# 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 'Streubel, Rainer' _publ_contact_author_email jahns-streubel@t-online.de _publ_section_title ; Two unprecedented NLO-active coordination polymers constructed by a semi-rigid tetrahedral linker ; _publ_author_name 'Rainer Streubel' data_str018_m_compound_4 _database_code_depnum_ccdc_archive 'CCDC 777321' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [5-Bis(trimethylsilyl)methyl-2,2-dimethyl-4-ferrocenyl-1,3,5- oxazaphosphol-3-ene-kappaP]perntacarbonyltungsten(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 Fe N O6 P Si2 W' _chemical_formula_sum 'C26 H34 Fe N O6 P Si2 W' _chemical_formula_weight 783.39 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' Si Si 0.0817 0.0704 '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' Fe Fe 0.3463 0.8444 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7925(1) _cell_length_b 12.2414(1) _cell_length_c 21.4230(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.969(1) _cell_angle_gamma 90.00 _cell_volume 3054.74(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5746 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 4.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48199 _exptl_absorpt_correction_T_max 0.53633 _exptl_absorpt_process_details 'MULABS (Platon, cf. Blessing, 1995)' _exptl_special_details ; dx = 40 mm, 50 sec./deg., 1 deg., 2 sets, 237 frames, mos.= 0.398(1) deg. ; _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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17330 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6866 _reflns_number_gt 5980 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0076P)^2^+0.1287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 6866 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0438 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.578070(8) 0.287856(7) 0.537534(4) 0.01621(4) Uani 1 1 d . . . C1A C 0.4689(2) 0.3106(2) 0.45628(13) 0.0280(6) Uani 1 1 d . . . O1A O 0.40831(18) 0.32234(17) 0.40969(9) 0.0462(5) Uani 1 1 d . . . C1B C 0.4910(2) 0.14686(19) 0.55163(11) 0.0220(5) Uani 1 1 d . . . O1B O 0.44216(16) 0.06808(13) 0.55766(9) 0.0346(5) Uani 1 1 d . . . C1C C 0.6596(2) 0.4268(2) 0.51873(13) 0.0302(6) Uani 1 1 d . . . O1C O 0.70309(17) 0.50582(14) 0.50664(11) 0.0538(6) Uani 1 1 d . . . C1D C 0.4802(2) 0.38006(18) 0.58813(12) 0.0234(6) Uani 1 1 d . . . O1D O 0.42893(16) 0.43338(13) 0.61718(9) 0.0338(5) Uani 1 1 d . . . C1E C 0.6827(2) 0.19620(18) 0.49104(12) 0.0227(6) Uani 1 1 d . . . O1E O 0.73957(17) 0.14284(14) 0.46532(8) 0.0351(5) Uani 1 1 d . . . P1 P 0.71063(5) 0.24811(4) 0.63857(3) 0.01218(12) Uani 1 1 d . . . C1 C 0.8651(2) 0.21553(15) 0.63411(10) 0.0135(5) Uani 1 1 d . . . N1 N 0.88832(16) 0.11490(13) 0.64764(9) 0.0158(4) Uani 1 1 d . . . C2 C 0.7924(2) 0.05159(16) 0.66234(11) 0.0159(5) Uani 1 1 d . . . O1 O 0.69498(13) 0.12481(10) 0.66461(7) 0.0153(3) Uani 1 1 d . . . C3 C 0.69407(19) 0.33564(16) 0.70629(10) 0.0138(5) Uani 1 1 d . . . H3 H 0.6513 0.4001 0.6858 0.017 Uiso 1 1 calc R . . Si1 Si 0.58684(6) 0.27439(5) 0.75626(3) 0.01852(15) Uani 1 1 d . . . C4 C 0.4671(2) 0.19415(17) 0.71051(12) 0.0239(6) Uani 1 1 d . . . H4A H 0.4269 0.2394 0.6763 0.036 Uiso 1 1 calc R . . H4B H 0.4132 0.1719 0.7386 0.036 Uiso 1 1 calc R . . H4C H 0.4983 0.1291 0.6926 0.036 Uiso 1 1 calc R . . C5 C 0.6599(2) 0.18542(18) 0.82090(12) 0.0265(6) Uani 1 1 d . . . H5A H 0.6988 0.1253 0.8027 0.040 Uiso 1 1 calc R . . H5B H 0.6028 0.1556 0.8450 0.040 Uiso 1 1 calc R . . H5C H 0.7164 0.2285 0.8490 0.040 Uiso 1 1 calc R . . C6 C 0.5123(2) 0.38875(18) 0.79125(13) 0.0304(7) Uani 1 1 d . . . H6A H 0.4737 0.4355 0.7573 0.046 Uiso 1 1 calc R . . H6B H 0.5688 0.4319 0.8194 0.046 Uiso 1 1 calc R . . H6C H 0.4555 0.3587 0.8154 0.046 Uiso 1 1 calc R . . Si2 Si 0.82514(6) 0.40126(4) 0.75589(3) 0.01586(14) Uani 1 1 d . . . C7 C 0.9366(2) 0.29723(16) 0.78474(11) 0.0207(5) Uani 1 1 d . . . H7A H 0.9030 0.2406 0.8085 0.031 Uiso 1 1 calc R . . H7B H 1.0004 0.3325 0.8122 0.031 Uiso 1 1 calc R . . H7C H 0.9651 0.2639 0.7486 0.031 Uiso 1 1 calc R . . C8 C 0.8764(2) 0.51546(16) 0.70918(11) 0.0223(6) Uani 1 1 d . . . H8A H 0.8130 0.5663 0.6960 0.033 Uiso 1 1 calc R . . H8B H 0.9036 0.4856 0.6717 0.033 Uiso 1 1 calc R . . H8C H 0.9393 0.5542 0.7354 0.033 Uiso 1 1 calc R . . C9 C 0.7892(2) 0.47126(17) 0.82791(11) 0.0240(6) Uani 1 1 d . . . H9A H 0.7306 0.5271 0.8153 0.036 Uiso 1 1 calc R . . H9B H 0.8584 0.5058 0.8509 0.036 Uiso 1 1 calc R . . H9C H 0.7598 0.4175 0.8553 0.036 Uiso 1 1 calc R . . C10 C 0.9554(2) 0.29070(15) 0.61915(11) 0.0145(5) Uani 1 1 d . . . C11 C 1.0745(2) 0.28140(16) 0.64489(11) 0.0174(5) Uani 1 1 d . . . H11 H 1.1082 0.2243 0.6716 0.021 Uiso 1 1 calc R . . C12 C 1.1336(2) 0.37186(17) 0.62380(11) 0.0201(5) Uani 1 1 d . . . H12 H 1.2133 0.3868 0.6346 0.024 Uiso 1 1 calc R . . C13 C 1.0525(2) 0.43592(17) 0.58374(11) 0.0194(5) Uani 1 1 d . . . H13 H 1.0689 0.5010 0.5627 0.023 Uiso 1 1 calc R . . C14 C 0.9429(2) 0.38692(15) 0.58037(11) 0.0179(5) Uani 1 1 d . . . H14 H 0.8735 0.4131 0.5566 0.021 Uiso 1 1 calc R . . Fe1 Fe 1.05553(3) 0.28136(2) 0.548917(15) 0.01318(8) Uani 1 1 d . . . C15 C 1.0984(2) 0.29289(17) 0.46012(11) 0.0213(6) Uani 1 1 d . . . H15 H 1.1097 0.3586 0.4383 0.026 Uiso 1 1 calc R . . C16 C 1.1842(2) 0.23487(17) 0.50054(11) 0.0205(5) Uani 1 1 d . . . H16 H 1.2629 0.2546 0.5106 0.025 Uiso 1 1 calc R . . C17 C 1.1312(2) 0.14133(17) 0.52334(11) 0.0218(6) Uani 1 1 d . . . H17 H 1.1683 0.0874 0.5512 0.026 Uiso 1 1 calc R . . C18 C 1.0131(2) 0.14328(17) 0.49703(11) 0.0226(6) Uani 1 1 d . . . H18 H 0.9573 0.0909 0.5045 0.027 Uiso 1 1 calc R . . C19 C 0.9923(2) 0.23660(18) 0.45763(11) 0.0227(6) Uani 1 1 d . . . H19 H 0.9207 0.2576 0.4339 0.027 Uiso 1 1 calc R . . C20 C 0.8204(2) -0.00186(17) 0.72672(11) 0.0210(5) Uani 1 1 d . . . H20A H 0.7543 -0.0447 0.7352 0.031 Uiso 1 1 calc R . . H20B H 0.8381 0.0546 0.7592 0.031 Uiso 1 1 calc R . . H20C H 0.8870 -0.0500 0.7274 0.031 Uiso 1 1 calc R . . C21 C 0.7575(2) -0.03137(16) 0.61002(11) 0.0235(6) Uani 1 1 d . . . H21A H 0.6932 -0.0752 0.6200 0.035 Uiso 1 1 calc R . . H21B H 0.8227 -0.0794 0.6064 0.035 Uiso 1 1 calc R . . H21C H 0.7343 0.0069 0.5699 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01219(6) 0.01929(6) 0.01685(6) 0.00310(4) 0.00135(4) -0.00060(4) C1A 0.0167(14) 0.0440(15) 0.0235(15) 0.0081(12) 0.0033(12) -0.0029(12) O1A 0.0263(12) 0.0839(14) 0.0260(12) 0.0119(11) -0.0030(10) 0.0015(11) C1B 0.0176(14) 0.0278(13) 0.0203(13) -0.0030(10) 0.0023(11) 0.0037(11) O1B 0.0339(12) 0.0275(9) 0.0428(12) -0.0015(8) 0.0070(10) -0.0128(9) C1C 0.0183(15) 0.0267(13) 0.0420(17) 0.0129(12) -0.0065(12) 0.0014(12) O1C 0.0251(12) 0.0360(11) 0.0943(19) 0.0403(11) -0.0094(12) -0.0059(9) C1D 0.0179(14) 0.0197(12) 0.0309(15) 0.0041(10) -0.0016(12) 0.0023(11) O1D 0.0248(11) 0.0321(10) 0.0447(12) -0.0041(8) 0.0065(9) 0.0105(8) C1E 0.0183(14) 0.0306(13) 0.0190(14) -0.0010(10) 0.0017(11) -0.0040(11) O1E 0.0299(12) 0.0494(11) 0.0284(11) -0.0076(9) 0.0121(9) 0.0027(10) P1 0.0117(3) 0.0108(3) 0.0149(3) 0.0004(2) 0.0048(2) 0.0000(2) C1 0.0115(12) 0.0190(11) 0.0109(11) -0.0013(8) 0.0044(9) -0.0003(9) N1 0.0148(11) 0.0139(9) 0.0208(11) -0.0003(7) 0.0093(9) 0.0004(8) C2 0.0125(13) 0.0138(11) 0.0231(13) -0.0006(9) 0.0082(10) 0.0028(9) O1 0.0131(9) 0.0100(7) 0.0245(9) 0.0026(6) 0.0080(7) 0.0017(6) C3 0.0148(12) 0.0105(10) 0.0174(12) -0.0001(8) 0.0061(10) 0.0005(9) Si1 0.0186(4) 0.0156(3) 0.0244(4) -0.0027(3) 0.0126(3) -0.0018(3) C4 0.0195(14) 0.0198(12) 0.0347(16) -0.0008(10) 0.0117(12) -0.0036(10) C5 0.0358(17) 0.0219(12) 0.0260(15) -0.0005(10) 0.0182(13) -0.0018(12) C6 0.0266(16) 0.0280(13) 0.0410(17) -0.0084(11) 0.0188(14) -0.0014(12) Si2 0.0165(4) 0.0159(3) 0.0158(3) -0.0020(2) 0.0042(3) -0.0019(3) C7 0.0193(14) 0.0239(12) 0.0188(13) -0.0005(9) 0.0029(11) -0.0033(10) C8 0.0230(15) 0.0182(11) 0.0264(14) -0.0026(10) 0.0059(12) -0.0054(10) C9 0.0300(16) 0.0214(12) 0.0218(14) -0.0055(10) 0.0083(12) -0.0047(11) C10 0.0139(13) 0.0159(11) 0.0156(12) -0.0041(8) 0.0079(10) -0.0004(9) C11 0.0161(13) 0.0218(12) 0.0150(13) -0.0020(9) 0.0050(10) 0.0004(10) C12 0.0143(13) 0.0260(12) 0.0218(13) -0.0087(10) 0.0079(10) -0.0072(11) C13 0.0224(14) 0.0124(11) 0.0266(14) -0.0031(9) 0.0137(11) -0.0037(10) C14 0.0163(13) 0.0143(11) 0.0252(14) -0.0015(9) 0.0100(11) 0.0038(10) Fe1 0.01251(18) 0.01316(16) 0.01508(18) -0.00016(12) 0.00589(14) -0.00039(12) C15 0.0295(16) 0.0220(12) 0.0153(13) 0.0013(9) 0.0126(12) 0.0002(11) C16 0.0208(14) 0.0213(12) 0.0223(14) -0.0031(10) 0.0127(12) 0.0004(10) C17 0.0284(15) 0.0168(11) 0.0229(14) 0.0005(10) 0.0127(12) 0.0068(11) C18 0.0301(16) 0.0153(11) 0.0249(14) -0.0068(10) 0.0122(12) -0.0060(11) C19 0.0273(16) 0.0233(12) 0.0170(13) -0.0045(10) 0.0022(11) -0.0024(11) C20 0.0182(14) 0.0177(11) 0.0281(14) 0.0075(10) 0.0068(11) 0.0042(10) C21 0.0288(15) 0.0178(12) 0.0257(14) -0.0039(10) 0.0102(12) -0.0030(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 W1 C1A 2.017(3) . ? W1 C1C 2.025(3) . ? W1 C1E 2.039(2) . ? W1 C1D 2.042(2) . ? W1 C1B 2.055(2) . ? W1 P1 2.5121(6) . ? C1A O1A 1.142(3) . ? C1B O1B 1.141(3) . ? C1C O1C 1.143(3) . ? C1D O1D 1.139(3) . ? C1E O1E 1.138(3) . ? P1 O1 1.6296(14) . ? P1 C3 1.838(2) . ? P1 C1 1.882(2) . ? C1 N1 1.285(2) . ? C1 C10 1.480(3) . ? N1 C2 1.446(3) . ? C2 O1 1.464(2) . ? C2 C20 1.516(3) . ? C2 C21 1.521(3) . ? C3 Si2 1.911(2) . ? C3 Si1 1.931(2) . ? C3 H3 1.0000 . ? Si1 C5 1.864(3) . ? Si1 C4 1.867(3) . ? Si1 C6 1.871(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si2 C7 1.865(2) . ? Si2 C9 1.870(2) . ? Si2 C8 1.873(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.431(3) . ? C10 C14 1.436(3) . ? C10 Fe1 2.056(2) . ? C11 C12 1.420(3) . ? C11 Fe1 2.033(2) . ? C11 H11 0.9500 . ? C12 C13 1.418(3) . ? C12 Fe1 2.047(2) . ? C12 H12 0.9500 . ? C13 C14 1.416(3) . ? C13 Fe1 2.036(2) . ? C13 H13 0.9500 . ? C14 Fe1 2.041(2) . ? C14 H14 0.9500 . ? Fe1 C18 2.042(2) . ? Fe1 C17 2.046(2) . ? Fe1 C16 2.048(2) . ? Fe1 C15 2.048(2) . ? Fe1 C19 2.056(2) . ? Fe1 Cp1 1.645(2) . ? Fe1 Cp2 1.653(2) . ? C15 C16 1.417(3) . ? C15 C19 1.422(3) . ? C15 H15 0.9500 . ? C16 C17 1.427(3) . ? C16 H16 0.9500 . ? C17 C18 1.418(4) . ? C17 H17 0.9500 . ? C18 C19 1.419(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 C1A W1 C1C 88.38(11) . . ? C1A W1 C1E 90.45(10) . . ? C1C W1 C1E 91.30(9) . . ? C1A W1 C1D 92.54(10) . . ? C1C W1 C1D 88.09(10) . . ? C1E W1 C1D 176.93(10) . . ? C1A W1 C1B 88.64(10) . . ? C1C W1 C1B 176.91(10) . . ? C1E W1 C1B 87.92(9) . . ? C1D W1 C1B 92.84(9) . . ? C1A W1 P1 176.67(7) . . ? C1C W1 P1 94.76(8) . . ? C1E W1 P1 88.38(7) . . ? C1D W1 P1 88.68(7) . . ? C1B W1 P1 88.21(7) . . ? O1A C1A W1 178.8(3) . . ? O1B C1B W1 178.1(2) . . ? O1C C1C W1 177.9(2) . . ? O1D C1D W1 177.7(2) . . ? O1E C1E W1 178.3(2) . . ? O1 P1 C3 103.77(8) . . ? O1 P1 C1 89.04(8) . . ? C3 P1 C1 112.74(10) . . ? O1 P1 W1 112.70(6) . . ? C3 P1 W1 116.02(8) . . ? C1 P1 W1 118.33(7) . . ? N1 C1 C10 120.6(2) . . ? N1 C1 P1 111.45(16) . . ? C10 C1 P1 127.89(15) . . ? C1 N1 C2 114.59(18) . . ? N1 C2 O1 108.88(15) . . ? N1 C2 C20 111.2(2) . . ? O1 C2 C20 107.17(16) . . ? N1 C2 C21 109.14(17) . . ? O1 C2 C21 108.09(19) . . ? C20 C2 C21 112.20(18) . . ? C2 O1 P1 115.12(12) . . ? P1 C3 Si2 120.51(12) . . ? P1 C3 Si1 111.74(10) . . ? Si2 C3 Si1 113.44(11) . . ? P1 C3 H3 102.8 . . ? Si2 C3 H3 102.8 . . ? Si1 C3 H3 102.8 . . ? C5 Si1 C4 107.85(11) . . ? C5 Si1 C6 109.33(12) . . ? C4 Si1 C6 103.89(12) . . ? C5 Si1 C3 111.84(11) . . ? C4 Si1 C3 114.85(10) . . ? C6 Si1 C3 108.70(10) . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 Si2 C9 106.15(11) . . ? C7 Si2 C8 114.65(11) . . ? C9 Si2 C8 103.42(10) . . ? C7 Si2 C3 111.38(10) . . ? C9 Si2 C3 112.56(11) . . ? C8 Si2 C3 108.48(10) . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 . . ? C11 C10 C14 107.10(19) . . ? C11 C10 C1 124.3(2) . . ? C14 C10 C1 128.6(2) . . ? C11 C10 Fe1 68.68(12) . . ? C14 C10 Fe1 68.94(12) . . ? C1 C10 Fe1 129.71(14) . . ? C12 C11 C10 108.5(2) . . ? C12 C11 Fe1 70.14(13) . . ? C10 C11 Fe1 70.36(13) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe1 C11 H11 125.3 . . ? C13 C12 C11 107.8(2) . . ? C13 C12 Fe1 69.28(14) . . ? C11 C12 Fe1 69.13(13) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? Fe1 C12 H12 127.0 . . ? C14 C13 C12 108.72(19) . . ? C14 C13 Fe1 69.87(11) . . ? C12 C13 Fe1 70.07(12) . . ? C14 C13 H13 125.6 . . ? C12 C13 H13 125.6 . . ? Fe1 C13 H13 126.0 . . ? C13 C14 C10 107.9(2) . . ? C13 C14 Fe1 69.50(12) . . ? C10 C14 Fe1 70.03(12) . . ? C13 C14 H14 126.0 . . ? C10 C14 H14 126.0 . . ? Fe1 C14 H14 126.0 . . ? C11 Fe1 C13 68.57(9) . . ? C11 Fe1 C14 68.93(9) . . ? C13 Fe1 C14 40.64(9) . . ? C11 Fe1 C18 121.98(9) . . ? C13 Fe1 C18 162.14(11) . . ? C14 Fe1 C18 125.95(10) . . ? C11 Fe1 C17 106.69(9) . . ? C13 Fe1 C17 155.50(10) . . ? C14 Fe1 C17 162.17(9) . . ? C18 Fe1 C17 40.60(10) . . ? C11 Fe1 C12 40.73(8) . . ? C13 Fe1 C12 40.65(9) . . ? C14 Fe1 C12 68.59(10) . . ? C18 Fe1 C12 156.47(10) . . ? C17 Fe1 C12 120.11(10) . . ? C11 Fe1 C16 122.60(10) . . ? C13 Fe1 C16 120.04(9) . . ? C14 Fe1 C16 156.18(8) . . ? C18 Fe1 C16 68.43(9) . . ? C17 Fe1 C16 40.81(8) . . ? C12 Fe1 C16 105.58(10) . . ? C11 Fe1 C15 159.27(10) . . ? C13 Fe1 C15 107.30(9) . . ? C14 Fe1 C15 122.04(9) . . ? C18 Fe1 C15 68.06(9) . . ? C17 Fe1 C15 68.16(9) . . ? C12 Fe1 C15 123.01(9) . . ? C16 Fe1 C15 40.47(10) . . ? C11 Fe1 C10 40.96(9) . . ? C13 Fe1 C10 68.60(8) . . ? C14 Fe1 C10 41.03(8) . . ? C18 Fe1 C10 108.94(9) . . ? C17 Fe1 C10 124.52(8) . . ? C12 Fe1 C10 68.65(9) . . ? C16 Fe1 C10 160.35(9) . . ? C15 Fe1 C10 158.31(11) . . ? C11 Fe1 C19 158.18(9) . . ? C13 Fe1 C19 124.87(10) . . ? C14 Fe1 C19 108.95(10) . . ? C18 Fe1 C19 40.51(9) . . ? C17 Fe1 C19 68.32(10) . . ? C12 Fe1 C19 160.42(9) . . ? C16 Fe1 C19 68.40(10) . . ? C15 Fe1 C19 40.54(10) . . ? C10 Fe1 C19 123.13(10) . . ? Cp1 Fe1 Cp2 178.2(1) . . ? C16 C15 C19 108.7(2) . . ? C16 C15 Fe1 69.76(13) . . ? C19 C15 Fe1 70.03(13) . . ? C16 C15 H15 125.6 . . ? C19 C15 H15 125.6 . . ? Fe1 C15 H15 126.2 . . ? C15 C16 C17 107.6(2) . . ? C15 C16 Fe1 69.77(13) . . ? C17 C16 Fe1 69.54(12) . . ? C15 C16 H16 126.2 . . ? C17 C16 H16 126.2 . . ? Fe1 C16 H16 126.0 . . ? C18 C17 C16 107.8(2) . . ? C18 C17 Fe1 69.54(12) . . ? C16 C17 Fe1 69.65(12) . . ? C18 C17 H17 126.1 . . ? C16 C17 H17 126.1 . . ? Fe1 C17 H17 126.3 . . ? C17 C18 C19 108.5(2) . . ? C17 C18 Fe1 69.86(13) . . ? C19 C18 Fe1 70.27(12) . . ? C17 C18 H18 125.7 . . ? C19 C18 H18 125.7 . . ? Fe1 C18 H18 125.7 . . ? C18 C19 C15 107.4(2) . . ? C18 C19 Fe1 69.21(13) . . ? C15 C19 Fe1 69.43(14) . . ? C18 C19 H19 126.3 . . ? C15 C19 H19 126.3 . . ? Fe1 C19 H19 126.6 . . ? C2 C20 H20A 109.5 . . ? C2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1C W1 C1A O1A 90(12) . . . . ? C1E W1 C1A O1A -1(12) . . . . ? C1D W1 C1A O1A 178(100) . . . . ? C1B W1 C1A O1A -89(12) . . . . ? P1 W1 C1A O1A -70(12) . . . . ? C1A W1 C1B O1B 35(6) . . . . ? C1C W1 C1B O1B 20(7) . . . . ? C1E W1 C1B O1B -56(6) . . . . ? C1D W1 C1B O1B 127(6) . . . . ? P1 W1 C1B O1B -144(6) . . . . ? C1A W1 C1C O1C 9(7) . . . . ? C1E W1 C1C O1C 99(7) . . . . ? C1D W1 C1C O1C -84(7) . . . . ? C1B W1 C1C O1C 24(8) . . . . ? P1 W1 C1C O1C -172(7) . . . . ? C1A W1 C1D O1D -130(5) . . . . ? C1C W1 C1D O1D -42(5) . . . . ? C1E W1 C1D O1D 37(6) . . . . ? C1B W1 C1D O1D 141(5) . . . . ? P1 W1 C1D O1D 53(5) . . . . ? C1A W1 C1E O1E -87(8) . . . . ? C1C W1 C1E O1E -176(100) . . . . ? C1D W1 C1E O1E 106(8) . . . . ? C1B W1 C1E O1E 1(8) . . . . ? P1 W1 C1E O1E 90(8) . . . . ? C1A W1 P1 O1 -6.7(13) . . . . ? C1C W1 P1 O1 -167.23(9) . . . . ? C1E W1 P1 O1 -76.06(9) . . . . ? C1D W1 P1 O1 104.80(9) . . . . ? C1B W1 P1 O1 11.91(8) . . . . ? C1A W1 P1 C3 -126.1(13) . . . . ? C1C W1 P1 C3 73.34(11) . . . . ? C1E W1 P1 C3 164.51(10) . . . . ? C1D W1 P1 C3 -14.63(10) . . . . ? C1B W1 P1 C3 -107.52(10) . . . . ? C1A W1 P1 C1 95.1(13) . . . . ? C1C W1 P1 C1 -65.40(10) . . . . ? C1E W1 P1 C1 25.76(10) . . . . ? C1D W1 P1 C1 -153.38(10) . . . . ? C1B W1 P1 C1 113.74(9) . . . . ? O1 P1 C1 N1 4.81(17) . . . . ? C3 P1 C1 N1 109.35(17) . . . . ? W1 P1 C1 N1 -110.62(15) . . . . ? O1 P1 C1 C10 -173.6(2) . . . . ? C3 P1 C1 C10 -69.0(2) . . . . ? W1 P1 C1 C10 71.0(2) . . . . ? C10 C1 N1 C2 178.9(2) . . . . ? P1 C1 N1 C2 0.4(2) . . . . ? C1 N1 C2 O1 -6.4(3) . . . . ? C1 N1 C2 C20 -124.2(2) . . . . ? C1 N1 C2 C21 111.4(2) . . . . ? N1 C2 O1 P1 10.4(2) . . . . ? C20 C2 O1 P1 130.84(15) . . . . ? C21 C2 O1 P1 -108.03(16) . . . . ? C3 P1 O1 C2 -121.74(15) . . . . ? C1 P1 O1 C2 -8.55(15) . . . . ? W1 P1 O1 C2 111.95(14) . . . . ? O1 P1 C3 Si2 104.05(12) . . . . ? C1 P1 C3 Si2 9.23(15) . . . . ? W1 P1 C3 Si2 -131.77(10) . . . . ? O1 P1 C3 Si1 -33.01(14) . . . . ? C1 P1 C3 Si1 -127.83(11) . . . . ? W1 P1 C3 Si1 91.17(11) . . . . ? P1 C3 Si1 C5 90.95(14) . . . . ? Si2 C3 Si1 C5 -49.28(14) . . . . ? P1 C3 Si1 C4 -32.39(16) . . . . ? Si2 C3 Si1 C4 -172.62(11) . . . . ? P1 C3 Si1 C6 -148.24(13) . . . . ? Si2 C3 Si1 C6 71.53(15) . . . . ? P1 C3 Si2 C7 -53.46(15) . . . . ? Si1 C3 Si2 C7 82.94(13) . . . . ? P1 C3 Si2 C9 -172.55(12) . . . . ? Si1 C3 Si2 C9 -36.15(14) . . . . ? P1 C3 Si2 C8 73.63(14) . . . . ? Si1 C3 Si2 C8 -149.98(11) . . . . ? N1 C1 C10 C11 -30.6(3) . . . . ? P1 C1 C10 C11 147.67(18) . . . . ? N1 C1 C10 C14 152.8(2) . . . . ? P1 C1 C10 C14 -29.0(3) . . . . ? N1 C1 C10 Fe1 59.1(3) . . . . ? P1 C1 C10 Fe1 -122.68(18) . . . . ? C14 C10 C11 C12 1.6(2) . . . . ? C1 C10 C11 C12 -175.64(19) . . . . ? Fe1 C10 C11 C12 60.03(15) . . . . ? C14 C10 C11 Fe1 -58.43(14) . . . . ? C1 C10 C11 Fe1 124.3(2) . . . . ? C10 C11 C12 C13 -1.5(2) . . . . ? Fe1 C11 C12 C13 58.69(15) . . . . ? C10 C11 C12 Fe1 -60.17(15) . . . . ? C11 C12 C13 C14 0.8(2) . . . . ? Fe1 C12 C13 C14 59.37(15) . . . . ? C11 C12 C13 Fe1 -58.60(15) . . . . ? C12 C13 C14 C10 0.2(2) . . . . ? Fe1 C13 C14 C10 59.72(14) . . . . ? C12 C13 C14 Fe1 -59.50(15) . . . . ? C11 C10 C14 C13 -1.1(2) . . . . ? C1 C10 C14 C13 176.0(2) . . . . ? Fe1 C10 C14 C13 -59.38(14) . . . . ? C11 C10 C14 Fe1 58.26(14) . . . . ? C1 C10 C14 Fe1 -124.7(2) . . . . ? C12 C11 Fe1 C13 -37.51(13) . . . . ? C10 C11 Fe1 C13 81.61(13) . . . . ? C12 C11 Fe1 C14 -81.25(14) . . . . ? C10 C11 Fe1 C14 37.87(11) . . . . ? C12 C11 Fe1 C18 158.67(14) . . . . ? C10 C11 Fe1 C18 -82.21(15) . . . . ? C12 C11 Fe1 C17 117.03(14) . . . . ? C10 C11 Fe1 C17 -123.85(13) . . . . ? C10 C11 Fe1 C12 119.12(18) . . . . ? C12 C11 Fe1 C16 75.29(15) . . . . ? C10 C11 Fe1 C16 -165.59(11) . . . . ? C12 C11 Fe1 C15 44.8(3) . . . . ? C10 C11 Fe1 C15 163.9(2) . . . . ? C12 C11 Fe1 C10 -119.12(18) . . . . ? C12 C11 Fe1 C19 -169.8(2) . . . . ? C10 C11 Fe1 C19 -50.6(3) . . . . ? C14 C13 Fe1 C11 -82.20(15) . . . . ? C12 C13 Fe1 C11 37.57(13) . . . . ? C12 C13 Fe1 C14 119.77(19) . . . . ? C14 C13 Fe1 C18 47.4(3) . . . . ? C12 C13 Fe1 C18 167.2(3) . . . . ? C14 C13 Fe1 C17 -165.5(2) . . . . ? C12 C13 Fe1 C17 -45.7(3) . . . . ? C14 C13 Fe1 C12 -119.77(19) . . . . ? C14 C13 Fe1 C16 161.60(14) . . . . ? C12 C13 Fe1 C16 -78.63(15) . . . . ? C14 C13 Fe1 C15 119.35(15) . . . . ? C12 C13 Fe1 C15 -120.88(14) . . . . ? C14 C13 Fe1 C10 -38.05(14) . . . . ? C12 C13 Fe1 C10 81.72(14) . . . . ? C14 C13 Fe1 C19 78.21(16) . . . . ? C12 C13 Fe1 C19 -162.01(13) . . . . ? C13 C14 Fe1 C11 81.25(15) . . . . ? C10 C14 Fe1 C11 -37.81(13) . . . . ? C10 C14 Fe1 C13 -119.1(2) . . . . ? C13 C14 Fe1 C18 -163.81(14) . . . . ? C10 C14 Fe1 C18 77.13(17) . . . . ? C13 C14 Fe1 C17 160.2(3) . . . . ? C10 C14 Fe1 C17 41.1(4) . . . . ? C13 C14 Fe1 C12 37.40(13) . . . . ? C10 C14 Fe1 C12 -81.65(14) . . . . ? C13 C14 Fe1 C16 -42.6(3) . . . . ? C10 C14 Fe1 C16 -161.6(2) . . . . ? C13 C14 Fe1 C15 -79.02(17) . . . . ? C10 C14 Fe1 C15 161.93(14) . . . . ? C13 C14 Fe1 C10 119.1(2) . . . . ? C13 C14 Fe1 C19 -121.88(14) . . . . ? C10 C14 Fe1 C19 119.06(14) . . . . ? C13 C12 Fe1 C11 -119.55(19) . . . . ? C11 C12 Fe1 C13 119.55(19) . . . . ? C13 C12 Fe1 C14 -37.39(12) . . . . ? C11 C12 Fe1 C14 82.16(14) . . . . ? C13 C12 Fe1 C18 -170.2(2) . . . . ? C11 C12 Fe1 C18 -50.6(3) . . . . ? C13 C12 Fe1 C17 159.93(13) . . . . ? C11 C12 Fe1 C17 -80.53(15) . . . . ? C13 C12 Fe1 C16 118.23(13) . . . . ? C11 C12 Fe1 C16 -122.23(14) . . . . ? C13 C12 Fe1 C15 77.74(16) . . . . ? C11 C12 Fe1 C15 -162.71(13) . . . . ? C13 C12 Fe1 C10 -81.60(14) . . . . ? C11 C12 Fe1 C10 37.94(13) . . . . ? C13 C12 Fe1 C19 49.1(3) . . . . ? C11 C12 Fe1 C19 168.6(3) . . . . ? C14 C10 Fe1 C11 119.24(18) . . . . ? C1 C10 Fe1 C11 -117.5(2) . . . . ? C11 C10 Fe1 C13 -81.54(14) . . . . ? C14 C10 Fe1 C13 37.70(14) . . . . ? C1 C10 Fe1 C13 161.0(2) . . . . ? C11 C10 Fe1 C14 -119.24(18) . . . . ? C1 C10 Fe1 C14 123.3(3) . . . . ? C11 C10 Fe1 C18 117.31(13) . . . . ? C14 C10 Fe1 C18 -123.45(14) . . . . ? C1 C10 Fe1 C18 -0.2(2) . . . . ? C11 C10 Fe1 C17 74.90(16) . . . . ? C14 C10 Fe1 C17 -165.86(14) . . . . ? C1 C10 Fe1 C17 -42.6(3) . . . . ? C11 C10 Fe1 C12 -37.74(12) . . . . ? C14 C10 Fe1 C12 81.50(14) . . . . ? C1 C10 Fe1 C12 -155.2(2) . . . . ? C11 C10 Fe1 C16 38.6(3) . . . . ? C14 C10 Fe1 C16 157.8(3) . . . . ? C1 C10 Fe1 C16 -78.9(4) . . . . ? C11 C10 Fe1 C15 -164.6(2) . . . . ? C14 C10 Fe1 C15 -45.4(3) . . . . ? C1 C10 Fe1 C15 77.9(3) . . . . ? C11 C10 Fe1 C19 159.93(12) . . . . ? C14 C10 Fe1 C19 -80.83(15) . . . . ? C1 C10 Fe1 C19 42.4(2) . . . . ? C11 Fe1 C15 