# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _audit_creation_date 'Mon Jan 27 18:29:41 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hiromi Tobita' 'Masatoshi Iwata' 'Masaaki Okazaki' _publ_contact_author_name 'Prof Hiromi Tobita' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Aramaki-za-Aoba, Aoba-ku Sendai Miyagi 980-8578 JAPAN ; _publ_contact_author_email TOBITA@INORG.CHEM.TOHOKU.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; Insertion of Pyridine into an Iron Silicon Bond: Structure of the Product Cp*(CO)Fe{h3(C,C,C)-C5H5NSiMe2NPh2} ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ data_complex_3 _database_code_CSD 216673 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H36 Fe N2 O Si ' _chemical_formula_moiety 'C30 H36 Fe N2 O Si ' _chemical_formula_weight 524.56 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 17.1694(6) _cell_length_b 9.0939(4) _cell_length_c 18.5947(6) _cell_angle_alpha 90 _cell_angle_beta 109.099(2) _cell_angle_gamma 90 _cell_volume 2743.5(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 21889 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.901 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 26166 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.9965 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.9965 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6255 _reflns_number_gt 4963 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1320 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4963 _refine_ls_number_parameters 316 _refine_ls_goodness_of_fit_ref 1.412 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.79 _refine_diff_density_min -0.71 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12903(2) 0.20073(4) 0.13790(2) 0.0209(1) Uani 1.00 d . . . Si1 Si 0.33099(5) 0.01942(9) 0.32180(4) 0.0268(2) Uani 1.00 d . . . O1 O 0.2073(2) -0.0651(3) 0.1108(1) 0.0437(7) Uani 1.00 d . . . N1 N 0.3678(1) 0.1334(3) 0.4014(1) 0.0250(6) Uani 1.00 d . . . N2 N 0.2243(1) 0.0385(2) 0.2838(1) 0.0225(5) Uani 1.00 d . . . C1 C 0.3798(2) 0.0806(5) 0.2518(2) 0.0462(10) Uani 1.00 d . . . C2 C 0.3557(2) -0.1761(4) 0.3468(2) 0.0445(9) Uani 1.00 d . . . C3 C 0.4324(2) 0.2362(3) 0.4026(1) 0.0238(7) Uani 1.00 d . . . C4 C 0.4136(2) 0.3774(3) 0.3751(2) 0.0319(8) Uani 1.00 d . . . C5 C 0.4749(2) 0.4722(3) 0.3721(2) 0.0403(9) Uani 1.00 d . . . C6 C 0.5565(2) 0.4277(3) 0.3979(2) 0.0343(8) Uani 1.00 d . . . C7 C 0.5762(2) 0.2884(3) 0.4268(2) 0.0346(8) Uani 1.00 d . . . C8 C 0.5144(2) 0.1923(3) 0.4289(2) 0.0299(7) Uani 1.00 d . . . C9 C 0.3487(2) 0.1165(3) 0.4691(1) 0.0223(6) Uani 1.00 d . . . C10 C 0.3933(2) 0.1911(3) 0.5359(2) 0.0272(7) Uani 1.00 d . . . C11 C 0.3758(2) 0.1697(3) 0.6026(2) 0.0351(8) Uani 1.00 d . . . C12 C 0.3139(2) 0.0749(4) 0.6055(2) 0.0370(9) Uani 1.00 d . . . C13 C 0.2678(2) 0.0030(3) 0.5389(2) 0.0340(8) Uani 1.00 d . . . C14 C 0.2849(2) 0.0235(3) 0.4723(2) 0.0283(7) Uani 1.00 d . . . C15 C 0.1917(2) 0.1820(3) 0.2573(1) 0.0249(7) Uani 1.00 d . . . C16 C 0.1057(2) 0.2052(3) 0.2361(2) 0.0266(7) Uani 1.00 d . . . C17 C 0.0576(2) 0.0873(3) 0.1957(2) 0.0289(7) Uani 1.00 d . . . C18 C 0.0900(2) -0.0596(3) 0.2227(2) 0.0284(7) Uani 1.00 d . . . C19 C 0.1684(2) -0.0772(3) 0.2657(1) 0.0253(7) Uani 1.00 d . . . C20 C 0.1748(2) 0.0392(3) 0.1232(1) 0.0270(7) Uani 1.00 d . . . C21 C 0.0803(3) 0.4146(4) 0.1114(2) 0.047(1) Uani 1.00 d . . . C22 C 0.1627(2) 0.4163(3) 0.1181(2) 0.0400(9) Uani 1.00 d . . . C23 C 0.1745(2) 0.3195(4) 0.0646(2) 0.0350(8) Uani 1.00 d . . . C24 C 0.0966(2) 0.2548(3) 0.0229(2) 0.0358(8) Uani 1.00 d . . . C25 C 0.0375(2) 0.3153(4) 0.0521(2) 0.0468(10) Uani 1.00 d . . . C26 C 0.0417(5) 0.5153(6) 0.1550(3) 0.109(2) Uani 1.00 d . . . C27 C 0.2290(4) 0.5130(5) 0.1703(3) 0.084(2) Uani 1.00 d . . . C28 C 0.2531(3) 0.2912(6) 0.0474(3) 0.080(2) Uani 1.00 d . . . C29 C 0.0806(4) 0.1524(5) -0.0433(2) 0.092(2) Uani 1.00 d . . . C30 C -0.0530(3) 0.2888(7) 0.0269(4) 0.107(2) Uani 1.00 d . . . H1 H 0.3613 0.0204 0.2077 0.0555 Uiso 1.00 calc . . . H2 H 0.3649 0.1801 0.2380 0.0555 Uiso 1.00 calc . . . H3 H 0.4379 0.0735 0.2735 0.0555 Uiso 1.00 calc . . . H4 H 0.3337 -0.2356 0.3026 0.0545 Uiso 1.00 calc . . . H5 H 0.3316 -0.2055 0.3841 0.0545 Uiso 1.00 calc . . . H6 H 0.4135 -0.1889 0.3666 0.0545 Uiso 1.00 calc . . . H7 H 0.3578 0.4090 0.3580 0.0388 Uiso 1.00 calc . . . H8 H 0.4611 0.5684 0.3519 0.0485 Uiso 1.00 calc . . . H9 H 0.5988 0.4935 0.3958 0.0417 Uiso 1.00 calc . . . H10 H 0.6321 0.2580 0.4456 0.0414 Uiso 1.00 calc . . . H11 H 0.5283 0.0961 0.4486 0.0364 Uiso 1.00 calc . . . H12 H 0.4360 0.2570 0.5353 0.0329 Uiso 1.00 calc . . . H13 H 0.4068 0.2207 0.6475 0.0421 Uiso 1.00 calc . . . H14 H 0.3028 0.0594 0.6517 0.0444 Uiso 1.00 calc . . . H15 H 0.2243 -0.0608 0.5397 0.0406 Uiso 1.00 calc . . . H16 H 0.2531 -0.0273 0.4276 0.0340 Uiso 1.00 calc . . . H17 H 0.2291 0.2570 0.2830 0.0413 Uiso 1.00 calc . . . H18 H 0.0794 0.2943 0.2425 0.0413 Uiso 1.00 calc . . . H19 H 0.0011 0.1005 0.1731 0.0413 Uiso 1.00 calc . . . H20 H 0.0546 -0.1431 0.2092 0.0346 Uiso 1.00 calc . . . H21 H 0.1868 -0.1726 0.2851 0.0303 Uiso 1.00 calc . . . H22 H 0.0493 0.6155 0.1429 0.1131 Uiso 1.00 calc . . . H23 H -0.0157 0.4959 0.1412 0.1131 Uiso 1.00 calc . . . H24 H 0.0669 0.5010 0.2081 0.1131 Uiso 1.00 calc . . . H25 H 0.2511 0.5762 0.1396 0.0992 Uiso 1.00 calc . . . H26 H 0.2091 0.5693 0.2018 0.0992 Uiso 1.00 calc . . . H27 H 0.2741 0.4521 0.2002 0.0992 Uiso 1.00 calc . . . H28 H 0.2457 0.3177 -0.0042 0.0921 Uiso 1.00 calc . . . H29 H 0.2971 0.3427 0.0806 0.0921 Uiso 1.00 calc . . . H30 H 0.2649 0.1866 0.0523 0.0921 Uiso 1.00 calc . . . H31 H 0.0440 0.1981 -0.0874 0.1051 Uiso 1.00 calc . . . H32 H 0.1300 0.1267 -0.0511 0.1051 Uiso 1.00 calc . . . H33 H 0.0542 0.0652 -0.0328 0.1051 Uiso 1.00 calc . . . H34 H -0.0817 0.3790 0.0094 0.1207 Uiso 1.00 calc . . . H35 H -0.0680 0.2195 -0.0136 0.1207 Uiso 1.00 calc . . . H36 H -0.0687 0.2523 0.0681 0.1207 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0203(2) 0.0222(2) 