data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H52 Fe N4 Si2 U, C6 H12' _chemical_formula_sum 'C43 H64 Fe N4 Si2 U' _chemical_formula_weight 987.04 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' 'Si' 'Si' 0.0817 0.0704 '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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.538(3) _cell_length_b 9.827(2) _cell_length_c 27.945(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.981(2) _cell_angle_gamma 90.00 _cell_volume 4343.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9969 _cell_measurement_theta_min 3.86 _cell_measurement_theta_max 28.98 _exptl_crystal_description block _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 4.146 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7327 _exptl_absorpt_correction_T_max 0.8517 _exptl_absorpt_process_details 'Sadabs (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41564 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 30.63 _reflns_number_total 12610 _reflns_number_gt 10166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX11' _computing_cell_refinement 'Bruker APEX11' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0308P)^2^+1.3036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12610 _refine_ls_number_parameters 473 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.248197(6) 0.825395(9) 0.423854(4) 0.01833(3) Uani 1 1 d . . . Fe1 Fe 0.26183(2) 0.49555(4) 0.413239(15) 0.01887(8) Uani 1 1 d . . . Si2 Si 0.12283(5) 0.83853(8) 0.29535(3) 0.02341(17) Uani 1 1 d . . . Si1 Si 0.30466(5) 0.78080(8) 0.55714(3) 0.02044(16) Uani 1 1 d . . . N2 N 0.19611(15) 0.7588(2) 0.34454(9) 0.0212(5) Uani 1 1 d . . . N1 N 0.30339(14) 0.7265(2) 0.49782(9) 0.0199(5) Uani 1 1 d . . . N3 N 0.11252(15) 0.8066(2) 0.43584(9) 0.0229(5) Uani 1 1 d . . . N4 N 0.04560(15) 1.0019(2) 0.43272(9) 0.0230(5) Uani 1 1 d . . . C1 C 0.33226(19) 1.0389(3) 0.42649(12) 0.0268(6) Uani 1 1 d . . . H1A H 0.3021 1.1106 0.4032 0.032 Uiso 1 1 calc R . . H1B H 0.3574 1.0758 0.4606 0.032 Uiso 1 1 calc R . . C4 C 0.4927(2) 0.7793(4) 0.37058(16) 0.0426(9) Uani 1 1 d . . . H4A H 0.5272 0.7202 0.3581 0.051 Uiso 1 1 calc R . . C3 C 0.4956(2) 0.7760(4) 0.41996(16) 0.0437(9) Uani 1 1 d . . . H3A H 0.5327 0.7141 0.4419 0.052 Uiso 1 1 calc R . . C5 C 0.4378(2) 0.8713(4) 0.33882(14) 0.0402(8) Uani 1 1 d . . . H5A H 0.4349 0.8743 0.3044 0.048 Uiso 1 1 calc R . . C2 C 0.39069(18) 0.9581(3) 0.40769(12) 0.0248(6) Uani 1 1 d . . . C7 C 0.12019(17) 0.9431(3) 0.43204(11) 0.0216(6) Uani 1 1 d . . . C13 C -0.01136(18) 0.9012(3) 0.43726(11) 0.0235(6) Uani 1 1 d . . . C9 C -0.0077(2) 0.6547(3) 0.44321(13) 0.0315(7) Uani 1 1 d . . . H9A H 0.0208 0.5703 0.4443 