Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email TOBITA@INORG.CHEM.TOHOKU.AC.JP _publ_contact_author_name 'Prof Hiromi Tobita' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name H.Tobita M.Iwata H.Ogino M.Okazaki data_of_1-Ph _database_code_CSD 200912 _audit_creation_date 'Tue Jan 28 13:58:04 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H39 Fe N O3 Si ' _chemical_formula_moiety 'C30 H39 Fe N O3 Si ' _chemical_formula_weight 545.58 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.4866(8) _cell_length_b 9.4172(5) _cell_length_c 17.867(2) _cell_angle_alpha 96.519(5) _cell_angle_beta 97.382(3) _cell_angle_gamma 93.474(1) _cell_volume 1402.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7442 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.931 #------------------------------------------------------------------------------ # 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 11070 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.8564 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.8564 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # 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 5470 _reflns_number_gt 4806 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1798 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5470 _refine_ls_number_parameters 325 _refine_ls_goodness_of_fit_ref 1.630 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.09500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0012 _refine_diff_density_max 0.28 _refine_diff_density_min -0.61 _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) ; Si Si 0.082 0.070 ;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) ; #------------------------------------------------------------------------------ # 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 -0.43767(4) 0.21113(4) -0.14189(2) 0.0174(1) Uani 1.00 d . . . Si Si -0.14590(9) -0.32214(8) -0.35739(4) 0.0182(2) Uani 1.00 d . . . O1 O -0.1498(2) -0.2997(2) -0.2644(1) 0.0219(5) Uani 1.00 d . . . O2 O -0.3742(3) 0.2179(3) -0.2975(1) 0.0348(7) Uani 1.00 d . . . O3 O -0.6562(3) -0.0446(3) -0.1691(1) 0.0376(7) Uani 1.00 d . . . N N 0.0360(3) -0.3878(2) -0.3762(1) 0.0184(6) Uani 1.00 d . . . C1 C -0.2441(3) 0.0909(3) -0.1216(2) 0.0206(7) Uani 1.00 d . . . C2 C -0.2166(4) -0.0303(3) -0.1819(2) 0.0232(7) Uani 1.00 d . . . C3 C -0.0843(4) -0.1208(3) -0.1530(2) 0.0223(7) Uani 1.00 d . . . C4 C -0.0217(4) -0.2124(3) -0.2165(2) 0.0245(7) Uani 1.00 d . . . C5 C -0.1589(4) -0.1478(3) -0.3954(2) 0.0258(8) Uani 1.00 d . . . C6 C -0.3201(4) -0.4467(3) -0.3976(2) 0.0267(8) Uani 1.00 d . . . C7 C 0.1584(3) -0.2917(3) -0.3958(1) 0.0182(6) Uani 1.00 d . . . C8 