0.0206(2) 0.0001(1) 0.0073(1) 0.0030(1) Si1 0.0201(4) 0.0353(4) 0.0226(4) 0.0016(3) 0.0036(3) -0.0065(3) O1 0.062(2) 0.039(1) 0.029(1) 0.018(1) 0.014(1) -0.0039(9) N1 0.021(1) 0.031(1) 0.022(1) -0.0032(10) 0.0054(9) -0.0034(9) N2 0.021(1) 0.022(1) 0.020(1) 0.0008(9) 0.0024(8) 0.0005(8) C1 0.031(2) 0.081(3) 0.029(2) -0.009(2) 0.013(1) -0.015(2) C2 0.031(2) 0.039(2) 0.051(2) 0.014(1) -0.003(1) -0.013(1) C3 0.021(1) 0.027(1) 0.022(1) 0.000(1) 0.006(1) -0.0026(10) C4 0.023(1) 0.030(2) 0.039(2) 0.010(1) 0.006(1) 0.002(1) C5 0.037(2) 0.026(2) 0.055(2) 0.005(1) 0.011(1) 0.009(1) C6 0.030(2) 0.030(2) 0.043(2) -0.004(1) 0.011(1) 0.002(1) C7 0.022(1) 0.036(2) 0.044(2) 0.005(1) 0.008(1) 0.001(1) C8 0.023(1) 0.025(1) 0.037(2) 0.004(1) 0.003(1) 0.005(1) C9 0.021(1) 0.020(1) 0.025(1) 0.005(1) 0.0058(10) 0.0006(10) C10 0.025(1) 0.027(1) 0.027(1) -0.001(1) 0.006(1) -0.006(1) C11 0.041(2) 0.038(2) 0.026(1) 0.000(1) 0.010(1) -0.010(1) C12 0.045(2) 0.045(2) 0.025(1) -0.002(1) 0.017(1) -0.004(1) C13 0.034(2) 0.039(2) 0.032(2) -0.004(1) 0.014(1) -0.002(1) C14 0.027(1) 0.030(1) 0.025(1) 0.000(1) 0.004(1) -0.001(1) C15 0.027(1) 0.023(1) 0.023(1) -0.002(1) 0.006(1) -0.0017(10) C16 0.030(1) 0.029(1) 0.025(1) 0.007(1) 0.013(1) 0.007(1) C17 0.021(1) 0.036(2) 0.029(1) 0.000(1) 0.007(1) 0.010(1) C18 0.027(1) 0.029(1) 0.026(1) -0.008(1) 0.003(1) 0.005(1) C19 0.029(1) 0.024(1) 0.022(1) -0.002(1) 0.005(1) 0.0038(10) C20 0.035(2) 0.029(1) 0.015(1) 0.000(1) 0.006(1) 0.0012(10) C21 0.073(3) 0.033(2) 0.050(2) 0.022(2) 0.040(2) 0.022(1) C22 0.062(2) 0.030(2) 0.027(2) -0.014(2) 0.013(1) 0.005(1) C23 0.032(2) 0.047(2) 0.029(1) 0.000(1) 0.014(1) 0.015(1) C24 0.048(2) 0.027(1) 0.024(1) -0.001(1) 0.000(1) 0.005(1) C25 0.022(2) 0.054(2) 0.060(2) 0.004(1) 0.006(1) 0.042(2) C26 0.187(6) 0.085(4) 0.098(4) 0.096(4) 0.104(4) 0.065(3) C27 0.133(5) 0.047(2) 0.049(2) -0.045(3) -0.003(3) 0.005(2) C28 0.053(3) 0.126(4) 0.080(3) 0.021(3) 0.047(2) 0.053(3) C29 0.187(6) 0.044(2) 0.021(2) 0.009(3) 0.000(2) 0.003(2) C30 0.030(2) 0.127(5) 0.138(5) -0.006(3) -0.006(3) 0.106(4) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag FE1 C15 2.134(3) . . yes FE1 C16 1.995(3) . . yes FE1 C17 2.141(3) . . yes FE1 C20 1.730(3) . . yes FE1 C21 2.111(3) . . yes FE1 C22 2.110(3) . . yes FE1 C23 2.082(3) . . yes FE1 C24 2.085(3) . . yes FE1 C25 2.112(3) . . yes SI1 N1 1.747(2) . . yes SI1 N2 1.742(2) . . yes SI1 C1 1.850(4) . . yes SI1 C2 1.852(4) . . yes O1 C20 1.161(4) . . yes N1 C3 1.444(4) . . yes N1 C9 1.410(4) . . yes N2 C15 1.442(3) . . yes N2 C19 1.390(3) . . yes C3 C4 1.381(4) . . yes C3 C8 1.389(4) . . yes C4 C5 1.375(4) . . yes C5 C6 1.385(4) . . yes C6 C7 1.375(4) . . yes C7 C8 1.386(4) . . yes C9 C10 1.402(4) . . yes C9 C14 1.400(4) . . yes C10 C11 1.383(4) . . yes C11 C12 1.382(5) . . yes C12 C13 1.394(4) . . yes C13 C14 1.376(4) . . yes C15 C16 1.413(4) . . yes C16 C17 1.412(4) . . yes C17 C18 1.471(4) . . yes C18 C19 1.332(4) . . yes C21 C22 1.380(5) . . yes C21 C25 1.429(6) . . yes C21 C26 