C16 41.2(3) . . . . ? C13 Fe1 C15 C16 116.28(14) . . . . ? C14 Fe1 C15 C16 158.32(13) . . . . ? C18 Fe1 C15 C16 -82.04(15) . . . . ? C17 Fe1 C15 C16 -38.13(14) . . . . ? C12 Fe1 C15 C16 74.46(16) . . . . ? C10 Fe1 C15 C16 -168.25(19) . . . . ? C19 Fe1 C15 C16 -119.86(19) . . . . ? C11 Fe1 C15 C19 161.1(2) . . . . ? C13 Fe1 C15 C19 -123.86(14) . . . . ? C14 Fe1 C15 C19 -81.82(15) . . . . ? C18 Fe1 C15 C19 37.82(14) . . . . ? C17 Fe1 C15 C19 81.73(15) . . . . ? C12 Fe1 C15 C19 -165.68(14) . . . . ? C16 Fe1 C15 C19 119.86(19) . . . . ? C10 Fe1 C15 C19 -48.4(3) . . . . ? C19 C15 C16 C17 0.1(3) . . . . ? Fe1 C15 C16 C17 59.52(15) . . . . ? C19 C15 C16 Fe1 -59.39(16) . . . . ? C11 Fe1 C16 C15 -163.93(13) . . . . ? C13 Fe1 C16 C15 -81.46(17) . . . . ? C14 Fe1 C16 C15 -50.8(3) . . . . ? C18 Fe1 C16 C15 81.04(15) . . . . ? C17 Fe1 C16 C15 118.7(2) . . . . ? C12 Fe1 C16 C15 -122.99(14) . . . . ? C10 Fe1 C16 C15 167.1(2) . . . . ? C19 Fe1 C16 C15 37.32(13) . . . . ? C11 Fe1 C16 C17 77.36(17) . . . . ? C13 Fe1 C16 C17 159.82(15) . . . . ? C14 Fe1 C16 C17 -169.6(2) . . . . ? C18 Fe1 C16 C17 -37.68(15) . . . . ? C12 Fe1 C16 C17 118.29(15) . . . . ? C15 Fe1 C16 C17 -118.7(2) . . . . ? C10 Fe1 C16 C17 48.3(3) . . . . ? C19 Fe1 C16 C17 -81.40(16) . . . . ? C15 C16 C17 C18 -0.4(2) . . . . ? Fe1 C16 C17 C18 59.28(15) . . . . ? C15 C16 C17 Fe1 -59.67(15) . . . . ? C11 Fe1 C17 C18 119.98(14) . . . . ? C13 Fe1 C17 C18 -165.2(2) . . . . ? C14 Fe1 C17 C18 47.0(4) . . . . ? C12 Fe1 C17 C18 162.19(13) . . . . ? C16 Fe1 C17 C18 -119.1(2) . . . . ? C15 Fe1 C17 C18 -81.31(15) . . . . ? C10 Fe1 C17 C18 78.62(17) . . . . ? C19 Fe1 C17 C18 -37.51(13) . . . . ? C11 Fe1 C17 C16 -120.88(15) . . . . ? C13 Fe1 C17 C16 -46.0(3) . . . . ? C14 Fe1 C17 C16 166.2(3) . . . . ? C18 Fe1 C17 C16 119.1(2) . . . . ? C12 Fe1 C17 C16 -78.67(17) . . . . ? C15 Fe1 C17 C16 37.82(16) . . . . ? C10 Fe1 C17 C16 -162.24(15) . . . . ? C19 Fe1 C17 C16 81.63(16) . . . . ? C16 C17 C18 C19 0.5(2) . . . . ? Fe1 C17 C18 C19 59.85(15) . . . . ? C16 C17 C18 Fe1 -59.35(15) . . . . ? C11 Fe1 C18 C17 -77.99(16) . . . . ? C13 Fe1 C18 C17 159.8(3) . . . . ? C14 Fe1 C18 C17 -163.93(13) . . . . ? C12 Fe1 C18 C17 -41.5(3) . . . . ? C16 Fe1 C18 C17 37.87(13) . . . . ? C15 Fe1 C18 C17 81.59(15) . . . . ? C10 Fe1 C18 C17 -121.36(14) . . . . ? C19 Fe1 C18 C17 119.4(2) . . . . ? C11 Fe1 C18 C19 162.57(15) . . . . ? C13 Fe1 C18 C19 40.3(3) . . . . ? C14 Fe1 C18 C19 76.63(17) . . . . ? C17 Fe1 C18 C19 -119.4(2) . . . . ? C12 Fe1 C18 C19 -160.9(2) . . . . ? C16 Fe1 C18 C19 -81.57(15) . . . . ? C15 Fe1 C18 C19 -37.84(15) . . . . ? C10 Fe1 C18 C19 119.21(15) . . . . ? C17 C18 C19 C15 -0.4(2) . . . . ? Fe1 C18 C19 C15 59.18(15) . . . . ? C17 C18 C19 Fe1 -59.60(15) . . . . ? C16 C15 C19 C18 0.2(3) . . . . ? Fe1 C15 C19 C18 -59.04(15) . . . . ? C16 C15 C19 Fe1 59.22(16) . . . . ? C11 Fe1 C19 C18 -43.1(3) . . . . ? C13 Fe1 C19 C18 -166.00(14) . . . . ? C14 Fe1 C19 C18 -123.62(14) . . . . ? C17 Fe1 C19 C18 37.58(14) . . . . ? C12 Fe1 C19 C18 157.1(3) . . . . ? C16 Fe1 C19 C18 81.64(15) . . . . ? C15 Fe1 C19 C18 118.9(2) . . . . ? C10 Fe1 C19 C18 -80.37(16) . . . . ? C11 Fe1 C19 C15 -162.0(2) . . . . ? C13 Fe1 C19 C15 75.10(17) . . . . ? C14 Fe1 C19 C15 117.48(14) . . . . ? C18 Fe1 C19 C15 -118.9(2) . . . . ? C17 Fe1 C19 C15 -81.32(15) . . . . ? C12 Fe1 C19 C15 38.2(4) . . . . ? C16 Fe1 C19 C15 -37.26(13) . . . . ? C10 Fe1 C19 C15 160.73(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9 H9C O1E 0.98 2.52 3.391(3) 148.4 4_566 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.772 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.085 data_str021_m_compound_6a _database_code_depnum_ccdc_archive 'CCDC 777322' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [5-Bis(trimethylsilyl)methyl-2,4-bisferrocenyl-1,3,5- oxazaphosphol-3-ene-kappaP]pentacarbonyltungsten(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H38 Fe2 N O6 P Si2 W' _chemical_formula_sum 'C34 H38 Fe2 N O6 P Si2 W' _chemical_formula_weight 939.35 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' Si Si 0.0817 0.0704 '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' Fe Fe 0.3463 0.8444 '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 orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 18.8898(2) _cell_length_b 28.5021(3) _cell_length_c 13.8338(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7448.10(12) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8860 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 4.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36587 _exptl_absorpt_correction_T_max 0.53554 _exptl_absorpt_process_details 'MULABS (Platon, cf. Blessing, 1995)' _exptl_special_details ; dx = 40 mm, 40 sec./deg., 1 deg., 2 sets, 219 frames, mos.= 0.405(1) deg. ; _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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37905 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8475 _reflns_number_gt 6332 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 8475 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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 W1 W 0.407536(6) 0.259586(4) 0.151060(9) 0.02649(4) Uani 1 1 d . . . C1A C 0.35131(17) 0.20091(11) 0.1291(3) 0.0469(9) Uani 1 1 d . . . O1A O 0.32027(13) 0.16713(8) 0.1133(2) 0.0720(9) Uani 1 1 d . . . C1B C 0.48186(16) 0.23421(9) 0.0595(2) 0.0310(7) Uani 1 1 d . . . O1B O 0.52330(12) 0.22018(7) 0.00630(16) 0.0436(6) Uani 1 1 d . . . C1C C 0.33452(18) 0.28559(10) 0.2478(3) 0.0416(8) Uani 1 1 d . . . O1C O 0.29557(14) 0.29885(8) 0.3038(2) 0.0630(8) Uani 1 1 d . . . C1D C 0.35764(17) 0.28707(10) 0.0317(3) 0.0390(8) Uani 1 1 d . . . O1D O 0.33118(13) 0.30019(8) -0.03705(18) 0.0601(7) Uani 1 1 d . . . C1E C 0.45931(17) 0.22892(10) 0.2645(2) 0.0363(8) Uani 1 1 d . . . O1E O 0.48803(14) 0.21091(8) 0.32646(17) 0.0567(7) Uani 1 1 d . . . P1 P 0.48115(4) 0.33155(2) 0.17338(5) 0.01938(15) Uani 1 1 d . . . C1 C 0.43555(13) 0.38548(8) 0.22049(19) 0.0184(6) Uani 1 1 d . . . N1 N 0.45554(11) 0.39615(7) 0.30523(16) 0.0212(5) Uani 1 1 d . . . C2 C 0.50854(14) 0.36455(8) 0.34406(19) 0.0219(6) Uani 1 1 d . . . H2 H 0.4866 0.3459 0.3975 0.026 Uiso 1 1 calc R . . O1 O 0.53186(9) 0.33224(5) 0.26901(13) 0.0251(4) Uani 1 1 d . . . C3 C 0.54366(14) 0.34290(8) 0.07580(19) 0.0224(6) Uani 1 1 d . . . H3 H 0.5276 0.3205 0.0248 0.027 Uiso 1 1 calc R . . Si1 Si 0.54170(4) 0.40153(2) 0.00914(6) 0.02414(17) Uani 1 1 d . . . C4 C 0.61146(16) 0.40260(10) -0.0866(2) 0.0342(7) Uani 1 1 d . . . H4A H 0.6583 0.4001 -0.0564 0.051 Uiso 1 1 calc R . . H4B H 0.6084 0.4321 -0.1227 0.051 Uiso 1 1 calc R . . H4C H 0.6043 0.3762 -0.1308 0.051 Uiso 1 1 calc R . . C5 C 0.55860(16) 0.45193(9) 0.0923(2) 0.0309(7) Uani 1 1 d . . . H5A H 0.6039 0.4473 0.1255 0.046 Uiso 1 1 calc R . . H5B H 0.5204 0.4539 0.1402 0.046 Uiso 1 1 calc R . . H5C H 0.5603 0.4811 0.0550 0.046 Uiso 1 1 calc R . . C6 C 0.45712(15) 0.40649(9) -0.0586(2) 0.0308(7) Uani 1 1 d . . . H6A H 0.4515 0.3792 -0.1009 0.046 Uiso 1 1 calc R . . H6B H 0.4577 0.4351 -0.0978 0.046 Uiso 1 1 calc R . . H6C H 0.4175 0.4078 -0.0129 0.046 Uiso 1 1 calc R . . Si2 Si 0.63677(4) 0.31981(3) 0.10637(7) 0.0329(2) Uani 1 1 d . . . C7 C 0.63778(17) 0.26593(10) 0.1844(3) 0.0435(9) Uani 1 1 d . . . H7A H 0.6160 0.2731 0.2470 0.065 Uiso 1 1 calc R . . H7B H 0.6868 0.2557 0.1944 0.065 Uiso 1 1 calc R . . H7C H 0.6111 0.2408 0.1525 0.065 Uiso 1 1 calc R . . C8 C 0.69089(16) 0.36572(11) 0.1677(2) 0.0422(8) Uani 1 1 d . . . H8A H 0.6677 0.3750 0.2281 0.063 Uiso 1 1 calc R . . H8B H 0.6954 0.3931 0.1253 0.063 Uiso 1 1 calc R . . H8C H 0.7380 0.3532 0.1820 0.063 Uiso 1 1 calc R . . C9 C 0.67906(18) 0.30084(11) -0.0095(3) 0.0534(10) Uani 1 1 d . . . H9A H 0.6498 0.2767 -0.0402 0.080 Uiso 1 1 calc R . . H9B H 0.7262 0.2880 0.0039 0.080 Uiso 1 1 calc R . . H9C H 0.6834 0.3279 -0.0529 0.080 Uiso 1 1 calc R . . C10 C 0.38113(14) 0.41307(8) 0.16917(17) 0.0188(6) Uani 1 1 d . . . C11 C 0.32067(14) 0.39575(9) 0.11865(19) 0.0252(6) Uani 1 1 d . . . H11 H 0.3073 0.3637 0.1130 0.030 Uiso 1 1 calc R . . C12 C 0.28408(15) 0.43431(10) 0.0785(2) 0.0303(7) Uani 1 1 d . . . H12 H 0.2419 0.4326 0.0412 0.036 Uiso 1 1 calc R . . C13 C 0.32077(15) 0.47581(10) 0.1032(2) 0.0307(7) Uani 1 1 d . . . H13 H 0.3079 0.5068 0.0847 0.037 Uiso 1 1 calc R . . C14 C 0.38041(14) 0.46317(9) 0.16040(19) 0.0263(6) Uani 1 1 d . . . H14 H 0.4138 0.4842 0.1879 0.032 Uiso 1 1 calc R . . Fe1 Fe 0.28969(2) 0.440977(13) 0.22455(3) 0.02478(10) Uani 1 1 d . . . C15 C 0.2799(2) 0.41990(14) 0.3632(2) 0.0581(11) Uani 1 1 d . . . H15 H 0.3127 0.4003 0.3959 0.070 Uiso 1 1 calc R . . C16 C 0.2212(2) 0.40517(13) 0.3122(3) 0.0544(10) Uani 1 1 d . . . H16 H 0.2062 0.3736 0.3043 0.065 Uiso 1 1 calc R . . C17 C 0.18805(17) 0.44428(12) 0.2745(3) 0.0489(9) Uani 1 1 d . . . H17 H 0.1464 0.4438 0.2361 0.059 Uiso 1 1 calc R . . C18 C 0.22446(19) 0.48419(12) 0.3011(3) 0.0475(9) Uani 1 1 d . . . H18 H 0.2126 0.5155 0.2842 0.057 Uiso 1 1 calc R . . C19 C 0.2827(2) 0.46993(14) 0.3580(2) 0.0561(11) Uani 1 1 d . . . H19 H 0.3170 0.4898 0.3871 0.067 Uiso 1 1 calc R . . C20 C 0.57073(15) 0.39029(9) 0.38365(19) 0.0229(6) Uani 1 1 d . . . C21 C 0.62753(15) 0.37007(10) 0.4375(2) 0.0295(7) Uani 1 1 d . . . H21 H 0.6327 0.3378 0.4534 0.035 Uiso 1 1 calc R . . C22 C 0.67468(15) 0.40646(10) 0.4631(2) 0.0372(7) Uani 1 1 d . . . H22 H 0.7169 0.4029 0.4996 0.045 Uiso 1 1 calc R . . C23 C 0.64836(15) 0.44907(10) 0.4251(2) 0.0339(7) Uani 1 1 d . . . H23 H 0.6698 0.4790 0.4318 0.041 Uiso 1 1 calc R . . C24 C 0.58440(15) 0.43941(9) 0.37535(19) 0.0254(6) Uani 1 1 d . . . H24 H 0.5557 0.4616 0.3424 0.031 Uiso 1 1 calc R . . Fe2 Fe 0.57637(2) 0.419113(14) 0.51785(3) 0.02688(10) Uani 1 1 d . . . C25 C 0.54670(17) 0.46643(10) 0.6224(2) 0.0351(7) Uani 1 1 d . . . H25 H 0.5586 0.4988 0.6244 0.042 Uiso 1 1 calc R . . C26 C 0.58647(19) 0.42929(11) 0.6640(2) 0.0442(9) Uani 1 1 d . . . H26 H 0.6295 0.4323 0.6989 0.053 Uiso 1 1 calc R . . C27 C 0.5502(2) 0.38702(11) 0.6440(2) 0.0474(9) Uani 1 1 d . . . H27 H 0.5650 0.3565 0.6628 0.057 Uiso 1 1 calc R . . C28 C 0.48819(18) 0.39784(10) 0.5910(2) 0.0399(8) Uani 1 1 d . . . H28 H 0.4539 0.3760 0.5688 0.048 Uiso 1 1 calc R . . C29 C 0.48625(16) 0.44695(10) 0.5772(2) 0.0347(7) Uani 1 1 d . . . H29 H 0.4506 0.4639 0.5436 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02641(7) 0.01994(7) 0.03310(7) -0.00203(5) 0.00281(6) -0.00487(5) C1A 0.035(2) 0.0291(19) 0.076(3) -0.0095(17) 0.0092(18) -0.0034(15) O1A 0.0478(16) 0.0355(14) 0.133(3) -0.0178(15) 0.0099(16) -0.0205(12) C1B 0.0347(18) 0.0208(16) 0.0374(19) -0.0016(13) -0.0028(15) -0.0039(12) O1B 0.0547(16) 