . . C9 C -0.4944(10) 0.5285(8) 0.2588(15) 0.026(6) Uani 1 1 d . . . H9 H -0.5343 0.4644 0.2556 0.032 Uiso 1 1 calc R . . C10 C -0.4533(13) 0.5817(8) 0.3636(11) 0.087(5) Uani 1 1 d . . . H10 H -0.4579 0.5582 0.4397 0.105 Uiso 1 1 calc R . . C11 C -0.4060(10) 0.6742(7) 0.3266(9) 0.054(3) Uani 1 1 d . . . H11 H -0.3752 0.7269 0.3747 0.065 Uiso 1 1 calc R . . C12 C -0.4111(9) 0.6769(6) 0.2094(9) 0.048(3) Uani 1 1 d . . . H12 H -0.3820 0.7316 0.1649 0.057 Uiso 1 1 calc R . . C13 C -0.4649(10) 0.5882(7) 0.1643(10) 0.058(3) Uani 1 1 d . . . H13 H -0.4785 0.5719 0.0861 0.069 Uiso 1 1 calc R . . C14 C -0.4462(8) 0.3012(6) 0.0849(7) 0.038(2) Uani 1 1 d . . . H14A H -0.4887 0.3667 0.0874 0.058 Uiso 1 1 calc R . . H14B H -0.4738 0.2590 0.1480 0.058 Uiso 1 1 calc R . . H14C H -0.4671 0.2676 0.0125 0.058 Uiso 1 1 calc R . . C15 C -0.3305(9) 0.3633(6) -0.1430(7) 0.037(2) Uani 1 1 d . . . H15A H -0.3518 0.4110 -0.0828 0.055 Uiso 1 1 calc R . . H15B H -0.4078 0.3393 -0.1815 0.055 Uiso 1 1 calc R . . H15C H -0.2776 0.3971 -0.1983 0.055 Uiso 1 1 calc R . . C16 C -0.1898(9) 0.2198(6) -0.1741(6) 0.042(3) Uani 1 1 d . . . H16A H -0.1184 0.2605 -0.1983 0.063 Uiso 1 1 calc R . . H16B H -0.2435 0.2029 -0.2406 0.063 Uiso 1 1 calc R . . H16C H -0.1588 0.1576 -0.1381 0.063 Uiso 1 1 calc R . . C17 C -0.0189(8) -0.0031(6) 0.0717(6) 0.033(2) Uani 1 1 d . . . H17A H -0.0072 -0.0658 0.0291 0.049 Uiso 1 1 calc R . . H17B H 0.0507 0.0054 0.1273 0.049 Uiso 1 1 calc R . . H17C H -0.0207 0.0542 0.0189 0.049 Uiso 1 1 calc R . . C18 C -0.1585(13) -0.1246(7) 0.2362(8) 0.053(3) Uani 1 1 d . . . H18A H -0.1603 -0.1843 0.1869 0.080 Uiso 1 1 calc R . . H18B H -0.2295 -0.1271 0.2874 0.080 Uiso 1 1 calc R . . H18C H -0.0795 -0.1236 0.2813 0.080 Uiso 1 1 calc R . . C19 C -0.2980(9) -0.0293(7) 0.0371(7) 0.051(3) Uani 1 1 d . . . H19A H -0.3027 0.0291 -0.0140 0.076 Uiso 1 1 calc R . . H19B H -0.3785 -0.0376 0.0744 0.076 Uiso 1 1 calc R . . H19C H -0.2798 -0.0902 -0.0069 0.076 Uiso 1 1 calc R . . C20 C -0.3260(8) 0.2029(6) 0.4537(6) 0.035(2) Uani 1 1 d . . . H20A H -0.3442 0.1860 0.5327 0.053 Uiso 1 1 calc R . . H20B H -0.4010 0.2321 0.4163 0.053 Uiso 1 1 calc R . . H20C H -0.2570 0.2518 0.4525 0.053 Uiso 1 1 calc R . . C21 C -0.4219(10) 0.0037(7) 0.3529(8) 0.058(3) Uani 1 1 d . . . H21A H -0.4443 -0.0277 0.4251 0.086 Uiso 1 1 calc R . . H21B H -0.4031 -0.0490 0.2974 0.086 Uiso 1 1 calc R . . H21C H -0.4924 0.0448 0.3239 0.086 Uiso 1 1 calc R . . C22 C -0.1665(10) 0.0232(6) 0.4788(7) 0.050(3) Uani 1 1 d . . . H22A H -0.1042 0.0726 0.5065 0.074 Uiso 1 1 calc R . . H22B H -0.1238 -0.0320 0.4400 0.074 Uiso 1 1 calc