1.511(6) . . yes C22 C23 1.393(5) . . yes C22 C27 1.512(5) . . yes C23 C24 1.435(4) . . yes C23 C28 1.506(5) . . yes C24 C25 1.410(5) . . yes C24 C29 1.495(5) . . yes C25 C30 1.489(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 FE1 C16 39.8(1) . . . yes C15 FE1 C17 67.4(1) . . . yes C15 FE1 C20 89.8(1) . . . yes C15 FE1 C21 110.0(1) . . . yes C15 FE1 C22 100.5(1) . . . yes C15 FE1 C23 123.6(1) . . . yes C15 FE1 C24 163.9(1) . . . yes C15 FE1 C25 145.3(1) . . . yes C16 FE1 C17 39.7(1) . . . yes C16 FE1 C20 113.6(1) . . . yes C16 FE1 C21 90.7(1) . . . yes C16 FE1 C22 106.8(1) . . . yes C16 FE1 C23 145.1(1) . . . yes C16 FE1 C24 150.3(1) . . . yes C16 FE1 C25 111.1(1) . . . yes C17 FE1 C20 92.0(1) . . . yes C17 FE1 C21 108.2(1) . . . yes C17 FE1 C22 140.3(1) . . . yes C17 FE1 C23 167.9(1) . . . yes C17 FE1 C24 128.6(1) . . . yes C17 FE1 C25 102.1(1) . . . yes C20 FE1 C21 155.8(1) . . . yes C20 FE1 C22 126.6(1) . . . yes C20 FE1 C23 92.9(1) . . . yes C20 FE1 C24 91.2(1) . . . yes C20 FE1 C25 124.3(2) . . . yes C21 FE1 C22 38.2(1) . . . yes C21 FE1 C23 64.8(1) . . . yes C21 FE1 C24 65.9(1) . . . yes C21 FE1 C25 39.6(2) . . . yes C22 FE1 C23 38.8(1) . . . yes C22 FE1 C24 66.3(1) . . . yes C22 FE1 C25 65.7(1) . . . yes C23 FE1 C24 40.3(1) . . . yes C23 FE1 C25 66.1(1) . . . yes C24 FE1 C25 39.2(1) . . . yes N1 SI1 N2 109.0(1) . . . yes N1 SI1 C1 107.2(1) . . . yes N1 SI1 C2 111.6(1) . . . yes N2 SI1 C1 110.0(1) . . . yes N2 SI1 C2 108.8(1) . . . yes C1 SI1 C2 110.2(2) . . . yes SI1 N1 C3 117.5(2) . . . yes SI1 N1 C9 124.5(2) . . . yes C3 N1 C9 117.3(2) . . . yes SI1 N2 C15 118.0(2) . . . yes SI1 N2 C19 125.0(2) . . . yes C15 N2 C19 116.3(2) . . . yes N1 C3 C4 120.7(2) . . . yes N1 C3 C8 120.2(3) . . . yes C4 C3 C8 119.0(3) . . . yes C3 C4 C5 120.6(3) . . . yes C4 C5 C6 120.3(3) . . . yes C5 C6 C7 119.7(3) . . . yes C6 C7 C8 120.0(3) . . . yes C3 C8 C7 120.4(3) . . . yes N1 C9 C10 121.3(2) . . . yes N1 C9 C14 121.2(2) . . . yes C10 C9 C14 117.5(3) . . . yes C9 C10 C11 120.7(3) . . . yes C10 C11 C12 121.1(3) . . . yes C11 C12 C13 118.6(3) . . . yes C12 C13 C14 120.6(3) . . . yes C9 C14 C13 121.4(3) . . . yes FE1 C15 N2 115.7(2) . . . yes FE1 C15 C16 64.8(1) . . . yes N2 C15 C16 119.0(2) . . . yes FE1 C16 C15 75.4(2) . . . yes FE1 C16 C17 75.8(2) . . . yes C15 C16 C17 114.3(2) . . . yes FE1 C17 C16 64.5(2) . . . yes FE1 C17 C18 113.2(2) . . . yes C16 C17 C18 114.7(2) . . . yes C17 C18 C19 120.6(2) . . . yes N2 C19 C18 122.5(2) . . . yes FE1 C20 O1 176.3(3) . . . yes FE1 C21 C22 70.9(2) . . . yes FE1 C21 C25 70.3(2) . . . yes FE1 C21 C26 130.0(2) . . . yes C22 C21 C25 109.2(3) . . . yes C22 C21 C26 124.1(5) . . . yes C25 C21 C26 126.3(5) . . . yes FE1 C22 C21 70.9(2) . . . yes FE1 C22 C23 69.5(2) . . . yes FE1 C22 C27 128.3(2) . . . yes C21 C22 C23 108.3(3) . . . yes C21 C22 C27 126.8(4) . . . yes C23 C22 C27 124.9(4) . . . yes FE1 C23 C22 71.7(2) . . . yes FE1 C23 C24 70.0(2) . . . yes FE1 C23 C28 127.2(2) . . . yes C22 C23 C24 108.5(3) . . . yes