0.038 Uiso 1 1 calc R . . C14 C 0.0269(2) 1.1468(3) 0.42789(13) 0.0289(7) Uani 1 1 d . . . H14A H 0.0778 1.1969 0.4273 0.043 Uiso 1 1 calc R . . H14B H 0.0083 1.1774 0.4564 0.043 Uiso 1 1 calc R . . H14C H -0.0181 1.1636 0.3967 0.043 Uiso 1 1 calc R . . C8 C 0.03242(18) 0.7778(3) 0.43926(11) 0.0241(6) Uani 1 1 d . . . C12 C -0.09379(19) 0.9065(3) 0.43964(12) 0.0297(7) Uani 1 1 d . . . H12A H -0.1227 0.9905 0.4385 0.036 Uiso 1 1 calc R . . C10 C -0.0896(2) 0.6595(3) 0.44546(14) 0.0378(8) Uani 1 1 d . . . H10A H -0.1180 0.5771 0.4482 0.045 Uiso 1 1 calc R . . C11 C -0.1320(2) 0.7838(4) 0.44379(14) 0.0379(8) Uani 1 1 d . . . H11A H -0.1885 0.7837 0.4456 0.046 Uiso 1 1 calc R . . C16 C 0.23911(18) 0.4889(3) 0.48204(11) 0.0227(6) Uani 1 1 d . . . H16A H 0.1835 0.5065 0.4883 0.027 Uiso 1 1 calc R . . C15 C 0.30421(18) 0.5885(3) 0.48483(11) 0.0207(6) Uani 1 1 d . . . C21 C 0.15006(18) 0.5156(3) 0.35608(11) 0.0252(6) Uani 1 1 d . . . H21A H 0.0930 0.5335 0.3602 0.030 Uiso 1 1 calc R . . C17 C 0.26780(19) 0.3611(3) 0.46989(12) 0.0252(6) Uani 1 1 d . . . H17A H 0.2366 0.2728 0.4668 0.030 Uiso 1 1 calc R . . C20 C 0.20868(18) 0.6176(3) 0.34856(11) 0.0218(6) Uani 1 1 d . . . C23 C 0.2687(2) 0.4041(3) 0.34913(12) 0.0293(7) Uani 1 1 d . . . H23A H 0.3087 0.3299 0.3468 0.035 Uiso 1 1 calc R . . C19 C 0.37148(17) 0.5204(3) 0.47182(10) 0.0214(6) Uani 1 1 d . . . H19A H 0.4250 0.5636 0.4695 0.026 Uiso 1 1 calc R . . C18 C 0.34963(19) 0.3801(3) 0.46353(11) 0.0240(6) Uani 1 1 d . . . H18A H 0.3857 0.3076 0.4552 0.029 Uiso 1 1 calc R . . C22 C 0.1868(2) 0.3859(3) 0.35476(11) 0.0286(7) Uani 1 1 d . . . H22A H 0.1597 0.2965 0.3575 0.034 Uiso 1 1 calc R . . C24 C 0.28318(19) 0.5461(3) 0.34623(11) 0.0247(6) Uani 1 1 d . . . H24A H 0.3358 0.5888 0.3423 0.030 Uiso 1 1 calc R . . C25 C 0.40026(19) 0.7115(3) 0.60616(12) 0.0293(7) Uani 1 1 d . . . C26 C 0.30892(19) 0.9708(3) 0.55531(12) 0.0280(6) Uani 1 1 d . . . H26A H 0.2653 1.0043 0.5258 0.042 Uiso 1 1 calc R . . H26B H 0.3647 0.9996 0.5536 0.042 Uiso 1 1 calc R . . H26C H 0.2989 1.0082 0.5856 0.042 Uiso 1 1 calc R . . C33 C 0.14169(19) 1.0252(3) 0.30759(12) 0.0284(7) Uani 1 1 d . . . H33A H 0.1388 1.0466 0.3413 0.043 Uiso 1 1 calc R . . H33B H 0.0984 1.0772 0.2829 0.043 Uiso 1 1 calc R . . H33C H 0.1977 1.0493 0.3049 0.043 Uiso 1 1 calc R . . C32 C 0.0118(2) 0.7978(3) 0.29469(13) 0.0341(7) Uani 1 1 d . . . H32A H 0.0009 0.8358 0.3246 0.051 Uiso 1 1 calc R . . H32B H 0.0043 0.6988 0.2943 0.051 Uiso 1 1 calc R . . H32C H -0.0279 0.8373 0.2648 0.051 Uiso 1 1 calc R . . C37 C 0.0878(2) 0.8866(4) 0.19164(13) 0.0407(8) Uani 1 1 d . . . H37A H 0.0953 0.8598 0.1594 0.061 Uiso 1 1 calc R . . H37B H 0.1075 0.9803 0.1994 