R . . H22C H -0.2122 -0.0039 0.5432 0.074 Uiso 1 1 calc R . . C23 C 0.1671(8) 0.2143(5) 0.1360(8) 0.034(2) Uani 1 1 d . . . C24 C 0.1148(9) 0.0983(6) 0.3347(7) 0.034(2) Uani 1 1 d . . . C25 C 0.0160(8) 0.2764(5) 0.4417(7) 0.031(2) Uani 1 1 d . . . C26 C 0.1025(8) 0.3943(6) 0.2445(7) 0.0283(19) Uani 1 1 d . . . C27 C 0.2639(10) 0.2664(8) 0.3588(7) 0.047(3) Uani 1 1 d . . . O1 O 0.2109(6) 0.1960(4) 0.0491(5) 0.0476(18) Uani 1 1 d . . . O2 O 0.1351(6) 0.0150(4) 0.3590(5) 0.0463(17) Uani 1 1 d . . . O3 O -0.0236(6) 0.2930(4) 0.5310(5) 0.0392(16) Uani 1 1 d . . . O4 O 0.1248(6) 0.4750(4) 0.2193(5) 0.0367(15) Uani 1 1 d . . . O5 O 0.3655(7) 0.2827(5) 0.3939(6) 0.071(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02706(17) 0.02511(14) 0.02568(14) -0.0009(2) -0.00425(11) 0.0032(2) Fe1 0.0327(8) 0.0231(6) 0.0366(7) -0.0026(5) 0.0074(6) 0.0060(5) P1 0.0272(13) 0.0201(16) 0.0202(9) 0.0008(7) 0.0016(9) 0.0012(8) Si1 0.028(2) 0.0189(15) 0.0305(17) -0.0021(12) -0.0001(15) 0.0006(13) Si2 0.0314(15) 0.0291(12) 0.0283(12) 0.0013(9) 0.0046(11) -0.0070(10) N1 0.025(4) 0.022(4) 0.031(4) 0.000(3) -0.011(3) 0.010(3) N2 0.021(4) 0.024(4) 0.021(3) -0.002(3) -0.001(3) -0.001(3) N3 0.033(5) 0.035(5) 0.024(4) -0.001(2) -0.006(3) 0.003(3) C1 0.029(6) 0.029(5) 0.019(4) -0.001(3) 0.004(4) -0.001(4) C2 0.035(5) 0.016(5) 0.024(4) 0.002(3) 0.000(4) -0.002(3) C3 0.036(7) 0.023(5) 0.040(5) -0.001(4) 0.004(4) -0.007(5) C4 0.019(5) 0.028(5) 0.024(4) -0.003(4) 0.000(4) 0.005(4) C5 0.051(7) 0.022(5) 0.035(5) -0.002(3) -0.011(4) 0.008(4) C6 0.042(6) 0.021(5) 0.052(6) -0.013(4) -0.021(5) 0.011(4) C7 0.023(6) 0.025(5) 0.068(8) 0.004(4) 0.001(5) 0.009(4) C8 0.020(7) 0.017(5) 0.032(6) -0.001(4) 0.003(5) 0.008(4) C9 0.041(7) 0.031(5) 0.038(6) -0.002(4) 0.023(5) 0.006(4) C10 0.040(7) 0.045(7) 0.059(7) 0.013(6) 0.034(7) 0.019(6) C11 0.052(8) 0.037(6) 0.074(8) -0.006(5) 0.022(6) 0.017(5) C12 0.040(7) 0.029(5) 0.073(7) -0.006(4) -0.001(6) 0.016(4) C13 0.033(7) 0.039(6) 0.100(9) -0.008(6) -0.012(6) 0.013(5) C14 0.021(6) 0.045(5) 0.049(6) -0.008(4) -0.011(4) -0.003(4) C15 0.039(6) 0.032(5) 0.038(5) 0.011(4) -0.020(4) -0.007(4) C16 0.057(7) 0.037(7) 0.033(5) -0.003(3) -0.011(5) 0.003(4) C17 0.035(6) 0.033(5) 0.030(5) -0.007(3) 0.005(4) 0.004(4) C18 0.080(10) 0.037(6) 0.044(6) -0.008(5) 0.010(6) 0.011(6) C19 0.038(7) 0.080(7) 0.035(5) -0.009(5) -0.002(5) -0.008(5) C20 0.029(6) 0.041(5) 0.037(5) 0.005(3) 0.013(4) -0.004(4) C21 0.057(8) 0.054(6) 0.063(7) -0.008(5) 0.023(6) -0.028(6) C22 0.057(8) 0.041(6) 0.051(6) 0.010(4) 0.005(5) 0.002(5) C23 0.024(5) 0.021(5) 0.056(6) 0.003(3) -0.007(5) -0.006(3) C24 0.038(6) 