C22 C23 C28 127.6(4) . . . yes C24 C23 C28 123.8(4) . . . yes FE1 C24 C23 69.7(2) . . . yes FE1 C24 C25 71.4(2) . . . yes FE1 C24 C29 127.8(2) . . . yes C23 C24 C25 107.1(3) . . . yes C23 C24 C29 126.0(4) . . . yes C25 C24 C29 126.8(4) . . . yes FE1 C25 C21 70.2(2) . . . yes FE1 C25 C24 69.3(2) . . . yes FE1 C25 C30 126.9(2) . . . yes C21 C25 C24 106.9(3) . . . yes C21 C25 C30 124.4(5) . . . yes C24 C25 C30 128.6(5) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_complex_2 _database_code_CSD 216674 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H36 Fe N2 O Si ' _chemical_formula_moiety 'C30 H36 Fe N2 O Si ' _chemical_formula_weight 524.56 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.4245(4) _cell_length_b 16.9079(5) _cell_length_c 13.8660(3) _cell_angle_alpha 90 _cell_angle_beta 92.431(2) _cell_angle_gamma 90 _cell_volume 2676.0(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24561 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.866 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 25124 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.40 _diffrn_measured_fraction_theta_max 0.9984 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6079 _reflns_number_gt 5370 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.1193 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6079 _refine_ls_number_parameters 316 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0008 _refine_diff_density_max 0.25 _refine_diff_density_min -0.51 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.18326(2) 0.04146(1) 0.30258(1) 0.02087(7) Uani 1.00 d . . . Si Si 0.19183(3) 0.12573(2) 0.16984(3) 0.0229(1) Uani 1.00 d . . . O O -0.0619(1) 0.08089(8) 0.28438(10) 0.0429(4) Uani 1.00 d . . . N1 N 0.3241(1) 0.12839(8) 0.10393(9) 0.0288(3) Uani 1.00 d . . . N2 N 0.2374(1) 0.12533(7) 0.39481(9) 0.0262(3) Uani 1.00 d . . . C1 C 0.1557(2) 0.23276(9) 0.1979(1) 0.0352(4) Uani 1.00 d . . . C2 C 0.0764(2) 0.1020(1) 0.0728(1) 0.0380(4) Uani 1.00 d . . . C3 C 0.4369(1) 0.13645(9) 0.1488(1) 0.0298(4) Uani 1.00 d . . . C4 C 0.5338(2) 0.0992(1) 0.1087(1) 0.0368(4) Uani 1.00 d . . . C5 C 0.6440(2) 0.1049(1) 0.1552(2) 0.0424(5) Uani 1.00 d . . . C6 C 0.6606(2) 0.1460(1) 0.2392(2) 0.0450(5) Uani 1.00 d . . . C7 C 0.5669(2) 0.1840(1) 0.2786(2) 0.0459(5) Uani 1.00 d . . . C8 C 0.4556(1) 0.1796(1) 0.2331(1) 0.0382(4) Uani 1.00 d . . . C9 C 0.3221(1) 0.1419(1) 0.0017(1) 0.0341(4) Uani 1.00 d . . . C10 C 0.3573(2) 0.2147(1) -0.0337(2) 0.0540(6) Uani 1.00 d . . . C11 C 0.3590(2) 0.2279(2) -0.1321(2) 0.0696(8) Uani 1.00 d . . . C12 C 0.3239(2) 0.1712(2) -0.1959(2) 0.0676(8) Uani 1.00 d . . . C13 C 0.2879(2) 0.0989(2) -0.1634(1) 0.0626(7) Uani 1.00 d . . . C14 C 0.2886(2) 0.0846(1) -0.0637(1) 0.0493(6) Uani 1.00 d . . . C15 C 0.0388(1) 0.06942(10) 0.2930(1) 0.0294(4) Uani 1.00 d . . . C16 C 0.3500(2) 0.1315(1) 0.4288(1) 0.0357(4) Uani 1.00 d . . . C17 C 0.3878(2) 0.1864(1) 0.4974(1) 0.0418(5) Uani 1.00 d . . . C18 C 0.3094(2) 0.2394(1) 0.5336(1) 