0.061 Uiso 1 1 calc R . . H37C H 0.0278 0.8807 0.1898 0.061 Uiso 1 1 calc R . . C34 C 0.1393(2) 0.7906(3) 0.23298(12) 0.0284(7) Uani 1 1 d . . . C35 C 0.2329(2) 0.8033(4) 0.23647(13) 0.0353(8) Uani 1 1 d . . . H35A H 0.2408 0.7838 0.2037 0.053 Uiso 1 1 calc R . . H35B H 0.2656 0.7383 0.2612 0.053 Uiso 1 1 calc R . . H35C H 0.2522 0.8960 0.2467 0.053 Uiso 1 1 calc R . . C36 C 0.1101(2) 0.6435(3) 0.21884(14) 0.0391(8) Uani 1 1 d . . . H36A H 0.1225 0.6184 0.1878 0.059 Uiso 1 1 calc R . . H36B H 0.0491 0.6366 0.2140 0.059 Uiso 1 1 calc R . . H36C H 0.1401 0.5818 0.2457 0.059 Uiso 1 1 calc R . . C6 C 0.38800(19) 0.9574(3) 0.35696(12) 0.0324(7) Uani 1 1 d . . . H6A H 0.3507 1.0181 0.3345 0.039 Uiso 1 1 calc R . . C28 C 0.20634(19) 0.7292(3) 0.57273(12) 0.0291(7) Uani 1 1 d . . . H28A H 0.1567 0.7578 0.5458 0.044 Uiso 1 1 calc R . . H28B H 0.2053 0.7726 0.6041 0.044 Uiso 1 1 calc R . . H28C H 0.2056 0.6301 0.5765 0.044 Uiso 1 1 calc R . . C30 C 0.4124(2) 0.7896(4) 0.65560(13) 0.0419(9) Uani 1 1 d . . . H30A H 0.4596 0.7498 0.6816 0.063 Uiso 1 1 calc R . . H30B H 0.3606 0.7834 0.6658 0.063 Uiso 1 1 calc R . . H30C H 0.4247 0.8854 0.6508 0.063 Uiso 1 1 calc R . . C29 C 0.4791(2) 0.7276(4) 0.58895(14) 0.0445(9) Uani 1 1 d . . . H29A H 0.5283 0.6916 0.6147 0.067 Uiso 1 1 calc R . . H29B H 0.4881 0.8242 0.5834 0.067 Uiso 1 1 calc R . . H29C H 0.4717 0.6773 0.5577 0.067 Uiso 1 1 calc R . . C31 C 0.3879(3) 0.5591(4) 0.61570(15) 0.0495(10) Uani 1 1 d . . . H31A H 0.4393 0.5234 0.6397 0.074 Uiso 1 1 calc R . . H31B H 0.3767 0.5088 0.5841 0.074 Uiso 1 1 calc R . . H31C H 0.3400 0.5483 0.6293 0.074 Uiso 1 1 calc R . . C38 C 0.4451(2) 0.8619(3) 0.43855(14) 0.0325(7) Uani 1 1 d . . . H38A H 0.4473 0.8558 0.4728 0.039 Uiso 1 1 calc R . . C1S C 0.7860(4) 0.7748(6) 0.3049(3) 0.104(2) Uani 1 1 d D . . H1SA H 0.8044 0.7469 0.2757 0.157 Uiso 1 1 calc R . . H1SB H 0.8358 0.7835 0.3348 0.157 Uiso 1 1 calc R . . C2S C 0.7208(5) 0.6828(7) 0.3136(3) 0.114(3) Uani 1 1 d . . . H2SA H 0.7177 0.6924 0.3483 0.171 Uiso 1 1 calc R . . H2SB H 0.7340 0.5869 0.3080 0.171 Uiso 1 1 calc R . . C3S C 0.6367(4) 0.7258(7) 0.2759(2) 0.0971(19) Uani 1 1 d . . . H3SA H 0.6353 0.7032 0.2412 0.146 Uiso 1 1 calc R . . H3SB H 0.5877 0.6831 0.2836 0.146 Uiso 1 1 calc R . . C4S C 0.6387(3) 0.8796(6) 0.2844(2) 0.0762(15) Uani 1 1 d . . . H4SA H 0.6243 0.8956 0.3163 0.114 Uiso 1 1 calc R . . C5S C 0.7288(5) 0.9117(7) 0.2942(3) 0.119(3) Uani 1 1 d D . . H5SA H 0.7470 0.9730 0.3235 0.179 Uiso 1 1 calc R . . H5SB H 0.7375 0.9599 0.2650 0.179 Uiso 1 1 calc R . . C6S C 0.5798(3) 0.9737(6) 0.24382(16) 0.0710(14) Uani 1 1 d . . . H6SA H 0.5207 0.9570 0.2424 0.106 Uiso 1 1 calc R . . H6SB H 0.5877 