0.036(5) 0.026(5) -0.007(4) 0.000(4) 0.009(4) C25 0.025(5) 0.022(5) 0.047(6) 0.003(3) -0.013(4) 0.002(3) C26 0.026(5) 0.028(5) 0.030(5) -0.003(4) -0.002(4) 0.001(4) C27 0.048(7) 0.063(9) 0.029(4) -0.007(4) -0.015(4) 0.000(6) O1 0.042(5) 0.060(4) 0.041(4) -0.008(3) 0.016(3) -0.006(3) O2 0.060(5) 0.033(4) 0.046(4) 0.005(3) -0.008(3) 0.021(3) O3 0.054(5) 0.039(3) 0.025(3) -0.008(2) 0.005(3) 0.001(3) O4 0.037(4) 0.027(3) 0.045(4) 0.008(3) -0.005(3) -0.005(3) O5 0.033(5) 0.096(7) 0.083(5) 0.002(4) -0.022(4) -0.009(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 W1 C27 1.994(10) . ? W1 C24 2.023(9) . ? W1 C25 2.026(9) . ? W1 C23 2.036(9) . ? W1 C26 2.054(8) . ? W1 P1 2.528(2) . ? Fe1 C12 2.021(9) . ? Fe1 C10 2.027(10) . ? Fe1 C7 2.032(11) . ? Fe1 C5 2.032(8) . ? Fe1 C9 2.034(11) . ? Fe1 C6 2.036(9) . ? Fe1 C11 2.043(9) . ? Fe1 C13 2.046(10) . ? Fe1 C4 2.055(8) . ? Fe1 C8 2.066(10) . ? P1 N2 1.691(5) . ? P1 C3 1.844(9) . ? P1 C1 1.901(8) . ? Si1 C18 1.856(10) . ? Si1 C17 1.863(9) . ? Si1 C19 1.872(10) . ? Si1 C3 1.893(9) . ? Si2 C20 1.865(8) . ? Si2 C22 1.871(9) . ? Si2 C21 1.878(10) . ? Si2 C3 1.892(9) . ? N1 C2 1.419(9) . ? N1 C14 1.455(10) . ? N1 C1 1.471(10) . ? N2 C2 1.302(10) . ? N3 C2 1.348(9) . ? N3 C16 1.458(9) . ? N3 C15 1.467(9) . ? C1 C4 1.478(10) . ? C1 H1 1.0000 . ? C3 H3 1.0000 . ? C4 C5 1.428(11) . ? C4 C8 1.432(12) . ? C5 C6 1.411(11) . ? C5 H5 0.9500 . ? C6 C7 1.436(13) . ? C6 H6 0.9500 . ? C7 C8 1.443(13) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C13 1.406(16) . ? C9 C10 1.474(18) . ? C9 H9 0.9500 . ? C10 C11 1.399(14) . ? C10 H10 0.9500 . ? C11 C12 1.377(13) . ? C11 H11 0.9500 . ? C12 C13 1.404(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O1 1.160(9) . ? C24 O2 1.159(9) . ? C25 O3 1.163(9) . ? C26 O4 1.135(9) . ? C27 O5 1.167(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 C27 W1 C24 86.1(4) . . ? C27 W1 C25 90.0(4) . . ? C24 W1 C25 90.9(3) . . ? C27 W1 C23 90.7(4) . . ? C24 W1 C23 89.7(3) . . ? C25 W1 C23 179.1(4) . . ? C27 W1 C26 85.1(4) . . ? C24 W1 C26 170.3(4) . . ? C25 W1 C26 93.2(3) . . ? C23 W1 C26 86.3(3) . . ? C27 W1 P1 178.3(3) . . ? C24 W1 P1 95.5(3) . . ? C25 W1 P1 90.5(2) . . ? C23 W1 P1 88.8(3) . . ? C26 W1 P1 93.3(3) . . ? C12 Fe1 C10 68.0(4) . . ? C12 Fe1 C7 104.8(4) . . ? C10 Fe1 C7 150.6(5) . . ? C12 Fe1 C5 162.1(4) . . ? C10 Fe1 C5 108.6(5) . . ? C7 Fe1 C5 69.0(4) . . ? C12 Fe1 C9 67.1(5) . . ? C10 Fe1 C9 42.6(5) . . ? C7 Fe1 C9 162.7(6) . . ? C5 Fe1 C9 123.2(5) . . ? C12 Fe1 C6 124.0(4) . . ? C10 Fe1 C6 117.5(5) . . ? C7 Fe1 C6 41.4(4) . . ? C5 Fe1 C6 40.6(3) . . ? C9 Fe1 C6 155.8(6) . . ? C12 Fe1 