0.0338(12) 0.0423(14) -0.0133(10) 0.0120(12) 0.0000(10) C1C 0.042(2) 0.0282(17) 0.055(2) 0.0029(16) 0.0146(18) -0.0031(14) O1C 0.0685(19) 0.0464(15) 0.074(2) 0.0013(13) 0.0417(16) 0.0034(12) C1D 0.038(2) 0.0304(18) 0.048(2) -0.0121(16) -0.0085(17) 0.0017(13) O1D 0.0733(19) 0.0572(15) 0.0497(17) -0.0166(12) -0.0307(15) 0.0175(13) C1E 0.044(2) 0.0258(16) 0.039(2) 0.0051(14) 0.0078(17) -0.0036(13) O1E 0.081(2) 0.0457(15) 0.0440(16) 0.0169(12) -0.0032(14) 0.0049(13) P1 0.0215(4) 0.0176(4) 0.0191(4) -0.0003(3) -0.0016(3) -0.0009(3) C1 0.0199(14) 0.0172(13) 0.0180(15) 0.0010(11) 0.0018(11) -0.0048(10) N1 0.0204(12) 0.0237(12) 0.0195(13) -0.0001(9) -0.0018(10) -0.0003(9) C2 0.0262(15) 0.0227(15) 0.0170(14) 0.0027(11) -0.0024(12) 0.0022(11) O1 0.0297(11) 0.0227(10) 0.0229(11) -0.0026(8) -0.0067(9) 0.0066(8) C3 0.0257(15) 0.0211(14) 0.0203(15) -0.0023(11) 0.0033(12) -0.0021(11) Si1 0.0285(4) 0.0235(4) 0.0204(4) 0.0022(3) 0.0016(3) -0.0022(3) C4 0.0407(19) 0.0361(17) 0.0259(17) 0.0066(13) 0.0068(14) -0.0038(13) C5 0.0351(18) 0.0257(15) 0.0319(18) 0.0019(13) -0.0025(14) -0.0041(12) C6 0.0367(18) 0.0319(16) 0.0237(16) -0.0008(12) -0.0004(14) 0.0036(13) Si2 0.0257(5) 0.0319(4) 0.0410(5) 0.0059(4) 0.0059(4) 0.0048(3) C7 0.0308(19) 0.040(2) 0.059(2) 0.0110(16) 0.0026(17) 0.0138(14) C8 0.0251(18) 0.053(2) 0.049(2) 0.0072(16) 0.0001(15) -0.0018(14) C9 0.052(2) 0.045(2) 0.063(3) 0.0014(17) 0.022(2) 0.0175(16) C10 0.0195(14) 0.0243(15) 0.0126(14) -0.0007(10) 0.0007(11) 0.0010(11) C11 0.0237(16) 0.0301(16) 0.0220(15) -0.0079(12) -0.0012(12) 0.0006(12) C12 0.0226(16) 0.0504(19) 0.0180(16) -0.0056(13) -0.0051(12) 0.0074(13) C13 0.0291(17) 0.0353(17) 0.0278(17) 0.0110(13) 0.0026(14) 0.0073(13) C14 0.0251(15) 0.0254(16) 0.0283(17) 0.0019(12) -0.0016(13) -0.0002(12) Fe1 0.0245(2) 0.0292(2) 0.0206(2) -0.00344(17) 0.00155(17) 0.00383(16) C15 0.074(3) 0.076(3) 0.024(2) 0.0116(18) 0.018(2) 0.038(2) C16 0.065(3) 0.049(2) 0.050(3) 0.0036(18) 0.033(2) 0.0002(19) C17 0.0278(19) 0.070(3) 0.049(2) -0.0063(19) 0.0123(17) 0.0019(17) C18 0.050(2) 0.045(2) 0.047(2) -0.0066(17) 0.0193(19) 0.0160(17) C19 0.053(2) 0.088(3) 0.027(2) -0.0328(18) 0.0153(18) -0.015(2) C20 0.0254(15) 0.0285(16) 0.0147(14) -0.0026(11) -0.0024(12) 0.0008(11) C21 0.0269(17) 0.0330(16) 0.0285(17) -0.0018(13) -0.0037(13) 0.0043(12) C22 0.0196(16) 0.057(2) 0.0349(19) -0.0057(15) -0.0099(14) 0.0032(14) C23 0.0305(18) 0.0386(18) 0.0325(18) -0.0042(14) 0.0013(14) -0.0102(13) C24 0.0320(17) 0.0257(16) 0.0187(15) -0.0011(11) 0.0029(12) -0.0019(12) Fe2 0.0323(2) 0.0301(2) 0.0182(2) -0.00183(17) -0.00491(18) -0.00165(17) C25 0.048(2) 0.0321(17) 0.0255(17) -0.0063(13) -0.0014(15) -0.0021(14) C26 0.068(3) 0.046(2) 0.0185(17) -0.0090(14) -0.0115(16) 0.0044(17) C27 0.083(3) 0.038(2) 0.0212(18) 0.0061(14) 0.0064(18) 0.0085(18) C28 0.050(2) 0.0406(19) 0.0292(19) -0.0056(14) 0.0157(16) -0.0127(15) C29 0.0384(19) 0.0406(19) 0.0250(17) -0.0026(14) 0.0049(14) 0.0003(14) _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 C1A 2.004(3) . ? W1 C1B 2.024(3) . ? W1 C1E 2.045(3) . ? W1 C1D 2.056(3) . ? W1 C1C 2.060(3) . ? W1 P1 2.4973(7) . ? C1A O1A 1.148(3) . ? C1B O1B 1.147(3) . ? C1C O1C 1.133(3) . ? C1D O1D 1.138(3) . ? C1E O1E 1.137(4) . ? P1 O1 1.6334(18) . ? P1 C3 1.822(3) . ? P1 C1 1.879(2) . ? C1 N1 1.269(3) . ? C1 C10 1.476(3) . ? N1 C2 1.450(3) . ? C2 O1 1.456(3) . ? C2 C20 1.489(4) . ? C2 H2 1.0000 . ? C3 Si1 1.909(2) . ? C3 Si2 1.925(3) . ? C3 H3 1.0000 . ? Si1 C6 1.858(3) . ? Si1 C5 1.868(3) . ? Si1 C4 1.868(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si2 C8 1.865(3) . ? Si2 C9 1.871(3) . ? Si2 C7 1.877(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.427(4) . ? C10 C14 1.433(4) . ? C10 Fe1 2.050(3) . ? C11 C12 1.412(4) . ? C11 Fe1 2.037(3) . ? C11 H11 0.9500 . ? C12 C13 1.413(4) . ? C12 Fe1 2.032(3) . ? C12 H12 0.9500 . ? C13 C14 1.423(4) . ? C13 Fe1 2.037(3) . ? C13 H13 0.9500 . ? C14 Fe1 2.031(3) . ? C14 H14 0.9500 . ? Fe1 C15 2.018(3) . ? Fe1 C19 2.026(3) . ? Fe1 C18 2.039(3) . ? Fe1 C17 2.043(3) . ? Fe1 C16 2.045(3) . ? Fe1 Cp1' 1.640(2) . ? Fe1 Cp1 1.651(2) . ? C15 C16 1.380(6) . ? C15 C19 1.429(5) . ? C15 H15 0.9500 . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.412(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.428(4) . ? C20 C24 1.428(4) . ? C20 Fe2 2.033(3) . ? C21 C22 1.412(4) . ? C21 Fe2 2.030(3) . ? C21 H21 0.9500 . ? C22 C23 1.413(4) . ? C22 Fe2 2.038(3) . ? C22 H22 0.9500 . ? C23 C24 1.418(4) . ? C23 Fe2 2.055(3) . ? C23 H23 0.9500 . ? C24 Fe2 2.060(3) . ? C24 H24 0.9500 . ? Fe2 C27 2.031(3) . ? Fe2 C28 2.041(3) . ? Fe2 C29 2.050(3) . ? Fe2 C26 2.051(3) . ? Fe2 C25 2.055(3) . ? Fe2 Cp2' 1.648(2) . ? Fe2 Cp2 1.654(2) . ? C25 C29 1.415(4) . ? C25 C26 1.420(4) . ? C25 H25 0.9500 . ? C26 C27 1.413(5) . ? C26 H26 0.9500 . ? C27 C28 1.416(5) . ? C27 H27 0.9500 . ? C28 C29 1.413(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A W1 C1B 88.55(12) . . ? C1A W1 C1E 90.74(13) . . ? C1B W1 C1E 89.74(12) . . ? C1A W1 C1D 87.33(13) . . ? C1B W1 C1D 87.24(12) . . ? C1E W1 C1D 176.45(12) . . ? C1A W1 C1C 92.52(12) . . ? C1B W1 C1C 178.03(13) . . ? C1E W1 C1C 88.59(13) . . ? C1D W1 C1C 94.47(13) . . ? C1A W1 P1 177.66(10) . . ? C1B W1 P1 89.12(8) . . ? C1E W1 P1 89.42(8) . . ? C1D W1 P1 92.38(8) . . ? C1C W1 P1 89.82(8) . . ? O1A C1A W1 177.5(3) . . ? O1B C1B W1 178.8(3) . . ? O1C C1C W1 177.3(3) . . ? O1D C1D W1 176.3(3) . . ? O1E C1E W1 178.4(3) . . ? O1 P1 C3 102.58(11) . . ? O1 P1 C1 88.75(10) . . ? C3 P1 C1 114.13(11) . . ? O1 P1 W1 115.88(7) . . ? C3 P1 W1 114.52(8) . . ? C1 P1 W1 117.36(8) . . ? N1 C1 C10 121.6(2) . . ? N1 C1 P1 112.34(19) . . ? C10 C1 P1 126.03(19) . . ? C1 N1 C2 113.5(2) . . ? N1 C2 O1 109.7(2) . . ? N1 C2 C20 112.0(2) . . ? O1 C2 C20 109.6(2) . . ? N1 C2 H2 108.5 . . ? O1 C2 H2 108.5 . . ? C20 C2 H2 108.5 . . ? C2 O1 P1 114.06(14) . . ? P1 C3 Si1 120.04(13) . . ? P1 C3 Si2 111.63(13) . . ? Si1 C3 Si2 115.03(13) . . ? P1 C3 H3 102.3 . . ? Si1 C3 H3 102.3 . . ? Si2 C3 H3 102.3 . . ? C6 Si1 C5 113.53(13) . . ? C6 Si1 C4 104.34(14) . . ? C5 Si1 C4 107.67(13) . . ? C6 Si1 C3 109.09(12) . . ? C5 Si1 C3 111.85(12) . . ? C4 Si1 C3 110.06(12) . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 Si2 C9 111.02(15) . . ? C8 Si2 C7 107.87(15) . . ? C9 Si2 C7 104.58(15) . . ? C8 Si2 C3 111.16(12) . . ? C9 Si2 C3 107.50(14) . . ? C7 Si2 C3 114.54(13) . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 . . ? C11 C10 C14 107.2(2) . . ? C11 C10 C1 127.5(2) . . ? C14 C10 C1 125.3(2) . . ? C11 C10 Fe1 69.08(15) . . ? C14 C10 Fe1 68.72(15) . . ? C1 C10 Fe1 127.86(18) . . ? C12 C11 C10 108.4(2) . . ? C12 C11 Fe1 69.51(15) . . ? C10 C11 Fe1 70.05(14) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Fe1 C11 H11 126.2 . . ? C11 C12 C13 108.4(2) . . ? C11 C12 Fe1 69.88(16) . . ? C13 C12 Fe1 69.87(16) . . ? C11 C12 H12 125.8 . . ? C13 C12 H12 125.8 . . ? Fe1 C12 H12 126.0 . . ? C12 C13 C14 108.1(2) . . ? C12 C13 Fe1 69.50(16) . . ? C14 C13 Fe1 69.28(15) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Fe1 C13 H13 126.8 . . ? C13 C14 C10 107.9(2) . . ? C13 C14 Fe1 69.76(16) . . ? C10 C14 Fe1 70.17(15) . . ? C13 C14 H14 126.1 . . ? C10 C14 H14 126.1 . . ? Fe1 C14 H14 125.6 . . ? C15 Fe1 C19 41.38(15) . . ? C15 Fe1 C14 125.80(15) . . ? C19 Fe1 C14 109.05(13) . . ? C15 Fe1 C12 155.81(15) . . ? C19 Fe1 C12 160.12(15) . . ? C14 Fe1 C12 68.82(11) . . ? C15 Fe1 C11 121.41(13) . . ? C19 Fe1 C11 158.68(15) . . ? C14 Fe1 C11 68.93(11) . . ? C12 Fe1 C11 40.61(10) . . ? C15 Fe1 C13 162.69(17) . . ? C19 Fe1 C13 124.84(14) . . ? C14 Fe1 C13 40.96(10) . . ? C12 Fe1 C13 40.63(11) . . ? C11 Fe1 C13 68.45(11) . . ? C15 Fe1 C18 68.36(14) . . ? C19 Fe1 C18 40.65(15) . . ? C14 Fe1 C18 123.28(13) . . ? C12 Fe1 C18 122.77(13) . . ? C11 Fe1 C18 158.33(14) . . ? C13 Fe1 C18 107.93(13) . . ? C15 Fe1 C17 66.83(15) . . ? C19 Fe1 C17 67.14(14) . . ? C14 Fe1 C17 157.91(13) . . ? C12 Fe1 C17 106.96(13) . . ? C11 Fe1 C17 122.85(13) . . ? C13 Fe1 C17 121.82(13) . . ? C18 Fe1 C17 39.50(13) . . ? C15 Fe1 C16 39.70(16) . . ? C19 Fe1 C16 67.79(15) . . ? C14 Fe1 C16 161.43(14) . . ? C12 Fe1 C16 120.63(15) . . ? C11 Fe1 C16 106.98(13) . . ? C13 Fe1 C16 156.05(15) . . ? C18 Fe1 C16 67.14(14) . . ? C17 Fe1 C16 39.48(13) . . ? C15 Fe1 C10 108.44(13) . . ? C19 Fe1 C10 123.61(14) . . ? C14 Fe1 C10 41.12(10) . . ? C12 Fe1 C10 68.66(10) . . ? C11 Fe1 C10 40.87(10) . . ? C13 Fe1 C10 68.79(10) . . ? C18 Fe1 C10 159.66(13) . . ? C17 Fe1 C10 159.42(12) . . ? C16 Fe1 C10 124.09(12) . . ? Cp1' Fe1 Cp1 178.0(1) . . ? C16 C15 C19 107.9(3) . . ? C16 C15 Fe1 71.2(2) . . ? C19 C15 Fe1 69.62(18) . . ? C16 C15 H15 126.1 . . ? C19 C15 H15 126.1 . . ? Fe1 C15 H15 124.7 . . ? C15 C16 C17 108.2(3) . . ? C15 C16 Fe1 69.1(2) . . ? C17 C16 Fe1 70.17(19) . . ? C15 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Fe1 C16 H16 126.4 . . ? C18 C17 C16 109.8(3) . . ? C18 C17 Fe1 70.09(18) . . ? C16 C17 Fe1 70.35(19) . . ? C18 C17 H17 125.1 . . ? C16 C17 H17 125.1 . . ? Fe1 C17 H17 126.1 . . ? C17 C18 C19 107.4(3) . . ? C17 C18 Fe1 70.41(18) . . ? C19 C18 Fe1 69.20(18) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? Fe1 C18 H18 125.7 . . ? C18 C19 C15 106.7(3) . . ? C18 C19 Fe1 70.15(18) . . ? C15 C19 Fe1 69.00(18) . . ? C18 C19 H19 126.7 . . ? C15 C19 H19 126.7 . . ? Fe1 C19 H19 125.8 . . ? C21 C20 C24 107.6(2) . . ? C21 C20 C2 125.9(2) . . ? C24 C20 C2 126.6(2) . . ? C21 C20 Fe2 69.34(15) . . ? C24 C20 Fe2 70.60(14) . . ? C2 C20 Fe2 125.18(19) . . ? C22 C21 C20 108.0(2) . . ? C22 C21 Fe2 69.97(16) . . ? C20 C21 Fe2 69.52(15) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Fe2 C21 H21 126.1 . . ? C21 C22 C23 108.4(3) . . ? C21 C22 Fe2 69.41(16) . . ? C23 C22 Fe2 70.46(16) . . ? C21 C22 H22 125.8 . . ? C23 C22 H22 125.8 . . ? Fe2 C22 H22 125.9 . . ? C22 C23 C24 108.3(2) . . ? C22 C23 Fe2 69.15(17) . . ? C24 C23 Fe2 70.04(16) . . ? C22 C23 H23 125.9 . . ? C24 C23 H23 125.9 . . ? Fe2 C23 H23 126.5 . . ? C23 C24 C20 107.8(2) . . ? C23 C24 Fe2 69.66(16) . . ? C20 C24 Fe2 68.56(15) . . ? C23 C24 H24 126.1 . . ? C20 C24 H24 126.1 . . ? Fe2 C24 H24 127.2 . . ? C21 Fe2 C27 106.01(12) . . ? C21 Fe2 C20 41.14(11) . . ? C27 Fe2 C20 126.14(12) . . ? C21 Fe2 C22 40.62(11) . . ? C27 Fe2 C22 117.47(14) . . ? C20 Fe2 C22 68.69(11) . . ? C21 Fe2 C28 117.09(12) . . ? C27 Fe2 C28 40.69(13) . . ? C20 Fe2 C28 106.87(12) . . ? C22 Fe2 C28 151.10(12) . . ? C21 Fe2 C29 151.77(11) . . ? C27 Fe2 C29 68.17(13) . . ? C20 Fe2 C29 118.61(12) . . ? C22 Fe2 C29 166.97(12) . . ? C28 Fe2 C29 40.42(11) . . ? C21 Fe2 C26 126.33(12) . . ? C27 Fe2 C26 40.51(13) . . ? C20 Fe2 C26 164.17(12) . . ? C22 Fe2 C26 107.86(13) . . ? C28 Fe2 C26 68.23(14) . . ? C29 Fe2 C26 68.13(13) . . ? C21 Fe2 C25 165.16(12) . . ? C27 Fe2 C25 67.97(12) . . ? C20 Fe2 C25 153.30(11) . . ? C22 Fe2 C25 128.78(12) . . ? C28 Fe2 C25 67.88(12) . . ? C29 Fe2 C25 40.32(11) . . ? C26 Fe2 C25 40.47(12) . . ? C21 Fe2 C23 68.25(11) . . ? C27 Fe2 C23 152.15(14) . . ? C20 Fe2 C23 68.44(11) . . ? C22 Fe2 C23 40.40(11) . . ? C28 Fe2 C23 166.62(13) . . ? C29 Fe2 C23 129.70(12) . . ? C26 Fe2 C23 119.66(13) . . ? C25 Fe2 C23 110.30(12) . . ? C21 Fe2 C24 68.56(11) . . ? C27 Fe2 C24 165.12(13) . . ? C20 Fe2 C24 40.84(10) . . ? C22 Fe2 C24 68.08(12) . . ? C28 Fe2 C24 128.18(13) . . ? C29 Fe2 C24 109.63(12) . . ? C26 Fe2 C24 153.71(12) . . ? C25 Fe2 C24 120.60(11) . . ? C23 Fe2 C24 40.30(10) . . ? Cp2' Fe2 Cp2 178.3(1) . . ? C29 C25 C26 108.3(3) . . ? C29 C25 Fe2 69.66(16) . . ? C26 C25 Fe2 69.63(17) . . ? C29 C25 H25 125.9 . . ? C26 C25 H25 125.9 . . ? Fe2 C25 H25 126.4 . . ? C27 C26 C25 107.4(3) . . ? C27 C26 Fe2 68.97(17) . . ? C25 C26 Fe2 69.91(17) . . ? C27 C26 H26 126.3 . . ? C25 C26 H26 126.3 . . ? Fe2 C26 H26 126.4 . . ? C26 C27 C28 108.5(3) . . ? C26 C27 Fe2 70.52(18) . . ? C28 C27 Fe2 70.06(17) . . ? C26 C27 H27 125.8 . . ? C28 C27 H27 125.8 . . ? Fe2 C27 H27 125.2 . . ? C29 C28 C27 107.9(3) . . ? C29 C28 Fe2 70.12(17) . . ? C27 C28 Fe2 69.25(19) . . ? C29 C28 H28 126.1 . . ? C27 C28 H28 126.1 . . ? Fe2 C28 H28 126.1 . . ? C28 C29 C25 107.9(3) . . ? C28 C29 Fe2 69.47(17) . . ? C25 C29 Fe2 70.03(17) . . ? C28 C29 H29 126.0 . . ? C25 C29 H29 126.0 . . ? Fe2 C29 H29 126.1 . . ? 