0.9538 0.2111 0.106 Uiso 1 1 calc R . . H6SC H 0.5939 1.0692 0.2525 0.106 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 U1 0.01953(5) 0.01237(5) 0.02477(6) -0.00223(4) 0.00911(4) -0.00098(4) Fe1 0.02004(19) 0.01262(18) 0.0256(2) -0.00238(15) 0.00922(16) -0.00048(15) Si2 0.0230(4) 0.0191(4) 0.0267(4) -0.0014(3) 0.0052(3) 0.0009(3) Si1 0.0200(4) 0.0183(4) 0.0246(4) -0.0035(3) 0.0090(3) -0.0010(3) N2 0.0244(12) 0.0141(11) 0.0261(13) -0.0010(10) 0.0090(10) 0.0009(9) N1 0.0215(12) 0.0148(11) 0.0251(13) -0.0036(9) 0.0093(10) -0.0015(9) N3 0.0207(12) 0.0207(12) 0.0297(13) -0.0017(10) 0.0110(10) -0.0010(9) N4 0.0246(12) 0.0216(12) 0.0239(13) -0.0012(10) 0.0088(10) 0.0035(10) C1 0.0322(16) 0.0147(13) 0.0344(17) 0.0000(12) 0.0112(13) -0.0024(12) C4 0.038(2) 0.0306(18) 0.070(3) -0.0030(18) 0.033(2) -0.0040(15) C3 0.0346(19) 0.0296(18) 0.074(3) 0.0186(18) 0.0277(19) 0.0059(15) C5 0.0343(19) 0.049(2) 0.041(2) -0.0064(17) 0.0170(16) -0.0079(17) C2 0.0233(14) 0.0159(13) 0.0363(17) -0.0013(12) 0.0105(13) -0.0099(11) C7 0.0203(14) 0.0213(14) 0.0236(15) -0.0024(11) 0.0071(11) 0.0007(11) C13 0.0243(15) 0.0237(15) 0.0234(15) -0.0041(12) 0.0083(12) -0.0012(12) C9 0.0313(17) 0.0221(16) 0.046(2) -0.0024(14) 0.0193(15) -0.0006(13) C14 0.0301(16) 0.0235(15) 0.0347(18) 0.0022(13) 0.0118(14) 0.0062(12) C8 0.0225(14) 0.0256(14) 0.0260(16) -0.0049(12) 0.0101(12) -0.0018(12) C12 0.0247(15) 0.0286(16) 0.0374(19) -0.0033(14) 0.0114(14) 0.0015(13) C10 0.0357(18) 0.0307(18) 0.053(2) -0.0073(16) 0.0230(17) -0.0117(15) C11 0.0283(17) 0.043(2) 0.050(2) -0.0041(17) 0.0219(16) -0.0012(15) C16 0.0245(14) 0.0193(14) 0.0270(15) -0.0015(12) 0.0119(12) -0.0022(11) C15 0.0241(14) 0.0181(13) 0.0216(15) -0.0010(11) 0.0090(12) -0.0003(11) C21 0.0231(14) 0.0202(14) 0.0309(16) -0.0024(12) 0.0058(12) -0.0051(12) C17 0.0293(16) 0.0169(13) 0.0303(17) 0.0008(12) 0.0101(13) -0.0027(12) C20 0.0239(14) 0.0169(13) 0.0251(15) -0.0042(11) 0.0078(12) 0.0006(11) C23 0.0405(18) 0.0197(14) 0.0283(17) -0.0053(12) 0.0110(14) 0.0069(13) C19 0.0194(13) 0.0184(13) 0.0261(15) -0.0011(11) 0.0060(11) 0.0008(11) C18 0.0287(15) 0.0152(13) 0.0289(16) -0.0002(12) 0.0095(13) 0.0025(12) C22 0.0370(18) 0.0183(14) 0.0270(17) -0.0039(12) 0.0039(14) -0.0078(13) C24 0.0279(15) 0.0222(14) 0.0271(16) -0.0021(12) 0.0130(13) 0.0013(12) C25 0.0253(15) 0.0298(16) 0.0316(17) -0.0038(13) 0.0064(13) 0.0028(13) C26 0.0334(17) 0.0224(14) 0.0307(17) -0.0048(13) 0.0134(14) 0.0010(13) C33 0.0321(16) 0.0183(14) 0.0326(17) 0.0015(13) 0.0059(13) 0.0042(13) C32 0.0258(16) 0.0345(18) 0.040(2) -0.0019(15) 0.0069(14) 0.0001(14) C37 0.050(2) 0.0366(19) 0.0307(19) 0.0022(15) 0.0038(16) 0.0061(17) C34 0.0287(16) 0.0262(15) 