C11 39.6(4) . . ? C10 Fe1 C11 40.2(4) . . ? C7 Fe1 C11 116.2(4) . . ? C5 Fe1 C11 126.6(4) . . ? C9 Fe1 C11 68.0(4) . . ? C6 Fe1 C11 105.8(4) . . ? C12 Fe1 C13 40.4(4) . . ? C10 Fe1 C13 70.2(5) . . ? C7 Fe1 C13 123.8(5) . . ? C5 Fe1 C13 156.8(4) . . ? C9 Fe1 C13 40.3(5) . . ? C6 Fe1 C13 161.2(4) . . ? C11 Fe1 C13 68.2(4) . . ? C12 Fe1 C4 154.3(4) . . ? C10 Fe1 C4 129.5(4) . . ? C7 Fe1 C4 69.0(4) . . ? C5 Fe1 C4 40.9(3) . . ? C9 Fe1 C4 111.3(4) . . ? C6 Fe1 C4 68.7(3) . . ? C11 Fe1 C4 165.8(4) . . ? C13 Fe1 C4 121.1(4) . . ? C12 Fe1 C8 118.4(4) . . ? C10 Fe1 C8 167.4(5) . . ? C7 Fe1 C8 41.2(4) . . ? C5 Fe1 C8 68.8(4) . . ? C9 Fe1 C8 127.7(5) . . ? C6 Fe1 C8 69.1(4) . . ? C11 Fe1 C8 151.3(4) . . ? C13 Fe1 C8 107.0(4) . . ? C4 Fe1 C8 40.7(3) . . ? N2 P1 C3 105.1(4) . . ? N2 P1 C1 92.4(3) . . ? C3 P1 C1 101.5(4) . . ? N2 P1 W1 112.3(2) . . ? C3 P1 W1 119.4(4) . . ? C1 P1 W1 121.9(3) . . ? C18 Si1 C17 105.0(5) . . ? C18 Si1 C19 107.7(5) . . ? C17 Si1 C19 107.2(4) . . ? C18 Si1 C3 113.4(4) . . ? C17 Si1 C3 116.5(4) . . ? C19 Si1 C3 106.6(5) . . ? C20 Si2 C22 103.4(4) . . ? C20 Si2 C21 109.3(4) . . ? C22 Si2 C21 109.7(4) . . ? C20 Si2 C3 115.1(4) . . ? C22 Si2 C3 113.8(5) . . ? C21 Si2 C3 105.4(4) . . ? C2 N1 C14 122.2(6) . . ? C2 N1 C1 109.9(6) . . ? C14 N1 C1 119.6(6) . . ? C2 N2 P1 109.7(5) . . ? C2 N3 C16 117.9(7) . . ? C2 N3 C15 123.2(6) . . ? C16 N3 C15 114.0(6) . . ? N1 C1 C4 112.9(6) . . ? N1 C1 P1 101.0(5) . . ? C4 C1 P1 116.3(6) . . ? N1 C1 H1 108.8 . . ? C4 C1 H1 108.8 . . ? P1 C1 H1 108.8 . . ? N2 C2 N3 124.3(7) . . ? N2 C2 N1 120.1(6) . . ? N3 C2 N1 115.7(7) . . ? P1 C3 Si2 120.6(5) . . ? P1 C3 Si1 115.5(5) . . ? Si2 C3 Si1 116.7(5) . . ? P1 C3 H3 99.0 . . ? Si2 C3 H3 99.0 . . ? Si1 C3 H3 99.0 . . ? C5 C4 C8 108.1(8) . . ? C5 C4 C1 127.7(7) . . ? C8 C4 C1 124.1(8) . . ? C5 C4 Fe1 68.7(4) . . ? C8 C4 Fe1 70.1(5) . . ? C1 C4 Fe1 129.6(7) . . ? C6 C5 C4 108.8(7) . . ? C6 C5 Fe1 69.9(5) . . ? C4 C5 Fe1 70.4(5) . . ? C6 C5 H5 125.6 . . ? C4 C5 H5 125.6 . . ? Fe1 C5 H5 125.7 . . ? C5 C6 C7 107.9(8) . . ? C5 C6 Fe1 69.5(5) . . ? C7 C6 Fe1 69.2(5) . . ? C5 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Fe1 C6 H6 126.8 . . ? C6 C7 C8 107.9(8) . . ? C6 C7 Fe1 69.5(6) . . ? C8 C7 Fe1 70.7(6) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Fe1 C7 H7 125.4 . . ? C4 C8 C7 107.2(9) . . ? C4 C8 Fe1 69.2(5) . . ? C7 C8 Fe1 68.1(5) . . ? C4 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? Fe1 C8 H8 127.8 . . ? C13 C9 C10 108.9(10) . . ? C13 C9 Fe1 70.3(6) . . ? C10 C9 Fe1 68.5(7) . . ? C13 C9 H9 125.6 . . ? C10 C9 H9 125.6 . . ? Fe1 C9 H9 127.2 . . ? C11 C10 