0.0406(5) Uani 1.00 d . . . C19 C 0.1943(2) 0.2353(1) 0.4994(1) 0.0400(5) Uani 1.00 d . . . C20 C 0.1624(1) 0.17823(10) 0.4314(1) 0.0318(4) Uani 1.00 d . . . C21 C 0.1436(1) -0.07294(9) 0.2497(1) 0.0293(4) Uani 1.00 d . . . C22 C 0.2616(1) -0.05598(8) 0.2306(1) 0.0272(4) Uani 1.00 d . . . C23 C 0.3239(1) -0.04294(8) 0.3200(1) 0.0258(4) Uani 1.00 d . . . C24 C 0.2425(1) -0.05359(9) 0.3954(1) 0.0275(4) Uani 1.00 d . . . C25 C 0.1321(1) -0.07226(9) 0.3521(1) 0.0303(4) Uani 1.00 d . . . C26 C 0.0503(2) -0.0981(1) 0.1767(2) 0.0494(5) Uani 1.00 d . . . C27 C 0.3187(2) -0.06576(10) 0.1362(1) 0.0403(5) Uani 1.00 d . . . C28 C 0.4549(2) -0.0368(1) 0.3315(1) 0.0386(5) Uani 1.00 d . . . C29 C 0.2736(2) -0.0513(1) 0.5016(1) 0.0418(5) Uani 1.00 d . . . C30 C 0.0229(2) -0.0933(1) 0.4027(2) 0.0486(6) Uani 1.00 d . . . H1 H 0.2028 0.2566 0.2475 0.0436 Uiso 1.00 calc . . . H2 H 0.1681 0.2642 0.1439 0.0436 Uiso 1.00 calc . . . H3 H 0.0700 0.2327 0.2136 0.0436 Uiso 1.00 calc . . . H4 H -0.0022 0.0982 0.1037 0.0463 Uiso 1.00 calc . . . H5 H 0.0812 0.1344 0.0279 0.0463 Uiso 1.00 calc . . . H6 H 0.0911 0.0465 0.0417 0.0463 Uiso 1.00 calc . . . H7 H 0.5237 0.0666 0.0538 0.0441 Uiso 1.00 calc . . . H8 H 0.7031 0.0807 0.1237 0.0507 Uiso 1.00 calc . . . H9 H 0.7261 0.1471 0.2687 0.0538 Uiso 1.00 calc . . . H10 H 0.5780 0.2107 0.3361 0.0560 Uiso 1.00 calc . . . H11 H 0.3923 0.2060 0.2647 0.0457 Uiso 1.00 calc . . . H12 H 0.3732 0.2567 0.0084 0.0670 Uiso 1.00 calc . . . H13 H 0.3848 0.2718 -0.1580 0.0814 Uiso 1.00 calc . . . H14 H 0.3161 0.1893 -0.2702 0.0811 Uiso 1.00 calc . . . H15 H 0.2702 0.0473 -0.2017 0.0742 Uiso 1.00 calc . . . H16 H 0.2564 0.0284 -0.0405 0.0616 Uiso 1.00 calc . . . H17 H 0.4031 0.0970 0.3913 0.0416 Uiso 1.00 calc . . . H18 H 0.4715 0.1858 0.5155 0.0505 Uiso 1.00 calc . . . H19 H 0.3322 0.2821 0.5807 0.0484 Uiso 1.00 calc . . . H20 H 0.1347 0.2713 0.5200 0.0484 Uiso 1.00 calc . . . H21 H 0.0762 0.1770 0.4012 0.0381 Uiso 1.00 calc . . . H22 H -0.0169 -0.0830 0.1873 0.0613 Uiso 1.00 calc . . . H23 H 0.0689 -0.0775 0.1088 0.0613 Uiso 1.00 calc . . . H24 H 0.0357 -0.1566 0.1732 0.0613 Uiso 1.00 calc . . . H25 H 0.3558 -0.1113 0.1344 0.0507 Uiso 1.00 calc . . . H26 H 0.2532 -0.0618 0.0856 0.0507 Uiso 1.00 calc . . . H27 H 0.3636 -0.0253 0.1228 0.0507 Uiso 1.00 calc . . . H28 H 0.4903 -0.0866 0.3091 0.0473 Uiso 1.00 calc . . . H29 H 0.4856 0.0037 0.2875 0.0473 Uiso 1.00 calc . . . H30 H 0.4745 -0.0260 0.3949 0.0473 Uiso 1.00 calc . . . H31 H 0.3097 -0.0967 0.5231 0.0517 Uiso 1.00 calc . . . H32 H 0.3187 -0.0079 0.5225 0.0517 Uiso 1.00 calc . . . H33 H 0.2070 -0.0418 0.5379 0.0517 Uiso 1.00 calc . . . H34 H 0.0247 -0.0777 0.4644 0.0600 Uiso 1.00 calc . . . H35 H -0.0527 -0.0698 0.3689 0.0600 Uiso 1.00 calc . . . H36 H 0.0029 -0.1490 0.4022 0.0600 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe 0.0195(1) 0.0204(1) 0.0226(1) 0.00185(7) -0.00167(9) -0.00094(7) Si 0.0228(2) 0.0206(2) 0.0248(2) 0.0011(1) -0.0040(1) 0.0003(1) O 0.0218(6) 0.0494(8) 