0.0287(17) -0.0030(13) 0.0062(13) 0.0003(13) C35 0.0380(19) 0.041(2) 0.0290(17) -0.0012(15) 0.0125(14) -0.0008(15) C36 0.053(2) 0.0295(18) 0.0327(19) -0.0075(14) 0.0088(17) -0.0017(16) C6 0.0249(16) 0.0379(18) 0.0336(18) 0.0019(15) 0.0074(13) -0.0009(14) C28 0.0278(16) 0.0320(16) 0.0309(17) -0.0050(14) 0.0137(13) -0.0031(13) C30 0.0377(19) 0.051(2) 0.0321(19) -0.0073(17) 0.0028(15) 0.0094(17) C29 0.0202(16) 0.063(3) 0.047(2) -0.017(2) 0.0052(15) 0.0035(16) C31 0.055(2) 0.033(2) 0.048(2) 0.0049(17) -0.0026(19) 0.0082(18) C38 0.0253(16) 0.0310(17) 0.044(2) 0.0100(15) 0.0139(14) -0.0033(13) C1S 0.125(5) 0.088(4) 0.134(6) -0.030(4) 0.090(5) -0.027(4) C2S 0.100(5) 0.106(6) 0.155(7) 0.024(5) 0.066(5) 0.033(4) C3S 0.079(4) 0.102(5) 0.102(5) -0.016(4) 0.014(4) -0.006(4) C4S 0.071(4) 0.092(4) 0.067(3) -0.026(3) 0.023(3) -0.019(3) C5S 0.165(7) 0.106(6) 0.110(5) -0.014(4) 0.076(5) -0.064(5) C6S 0.055(3) 0.113(4) 0.045(3) -0.021(3) 0.013(2) -0.006(3) _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 U1 N1 2.225(2) . ? U1 N2 2.229(2) . ? U1 N3 2.371(2) . ? U1 C7 2.481(3) . ? U1 C1 2.506(3) . ? U1 C2 2.843(3) . ? U1 C20 2.867(3) . ? U1 C15 2.874(3) . ? U1 Fe1 3.2688(8) . ? Fe1 C23 2.037(3) . ? Fe1 C17 2.042(3) . ? Fe1 C18 2.044(3) . ? Fe1 C22 2.046(3) . ? Fe1 C24 2.065(3) . ? Fe1 C16 2.065(3) . ? Fe1 C21 2.069(3) . ? Fe1 C19 2.072(3) . ? Fe1 C15 2.124(3) . ? Fe1 C20 2.133(3) . ? Si2 N2 1.732(3) . ? Si2 C32 1.875(3) . ? Si2 C33 1.875(3) . ? Si2 C34 1.900(3) . ? Si1 N1 1.736(2) . ? Si1 C26 1.870(3) . ? Si1 C28 1.872(3) . ? Si1 C25 1.891(3) . ? N2 C20 1.402(4) . ? N1 C15 1.404(4) . ? N3 C7 1.355(3) . ? N3 C8 1.385(4) . ? N4 C7 1.367(3) . ? N4 C13 1.397(4) . ? N4 C14 1.455(4) . ? C1 C2 1.462(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C4 C3 1.367(5) . ? C4 C5 1.399(5) . ? C4 H4A 0.9500 . ? C3 C38 1.390(5) . ? C3 H3A 0.9500 . ? C5 C6 1.377(5) . ? C5 H5A 0.9500 . ? C2 C6 1.405(4) . ? C2 C38 1.412(4) . ? C13 C12 1.385(4) . ? C13 C8 1.406(4) . ? C9 C10 1.375(4) . ? C9 C8 1.399(4) . ? C9 H9A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 C11 1.382(5) . ? C12 H12A 0.9500 . ? C10 C11 1.403(5) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C16 C17 1.419(4) . ? C16 C15 1.441(4) . ? C16 H16A 1.0000 . ? C15 C19 1.433(4) . ? C21 C22 1.417(4) . ? C21 C20 1.452(4) . ? C21 H21A 1.0000 . ? C17 C18 1.428(4) . ? C17 H17A 1.0000 . ? C20 C24 1.436(4) . ? C23 C22 1.419(4) . ? C23 C24 1.422(4) . ? C23 H23A 1.0000 . ? C19 C18 1.427(4) . ? C19 H19A 1.0000 . ? C18 H18A 1.0000 . ? C22 H22A 1.0000 . ? C24 H24A 1.0000 . ? C25 C29 1.525(5) . ? C25 C30 1.542(5) . ? C25 C31 1.545(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C37 C34 