C9 105.0(10) . . ? C11 C10 Fe1 70.5(6) . . ? C9 C10 Fe1 68.9(5) . . ? C11 C10 H10 127.5 . . ? C9 C10 H10 127.5 . . ? Fe1 C10 H10 124.7 . . ? C12 C11 C10 109.3(10) . . ? C12 C11 Fe1 69.4(5) . . ? C10 C11 Fe1 69.3(5) . . ? C12 C11 H11 125.4 . . ? C10 C11 H11 125.4 . . ? Fe1 C11 H11 127.6 . . ? C11 C12 C13 111.0(9) . . ? C11 C12 Fe1 71.0(5) . . ? C13 C12 Fe1 70.7(5) . . ? C11 C12 H12 124.5 . . ? C13 C12 H12 124.5 . . ? Fe1 C12 H12 125.3 . . ? C12 C13 C9 105.7(11) . . ? C12 C13 Fe1 68.9(6) . . ? C9 C13 Fe1 69.4(7) . . ? C12 C13 H13 127.1 . . ? C9 C13 H13 127.1 . . ? Fe1 C13 H13 126.2 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C23 W1 179.0(8) . . ? O2 C24 W1 175.9(8) . . ? O3 C25 W1 177.3(7) . . ? O4 C26 W1 170.9(8) . . ? O5 C27 W1 176.1(9) . . ? 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 C27 W1 P1 N2 57(10) . . . . ? C24 W1 P1 N2 -107.3(4) . . . . ? C25 W1 P1 N2 161.8(3) . . . . ? C23 W1 P1 N2 -17.7(3) . . . . ? C26 W1 P1 N2 68.6(4) . . . . ? C27 W1 P1 C3 -180(100) . . . . ? C24 W1 P1 C3 16.4(4) . . . . ? C25 W1 P1 C3 -74.5(4) . . . . ? C23 W1 P1 C3 106.0(4) . . . . ? C26 W1 P1 C3 -167.8(4) . . . . ? C27 W1 P1 C1 -51(10) . . . . ? C24 W1 P1 C1 144.7(4) . . . . ? C25 W1 P1 C1 53.8(3) . . . . ? C23 W1 P1 C1 -125.7(3) . . . . ? C26 W1 P1 C1 -39.4(4) . . . . ? C3 P1 N2 C2 83.4(6) . . . . ? C1 P1 N2 C2 -19.2(6) . . . . ? W1 P1 N2 C2 -145.3(5) . . . . ? C2 N1 C1 C4 101.9(7) . . . . ? C14 N1 C1 C4 -109.2(8) . . . . ? C2 N1 C1 P1 -23.0(6) . . . . ? C14 N1 C1 P1 125.9(6) . . . . ? N2 P1 C1 N1 24.1(5) . . . . ? C3 P1 C1 N1 -81.8(5) . . . . ? W1 P1 C1 N1 142.4(4) . . . . ? N2 P1 C1 C4 -98.4(6) . . . . ? C3 P1 C1 C4 155.6(6) . . . . ? W1 P1 C1 C4 19.8(7) . . . . ? P1 N2 C2 N3 -170.9(6) . . . . ? P1 N2 C2 N1 8.4(9) . . . . ? C16 N3 C2 N2 8.7(11) . . . . ? C15 N3 C2 N2 -145.3(8) . . . . ? C16 N3 C2 N1 -170.6(6) . . . . ? C15 N3 C2 N1 35.3(10) . . . . ? C14 N1 C2 N2 -135.9(8) . . . . ? C1 N1 C2 N2 12.0(9) . . . . ? C14 N1 C2 N3 43.4(9) . . . . ? C1 N1 C2 N3 -168.7(6) . . . . ? N2 P1 C3 Si2 -163.2(6) . . . . ? C1 P1 C3 Si2 -67.5(7) . . . . ? W1 P1 C3 Si2 69.7(7) . . . . ? N2 P1 C3 Si1 47.5(7) . . . . ? C1 P1 C3 Si1 143.2(5) . . . . ? W1 P1 C3 Si1 -79.6(6) . . . . ? C20 Si2 C3 P1 32.3(8) . . . . ? C22 Si2 C3 P1 -86.8(7) . . . . ? C21 Si2 C3 P1 152.9(6) . . . . ? C20 Si2 C3 Si1 -178.7(5) . . . . ? C22 Si2 C3 Si1 62.2(7) . . . . ? C21 Si2 C3 Si1 -58.1(7) . . . . ? C18 Si1 C3 P1 135.8(6) . . . . ? C17 Si1 C3 P1 13.8(8) . . . . ? C19 Si1 C3 P1 -105.8(6) . . . . ? C18 Si1 C3 Si2 -14.7(8) . . . . ? C17 Si1 C3 Si2 -136.8(5) . . . . ? C19 Si1 C3 Si2 103.7(6) . . . . ? N1 