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 C1B W1 C1A O1A -26(7) . . . . ? C1E W1 C1A O1A -116(7) . . . . ? C1D W1 C1A O1A 61(7) . . . . ? C1C W1 C1A O1A 155(7) . . . . ? P1 W1 C1A O1A -22(10) . . . . ? C1A W1 C1B O1B 87(12) . . . . ? C1E W1 C1B O1B 177(100) . . . . ? C1D W1 C1B O1B -1(12) . . . . ? C1C W1 C1B O1B -151(11) . . . . ? P1 W1 C1B O1B -93(12) . . . . ? C1A W1 C1C O1C 82(6) . . . . ? C1B W1 C1C O1C -40(8) . . . . ? C1E W1 C1C O1C -8(6) . . . . ? C1D W1 C1C O1C 170(6) . . . . ? P1 W1 C1C O1C -98(6) . . . . ? C1A W1 C1D O1D -53(5) . . . . ? C1B W1 C1D O1D 36(5) . . . . ? C1E W1 C1D O1D 4(6) . . . . ? C1C W1 C1D O1D -145(5) . . . . ? P1 W1 C1D O1D 125(5) . . . . ? C1A W1 C1E O1E 34(11) . . . . ? C1B W1 C1E O1E -54(11) . . . . ? C1D W1 C1E O1E -23(12) . . . . ? C1C W1 C1E O1E 127(11) . . . . ? P1 W1 C1E O1E -143(11) . . . . ? C1A W1 P1 O1 -101(3) . . . . ? C1B W1 P1 O1 -97.08(11) . . . . ? C1E W1 P1 O1 -7.33(11) . . . . ? C1D W1 P1 O1 175.73(11) . . . . ? C1C W1 P1 O1 81.26(12) . . . . ? C1A W1 P1 C3 18(3) . . . . ? C1B W1 P1 C3 22.09(13) . . . . ? C1E W1 P1 C3 111.84(13) . . . . ? C1D W1 P1 C3 -65.10(13) . . . . ? C1C W1 P1 C3 -159.57(13) . . . . ? C1A W1 P1 C1 156(3) . . . . ? C1B W1 P1 C1 160.00(13) . . . . ? C1E W1 P1 C1 -110.26(13) . . . . ? C1D W1 P1 C1 72.80(13) . . . . ? C1C W1 P1 C1 -21.66(13) . . . . ? O1 P1 C1 N1 -7.12(19) . . . . ? C3 P1 C1 N1 -110.4(2) . . . . ? W1 P1 C1 N1 111.59(17) . . . . ? O1 P1 C1 C10 174.3(2) . . . . ? C3 P1 C1 C10 71.0(2) . . . . ? W1 P1 C1 C10 -67.0(2) . . . . ? C10 C1 N1 C2 179.1(2) . . . . ? P1 C1 N1 C2 0.4(3) . . . . ? C1 N1 C2 O1 7.8(3) . . . . ? C1 N1 C2 C20 129.7(2) . . . . ? N1 C2 O1 P1 -13.7(2) . . . . ? C20 C2 O1 P1 -137.04(18) . . . . ? C3 P1 O1 C2 125.94(17) . . . . ? C1 P1 O1 C2 11.48(17) . . . . ? W1 P1 O1 C2 -108.55(15) . . . . ? O1 P1 C3 Si1 -109.58(15) . . . . ? C1 P1 C3 Si1 -15.3(2) . . . . ? W1 P1 C3 Si1 124.03(12) . . . . ? O1 P1 C3 Si2 29.46(14) . . . . ? C1 P1 C3 Si2 123.79(13) . . . . ? W1 P1 C3 Si2 -96.94(12) . . . . ? P1 C3 Si1 C6 -65.93(18) . . . . ? Si2 C3 Si1 C6 156.34(14) . . . . ? P1 C3 Si1 C5 60.5(2) . . . . ? Si2 C3 Si1 C5 -77.22(17) . . . . ? P1 C3 Si1 C4 -179.84(16) . . . . ? Si2 C3 Si1 C4 42.42(18) . . . . ? P1 C3 Si2 C8 -90.63(16) . . . . ? Si1 C3 Si2 C8 50.60(18) . . . . ? P1 C3 Si2 C9 147.68(14) . . . . ? Si1 C3 Si2 C9 -71.10(17) . . . . ? P1 C3 Si2 C7 31.95(19) . . . . ? Si1 C3 Si2 C7 173.17(15) . . . . ? N1 C1 C10 C11 -132.3(3) . . . . ? P1 C1 C10 C11 46.2(4) . . . . ? N1 C1 C10 C14 48.5(4) . . . . ? P1 C1 C10 C14 -133.0(2) . . . . ? N1 C1 C10 Fe1 -40.8(3) . . . . ? P1 C1 C10 Fe1 137.72(17) . . . . ? C14 C10 C11 C12 0.8(3) . . . . ? C1 C10 C11 C12 -178.5(2) . . . . ? Fe1 C10 C11 C12 59.14(19) . . . . ? C14 C10 C11 Fe1 -58.33(18) . . . . ? C1 C10 C11 Fe1 122.3(3) . . . . ? C10 C11 C12 C13 0.0(3) . . . . ? Fe1 C11 C12 C13 59.44(19) . . . . ? C10 C11 C12 Fe1 -59.48(18) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? Fe1 C12 C13 C14 58.69(19) . . . . ? C11 C12 C13 Fe1 -59.45(19) . . . . ? C12 C13 C14 C10 1.3(3) . . . . ? Fe1 C13 C14 C10 60.08(18) . . . . ? C12 C13 C14 Fe1 -58.82(19) . . . . ? C11 C10 C14 C13 -1.3(3) . . . . ? C1 C10 C14 C13 178.1(2) . . . . ? Fe1 C10 C14 C13 -59.82(19) . . . . ? C11 C10 C14 Fe1 58.56(18) . . . . ? C1 C10 C14 Fe1 -122.1(2) . . . . ? C13 C14 Fe1 C15 -164.75(19) . . . . ? C10 C14 Fe1 C15 76.5(2) . . . . ? C13 C14 Fe1 C19 -121.6(2) . . . . ? C10 C14 Fe1 C19 119.66(19) . . . . ? C13 C14 Fe1 C12 37.32(15) . . . . ? C10 C14 Fe1 C12 -81.41(16) . . . . ? C13 C14 Fe1 C11 81.00(17) . . . . ? C10 C14 Fe1 C11 -37.73(15) . . . . ? C10 C14 Fe1 C13 -118.7(2) . . . . ? C13 C14 Fe1 C18 -78.8(2) . . . . ? C10 C14 Fe1 C18 162.49(17) . . . . ? C13 C14 Fe1 C17 -45.6(4) . . . . ? C10 C14 Fe1 C17 -164.3(3) . . . . ? C13 C14 Fe1 C16 161.5(4) . . . . ? C10 C14 Fe1 C16 42.8(5) . . . . ? C13 C14 Fe1 C10 118.7(2) . . . . ? C11 C12 Fe1 C15 -50.0(4) . . . . ? C13 C12 Fe1 C15 -169.6(3) . . . . ? C11 C12 Fe1 C19 169.5(4) . . . . ? C13 C12 Fe1 C19 50.0(5) . . . . ? C11 C12 Fe1 C14 81.93(17) . . . . ? C13 C12 Fe1 C14 -37.61(16) . . . . ? C13 C12 Fe1 C11 -119.5(2) . . . . ? C11 C12 Fe1 C13 119.5(2) . . . . ? C11 C12 Fe1 C18 -161.30(18) . . . . ? C13 C12 Fe1 C18 79.2(2) . . . . ? C11 C12 Fe1 C17 -121.04(18) . . . . ? C13 C12 Fe1 C17 119.42(18) . . . . ? C11 C12 Fe1 C16 -80.3(2) . . . . ? C13 C12 Fe1 C16 160.21(18) . . . . ? C11 C12 Fe1 C10 37.66(15) . . . . ? C13 C12 Fe1 C10 -81.88(17) . . . . ? C12 C11 Fe1 C15 158.4(2) . . . . ? C10 C11 Fe1 C15 -82.0(2) . . . . ? C12 C11 Fe1 C19 -170.2(3) . . . . ? C10 C11 Fe1 C19 -50.6(4) . . . . ? C12 C11 Fe1 C14 -81.64(17) . . . . ? C10 C11 Fe1 C14 37.95(15) . . . . ? C10 C11 Fe1 C12 119.6(2) . . . . ? C12 C11 Fe1 C13 -37.52(17) . . . . ? C10 C11 Fe1 C13 82.06(16) . . . . ? C12 C11 Fe1 C18 46.9(4) . . . . ? C10 C11 Fe1 C18 166.5(3) . . . . ? C12 C11 Fe1 C17 77.3(2) . . . . ? C10 C11 Fe1 C17 -163.11(17) . . . . ? C12 C11 Fe1 C16 117.5(2) . . . . ? C10 C11 Fe1 C16 -122.88(19) . . . . ? C12 C11 Fe1 C10 -119.6(2) . . . . ? C12 C13 Fe1 C15 165.5(4) . . . . ? C14 C13 Fe1 C15 45.8(5) . . . . ? C12 C13 Fe1 C19 -161.50(19) . . . . ? C14 C13 Fe1 C19 78.7(2) . . . . ? C12 C13 Fe1 C14 119.8(2) . . . . ? C14 C13 Fe1 C12 -119.8(2) . . . . ? C12 C13 Fe1 C11 37.50(16) . . . . ? C14 C13 Fe1 C11 -82.25(17) . . . . ? C12 C13 Fe1 C18 -119.78(19) . . . . ? C14 C13 Fe1 C18 120.47(18) . . . . ? C12 C13 Fe1 C17 -78.7(2) . . . . ? C14 C13 Fe1 C17 161.56(17) . . . . ? C12 C13 Fe1 C16 -45.9(4) . . . . ? C14 C13 Fe1 C16 -165.6(3) . . . . ? C12 C13 Fe1 C10 81.54(16) . . . . ? C14 C13 Fe1 C10 -38.21(15) . . . . ? C11 C10 Fe1 C15 117.0(2) . . . . ? C14 C10 Fe1 C15 -123.8(2) . . . . ? C1 C10 Fe1 C15 -4.9(3) . . . . ? C11 C10 Fe1 C19 160.28(19) . . . . ? C14 C10 Fe1 C19 -80.5(2) . . . . ? C1 C10 Fe1 C19 38.4(3) . . . . ? C11 C10 Fe1 C14 -119.2(2) . . . . ? C1 C10 Fe1 C14 118.9(3) . . . . ? C11 C10 Fe1 C12 -37.42(15) . . . . ? C14 C10 Fe1 C12 81.82(16) . . . . ? C1 C10 Fe1 C12 -159.3(2) . . . . ? C14 C10 Fe1 C11 119.2(2) . . . . ? C1 C10 Fe1 C11 -121.9(3) . . . . ? C11 C10 Fe1 C13 -81.16(17) . . . . ? C14 C10 Fe1 C13 38.07(16) . . . . ? C1 C10 Fe1 C13 157.0(2) . . . . ? C11 C10 Fe1 C18 -165.6(3) . . . . ? C14 C10 Fe1 C18 -46.4(4) . . . . ? C1 C10 Fe1 C18 72.5(4) . . . . ? C11 C10 Fe1 C17 44.0(4) . . . . ? C14 C10 Fe1 C17 163.2(3) . . . . ? C1 C10 Fe1 C17 -77.9(4) . . . . ? C11 C10 Fe1 C16 75.9(2) . . . . ? C14 C10 Fe1 C16 -164.8(2) . . . . ? C1 C10 Fe1 C16 -46.0(3) . . . . ? C19 Fe1 C15 C16 118.2(3) . . . . ? C14 Fe1 C15 C16 -163.94(19) . . . . ? C12 Fe1 C15 C16 -42.7(4) . . . . ? C11 Fe1 C15 C16 -78.5(2) . . . . ? C13 Fe1 C15 C16 160.7(4) . . . . ? C18 Fe1 C15 C16 79.8(2) . . . . ? C17 Fe1 C15 C16 37.0(2) . . . . ? C10 Fe1 C15 C16 -121.6(2) . . . . ? C14 Fe1 C15 C19 77.9(2) . . . . ? C12 Fe1 C15 C19 -160.9(3) . . . . ? C11 Fe1 C15 C19 163.4(2) . . . . ? C13 Fe1 C15 C19 42.5(5) . . . . ? C18 Fe1 C15 C19 -38.3(2) . . . . ? C17 Fe1 C15 C19 -81.2(2) . . . . ? C16 Fe1 C15 C19 -118.2(3) . . . . ? C10 Fe1 C15 C19 120.3(2) . . . . ? C19 C15 C16 C17 0.8(4) . . . . ? Fe1 C15 C16 C17 -59.5(2) . . . . ? C19 C15 C16 Fe1 60.3(2) . . . . ? C19 Fe1 C16 C15 -39.0(2) . . . . ? C14 Fe1 C16 C15 44.8(5) . . . . ? C12 Fe1 C16 C15 161.2(2) . . . . ? C11 Fe1 C16 C15 119.0(2) . . . . ? C13 Fe1 C16 C15 -166.0(3) . . . . ? C18 Fe1 C16 C15 -83.2(2) . . . . ? C17 Fe1 C16 C15 -119.5(3) . . . . ? C10 Fe1 C16 C15 77.5(2) . . . . ? C15 Fe1 C16 C17 119.5(3) . . . . ? C19 Fe1 C16 C17 80.5(2) . . . . ? C14 Fe1 C16 C17 164.3(4) . . . . ? C12 Fe1 C16 C17 -79.3(2) . . . . ? C11 Fe1 C16 C17 -121.4(2) . . . . ? C13 Fe1 C16 C17 -46.4(4) . . . . ? C18 Fe1 C16 C17 36.4(2) . . . . ? C10 Fe1 C16 C17 -163.00(19) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? Fe1 C16 C17 C18 -59.1(2) . . . . ? C15 C16 C17 Fe1 58.8(2) . . . . ? C15 Fe1 C17 C18 83.6(2) . . . . ? C19 Fe1 C17 C18 38.5(2) . . . . ? C14 Fe1 C17 C18 -46.0(4) . . . . ? C12 Fe1 C17 C18 -121.3(2) . . . . ? C11 Fe1 C17 C18 -162.9(2) . . . . ? C13 Fe1 C17 C18 -79.4(2) . . . . ? C16 Fe1 C17 C18 120.8(3) . . . . ? C10 Fe1 C17 C18 164.3(3) . . . . ? C15 Fe1 C17 C16 -37.2(2) . . . . ? C19 Fe1 C17 C16 -82.3(3) . . . . ? C14 Fe1 C17 C16 -166.8(3) . . . . ? C12 Fe1 C17 C16 117.9(2) . . . . ? C11 Fe1 C17 C16 76.3(3) . . . . ? C13 Fe1 C17 C16 159.8(2) . . . . ? C18 Fe1 C17 C16 -120.8(3) . . . . ? C10 Fe1 C17 C16 43.5(5) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? Fe1 C17 C18 C19 -59.6(2) . . . . ? C16 C17 C18 Fe1 59.3(2) . . . . ? C15 Fe1 C18 C17 -79.4(2) . . . . ? C19 Fe1 C18 C17 -118.4(3) . . . . ? C14 Fe1 C18 C17 161.1(2) . . . . ? C12 Fe1 C18 C17 76.4(2) . . . . ? C11 Fe1 C18 C17 42.0(4) . . . . ? C13 Fe1 C18 C17 118.6(2) . . . . ? C16 Fe1 C18 C17 -36.3(2) . . . . ? C10 Fe1 C18 C17 -164.2(3) . . . . ? C15 Fe1 C18 C19 39.0(2) . . . . ? C14 Fe1 C18 C19 -80.5(2) . . . . ? C12 Fe1 C18 C19 -165.3(2) . . . . ? C11 Fe1 C18 C19 160.3(3) . . . . ? C13 Fe1 C18 C19 -123.0(2) . . . . ? C17 Fe1 C18 C19 118.4(3) . . . . ? C16 Fe1 C18 C19 82.0(2) . . . . ? C10 Fe1 C18 C19 -45.8(5) . . . . ? C17 C18 C19 C15 0.7(4) . . . . ? Fe1 C18 C19 C15 -59.6(2) . . . . ? C17 