0.0573(8) 0.0064(5) -0.0007(5) -0.0018(6) N1 0.0276(7) 0.0282(6) 0.0304(6) -0.0022(5) 0.0005(5) 0.0025(5) N2 0.0287(6) 0.0253(6) 0.0246(6) 0.0019(5) -0.0012(5) 0.0007(5) C1 0.0410(9) 0.0253(7) 0.0394(8) 0.0083(7) 0.0008(7) 0.0024(7) C2 0.0349(9) 0.0471(10) 0.0308(8) -0.0056(7) -0.0100(6) 0.0063(7) C3 0.0247(7) 0.0233(7) 0.0414(8) -0.0018(6) 0.0024(6) 0.0057(6) C4 0.0337(9) 0.0305(8) 0.0468(9) 0.0013(7) 0.0092(7) 0.0052(7) C5 0.0298(9) 0.0333(8) 0.065(1) 0.0032(7) 0.0102(8) 0.0115(8) C6 0.0270(8) 0.0381(9) 0.069(1) -0.0009(7) -0.0064(8) 0.0108(9) C7 0.0340(9) 0.044(1) 0.059(1) -0.0014(8) -0.0100(8) -0.0075(9) C8 0.0273(8) 0.0350(9) 0.0521(10) 0.0020(7) -0.0022(7) -0.0056(7) C9 0.0331(8) 0.0345(8) 0.0350(8) 0.0034(7) 0.0042(6) 0.0133(7) C10 0.044(1) 0.050(1) 0.067(1) -0.0146(9) -0.0146(9) 0.032(1) C11 0.045(1) 0.091(2) 0.072(2) -0.016(1) -0.011(1) 0.058(2) C12 0.049(1) 0.108(2) 0.046(1) 0.023(1) 0.0132(10) 0.045(1) C13 0.092(2) 0.065(1) 0.0310(9) 0.032(1) 0.012(1) 0.0096(9) C14 0.079(2) 0.0388(10) 0.0309(9) 0.0122(10) 0.0090(9) 0.0069(7) C15 0.0274(8) 0.0281(7) 0.0328(8) 0.0020(6) 0.0013(6) -0.0004(6) C16 0.0327(9) 0.0341(8) 0.0394(8) 0.0029(7) -0.0083(7) -0.0056(7) C17 0.044(1) 0.0387(9) 0.0414(9) -0.0039(8) -0.0142(8) -0.0060(7) C18 0.059(1) 0.0325(8) 0.0299(8) -0.0090(8) -0.0019(7) -0.0062(7) C19 0.053(1) 0.0316(8) 0.0363(9) -0.0014(8) 0.0116(8) -0.0075(7) C20 0.0341(8) 0.0293(8) 0.0322(7) -0.0006(6) 0.0049(6) -0.0044(6) C21 0.0350(8) 0.0206(7) 0.0315(8) -0.0040(6) -0.0094(6) 0.0017(6) C22 0.0380(8) 0.0158(6) 0.0277(7) 0.0021(6) 0.0017(6) -0.0001(5) C23 0.0258(8) 0.0203(7) 0.0311(7) 0.0044(5) 0.0003(6) 0.0023(5) C24 0.0320(8) 0.0249(7) 0.0256(7) 0.0033(6) -0.0014(6) 0.0036(6) C25 0.0288(8) 0.0261(7) 0.0359(8) -0.0007(6) 0.0020(6) 0.0065(6) C26 0.056(1) 0.0338(9) 0.055(1) -0.0131(8) -0.0270(9) 0.0019(8) C27 0.065(1) 0.0221(7) 0.0345(8) 0.0044(8) 0.0145(8) -0.0012(6) C28 0.0261(8) 0.0341(9) 0.055(1) 0.0059(6) 0.0006(7) 0.0029(7) C29 0.053(1) 0.047(1) 0.0259(8) 0.0074(8) -0.0029(7) 0.0060(7) C30 0.0377(10) 0.046(1) 0.063(1) -0.0062(8) 0.0115(9) 0.0175(9) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag FE SI 2.3330(4) . . yes FE N2 1.991(1) . . yes FE C15 1.716(2) . . yes FE C21 2.111(2) . . yes FE C22 2.142(2) . . yes FE C23 2.155(1) . . yes FE C24 2.150(2) . . yes FE C25 2.132(2) . . yes SI N1 1.799(1) . . yes SI C1 1.900(2) . . yes SI C2 1.888(2) . . yes O C15 1.168(2) . . yes N1 C3 1.413(2) . . yes N1 C9 1.435(2) . . yes N2 C16 1.355(2) . . yes N2 C20 1.352(2) . . yes C3 C4 1.408(2) . . yes C3 C8 1.387(2) . . yes C4 C5 1.393(3) . . yes C5 C6 1.362(3) . . yes C6 C7 1.381(3) . . yes C7 C8 1.397(2) . . yes C9 C10 1.391(3) . . yes C9 C14 1.370(3) . . yes C10 C11 1.383(3) . . yes C11 C12 1.353(4) . . yes C12 C13 1.372(4) . . yes C13 C14 1.403(3) . . yes C16 C17 1.385(2) . . yes C17 C18 1.377(3) . . yes C18 C19 1.380(3) . . yes C19 C20 1.388(2) . . yes C21 C22 1.415(2) . . yes C21 C25 1.432(2) . . yes C21 C26 1.500(2) . . yes C22 C23 1.421(2) . . yes