C1 C4 C5 159.4(8) . . . . ? P1 C1 C4 C5 -84.6(10) . . . . ? N1 C1 C4 C8 -24.7(12) . . . . ? P1 C1 C4 C8 91.4(10) . . . . ? N1 C1 C4 Fe1 66.8(9) . . . . ? P1 C1 C4 Fe1 -177.1(4) . . . . ? C12 Fe1 C4 C5 162.3(8) . . . . ? C10 Fe1 C4 C5 -71.4(9) . . . . ? C7 Fe1 C4 C5 81.8(6) . . . . ? C9 Fe1 C4 C5 -116.7(7) . . . . ? C6 Fe1 C4 C5 37.4(5) . . . . ? C11 Fe1 C4 C5 -32.4(19) . . . . ? C13 Fe1 C4 C5 -160.5(6) . . . . ? C8 Fe1 C4 C5 119.7(8) . . . . ? C12 Fe1 C4 C8 42.6(11) . . . . ? C10 Fe1 C4 C8 168.9(8) . . . . ? C7 Fe1 C4 C8 -37.9(6) . . . . ? C5 Fe1 C4 C8 -119.7(8) . . . . ? C9 Fe1 C4 C8 123.6(8) . . . . ? C6 Fe1 C4 C8 -82.4(6) . . . . ? C11 Fe1 C4 C8 -152.1(16) . . . . ? C13 Fe1 C4 C8 79.7(7) . . . . ? C12 Fe1 C4 C1 -75.7(12) . . . . ? C10 Fe1 C4 C1 50.6(11) . . . . ? C7 Fe1 C4 C1 -156.2(9) . . . . ? C5 Fe1 C4 C1 122.0(10) . . . . ? C9 Fe1 C4 C1 5.3(10) . . . . ? C6 Fe1 C4 C1 159.3(8) . . . . ? C11 Fe1 C4 C1 89.6(18) . . . . ? C13 Fe1 C4 C1 -38.5(9) . . . . ? C8 Fe1 C4 C1 -118.3(10) . . . . ? C8 C4 C5 C6 -0.3(10) . . . . ? C1 C4 C5 C6 176.2(9) . . . . ? Fe1 C4 C5 C6 -59.5(6) . . . . ? C8 C4 C5 Fe1 59.2(6) . . . . ? C1 C4 C5 Fe1 -124.3(9) . . . . ? C12 Fe1 C5 C6 -34.9(15) . . . . ? C10 Fe1 C5 C6 -110.8(6) . . . . ? C7 Fe1 C5 C6 38.0(5) . . . . ? C9 Fe1 C5 C6 -155.7(6) . . . . ? C11 Fe1 C5 C6 -69.8(7) . . . . ? C13 Fe1 C5 C6 166.1(10) . . . . ? C4 Fe1 C5 C6 119.7(7) . . . . ? C8 Fe1 C5 C6 82.3(6) . . . . ? C12 Fe1 C5 C4 -154.6(12) . . . . ? C10 Fe1 C5 C4 129.5(6) . . . . ? C7 Fe1 C5 C4 -81.7(6) . . . . ? C9 Fe1 C5 C4 84.6(7) . . . . ? C6 Fe1 C5 C4 -119.7(7) . . . . ? C11 Fe1 C5 C4 170.6(5) . . . . ? C13 Fe1 C5 C4 46.4(13) . . . . ? C8 Fe1 C5 C4 -37.4(5) . . . . ? C4 C5 C6 C7 1.2(10) . . . . ? Fe1 C5 C6 C7 -58.7(6) . . . . ? C4 C5 C6 Fe1 59.8(6) . . . . ? C12 Fe1 C6 C5 167.7(5) . . . . ? C10 Fe1 C6 C5 86.9(6) . . . . ? C7 Fe1 C6 C5 -119.6(7) . . . . ? C9 Fe1 C6 C5 57.1(11) . . . . ? C11 Fe1 C6 C5 128.5(5) . . . . ? C13 Fe1 C6 C5 -162.9(11) . . . . ? C4 Fe1 C6 C5 -37.6(5) . . . . ? C8 Fe1 C6 C5 -81.3(5) . . . . ? C12 Fe1 C6 C7 -72.7(6) . . . . ? C10 Fe1 C6 C7 -153.5(5) . . . . ? C5 Fe1 C6 C7 119.6(7) . . . . ? C9 Fe1 C6 C7 176.7(9) . . . . ? C11 Fe1 C6 C7 -111.9(5) . . . . ? C13 Fe1 C6 C7 -43.3(14) . . . . ? C4 Fe1 C6 C7 81.9(5) . . . . ? C8 Fe1 C6 C7 38.2(5) . . . . ? C5 C6 C7 C8 -1.6(11) . . . . ? Fe1 C6 C7 C8 -60.5(7) . . . . ? C5 C6 C7 Fe1 58.9(7) . . . . ? C12 Fe1 C7 C6 125.0(5) . . . . ? C10 Fe1 C7 C6 53.6(10) . . . . ? C5 Fe1 C7 C6 -37.3(5) . . . . ? C9 Fe1 C7 C6 -175.4(12) . . . . ? C11 Fe1 C7 C6 84.3(6) . . . . ? C13 Fe1 C7 C6 164.6(5) . . . . ? C4 Fe1 C7 