1.542(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C34 C35 1.527(4) . ? C34 C36 1.538(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C6 H6A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C38 H38A 0.9500 . ? C1S C2S 1.481(8) . ? C1S C5S 1.622(7) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S C3S 1.538(9) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.529(8) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S C5S 1.468(8) . ? C4S C6S 1.564(7) . ? C4S H4SA 1.0000 . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 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 N1 U1 N2 136.91(9) . . ? N1 U1 N3 89.03(8) . . ? N2 U1 N3 90.62(9) . . ? N1 U1 C7 104.34(9) . . ? N2 U1 C7 97.83(9) . . ? N3 U1 C7 32.33(8) . . ? N1 U1 C1 105.37(9) . . ? N2 U1 C1 108.97(9) . . ? N3 U1 C1 126.93(9) . . ? C7 U1 C1 95.03(9) . . ? N1 U1 C2 102.35(9) . . ? N2 U1 C2 94.26(9) . . ? N3 U1 C2 157.08(8) . . ? C7 U1 C2 124.75(9) . . ? C1 U1 C2 30.92(9) . . ? N1 U1 C20 108.33(8) . . ? N2 U1 C20 28.60(8) . . ? N3 U1 C20 91.49(8) . . ? C7 U1 C20 112.46(9) . . ? C1 U1 C20 128.56(9) . . ? C2 U1 C20 103.41(8) . . ? N1 U1 C15 28.52(8) . . ? N2 U1 C15 108.41(8) . . ? N3 U1 C15 90.43(8) . . ? C7 U1 C15 117.33(9) . . ? C1 U1 C15 125.50(9) . . ? C2 U1 C15 109.10(8) . . ? C20 U1 C15 79.82(8) . . ? N1 U1 Fe1 68.32(6) . . ? N2 U1 Fe1 68.62(6) . . ? N3 U1 Fe1 91.65(6) . . ? C7 U1 Fe1 123.65(7) . . ? C1 U1 Fe1 141.31(7) . . ? C2 U1 Fe1 110.98(6) . . ? C20 U1 Fe1 40.02(6) . . ? C15 U1 Fe1 39.80(6) . . ? C23 Fe1 C17 113.20(12) . . ? C23 Fe1 C18 98.58(12) . . ? C17 Fe1 C18 40.90(12) . . ? C23 Fe1 C22 40.68(13) . . ? C17 Fe1 C22 99.16(12) . . ? C18 Fe1 C22 113.59(12) . . ? C23 Fe1 C24 40.57(11) . . ? C17 Fe1 C24 151.19(12) . . ? C18 Fe1 C24 118.80(12) . . ? C22 Fe1 C24 68.08(12) . . ? C23 Fe1 C16 151.28(12) . . ? C17 Fe1 C16 40.40(11) . . ? C18 Fe1 C16 68.17(12) . . ? C22 Fe1 C16 119.62(12) . . ? C24 Fe1 C16 167.89(11) . . ? C23 Fe1 C21 68.26(12) . . ? C17 Fe1 C21 119.33(12) . . ? C18 Fe1 C21 151.46(12) . . ? C22 Fe1 C21 40.27(12) . . ? C24 Fe1 C21 68.15(12) . . ? C16 Fe1 C21 110.93(12) . . ? C23 Fe1 C19 119.10(12) . . ? C17 Fe1 C19 68.35(12) . . ? C18 Fe1 C19 40.57(11) . . ? C22 Fe1 C19 151.61(12) . . ? C24 Fe1 C19 110.24(12) . . ? C16 Fe1 C19 67.88(11) . . ? C21 Fe1 C19 167.65(11) . . ? C23 Fe1 C15 158.54(12) . . ? C17 Fe1 C15 67.68(11) . . ? C18 Fe1 C15 67.56(11) . . ? C22 Fe1 C15 159.29(12) . . ? C24 Fe1 C15 130.84(11) . . ? C16 Fe1 C15 40.20(10) . . ? C21 Fe1 C15 131.37(11) . . ? C19 Fe1 C15 39.92(10) . . ? C23 Fe1 C20 67.53(12) . . ? C17 Fe1 C20 159.29(12) . . ? C18 Fe1 C20 158.25(11) . . ? C22 Fe1 C20 67.40(12) . . ? C24 Fe1 C20 39.97(11) . . ? C16 Fe1 C20 131.66(11) . . ? C21 