C18 C19 Fe1 60.3(2) . . . . ? C16 C15 C19 C18 -0.9(4) . . . . ? Fe1 C15 C19 C18 60.3(2) . . . . ? C16 C15 C19 Fe1 -61.3(2) . . . . ? C15 Fe1 C19 C18 -117.8(3) . . . . ? C14 Fe1 C19 C18 119.3(2) . . . . ? C12 Fe1 C19 C18 39.0(5) . . . . ? C11 Fe1 C19 C18 -160.0(3) . . . . ? C13 Fe1 C19 C18 76.4(2) . . . . ? C17 Fe1 C19 C18 -37.4(2) . . . . ? C16 Fe1 C19 C18 -80.3(2) . . . . ? C10 Fe1 C19 C18 162.60(19) . . . . ? C14 Fe1 C19 C15 -123.0(2) . . . . ? C12 Fe1 C19 C15 156.8(4) . . . . ? C11 Fe1 C19 C15 -42.3(5) . . . . ? C13 Fe1 C19 C15 -165.8(2) . . . . ? C18 Fe1 C19 C15 117.8(3) . . . . ? C17 Fe1 C19 C15 80.4(2) . . . . ? C16 Fe1 C19 C15 37.5(2) . . . . ? C10 Fe1 C19 C15 -79.6(3) . . . . ? N1 C2 C20 C21 171.7(3) . . . . ? O1 C2 C20 C21 -66.3(3) . . . . ? N1 C2 C20 C24 -8.0(4) . . . . ? O1 C2 C20 C24 114.0(3) . . . . ? N1 C2 C20 Fe2 83.0(3) . . . . ? O1 C2 C20 Fe2 -154.98(17) . . . . ? C24 C20 C21 C22 0.9(3) . . . . ? C2 C20 C21 C22 -178.8(3) . . . . ? Fe2 C20 C21 C22 -59.7(2) . . . . ? C24 C20 C21 Fe2 60.55(18) . . . . ? C2 C20 C21 Fe2 -119.2(3) . . . . ? C20 C21 C22 C23 -0.5(3) . . . . ? Fe2 C21 C22 C23 -59.9(2) . . . . ? C20 C21 C22 Fe2 59.4(2) . . . . ? C21 C22 C23 C24 -0.1(3) . . . . ? Fe2 C22 C23 C24 -59.3(2) . . . . ? C21 C22 C23 Fe2 59.2(2) . . . . ? C22 C23 C24 C20 0.6(3) . . . . ? Fe2 C23 C24 C20 -58.11(18) . . . . ? C22 C23 C24 Fe2 58.8(2) . . . . ? C21 C20 C24 C23 -0.9(3) . . . . ? C2 C20 C24 C23 178.8(3) . . . . ? Fe2 C20 C24 C23 58.80(19) . . . . ? C21 C20 C24 Fe2 -59.74(19) . . . . ? C2 C20 C24 Fe2 120.0(3) . . . . ? C22 C21 Fe2 C27 -113.7(2) . . . . ? C20 C21 Fe2 C27 127.16(18) . . . . ? C22 C21 Fe2 C20 119.1(2) . . . . ? C20 C21 Fe2 C22 -119.1(2) . . . . ? C22 C21 Fe2 C28 -156.07(18) . . . . ? C20 C21 Fe2 C28 84.83(19) . . . . ? C22 C21 Fe2 C29 172.7(2) . . . . ? C20 C21 Fe2 C29 53.6(3) . . . . ? C22 C21 Fe2 C26 -74.2(2) . . . . ? C20 C21 Fe2 C26 166.73(18) . . . . ? C22 C21 Fe2 C25 -49.9(5) . . . . ? C20 C21 Fe2 C25 -169.0(4) . . . . ? C22 C21 Fe2 C23 37.41(17) . . . . ? C20 C21 Fe2 C23 -81.69(18) . . . . ? C22 C21 Fe2 C24 80.90(18) . . . . ? C20 C21 Fe2 C24 -38.19(16) . . . . ? C24 C20 Fe2 C21 -118.3(2) . . . . ? C2 C20 Fe2 C21 120.0(3) . . . . ? C21 C20 Fe2 C27 -71.5(2) . . . . ? C24 C20 Fe2 C27 170.12(19) . . . . ? C2 C20 Fe2 C27 48.5(3) . . . . ? C21 C20 Fe2 C22 37.63(16) . . . . ? C24 C20 Fe2 C22 -80.71(17) . . . . ? C2 C20 Fe2 C22 157.7(3) . . . . ? C21 C20 Fe2 C28 -112.10(18) . . . . ? C24 C20 Fe2 C28 129.56(17) . . . . ? C2 C20 Fe2 C28 7.9(3) . . . . ? C21 C20 Fe2 C29 -154.29(17) . . . . ? C24 C20 Fe2 C29 87.36(18) . . . . ? C2 C20 Fe2 C29 -34.3(3) . . . . ? C21 C20 Fe2 C26 -42.7(5) . . . . ? C24 C20 Fe2 C26 -161.0(4) . . . . ? C2 C20 Fe2 C26 77.4(5) . . . . ? C21 C20 Fe2 C25 173.7(2) . . . . ? C24 C20 Fe2 C25 55.4(3) . . . . ? C2 C20 Fe2 C25 -66.2(4) . . . . ? C21 C20 Fe2 C23 81.17(18) . . . . ? C24 C20 Fe2 C23 -37.17(16) . . . . ? C2 C20 Fe2 C23 -158.8(3) . . . . ? C21 C20 Fe2 C24 118.3(2) . . . . ? C2 C20 Fe2 C24 -121.6(3) . . . . ? C23 C22 Fe2 C21 119.5(2) . . . . ? C21 C22 Fe2 C27 82.6(2) . . . . ? C23 C22 Fe2 C27 -157.94(18) . . . . ? C21 C22 Fe2 C20 -38.10(16) . . . . ? C23 C22 Fe2 C20 81.36(18) . . . . ? C21 C22 Fe2 C28 48.3(3) . . . . ? C23 C22 Fe2 C28 167.8(2) . . . . ? C21 C22 Fe2 C29 -164.6(5) . . . . ? C23 C22 Fe2 C29 -45.1(6) . . . . ? C21 C22 Fe2 C26 125.48(18) . . . . ? C23 C22 Fe2 C26 -115.06(18) . . . . ? C21 C22 Fe2 C25 165.45(17) . . . . ? C23 C22 Fe2 C25 -75.1(2) . . . . ? C21 C22 Fe2 C23 -119.5(2) . . . . ? C21 C22 Fe2 C24 -82.18(18) . . . . ? C23 C22 Fe2 C24 37.28(16) . . . . ? C22 C23 Fe2 C21 -37.61(17) . . . . ? C24 C23 Fe2 C21 82.08(17) . . . . ? C22 C23 Fe2 C27 45.5(3) . . . . ? C24 C23 Fe2 C27 165.2(2) . . . . ? C22 C23 Fe2 C20 -82.03(18) . . . . ? C24 C23 Fe2 C20 37.65(15) . . . . ? C24 C23 Fe2 C22 119.7(2) . . . . ? C22 C23 Fe2 C28 -153.8(5) . . . . ? C24 C23 Fe2 C28 -34.1(6) . . . . ? C22 C23 Fe2 C29 168.01(17) . . . . ? C24 C23 Fe2 C29 -72.3(2) . . . . ? C22 C23 Fe2 C26 82.8(2) . . . . ? C24 C23 Fe2 C26 -157.47(17) . . . . ? C22 C23 Fe2 C25 126.56(18) . . . . ? C24 C23 Fe2 C25 -113.76(17) . . . . ? C22 C23 Fe2 C24 -119.7(2) . . . . ? C23 C24 Fe2 C21 -81.22(18) . . . . ? C20 C24 Fe2 C21 38.47(16) . . . . ? C23 C24 Fe2 C27 -152.3(5) . . . . ? C20 C24 Fe2 C27 -32.6(6) . . . . ? C23 C24 Fe2 C20 -119.7(2) . . . . ? C23 C24 Fe2 C22 -37.37(16) . . . . ? C20 C24 Fe2 C22 82.33(17) . . . . ? C23 C24 Fe2 C28 170.50(17) . . . . ? C20 C24 Fe2 C28 -69.8(2) . . . . ? C23 C24 Fe2 C29 128.91(17) . . . . ? C20 C24 Fe2 C29 -111.40(17) . . . . ? C23 C24 Fe2 C26 48.7(3) . . . . ? C20 C24 Fe2 C26 168.4(3) . . . . ? C23 C24 Fe2 C25 85.8(2) . . . . ? C20 C24 Fe2 C25 -154.55(16) . . . . ? C20 C24 Fe2 C23 119.7(2) . . . . ? C21 Fe2 C25 C29 -150.4(4) . . . . ? C27 Fe2 C25 C29 -81.8(2) . . . . ? C20 Fe2 C25 C29 45.9(3) . . . . ? C22 Fe2 C25 C29 169.97(18) . . . . ? C28 Fe2 C25 C29 -37.70(18) . . . . ? C26 Fe2 C25 C29 -119.6(3) . . . . ? C23 Fe2 C25 C29 128.08(18) . . . . ? C24 Fe2 C25 C29 84.6(2) . . . . ? C21 Fe2 C25 C26 -30.7(5) . . . . ? C27 Fe2 C25 C26 37.9(2) . . . . ? C20 Fe2 C25 C26 165.6(2) . . . . ? C22 Fe2 C25 C26 -70.4(2) . . . . ? C28 Fe2 C25 C26 81.9(2) . . . . ? C29 Fe2 C25 C26 119.6(3) . . . . ? C23 Fe2 C25 C26 -112.3(2) . . . . ? C24 Fe2 C25 C26 -155.74(19) . . . . ? C29 C25 C26 C27 0.1(4) . . . . ? Fe2 C25 C26 C27 -59.0(2) . . . . ? C29 C25 C26 Fe2 59.1(2) . . . . ? C21 Fe2 C26 C27 -70.5(2) . . . . ? C20 Fe2 C26 C27 -36.9(6) . . . . ? C22 Fe2 C26 C27 -111.6(2) . . . . ? C28 Fe2 C26 C27 37.9(2) . . . . ? C29 Fe2 C26 C27 81.5(2) . . . . ? C25 Fe2 C26 C27 118.8(3) . . . . ? C23 Fe2 C26 C27 -154.2(2) . . . . ? C24 Fe2 C26 C27 171.8(3) . . . . ? C21 Fe2 C26 C25 170.65(18) . . . . ? C27 Fe2 C26 C25 -118.8(3) . . . . ? C20 Fe2 C26 C25 -155.7(4) . . . . ? C22 Fe2 C26 C25 129.50(19) . . . . ? C28 Fe2 C26 C25 -81.0(2) . . . . ? C29 Fe2 C26 C25 -37.30(18) . . . . ? C23 Fe2 C26 C25 87.0(2) . . . . ? C24 Fe2 C26 C25 53.0(4) . . . . ? C25 C26 C27 C28 -0.5(4) . . . . ? Fe2 C26 C27 C28 -60.0(2) . . . . ? C25 C26 C27 Fe2 59.6(2) . . . . ? C21 Fe2 C27 C26 127.8(2) . . . . ? C20 Fe2 C27 C26 168.30(19) . . . . ? C22 Fe2 C27 C26 85.6(2) . . . . ? C28 Fe2 C27 C26 -119.0(3) . . . . ? C29 Fe2 C27 C26 -81.4(2) . . . . ? C25 Fe2 C27 C26 -37.82(19) . . . . ? C23 Fe2 C27 C26 54.2(3) . . . . ? C24 Fe2 C27 C26 -165.8(4) . . . . ? C21 Fe2 C27 C28 -113.14(18) . . . . ? C20 Fe2 C27 C28 -72.7(2) . . . . ? C22 Fe2 C27 C28 -155.33(17) . . . . ? C29 Fe2 C27 C28 37.61(17) . . . . ? C26 Fe2 C27 C28 119.0(3) . . . . ? C25 Fe2 C27 C28 81.23(19) . . . . ? C23 Fe2 C27 C28 173.3(2) . . . . ? C24 Fe2 C27 C28 -46.8(6) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? Fe2 C27 C28 C29 -59.7(2) . . . . ? C26 C27 C28 Fe2 60.3(2) . . . . ? C21 Fe2 C28 C29 -157.78(17) . . . . ? C27 Fe2 C28 C29 119.1(3) . . . . ? C20 Fe2 C28 C29 -114.57(18) . . . . ? C22 Fe2 C28 C29 169.1(2) . . . . ? C26 Fe2 C28 C29 81.40(19) . . . . ? C25 Fe2 C28 C29 37.61(17) . . . . ? C23 Fe2 C28 C29 -47.2(6) . . . . ? C24 Fe2 C28 C29 -74.7(2) . . . . ? C21 Fe2 C28 C27 83.1(2) . . . . ? C20 Fe2 C28 C27 126.34(18) . . . . ? C22 Fe2 C28 C27 50.0(3) . . . . ? C29 Fe2 C28 C27 -119.1(3) . . . . ? C26 Fe2 C28 C27 -37.69(18) . . . . ? C25 Fe2 C28 C27 -81.48(19) . . . . ? C23 Fe2 C28 C27 -166.3(5) . . . . ? C24 Fe2 C28 C27 166.23(17) . . . . ? C27 C28 C29 C25 -0.5(3) . . . . ? Fe2 C28 C29 C25 -59.7(2) . . . . ? C27 C28 C29 Fe2 59.2(2) . . . . ? C26 C25 C29 C28 0.2(3) . . . . ? Fe2 C25 C29 C28 59.3(2) . . . . ? C26 C25 C29 Fe2 -59.1(2) . . . . ? C21 Fe2 C29 C28 45.4(3) . . . . ? C27 Fe2 C29 C28 -37.86(19) . . . . ? C20 Fe2 C29 C28 82.5(2) . . . . ? C22 Fe2 C29 C28 -156.1(5) . . . . ? C26 Fe2 C29 C28 -81.7(2) . . . . ? C25 Fe2 C29 C28 -119.1(3) . . . . ? C23 Fe2 C29 C28 167.25(19) . . . . ? C24 Fe2 C29 C28 126.39(19) . . . . ? C21 Fe2 C29 C25 164.5(2) . . . . ? C27 Fe2 C29 C25 81.2(2) . . . . ? C20 Fe2 C29 C25 -158.43(17) . . . . ? C22 Fe2 C29 C25 -37.0(6) . . . . ? C28 Fe2 C29 C25 119.1(3) . . . . ? C26 Fe2 C29 C25 37.43(18) . . . . ? C23 Fe2 C29 C25 -73.7(2) . . . . ? C24 Fe2 C29 C25 -114.52(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 O1A 0.95 2.57 3.210(4) 125.4 2 C2 H2 O1B 1.00 2.51 3.309(3) 136.6 7_566 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.231 _refine_diff_density_min -1.754 _refine_diff_density_rms 0.094 #============================================================================== # _eof # End of Crystallographic Information File data_joerg142 _database_code_depnum_ccdc_archive 'CCDC 777798' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "joerg142 H.Helten ''HHE-DR05'' 100K 13.02.08" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Fe N3 O5 P Si2 W' _chemical_formula_weight 795.41 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0145(5) _cell_length_b 12.3033(4) _cell_length_c 16.1955(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.387(2) _cell_angle_gamma 90.00 _cell_volume 3104.31(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17522 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 4.337 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.2203 _exptl_absorpt_correction_T_max 0.5090 _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 21506 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6845 _reflns_number_gt 6005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo/Scalepack(Otwinowski & Minor 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+5.3885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6845 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _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 W W 0.930165(8) 0.265909(10) 0.500693(7) 0.01269(5) Uani 1 1 d . . . Fe Fe 0.66844(3) 0.27871(4) 0.72333(3) 0.01444(10) Uani 1 1 d . . . P P 0.76943(5) 0.28411(6) 0.48438(5) 0.01081(16) Uani 1 1 d . . . Si1 Si 0.70954(6) 0.03168(7) 0.45670(6) 0.01615(18) Uani 1 1 d . . . Si2 Si 0.59939(6) 0.22879(8) 0.35694(5) 0.01501(18) Uani 1 1 d . . . N1 N 0.72575(17) 0.4568(2) 0.55827(16) 0.0139(5) Uani 1 1 d . . . N2 N 0.73612(16) 0.3923(2) 0.42192(15) 0.0125(5) Uani 1 1 d . . . N3 N 0.69288(18) 0.5703(2) 0.43769(16) 0.0171(6) Uani 1 1 d . . . O1 O 1.13045(16) 0.2862(2) 0.52731(17) 0.0319(6) Uani 1 1 d . . . O2 O 0.89907(18) 0.3823(3) 0.32030(18) 0.0451(8) Uani 1 1 d . . . O3 O 0.93701(19) 0.4943(2) 0.5941(2) 0.0406(7) Uani 1 1 d . . . O4 O 0.95890(16) 0.1397(2) 0.67613(15) 0.0244(5) Uani 1 1 d . . . O5 O 0.94780(18) 0.0453(2) 0.40290(18) 0.0360(7) Uani 1 1 d . . . C1 C 0.74853(19) 0.3576(3) 0.57784(18) 0.0121(6) Uani 1 1 d . . . C2 C 0.71876(19) 0.4720(3) 0.46861(18) 0.0123(6) Uani 1 1 d . . . C3 C 