C6 -81.3(5) . . . . ? C8 Fe1 C7 C6 -118.6(7) . . . . ? C12 Fe1 C7 C8 -116.4(6) . . . . ? C10 Fe1 C7 C8 172.3(8) . . . . ? C5 Fe1 C7 C8 81.3(6) . . . . ? C9 Fe1 C7 C8 -56.8(16) . . . . ? C6 Fe1 C7 C8 118.6(7) . . . . ? C11 Fe1 C7 C8 -157.1(6) . . . . ? C13 Fe1 C7 C8 -76.8(7) . . . . ? C4 Fe1 C7 C8 37.4(5) . . . . ? C5 C4 C8 C7 -0.7(11) . . . . ? C1 C4 C8 C7 -177.4(9) . . . . ? Fe1 C4 C8 C7 57.6(6) . . . . ? C5 C4 C8 Fe1 -58.3(6) . . . . ? C1 C4 C8 Fe1 125.0(9) . . . . ? C6 C7 C8 C4 1.4(11) . . . . ? Fe1 C7 C8 C4 -58.4(6) . . . . ? C6 C7 C8 Fe1 59.8(7) . . . . ? C12 Fe1 C8 C4 -160.5(6) . . . . ? C10 Fe1 C8 C4 -43(3) . . . . ? C7 Fe1 C8 C4 119.6(8) . . . . ? C5 Fe1 C8 C4 37.6(5) . . . . ? C9 Fe1 C8 C4 -78.7(8) . . . . ? C6 Fe1 C8 C4 81.2(6) . . . . ? C11 Fe1 C8 C4 166.2(8) . . . . ? C13 Fe1 C8 C4 -118.2(6) . . . . ? C12 Fe1 C8 C7 79.9(7) . . . . ? C10 Fe1 C8 C7 -162(2) . . . . ? C5 Fe1 C8 C7 -82.0(6) . . . . ? C9 Fe1 C8 C7 161.7(7) . . . . ? C6 Fe1 C8 C7 -38.4(5) . . . . ? C11 Fe1 C8 C7 46.6(11) . . . . ? C13 Fe1 C8 C7 122.2(6) . . . . ? C4 Fe1 C8 C7 -119.6(8) . . . . ? C12 Fe1 C9 C13 38.8(6) . . . . ? C10 Fe1 C9 C13 120.7(9) . . . . ? C7 Fe1 C9 C13 -26.1(17) . . . . ? C5 Fe1 C9 C13 -157.9(6) . . . . ? C6 Fe1 C9 C13 161.3(8) . . . . ? C11 Fe1 C9 C13 81.8(7) . . . . ? C4 Fe1 C9 C13 -113.5(6) . . . . ? C8 Fe1 C9 C13 -70.2(8) . . . . ? C12 Fe1 C9 C10 -81.9(6) . . . . ? C7 Fe1 C9 C10 -146.7(13) . . . . ? C5 Fe1 C9 C10 81.4(7) . . . . ? C6 Fe1 C9 C10 40.6(12) . . . . ? C11 Fe1 C9 C10 -38.9(6) . . . . ? C13 Fe1 C9 C10 -120.7(9) . . . . ? C4 Fe1 C9 C10 125.8(6) . . . . ? C8 Fe1 C9 C10 169.1(6) . . . . ? C13 C9 C10 C11 2.9(12) . . . . ? Fe1 C9 C10 C11 61.7(8) . . . . ? C13 C9 C10 Fe1 -58.8(7) . . . . ? C12 Fe1 C10 C11 -36.0(7) . . . . ? C7 Fe1 C10 C11 45.1(13) . . . . ? C5 Fe1 C10 C11 125.2(7) . . . . ? C9 Fe1 C10 C11 -115.6(11) . . . . ? C6 Fe1 C10 C11 81.9(8) . . . . ? C13 Fe1 C10 C11 -79.3(8) . . . . ? C4 Fe1 C10 C11 166.1(6) . . . . ? C8 Fe1 C10 C11 -159(2) . . . . ? C12 Fe1 C10 C9 79.6(8) . . . . ? C7 Fe1 C10 C9 160.6(9) . . . . ? C5 Fe1 C10 C9 -119.2(7) . . . . ? C6 Fe1 C10 C9 -162.5(7) . . . . ? C11 Fe1 C10 C9 115.6(11) . . . . ? C13 Fe1 C10 C9 36.2(7) . . . . ? C4 Fe1 C10 C9 -78.3(9) . . . . ? C8 Fe1 C10 C9 -43(3) . . . . ? C9 C10 C11 C12 -2.7(12) . . . . ? Fe1 C10 C11 C12 57.9(8) . . . . ? C9 C10 C11 Fe1 -60.7(7) . . . . ? C10 Fe1 C11 C12 -121.3(11) . . . . ? C7 Fe1 C11 C12 81.5(7) . . . . ? C5 Fe1 C11 C12 164.0(6) . . . . ? C9 Fe1 C11 C12 -80.1(8) . . . . ? C6 Fe1 C11 C12 124.6(6) . . . . ? C13 Fe1 C11 C12 -36.5(7) . . . . ? C4 Fe1 C11 C12 -170.1(15) . . . . ? C8 