C22 C27 1.496(2) . . yes C23 C24 1.440(2) . . yes C23 C28 1.501(2) . . yes C24 C25 1.410(2) . . yes C24 C29 1.500(2) . . yes C25 C30 1.500(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag SI FE N2 92.84(4) . . . yes SI FE C15 80.97(5) . . . yes SI FE C21 107.53(4) . . . yes SI FE C22 93.99(4) . . . yes SI FE C23 115.89(4) . . . yes SI FE C24 154.95(5) . . . yes SI FE C25 145.72(5) . . . yes N2 FE C15 97.20(6) . . . yes N2 FE C21 158.79(5) . . . yes N2 FE C22 136.27(6) . . . yes N2 FE C23 100.93(5) . . . yes N2 FE C24 93.81(6) . . . yes N2 FE C25 121.17(6) . . . yes C15 FE C21 91.94(7) . . . yes C15 FE C22 126.53(7) . . . yes C15 FE C23 154.30(7) . . . yes C15 FE C24 121.98(7) . . . yes C15 FE C25 89.87(7) . . . yes C21 FE C22 38.86(6) . . . yes C21 FE C23 65.19(6) . . . yes C21 FE C24 65.20(6) . . . yes C21 FE C25 39.44(6) . . . yes C22 FE C23 38.60(6) . . . yes C22 FE C24 64.97(6) . . . yes C22 FE C25 65.31(6) . . . yes C23 FE C24 39.07(6) . . . yes C23 FE C25 65.16(6) . . . yes C24 FE C25 38.43(6) . . . yes FE SI N1 118.70(5) . . . yes FE SI C1 113.78(5) . . . yes FE SI C2 112.41(6) . . . yes N1 SI C1 105.95(7) . . . yes N1 SI C2 102.69(7) . . . yes C1 SI C2 101.40(8) . . . yes SI N1 C3 123.3(1) . . . yes SI N1 C9 121.8(1) . . . yes C3 N1 C9 113.3(1) . . . yes FE N2 C16 122.9(1) . . . yes FE N2 C20 121.8(1) . . . yes C16 N2 C20 115.2(1) . . . yes N1 C3 C4 120.1(2) . . . yes N1 C3 C8 121.8(1) . . . yes C4 C3 C8 118.1(2) . . . yes C3 C4 C5 119.8(2) . . . yes C4 C5 C6 121.4(2) . . . yes C5 C6 C7 119.5(2) . . . yes C6 C7 C8 120.2(2) . . . yes C3 C8 C7 120.9(2) . . . yes N1 C9 C10 119.8(2) . . . yes N1 C9 C14 122.3(1) . . . yes C10 C9 C14 117.9(2) . . . yes C9 C10 C11 120.6(2) . . . yes C10 C11 C12 120.9(2) . . . yes C11 C12 C13 120.1(2) . . . yes C12 C13 C14 119.2(2) . . . yes C9 C14 C13 121.4(2) . . . yes FE C15 O 173.4(1) . . . yes N2 C16 C17 123.7(2) . . . yes C16 C17 C18 119.9(2) . . . yes C17 C18 C19 117.9(2) . . . yes C18 C19 C20 119.1(2) . . . yes N2 C20 C19 124.3(2) . . . yes FE C21 C22 71.76(8) . . . yes FE C21 C25 71.06(9) . . . yes FE C21 C26 129.1(1) . . . yes C22 C21 C25 108.2(1) . . . yes C22 C21 C26 125.9(2) . . . yes C25 C21 C26 125.4(2) . . . yes FE C22 C21 69.38(9) . . . yes FE C22 C23 71.19(8) . . . yes FE C22 C27 134.4(1) . . . yes C21 C22 C23 108.3(1) . . . yes C21 C22 C27 126.6(2) . . . yes C23 C22 C27 124.1(2) . . . yes FE C23 C22 70.20(9) . . . yes FE C23 C24 70.28(9) . . . yes FE C23 C28 134.5(1) . . . yes C22 C23 C24 107.4(1) . . . yes C22 C23 C28 124.3(2) . . . yes C24 C23 C28 127.1(2) . . . yes FE C24 C23 70.65(8) . . . yes FE C24 C25 70.07(9) . . . yes FE C24 C29 128.5(1) . . . yes C23 C24 C25 108.2(1) . . . yes C23 C24 C29 125.2(2) . . . yes C25 C24 C29 126.4(2) . . . yes FE C25 C21 69.50(8) . . . yes FE C25 C24 71.49(9) . . . yes FE C25 C30 127.5(1) . . . yes C21 C25 C24 107.8(1) . . . yes C21 C25 C30 125.1(2) . . . yes C24 C25 C30 127.0(2) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------