0.68253(19) 0.1823(3) 0.45683(19) 0.0131(6) Uani 1 1 d . . . H3 H 0.6520 0.1892 0.5025 0.016 Uiso 1 1 calc R . . C4 C 0.8043(2) -0.0176(3) 0.5400(2) 0.0175(7) Uani 1 1 d . . . H4A H 0.8122 -0.0941 0.5326 0.026 Uiso 1 1 calc R . . H4B H 0.7942 -0.0048 0.5953 0.026 Uiso 1 1 calc R . . H4C H 0.8549 0.0208 0.5345 0.026 Uiso 1 1 calc R . . C5 C 0.7287(3) -0.0111(3) 0.3522(2) 0.0341(10) Uani 1 1 d . . . H5A H 0.7392 -0.0879 0.3529 0.051 Uiso 1 1 calc R . . H5B H 0.7777 0.0269 0.3419 0.051 Uiso 1 1 calc R . . H5C H 0.6791 0.0058 0.3081 0.051 Uiso 1 1 calc R . . C6 C 0.6154(2) -0.0395(3) 0.4830(3) 0.0346(10) Uani 1 1 d . . . H6A H 0.5639 -0.0196 0.4424 0.052 Uiso 1 1 calc R . . H6B H 0.6106 -0.0186 0.5388 0.052 Uiso 1 1 calc R . . H6C H 0.6236 -0.1167 0.4813 0.052 Uiso 1 1 calc R . . C7 C 0.6522(2) 0.2529(3) 0.2666(2) 0.0232(8) Uani 1 1 d . . . H7A H 0.6295 0.2029 0.2214 0.035 Uiso 1 1 calc R . . H7B H 0.7130 0.2420 0.2857 0.035 Uiso 1 1 calc R . . H7C H 0.6411 0.3260 0.2463 0.035 Uiso 1 1 calc R . . C8 C 0.5150(2) 0.1222(3) 0.3208(2) 0.0247(8) Uani 1 1 d . . . H8A H 0.4740 0.1479 0.2716 0.037 Uiso 1 1 calc R . . H8B H 0.4863 0.1074 0.3655 0.037 Uiso 1 1 calc R . . H8C H 0.5414 0.0569 0.3068 0.037 Uiso 1 1 calc R . . C9 C 0.5373(2) 0.3476(3) 0.3844(2) 0.0227(7) Uani 1 1 d . . . H9A H 0.5633 0.4140 0.3718 0.034 Uiso 1 1 calc R . . H9B H 0.5378 0.3454 0.4438 0.034 Uiso 1 1 calc R . . H9C H 0.4792 0.3441 0.3517 0.034 Uiso 1 1 calc R . . C10 C 0.6875(2) 0.5937(3) 0.3481(2) 0.0216(7) Uani 1 1 d . . . H10A H 0.7133 0.5354 0.3235 0.032 Uiso 1 1 calc R . . H10B H 0.7172 0.6603 0.3432 0.032 Uiso 1 1 calc R . . H10C H 0.6283 0.6008 0.3188 0.032 Uiso 1 1 calc R . . C11 C 0.6722(2) 0.6587(3) 0.4884(2) 0.0211(7) Uani 1 1 d . . . H11A H 0.6639 0.6308 0.5413 0.032 Uiso 1 1 calc R . . H11B H 0.6205 0.6938 0.4583 0.032 Uiso 1 1 calc R . . H11C H 0.7184 0.7103 0.4993 0.032 Uiso 1 1 calc R . . C12 C 0.76408(19) 0.3160(3) 0.66396(19) 0.0132(6) Uani 1 1 d . . . C13 C 0.7686(2) 0.2037(3) 0.6878(2) 0.0165(7) Uani 1 1 d . . . H13 H 0.769(2) 0.149(3) 0.655(2) 0.020 Uiso 1 1 d . . . C14 C 0.7803(2) 0.1970(3) 0.7769(2) 0.0186(7) Uani 1 1 d . . . H14 H 0.785(2) 0.134(3) 0.809(2) 0.022 Uiso 1 1 d . . . C15 C 0.7831(2) 0.3047(3) 0.8090(2) 0.0168(7) Uani 1 1 d . . . H15 H 0.786(2) 0.322(3) 0.867(2) 0.020 Uiso 1 1 d . . . C16 C 0.7724(2) 0.3784(3) 0.7404(2) 0.0145(6) Uani 1 1 d . . . H16 H 0.772(2) 0.454(3) 0.745(2) 0.017 Uiso 1 1 d . . . C17 C 0.5546(3) 0.2219(5) 0.6529(3) 0.0425(13) Uani 1 1 d . . . H17 H 0.551(3) 0.190(4) 0.615(3) 0.051 Uiso 1 1 d . . . C18 C 0.5663(3) 0.1873(4) 0.7385(3) 0.0436(12) Uani 1 1 d . . . H18 H 0.568(3) 0.123(4) 0.756(3) 0.052 Uiso 1 1 d . . . C19 C 0.5728(3) 0.2821(4) 0.7882(3) 0.0385(11) Uani 1 1 d . . . H19 H 0.583(3) 0.287(4) 0.846(3) 0.046 Uiso 1 1 d . . . C20 C 0.5658(3) 0.3725(4) 0.7345(3) 0.0363(10) Uani 1 1 d . . . H20 H 0.567(3) 0.438(4) 0.748(3) 0.044 Uiso 1 1 d . . . C21 C 0.5550(2) 0.3352(4) 0.6517(3) 0.0373(11) Uani 1 1 d . . . H21 H 0.557(3) 0.378(4) 0.602(3) 0.045 Uiso 1 1 d . . . C22 C 1.0575(2) 0.2783(3) 0.5171(2) 0.0215(7) Uani 1 1 d . . . C23 C 0.9099(2) 0.3425(3) 0.3852(2) 0.0252(8) Uani 1 1 d . . . C24 C 0.9336(2) 0.4122(3) 0.5613(2) 0.0229(8) Uani 1 1 d . . . C25 C 0.9474(2) 0.1855(3) 0.6135(2) 0.0166(7) Uani 1 1 d . . . C26 C 0.9378(2) 0.1231(3) 0.4381(2) 0.0231(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 W 0.01076(7) 0.01572(8) 0.01180(7) 0.00108(5) 0.00304(5) -0.00087(5) Fe 0.0168(2) 0.0174(2) 0.0104(2) -0.00165(17) 0.00587(17) -0.00417(18) P 0.0126(4) 0.0110(4) 0.0092(4) 0.0000(3) 0.0031(3) -0.0001(3) Si1 0.0158(4) 0.0115(4) 0.0198(4) -0.0036(4) 0.0015(3) -0.0008(3) Si2 0.0124(4) 0.0194(5) 0.0124(4) -0.0001(3) 0.0010(3) -0.0008(3) N1 0.0176(14) 0.0129(14) 0.0118(12) 0.0011(10) 0.0043(10) 0.0010(11) N2 0.0145(13) 0.0125(13) 0.0113(12) 0.0021(10) 0.0044(10) 0.0006(10) N3 0.0285(16) 0.0111(14) 0.0124(13) 0.0010(11) 0.0063(11) 0.0025(12) O1 0.0133(13) 0.0466(18) 0.0348(15) -0.0030(13) 0.0036(11) -0.0026(12) O2 0.0275(16) 0.076(2) 0.0342(16) 0.0326(16) 0.0114(12) 0.0103(15) O3 0.0405(18) 0.0226(16) 0.059(2) -0.0150(14) 0.0120(14) -0.0106(13) O4 0.0276(14) 0.0264(14) 0.0181(12) 0.0047(11) 0.0028(10) 0.0019(11) O5 0.0373(16) 0.0318(16) 0.0435(17) -0.0147(14) 0.0189(13) 0.0018(13) C1 0.0111(15) 0.0140(16) 0.0123(14) -0.0014(12) 0.0047(11) -0.0025(12) C2 0.0117(15) 0.0159(16) 0.0098(14) 0.0019(12) 0.0031(11) -0.0015(12) C3 0.0118(15) 0.0128(16) 0.0149(15) 0.0010(12) 0.0037(11) -0.0015(12) C4 0.0198(17) 0.0143(17) 0.0188(16) -0.0007(13) 0.0049(13) 0.0008(13) C5 0.039(2) 0.036(2) 0.0231(19) -0.0138(17) -0.0017(16) 0.0105(19) C6 0.021(2) 0.0166(19) 0.062(3) 0.0096(18) 0.0007(18) -0.0040(15) C7 0.0232(18) 0.032(2) 0.0138(16) -0.0027(14) 0.0032(13) -0.0027(15) C8 0.0211(18) 0.027(2) 0.0234(18) 0.0031(15) 0.0006(14) -0.0018(15) C9 0.0161(17) 0.029(2) 0.0208(17) 0.0013(15) -0.0002(13) 0.0038(15) C10 0.032(2) 0.0169(18) 0.0167(16) 0.0063(14) 0.0063(14) 0.0043(15) C11 0.0268(19) 0.0109(16) 0.0256(18) -0.0005(14) 0.0060(14) 0.0065(14) C12 0.0137(15) 0.0135(16) 0.0129(14) 0.0001(12) 0.0044(11) 0.0009(12) C13 0.0244(18) 0.0115(16) 0.0142(15) -0.0013(13) 0.0060(13) 0.0022(13) C14 0.0301(19) 0.0126(16) 0.0134(15) 0.0029(13) 0.0057(13) 0.0015(14) C15 0.0188(17) 0.0195(17) 0.0116(15) -0.0001(13) 0.0021(12) -0.0007(14) C16 0.0157(16) 0.0121(17) 0.0155(15) -0.0008(13) 0.0032(12) 0.0000(12) C17 0.023(2) 0.071(4) 0.036(2) -0.033(2) 0.0130(18) -0.023(2) C18 0.034(2) 0.043(3) 0.060(3) 0.002(2) 0.024(2) -0.019(2) C19 0.025(2) 0.071(3) 0.025(2) -0.004(2) 0.0157(16) -0.007(2) C20 0.021(2) 0.042(3) 0.046(3) -0.009(2) 0.0086(17) 0.0027(19) C21 0.0152(19) 0.064(3) 0.031(2) 0.008(2) 0.0023(15) -0.0032(19) C22 0.0214(19) 0.026(2) 0.0170(16) -0.0010(14) 0.0044(13) -0.0012(14) C23 0.0143(17) 0.035(2) 0.0273(19) 0.0059(17) 0.0075(14) 0.0018(15) C24 0.0155(17) 0.025(2) 0.0271(18) -0.0004(16) 0.0030(14) -0.0056(14) C25 0.0121(16) 0.0197(17) 0.0175(16) -0.0062(14) 0.0023(12) -0.0003(13) C26 0.0191(18) 0.029(2) 0.0221(17) -0.0004(16) 0.0074(14) -0.0003(15) _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 W C22 2.000(4) . ? W C25 2.040(3) . ? W C24 2.044(4) . ? W C26 2.046(4) . ? W C23 2.052(4) . ? W P 2.5359(8) . ? Fe C16 2.034(3) . ? Fe C17 2.037(4) . ? Fe C21 2.038(4) . ? Fe C12 2.040(3) . ? Fe C13 2.045(3) . ? Fe C18 2.046(4) . ? Fe C19 2.048(4) . ? Fe C20 2.050(4) . ? Fe C15 2.054(3) . ? Fe C14 2.062(4) . ? P N2 1.683(3) . ? P C3 1.849(3) . ? P C1 1.859(3) . ? Si1 C5 1.864(4) . ? Si1 C6 1.875(4) . ? Si1 C4 1.882(3) . ? Si1 C3 1.903(3) . ? Si2 C7 1.875(4) . ? Si2 C8 1.877(4) . ? Si2 C9 1.878(4) . ? Si2 C3 1.929(3) . ? N1 C1 1.292(4) . ? N1 C2 1.443(4) . ? N2 C2 1.307(4) . ? N3 C2 1.337(4) . ? N3 C11 1.447(4) . ? N3 C10 1.462(4) . ? O1 C22 1.145(4) . ? O2 C23 1.137(4) . ? O3 C24 1.137(4) . ? O4 C25 1.137(4) . ? O5 C26 1.145(4) . ? C1 C12 1.452(4) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.432(5) . ? C12 C16 1.436(4) . ? C13 C14 1.414(4) . ? C13 H13 0.86(4) . ? C14 C15 1.421(5) . ? C14 H14 0.92(4) . ? C15 C16 1.413(5) . ? C15 H15 0.96(4) . ? C16 H16 0.94(4) . ? C17 C21 1.395(7) . ? C17 C18 1.421(7) . ? C17 H17 0.72(5) . ? C18 C19 1.407(7) . ? C18 H18 0.84(5) . ? C19 C20 1.400(7) . ? C19 H19 0.91(5) . ? C20 C21 1.390(6) . ? C20 H20 0.83(5) . ? C21 H21 0.97(5) . ? 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 C22 W C25 89.74(13) . . ? C22 W C24 87.50(14) . . ? C25 W C24 90.80(13) . . ? C22 W C26 87.45(14) . . ? C25 W C26 90.92(13) . . ? C24 W C26 174.65(13) . . ? C22 W C23 91.58(14) . . ? C25 W C23 177.97(14) . . ? C24 W C23 90.80(15) . . ? C26 W C23 87.60(15) . . ? C22 W P 170.44(11) . . ? C25 W P 93.42(9) . . ? C24 W P 83.44(10) . . ? C26 W P 101.51(10) . . ? C23 W P 85.52(10) . . ? C16 Fe C17 151.75(18) . . ? C16 Fe C21 117.69(17) . . ? C17 Fe C21 40.0(2) . . ? C16 Fe C12 41.26(12) . . ? C17 Fe C12 119.05(15) . . ? C21 Fe C12 108.78(15) . . ? C16 Fe C13 68.89(13) . . ? C17 Fe C13 110.27(16) . . ? C21 Fe C13 130.34(15) . . ? C12 Fe C13 41.04(13) . . ? C16 Fe C18 165.19(17) . . ? C17 Fe C18 40.7(2) . . ? C21 Fe C18 67.9(2) . . ? C12 Fe C18 152.69(17) . . ? C13 Fe C18 119.12(18) . . ? C16 Fe C19 127.13(16) . . ? C17 Fe C19 67.38(17) . . ? C21 Fe C19 67.14(17) . . ? C12 Fe C19 165.71(17) . . ? C13 Fe C19 151.85(17) . . ? C18 Fe C19 40.2(2) . . ? C16 Fe C20 107.22(16) . . ? C17 Fe C20 67.08(19) . . ? C21 Fe C20 39.76(17) . . ? C12 Fe C20 128.27(16) . . ? C13 Fe C20 167.35(16) . . ? C18 Fe C20 67.6(2) . . ? C19 Fe C20 39.96(19) . . ? C16 Fe C15 40.43(13) . . ? C17 Fe C15 167.38(19) . . ? C21 Fe C15 150.57(18) . . ? C12 Fe C15 68.38(12) . . ? C13 Fe C15 67.87(13) . . ? C18 Fe C15 128.26(18) . . ? C19 Fe C15 107.97(15) . . ? C20 Fe C15 117.54(16) . . ? C16 Fe C14 68.49(14) . . ? C17 Fe C14 130.23(19) . . ? C21 Fe C14 168.16(17) . . ? C12 Fe C14 68.55(13) . . ? C13 Fe C14 40.26(12) . . ? C18 Fe C14 108.79(19) . . ? C19 Fe C14 118.29(16) . . ? C20 Fe C14 150.85(16) . . ? C15 Fe C14 40.38(14) . . ? N2 P C3 105.96(14) . . ? N2 P C1 90.74(13) . . ? C3 P C1 104.99(14) . . ? N2 P W 107.78(9) . . ? C3 P W 130.89(10) . . ? C1 P W 109.14(10) . . ? C5 Si1 C6 112.6(2) . . ? C5 Si1 C4 106.53(16) . . ? C6 Si1 C4 104.11(16) . . ? C5 Si1 C3 111.16(17) . . ? C6 Si1 C3 105.04(16) . . ? C4 Si1 C3 117.31(14) . . ? C7 Si2 C8 106.81(16) . . ? C7 Si2 C9 114.89(17) . . ? C8 Si2 C9 103.58(17) . . ? C7 Si2 C3 110.68(15) . . ? C8 Si2 C3 111.22(15) . . ? C9 Si2 C3 109.43(14) . . ? C1 N1 C2 108.7(3) . . ? C2 N2 P 109.0(2) . . ? C2 N3 C11 124.0(3) . . ? C2 N3 C10 119.5(3) . . ? C11 N3 C10 116.5(3) . . ? N1 C1 C12 123.0(3) . . ? N1 C1 P 110.7(2) . . ? C12 C1 P 126.0(2) . . ? N2 C2 N3 123.4(3) . . ? N2 C2 N1 120.5(3) . . ? N3 C2 N1 116.1(3) . . ? P C3 Si1 120.10(16) . . ? P C3 Si2 109.65(16) . . ? Si1 C3 Si2 113.63(16) . . ? P C3 H3 103.8 . . ? Si1 C3 H3 103.8 . . ? Si2 C3 H3 103.8 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 . . ? 