Fe1 C20 40.40(11) . . ? C19 Fe1 C20 130.68(11) . . ? C15 Fe1 C20 119.81(11) . . ? C23 Fe1 U1 122.70(9) . . ? C17 Fe1 U1 124.08(9) . . ? C18 Fe1 U1 122.81(8) . . ? C22 Fe1 U1 123.56(9) . . ? C24 Fe1 U1 83.01(8) . . ? C16 Fe1 U1 84.89(8) . . ? C21 Fe1 U1 84.61(8) . . ? C19 Fe1 U1 83.04(8) . . ? C15 Fe1 U1 60.02(8) . . ? C20 Fe1 U1 59.80(8) . . ? N2 Si2 C32 111.57(14) . . ? N2 Si2 C33 104.91(13) . . ? C32 Si2 C33 108.73(15) . . ? N2 Si2 C34 111.19(13) . . ? C32 Si2 C34 109.89(15) . . ? C33 Si2 C34 110.43(14) . . ? N1 Si1 C26 105.72(13) . . ? N1 Si1 C28 111.71(13) . . ? C26 Si1 C28 108.62(14) . . ? N1 Si1 C25 110.81(13) . . ? C26 Si1 C25 110.45(15) . . ? C28 Si1 C25 109.46(15) . . ? C20 N2 Si2 124.3(2) . . ? C20 N2 U1 101.86(17) . . ? Si2 N2 U1 129.36(12) . . ? C15 N1 Si1 123.06(19) . . ? C15 N1 U1 102.35(16) . . ? Si1 N1 U1 129.80(12) . . ? C7 N3 C8 108.8(2) . . ? C7 N3 U1 78.32(15) . . ? C8 N3 U1 171.7(2) . . ? C7 N4 C13 109.7(2) . . ? C7 N4 C14 125.5(2) . . ? C13 N4 C14 124.8(2) . . ? C2 C1 U1 87.35(16) . . ? C2 C1 H1A 114.1 . . ? U1 C1 H1A 114.1 . . ? C2 C1 H1B 114.1 . . ? U1 C1 H1B 114.1 . . ? H1A C1 H1B 111.3 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C4 C3 C38 121.0(3) . . ? C4 C3 H3A 119.5 . . ? C38 C3 H3A 119.5 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C6 C2 C38 116.1(3) . . ? C6 C2 C1 122.4(3) . . ? C38 C2 C1 121.0(3) . . ? C6 C2 U1 112.00(19) . . ? C38 C2 U1 90.36(17) . . ? C1 C2 U1 61.73(14) . . ? N3 C7 N4 108.2(2) . . ? N3 C7 U1 69.35(15) . . ? N4 C7 U1 174.8(2) . . ? C12 C13 N4 132.6(3) . . ? C12 C13 C8 122.2(3) . . ? N4 C13 C8 105.2(2) . . ? C10 C9 C8 118.1(3) . . ? C10 C9 H9A 121.0 . . ? C8 C9 H9A 121.0 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C8 C9 131.9(3) . . ? N3 C8 C13 108.2(3) . . ? C9 C8 C13 119.9(3) . . ? C11 C12 C13 116.9(3) . . ? C11 C12 H12A 121.6 . . ? C13 C12 H12A 121.6 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 121.8(3) . . ? C12 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C17 C16 C15 108.5(2) . . ? C17 C16 Fe1 68.94(17) . . ? C15 C16 Fe1 72.08(16) . . ? C17 C16 H16A 125.7 . . ? C15 C16 H16A 125.7 . . ? Fe1 C16 H16A 125.7 . . ? N1 C15 C19 125.7(2) . . ? N1 C15 C16 127.3(2) . . ? C19 C15 C16 107.0(2) . . ? N1 C15 Fe1 129.3(2) . . ? C19 C15 Fe1 68.11(16) . . ? C16 C15 Fe1 67.71(16) . . ? N1 C15 U1 49.14(13) . . ? C19 C15 U1 111.56(18) . . ? C16 C15 U1 114.35(19) . . ? Fe1 C15 U1 80.18(9) . . ? C22 C21 C20 107.9(3) . . ? C22 C21 Fe1 68.98(17) . . ? C20 C21 Fe1 72.17(17) . . ? C22 C21 H21A 126.0 . . ? C20 C21 H21A 126.0 . . ? Fe1 C21 H21A 126.0 . . ? C16 C17 C18 108.0(2) . . ? C16 C17 Fe1 70.66(17) . . ? C18 C17 Fe1 69.61(17) . . ? C16 C17 H17A 126.0 . . ? C18 C17 H17A 126.0 . . ? Fe1 C17 H17A 126.0 . . ? N2 C20 C24 126.1(3) . . ? N2 C20 C21 127.2(3) . . ? C24 C20 C21 106.6(3) . . ? N2 C20 Fe1 129.7(2) . . ? C24 C20 Fe1 67.45(17) . . ? C21 C20 Fe1 67.43(16) . . ? N2 C20 U1 49.53(13) . . ? C24 C20 U1 111.53(19) . . ? C21 C20 U1 113.85(19) . . ? Fe1 C20 U1 80.18(9) . . ? C22 C23 C24 108.2(3) . . ? C22 C23 Fe1 70.01(17) . . ? C24 C23 Fe1 70.78(17) . . ? C22 C23 H23A 125.9 . . ? C24 C23 H23A 125.9 . . ? Fe1 C23 H23A 125.9 . . ? C18 C19 C15 108.3(2) . . ? C18 C19 Fe1 68.65(17) . . ? C15 C19 Fe1 71.97(16) . . ? C18 C19 H19A 125.9 . . ? C15 C19 H19A 125.9 . . ? Fe1 C19 H19A 125.9 . . ? C19 C18 C17 108.1(2) . . ? C19 C18 Fe1 70.78(16) . . ? C17 C18 Fe1 69.49(17) . . ? C19 C18 H18A 125.9 . . ? C17 C18 H18A 125.9 . . ? Fe1 C18 H18A 125.9 . . ? C21 C22 C23 108.7(3) . . ? C21 C22 Fe1 70.75(17) . . ? C23 C22 Fe1 69.31(17) . . ? C21 C22 H22A 125.7 . . ? C23 C22 H22A 125.7 . . ? Fe1 C22 H22A 125.7 . . ? C23 C24 C20 108.4(3) . . ? C23 C24 Fe1 68.65(17) . . ? C20 C24 Fe1 72.58(17) . . ? C23 C24 H24A 125.8 . . ? C20 C24 H24A 125.8 . . ? Fe1 C24 H24A 125.8 . . ? C29 C25 C30 109.4(3) . . ? C29 C25 C31 108.8(3) . . ? C30 C25 C31 108.5(3) . . ? C29 C25 Si1 110.2(2) . . ? C30 C25 Si1 109.4(2) . . ? C31 C25 Si1 110.5(2) . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C34 C36 109.2(3) . . ? C35 C34 C37 109.0(3) . . ? C36 C34 C37 108.6(3) . . ? C35 C34 Si2 109.6(2) . . ? C36 C34 Si2 110.5(2) . . ? C37 C34 Si2 109.9(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C5 C6 C2 121.9(3) . . ? C5 C6 H6A 119.1 . . ? C2 C6 H6A 119.1 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C38 C2 121.6(3) . . ? C3 C38 H38A 119.2 . . ? C2 C38 H38A 119.2 . . ? C2S C1S C5S 97.0(5) . . ? C2S C1S H1SA 112.4 . . ? C5S C1S H1SA 112.4 . . ? C2S C1S H1SB 112.4 . . ? C5S C1S H1SB 112.3 . . ? H1SA C1S H1SB 109.9 . . ? C1S C2S C3S 106.1(6) . . ? C1S C2S H2SA 110.5 . . ? C3S C2S H2SA 110.5 . . ? C1S C2S H2SB 110.5 . . ? C3S C2S H2SB 110.5 . . ? H2SA C2S H2SB 108.7 . . ? C4S C3S C2S 101.0(5) . . ? C4S C3S H3SA 111.6 . . ? C2S C3S H3SA 111.6 . . ? C4S C3S H3SB 111.6 . . ? C2S C3S H3SB 111.6 . . ? H3SA C3S H3SB 109.4 . . ? C5S C4S C3S 102.5(5) . . ? C5S C4S C6S 113.1(5) . . ? C3S C4S C6S 119.4(4) . . ? C5S C4S H4SA 107.1 . . ? C3S C4S H4SA 107.1 . . ? C6S C4S H4SA 107.1 . . ? C4S C5S C1S 111.2(5) . . ? C4S C5S H5SA 109.4 . . ? C1S C5S H5SA 109.4 . . ? C4S C5S H5SB 109.4 . . ? C1S C5S H5SB 109.4 . . ? H5SA C5S H5SB 108.0 . . ? C4S C6S H6SA 109.5 . . ? C4S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C4S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.049 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.110 #===END