Fe1 C11 C12 49.3(12) . . . . ? C12 Fe1 C11 C10 121.3(11) . . . . ? C7 Fe1 C11 C10 -157.2(8) . . . . ? C5 Fe1 C11 C10 -74.7(10) . . . . ? C9 Fe1 C11 C10 41.1(9) . . . . ? C6 Fe1 C11 C10 -114.1(9) . . . . ? C13 Fe1 C11 C10 84.7(9) . . . . ? C4 Fe1 C11 C10 -49(2) . . . . ? C8 Fe1 C11 C10 170.5(10) . . . . ? C10 C11 C12 C13 1.7(12) . . . . ? Fe1 C11 C12 C13 59.6(7) . . . . ? C10 C11 C12 Fe1 -57.9(8) . . . . ? C10 Fe1 C12 C11 36.5(7) . . . . ? C7 Fe1 C12 C11 -113.4(7) . . . . ? C5 Fe1 C12 C11 -45.9(16) . . . . ? C9 Fe1 C12 C11 82.8(8) . . . . ? C6 Fe1 C12 C11 -72.6(8) . . . . ? C13 Fe1 C12 C11 121.5(10) . . . . ? C4 Fe1 C12 C11 174.4(8) . . . . ? C8 Fe1 C12 C11 -155.5(6) . . . . ? C10 Fe1 C12 C13 -85.0(8) . . . . ? C7 Fe1 C12 C13 125.2(7) . . . . ? C5 Fe1 C12 C13 -167.4(12) . . . . ? C9 Fe1 C12 C13 -38.7(7) . . . . ? C6 Fe1 C12 C13 165.9(6) . . . . ? C11 Fe1 C12 C13 -121.5(10) . . . . ? C4 Fe1 C12 C13 52.9(12) . . . . ? C8 Fe1 C12 C13 83.0(8) . . . . ? C11 C12 C13 C9 0.2(12) . . . . ? Fe1 C12 C13 C9 59.9(7) . . . . ? C11 C12 C13 Fe1 -59.8(7) . . . . ? C10 C9 C13 C12 -1.9(12) . . . . ? Fe1 C9 C13 C12 -59.6(7) . . . . ? C10 C9 C13 Fe1 57.7(8) . . . . ? C10 Fe1 C13 C12 78.9(7) . . . . ? C7 Fe1 C13 C12 -71.9(7) . . . . ? C5 Fe1 C13 C12 170.2(9) . . . . ? C9 Fe1 C13 C12 117.1(10) . . . . ? C6 Fe1 C13 C12 -38.9(15) . . . . ? C11 Fe1 C13 C12 35.8(6) . . . . ? C4 Fe1 C13 C12 -156.2(6) . . . . ? C8 Fe1 C13 C12 -114.1(6) . . . . ? C12 Fe1 C13 C9 -117.1(10) . . . . ? C10 Fe1 C13 C9 -38.2(6) . . . . ? C7 Fe1 C13 C9 171.0(7) . . . . ? C5 Fe1 C13 C9 53.1(13) . . . . ? C6 Fe1 C13 C9 -156.0(11) . . . . ? C11 Fe1 C13 C9 -81.3(7) . . . . ? C4 Fe1 C13 C9 86.7(7) . . . . ? C8 Fe1 C13 C9 128.8(7) . . . . ? C27 W1 C23 O1 48(45) . . . . ? C24 W1 C23 O1 -38(45) . . . . ? C25 W1 C23 O1 -170(35) . . . . ? C26 W1 C23 O1 133(45) . . . . ? P1 W1 C23 O1 -134(45) . . . . ? C27 W1 C24 O2 -35(10) . . . . ? C25 W1 C24 O2 -125(10) . . . . ? C23 W1 C24 O2 56(10) . . . . ? C26 W1 C24 O2 -10(12) . . . . ? P1 W1 C24 O2 144(10) . . . . ? C27 W1 C25 O3 -30(14) . . . . ? C24 W1 C25 O3 57(14) . . . . ? C23 W1 C25 O3 -172(41) . . . . ? C26 W1 C25 O3 -115(14) . . . . ? P1 W1 C25 O3 152(14) . . . . ? C27 W1 C26 O4 28(5) . . . . ? C24 W1 C26 O4 3(6) . . . . ? C25 W1 C26 O4 118(5) . . . . ? C23 W1 C26 O4 -63(5) . . . . ? P1 W1 C26 O4 -152(5) . . . . ? C24 W1 C27 O5 140(14) . . . . ? C25 W1 C27 O5 -129(14) . . . . ? C23 W1 C27 O5 51(14) . . . . ? C26 W1 C27 O5 -36(14) . . . . ? P1 W1 C27 O5 -24(22) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.159 _refine_diff_density_min -1.988 _refine_diff_density_rms 0.123