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 . . ? C13 C12 C16 107.1(3) . . ? C13 C12 C1 125.8(3) . . ? C16 C12 C1 126.9(3) . . ? C13 C12 Fe 69.66(18) . . ? C16 C12 Fe 69.14(17) . . ? C1 C12 Fe 123.5(2) . . ? C14 C13 C12 108.6(3) . . ? C14 C13 Fe 70.5(2) . . ? C12 C13 Fe 69.30(18) . . ? C14 C13 H13 125(2) . . ? C12 C13 H13 127(2) . . ? Fe C13 H13 130(2) . . ? C13 C14 C15 107.7(3) . . ? C13 C14 Fe 69.21(19) . . ? C15 C14 Fe 69.50(19) . . ? C13 C14 H14 127(2) . . ? C15 C14 H14 125(2) . . ? Fe C14 H14 126(2) . . ? C16 C15 C14 108.9(3) . . ? C16 C15 Fe 69.03(18) . . ? C14 C15 Fe 70.11(19) . . ? C16 C15 H15 127(2) . . ? C14 C15 H15 124(2) . . ? Fe C15 H15 122(2) . . ? C15 C16 C12 107.7(3) . . ? C15 C16 Fe 70.54(19) . . ? C12 C16 Fe 69.59(18) . . ? C15 C16 H16 125(2) . . ? C12 C16 H16 127(2) . . ? Fe C16 H16 126(2) . . ? C21 C17 C18 108.3(4) . . ? C21 C17 Fe 70.0(2) . . ? C18 C17 Fe 70.0(2) . . ? C21 C17 H17 122(4) . . ? C18 C17 H17 129(4) . . ? Fe C17 H17 123(4) . . ? C19 C18 C17 106.6(4) . . ? C19 C18 Fe 70.0(2) . . ? C17 C18 Fe 69.3(2) . . ? C19 C18 H18 127(4) . . ? C17 C18 H18 127(4) . . ? Fe C18 H18 127(4) . . ? C20 C19 C18 108.6(4) . . ? C20 C19 Fe 70.1(2) . . ? C18 C19 Fe 69.8(2) . . ? C20 C19 H19 123(3) . . ? C18 C19 H19 128(3) . . ? Fe C19 H19 123(3) . . ? C21 C20 C19 108.1(4) . . ? C21 C20 Fe 69.6(2) . . ? C19 C20 Fe 69.9(2) . . ? C21 C20 H20 124(3) . . ? C19 C20 H20 128(3) . . ? Fe C20 H20 127(3) . . ? C20 C21 C17 108.4(4) . . ? C20 C21 Fe 70.6(2) . . ? C17 C21 Fe 70.0(3) . . ? C20 C21 H21 127(3) . . ? C17 C21 H21 124(3) . . ? Fe C21 H21 118(3) . . ? O1 C22 W 179.2(3) . . ? O2 C23 W 178.1(4) . . ? O3 C24 W 178.3(3) . . ? O4 C25 W 178.3(3) . . ? O5 C26 W 175.2(3) . . ? 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 C22 W P N2 46.0(6) . . . . ? C25 W P N2 155.15(13) . . . . ? C24 W P N2 64.74(14) . . . . ? C26 W P N2 -113.21(14) . . . . ? C23 W P N2 -26.59(15) . . . . ? C22 W P C3 177.3(6) . . . . ? C25 W P C3 -73.57(16) . . . . ? C24 W P C3 -163.98(16) . . . . ? C26 W P C3 18.07(17) . . . . ? C23 W P C3 104.69(17) . . . . ? C22 W P C1 -51.2(6) . . . . ? C25 W P C1 57.94(14) . . . . ? C24 W P C1 -32.48(15) . . . . ? C26 W P C1 149.57(15) . . . . ? C23 W P C1 -123.80(15) . . . . ? C3 P N2 C2 109.9(2) . . . . ? C1 P N2 C2 4.1(2) . . . . ? W P N2 C2 -106.3(2) . . . . ? C2 N1 C1 C12 178.0(3) . . . . ? C2 N1 C1 P 4.2(3) . . . . ? N2 P C1 N1 -5.0(2) . . . . ? C3 P C1 N1 -111.8(2) . . . . ? W P C1 N1 104.1(2) . . . . ? N2 P C1 C12 -178.6(3) . . . . ? C3 P C1 C12 74.7(3) . . . . ? W P C1 C12 -69.5(3) . . . . ? P N2 C2 N3 178.2(3) . . . . ? P N2 C2 N1 -2.7(4) . . . . ? C11 N3 C2 N2 179.0(3) . . . . ? C10 N3 C2 N2 -3.3(5) . . . . ? C11 N3 C2 N1 -0.1(5) . . . . ? C10 N3 C2 N1 177.6(3) . . . . ? C1 N1 C2 N2 -1.2(4) . . . . ? C1 N1 C2 N3 177.9(3) . . . . ? N2 P C3 Si1 143.96(17) . . . . ? C1 P C3 Si1 -120.85(18) . . . . ? W P C3 Si1 12.1(2) . . . . ? N2 P C3 Si2 9.60(19) . . . . ? C1 P C3 Si2 104.79(16) . . . . ? W P C3 Si2 -122.29(12) . . . . ? C5 Si1 C3 P -86.9(2) . . . . ? C6 Si1 C3 P 151.0(2) . . . . ? C4 Si1 C3 P 36.0(2) . . . . ? C5 Si1 C3 Si2 45.8(2) . . . . ? C6 Si1 C3 Si2 -76.3(2) . . . . ? C4 Si1 C3 Si2 168.71(15) . . . . ? C7 Si2 C3 P 56.4(2) . . . . ? C8 Si2 C3 P 174.97(16) . . . . ? C9 Si2 C3 P -71.2(2) . . . . ? C7 Si2 C3 Si1 -81.1(2) . . . . ? C8 Si2 C3 Si1 37.4(2) . . . . ? C9 Si2 C3 Si1 151.28(17) . . . . ? N1 C1 C12 C13 163.7(3) . . . . ? P C1 C12 C13 -23.5(5) . . . . ? N1 C1 C12 C16 -12.1(5) . . . . ? P C1 C12 C16 160.7(3) . . . . ? N1 C1 C12 Fe 75.8(4) . . . . ? P C1 C12 Fe -111.4(3) . . . . ? C16 Fe C12 C13 118.5(3) . . . . ? C17 Fe C12 C13 -88.0(3) . . . . ? C21 Fe C12 C13 -130.6(2) . . . . ? C18 Fe C12 C13 -52.5(4) . . . . ? C19 Fe C12 C13 158.5(6) . . . . ? C20 Fe C12 C13 -170.6(2) . . . . ? C15 Fe C12 C13 80.7(2) . . . . ? C14 Fe C12 C13 37.12(19) . . . . ? C17 Fe C12 C16 153.5(2) . . . . ? C21 Fe C12 C16 110.9(2) . . . . ? C13 Fe C12 C16 -118.5(3) . . . . ? C18 Fe C12 C16 -171.0(4) . . . . ? C19 Fe C12 C16 40.0(7) . . . . ? C20 Fe C12 C16 70.9(3) . . . . ? C15 Fe C12 C16 -37.83(19) . . . . ? C14 Fe C12 C16 -81.4(2) . . . . ? C16 Fe C12 C1 -121.3(3) . . . . ? C17 Fe C12 C1 32.2(3) . . . . ? C21 Fe C12 C1 -10.4(3) . . . . ? C13 Fe C12 C1 120.2(3) . . . . ? C18 Fe C12 C1 67.7(5) . . . . ? C19 Fe C12 C1 -81.3(7) . . . . ? C20 Fe C12 C1 -50.4(3) . . . . ? C15 Fe C12 C1 -159.1(3) . . . . ? C14 Fe C12 C1 157.3(3) . . . . ? C16 C12 C13 C14 -0.6(4) . . . . ? C1 C12 C13 C14 -177.0(3) . . . . ? Fe C12 C13 C14 -59.8(2) . . . . ? C16 C12 C13 Fe 59.2(2) . . . . ? C1 C12 C13 Fe -117.2(3) . . . . ? C16 Fe C13 C14 81.2(2) . . . . ? C17 Fe C13 C14 -129.0(2) . . . . ? C21 Fe C13 C14 -169.8(2) . . . . ? C12 Fe C13 C14 119.6(3) . . . . ? C18 Fe C13 C14 -85.0(3) . . . . ? C19 Fe C13 C14 -49.3(4) . . . . ? C20 Fe C13 C14 155.5(7) . . . . ? C15 Fe C13 C14 37.6(2) . . . . ? C16 Fe C13 C12 -38.40(18) . . . . ? C17 Fe C13 C12 111.4(2) . . . . ? C21 Fe C13 C12 70.6(3) . . . . ? C18 Fe C13 C12 155.4(2) . . . . ? C19 Fe C13 C12 -168.9(3) . . . . ? C20 Fe C13 C12 35.8(8) . . . . ? C15 Fe C13 C12 -82.0(2) . . . . ? C14 Fe C13 C12 -119.6(3) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? Fe C13 C14 C15 -59.1(2) . . . . ? C12 C13 C14 Fe 59.1(2) . . . . ? C16 Fe C14 C13 -82.3(2) . . . . ? C17 Fe C14 C13 72.7(3) . . . . ? C21 Fe C14 C13 41.3(8) . . . . ? C12 Fe C14 C13 -37.8(2) . . . . ? C18 Fe C14 C13 113.2(2) . . . . ? C19 Fe C14 C13 156.0(2) . . . . ? C20 Fe C14 C13 -169.3(3) . . . . ? C15 Fe C14 C13 -119.2(3) . . . . ? C16 Fe C14 C15 36.93(19) . . . . ? C17 Fe C14 C15 -168.0(2) . . . . ? C21 Fe C14 C15 160.6(7) . . . . ? C12 Fe C14 C15 81.4(2) . . . . ? C13 Fe C14 C15 119.2(3) . . . . ? C18 Fe C14 C15 -127.6(2) . . . . ? C19 Fe C14 C15 -84.7(2) . . . . ? C20 Fe C14 C15 -50.0(4) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? Fe C14 C15 C16 -58.3(2) . . . . ? C13 C14 C15 Fe 58.9(2) . . . . ? C17 Fe C15 C16 167.0(7) . . . . ? C21 Fe C15 C16 -51.5(4) . . . . ? C12 Fe C15 C16 38.59(19) . . . . ? C13 Fe C15 C16 83.0(2) . . . . ? C18 Fe C15 C16 -166.6(2) . . . . ? C19 Fe C15 C16 -126.7(2) . . . . ? C20 Fe C15 C16 -84.4(2) . . . . ? C14 Fe C15 C16 120.5(3) . . . . ? C16 Fe C15 C14 -120.5(3) . . . . ? C17 Fe C15 C14 46.5(8) . . . . ? C21 Fe C15 C14 -172.0(3) . . . . ? C12 Fe C15 C14 -81.9(2) . . . . ? C13 Fe C15 C14 -37.50(19) . . . . ? C18 Fe C15 C14 72.9(3) . . . . ? C19 Fe C15 C14 112.8(2) . . . . ? C20 Fe C15 C14 155.1(2) . . . . ? C14 C15 C16 C12 -1.0(4) . . . . ? Fe C15 C16 C12 -59.9(2) . . . . ? C14 C15 C16 Fe 58.9(2) . . . . ? C13 C12 C16 C15 1.0(4) . . . . ? C1 C12 C16 C15 177.4(3) . . . . ? Fe C12 C16 C15 60.5(2) . . . . ? C13 C12 C16 Fe -59.6(2) . . . . ? C1 C12 C16 Fe 116.9(3) . . . . ? C17 Fe C16 C15 -174.0(3) . . . . ? C21 Fe C16 C15 154.2(2) . . . . ? C12 Fe C16 C15 -118.4(3) . . . . ? C13 Fe C16 C15 -80.2(2) . . . . ? C18 Fe C16 C15 45.3(8) . . . . ? C19 Fe C16 C15 73.0(3) . . . . ? C20 Fe C16 C15 112.5(2) . . . . ? C14 Fe C16 C15 -36.88(19) . . . . ? C17 Fe C16 C12 -55.6(4) . . . . ? C21 Fe C16 C12 -87.3(2) . . . . ? C13 Fe C16 C12 38.21(18) . . . . ? C18 Fe C16 C12 163.7(7) . . . . ? C19 Fe C16 C12 -168.5(2) . . . . ? C20 Fe C16 C12 -129.0(2) . . . . ? C15 Fe C16 C12 118.4(3) . . . . ? C14 Fe C16 C12 81.57(19) . . . . ? C16 Fe C17 C21 -46.4(4) . . . . ? C12 Fe C17 C21 -84.9(3) . . . . ? C13 Fe C17 C21 -129.3(2) . . . . ? C18 Fe C17 C21 119.2(4) . . . . ? C19 Fe C17 C21 80.9(3) . . . . ? C20 Fe C17 C21 37.4(3) . . . . ? C15 Fe C17 C21 151.6(6) . . . . ? C14 Fe C17 C21 -170.4(2) . . . . ? C16 Fe C17 C18 -165.6(3) . . . . ? C21 Fe C17 C18 -119.2(4) . . . . ? C12 Fe C17 C18 155.9(3) . . . . ? C13 Fe C17 C18 111.5(3) . . . . ? C19 Fe C17 C18 -38.3(3) . . . . ? C20 Fe C17 C18 -81.8(3) . . . . ? C15 Fe C17 C18 32.4(8) . . . . ? C14 Fe C17 C18 70.3(3) . . . . ? C21 C17 C18 C19 0.6(5) . . . . ? Fe C17 C18 C19 60.4(3) . . . . ? C21 C17 C18 Fe -59.8(3) . . . . ? C16 Fe C18 C19 35.1(9) . . . . ? C17 Fe C18 C19 -117.5(4) . . . . ? C21 Fe C18 C19 -80.2(3) . . . . ? C12 Fe C18 C19 -168.6(3) . . . . ? C13 Fe C18 C19 154.8(3) . . . . ? C20 Fe C18 C19 -37.1(3) . . . . ? C15 Fe C18 C19 71.1(3) . . . . ? C14 Fe C18 C19 111.9(3) . . . . ? C16 Fe C18 C17 152.6(6) . . . . ? C21 Fe C18 C17 37.3(3) . . . . ? C12 Fe C18 C17 -51.1(5) . . . . ? C13 Fe C18 C17 -87.7(3) . . . . ? C19 Fe C18 C17 117.5(4) . . . . ? C20 Fe C18 C17 80.4(3) . . . . ? C15 Fe C18 C17 -171.4(3) . . . . ? C14 Fe C18 C17 -130.6(3) . . . . ? C17 C18 C19 C20 -0.3(5) . . . . ? Fe C18 C19 C20 59.6(3) . . . . ? C17 C18 C19 Fe -59.9(3) . . . . ? C16 Fe C19 C20 71.0(3) . . . . ? C17 Fe C19 C20 -80.8(3) . . . . ? C21 Fe C19 C20 -37.3(3) . . . . ? C12 Fe C19 C20 38.9(7) . . . . ? C13 Fe C19 C20 -171.8(3) . . . . ? C18 Fe C19 C20 -119.6(4) . . . . ? C15 Fe C19 C20 111.7(3) . . . . ? C14 Fe C19 C20 154.4(2) . . . . ? C16 Fe C19 C18 -169.4(3) . . . . ? C17 Fe C19 C18 38.8(3) . . . . ? C21 Fe C19 C18 82.4(3) . . . . ? C12 Fe C19 C18 158.5(6) . . . . ? C13 Fe C19 C18 -52.1(5) . . . . ? C20 Fe C19 C18 119.6(4) . . . . ? C15 Fe C19 C18 -128.7(3) . . . . ? C14 Fe C19 C18 -86.0(3) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? Fe C19 C20 C21 59.4(3) . . . . ? C18 C19 C20 Fe -59.4(3) . . . . ? C16 Fe C20 C21 112.8(3) . . . . ? C17 Fe C20 C21 -37.6(3) . . . . ? C12 Fe C20 C21 72.1(3) . . . . ? C13 Fe C20 C21 42.8(9) . . . . ? C18 Fe C20 C21 -81.9(3) . . . . ? C19 Fe C20 C21 -119.3(4) . . . . ? C15 Fe C20 C21 155.4(3) . . . . ? C14 Fe C20 C21 -170.6(3) . . . . ? C16 Fe C20 C19 -127.9(3) . . . . ? C17 Fe C20 C19 81.6(3) . . . . ? C21 Fe C20 C19 119.3(4) . . . . ? C12 Fe C20 C19 -168.6(2) . . . . ? C13 Fe C20 C19 162.1(7) . . . . ? C18 Fe C20 C19 37.3(3) . . . . ? C15 Fe C20 C19 -85.4(3) . . . . ? C14 Fe C20 C19 -51.3(5) . . . . ? C19 C20 C21 C17 0.4(5) . . . . ? Fe C20 C21 C17 60.0(3) . . . . ? C19 C20 C21 Fe -59.6(3) . . . . ? C18 C17 C21 C20 -0.7(5) . . . . ? Fe C17 C21 C20 -60.4(3) . . . . ? C18 C17 C21 Fe 59.7(3) . . . . ? C16 Fe C21 C20 -83.8(3) . . . . ? C17 Fe C21 C20 119.0(4) . . . . ? C12 Fe C21 C20 -127.9(3) . . . . ? C13 Fe C21 C20 -168.7(3) . . . . ? C18 Fe C21 C20 81.1(3) . . . . ? C19 Fe C21 C20 37.4(3) . . . . ? C15 Fe C21 C20 -48.8(4) . . . . ? C14 Fe C21 C20 157.2(7) . . . . ? C16 Fe C21 C17 157.2(2) . . . . ? C12 Fe C21 C17 113.1(2) . . . . ? C13 Fe C21 C17 72.3(3) . . . . ? C18 Fe C21 C17 -37.9(3) . . . . ? C19 Fe C21 C17 -81.5(3) . . . . ? C20 Fe C21 C17 -119.0(4) . . . . ? C15 Fe C21 C17 -167.8(3) . . . . ? C14 Fe C21 C17 38.2(9) . . . . ? C25 W C22 O1 -70(27) . . . . ? C24 W C22 O1 21(27) . . . . ? C26 W C22 O1 -161(27) . . . . ? C23 W C22 O1 112(27) . . . . ? P W C22 O1 40(28) . . . . ? C22 W C23 O2 82(10) . . . . ? C25 W C23 O2 -49(12) . . . . ? C24 W C23 O2 169(10) . . . . ? C26 W C23 O2 -6(10) . . . . ? P W C23 O2 -107(10) . . . . ? C22 W C24 O3 35(12) . . . . ? C25 W C24 O3 125(12) . . . . ? C26 W C24 O3 16(13) . . . . ? C23 W C24 O3 -56(12) . . . . ? P W C24 O3 -142(12) . . . . ? C22 W C25 O4 -29(10) . . . . ? C24 W C25 O4 -116(10) . . . . ? C26 W C25 O4 59(10) . . . . ? C23 W C25 O4 102(11) . . . . ? P W C25 O4 160(10) . . . . ? C22 W C26 O5 -13(4) . . . . ? C25 W C26 O5 -103(4) . . . . ? C24 W C26 O5 6(5) . . . . ? C23 W C26 O5 78(4) . . . . ? P W C26 O5 163(4) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 3.694 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.113