C 0.1516(4) -0.2532(3) -0.4691(2) 0.0258(7) Uani 1.00 d . . . C9 C 0.2691(4) -0.1589(4) -0.4865(2) 0.0316(8) Uani 1.00 d . . . C10 C 0.3936(4) -0.1024(3) -0.4312(2) 0.0299(8) Uani 1.00 d . . . C11 C 0.4021(4) -0.1406(3) -0.3585(2) 0.0257(7) Uani 1.00 d . . . C12 C 0.2845(3) -0.2350(3) -0.3406(2) 0.0215(7) Uani 1.00 d . . . C13 C 0.0815(3) -0.5261(3) -0.3638(2) 0.0204(7) Uani 1.00 d . . . C14 C 0.2131(4) -0.5811(3) -0.3928(2) 0.0240(7) Uani 1.00 d . . . C15 C 0.2520(4) -0.7193(3) -0.3829(2) 0.0318(8) Uani 1.00 d . . . C16 C 0.1629(4) -0.8060(3) -0.3441(2) 0.0357(9) Uani 1.00 d . . . C17 C 0.0332(4) -0.7524(3) -0.3151(2) 0.0335(9) Uani 1.00 d . . . C18 C -0.0069(4) -0.6136(3) -0.3232(2) 0.0259(8) Uani 1.00 d . . . C19 C -0.3989(3) 0.2141(3) -0.2359(2) 0.0227(7) Uani 1.00 d . . . C20 C -0.5655(3) 0.0550(3) -0.1601(2) 0.0237(7) Uani 1.00 d . . . C21 C -0.6076(4) 0.3405(3) -0.0984(2) 0.0252(7) Uani 1.00 d . . . C22 C -0.4995(4) 0.4257(3) -0.1325(2) 0.0236(7) Uani 1.00 d . . . C23 C -0.3418(3) 0.4172(3) -0.0928(2) 0.0215(7) Uani 1.00 d . . . C24 C -0.3559(3) 0.3298(3) -0.0333(1) 0.0202(7) Uani 1.00 d . . . C25 C -0.5180(4) 0.2800(3) -0.0375(2) 0.0224(7) Uani 1.00 d . . . C26 C -0.7858(4) 0.3219(4) -0.1181(2) 0.0395(10) Uani 1.00 d . . . C27 C -0.5418(5) 0.5154(4) -0.1955(2) 0.0387(10) Uani 1.00 d . . . C28 C -0.1911(4) 0.4932(3) -0.1070(2) 0.0338(9) Uani 1.00 d . . . C29 C -0.2251(4) 0.3002(3) 0.0262(2) 0.0318(8) Uani 1.00 d . . . C30 C -0.5871(4) 0.1905(3) 0.0158(2) 0.0354(9) Uani 1.00 d . . . H1 H -0.1419 0.1567 -0.1141 0.0249 Uiso 1.00 calc . . . H2 H -0.2664 0.0503 -0.0745 0.0249 Uiso 1.00 calc . . . H3 H -0.3249 -0.0970 -0.1984 0.0283 Uiso 1.00 calc . . . H4 H -0.1865 0.0109 -0.2257 0.0283 Uiso 1.00 calc . . . H5 H 0.0090 -0.0596 -0.1253 0.0262 Uiso 1.00 calc . . . H6 H -0.1271 -0.1866 -0.1175 0.0262 Uiso 1.00 calc . . . H7 H 0.0536 -0.2783 -0.1961 0.0310 Uiso 1.00 calc . . . H8 H 0.0374 -0.1538 -0.2470 0.0310 Uiso 1.00 calc . . . H9 H -0.0784 -0.0911 -0.3769 0.0324 Uiso 1.00 calc . . . H10 H -0.1718 -0.1656 -0.4469 0.0324 Uiso 1.00 calc . . . H11 H -0.2512 -0.1139 -0.3840 0.0324 Uiso 1.00 calc . . . H12 H -0.4121 -0.4012 -0.3916 0.0325 Uiso 1.00 calc . . . H13 H -0.3379 -0.4472 -0.4381 0.0325 Uiso 1.00 calc . . . H14 H -0.3267 -0.5198 -0.3802 0.0325 Uiso 1.00 calc . . . H15 H 0.0701 -0.2934 -0.5058 0.0306 Uiso 1.00 calc . . . H16 H 0.2657 -0.1423 -0.5300 0.0371 Uiso 1.00 calc . . . H17 H 0.4637 -0.0448 -0.4391 0.0348 Uiso 1.00 calc . . . H18 H 0.4894 -0.0987 -0.3197 0.0312 Uiso 1.00 calc . . . H19 H 0.2899 -0.2564 -0.2876 0.0263 Uiso 1.00 calc . . . H20 H 0.2800 -0.5224 -0.4215 0.0291 Uiso 1.00 calc . . . H21 H 0.3179 -0.7422 -0.3999 0.0388 Uiso 1.00 calc . . . H22 H 0.1825 -0.8826 -0.3403 0.0436 Uiso 1.00 calc . . . H23 H -0.0373 -0.8178 -0.2881 0.0407 Uiso 1.00 calc . . . H24 H -0.0763 -0.5800 -0.3018 0.0311 Uiso 1.00 calc . . . H25 H -0.8462 0.3709 -0.0765 0.0477 Uiso 1.00 calc . . . H26 H -0.8157 0.3517 -0.1631 0.0477 Uiso 1.00 calc . . . H27 H -0.8271 0.2239 -0.1285 0.0477 Uiso 1.00 calc . . . H28 H -0.4459 0.5263 -0.2233 0.0492 Uiso 1.00 calc . . . H29 H -0.6219 0.4780 -0.2284 0.0492 Uiso 1.00 calc . . . H30 H -0.5659 0.6005 -0.1744 0.0492 Uiso 1.00 calc . . . H31 H -0.1073 0.4328 -0.1116 0.0429 Uiso 1.00 calc . . . H32 H -0.2033 0.5169 -0.1515 0.0429 Uiso 1.00 calc . . . H33 H -0.1674 0.5803 -0.0631 0.0429 Uiso 1.00 calc . . . H34 H -0.2401 0.2030 0.0403 0.0388 Uiso 1.00 calc . . . H35 H -0.1240 0.3112 0.0105 0.0388 Uiso 1.00 calc . . . H36 H -0.2207 0.3566 0.0680 0.0388 Uiso 1.00 calc . . . H37 H -0.6175 0.2497 0.0590 0.0443 Uiso 1.00 calc . . . H38 H -0.6876 0.1477 -0.0063 0.0443 Uiso 1.00 calc . . . H39 H -0.5190 0.1160 0.0312 0.0443 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 0.0164(3) 0.0183(3) 0.0175(2) 0.0021(2) 0.0035(1) -0.0005(1) Si 0.0158(4) 0.0186(4) 0.0204(4) 0.0018(3) 0.0047(3) 0.0002(3) O1 0.021(1) 0.0224(10) 0.0228(10) 0.0012(8) 0.0083(8) -0.0026(7) O2 0.038(1) 0.045(1) 0.025(1) 0.009(1) 0.0112(9) 0.0095(9) O3 0.034(1) 0.040(1) 0.036(1) -0.011(1) 0.0069(10) -0.0062(10) N 0.016(1) 0.018(1) 0.022(1) 0.0001(9) 0.0056(8) 0.0023(8) C1 0.020(1) 0.018(1) 0.023(1) 0.002(1) 0.003(1) 0.0000(9) C2 0.026(2) 0.024(1) 0.020(1) 0.008(1) 0.004(1) -0.0001(10) C3 0.023(1) 0.022(1) 0.021(1) 0.007(1) 0.003(1) -0.0010(9) C4 0.022(1) 0.027(1) 0.023(1) 0.004(1) 0.002(1) -0.003(1) C5 0.021(2) 0.026(1) 0.032(2) 0.007(1) 0.006(1) 0.007(1) C6 0.018(1) 0.032(2) 0.029(2) 0.002(1) 0.003(1) 0.001(1) C7 0.015(1) 0.019(1) 0.020(1) 0.002(1) 0.0053(9) 0.0001(9) C8 0.020(1) 0.037(2) 0.020(1) 0.001(1) 0.001(1) 0.002(1) C9 0.031(2) 0.044(2) 0.023(1) 0.000(1) 0.007(1) 0.015(1) C10 0.024(2) 0.032(2) 0.036(2) -0.002(1) 0.010(1) 0.010(1) C11 0.019(1) 0.031(2) 0.025(1) -0.001(1) 0.003(1) 0.001(1) C12 0.018(1) 0.027(1) 0.020(1) 0.003(1) 0.0036(10) 0.0011(10) C13 0.020(1) 0.018(1) 0.020(1) -0.002(1) -0.0013(10) -0.0025(9) C14 0.021(1) 0.024(1) 0.026(1) 0.002(1) 0.003(1) -0.003(1) C15 0.025(2) 0.032(2) 0.036(2) 0.010(1) 0.001(1) -0.007(1) C16 0.040(2) 0.017(1) 0.049(2) 0.006(1) 0.002(1) 0.004(1) C17 0.032(2) 0.025(2) 0.044(2) 0.002(1) 0.006(1) 0.008(1) C18 0.024(2) 0.025(1) 0.030(2) 0.003(1) 0.008(1) 0.004(1) C19 0.020(1) 0.023(1) 0.026(1) 0.006(1) 0.005(1) 0.0033(10) C20 0.021(1) 0.028(1) 0.022(1) 0.004(1) 0.005(1) -0.0017(10) C21 0.023(2) 0.025(1) 0.027(1) 0.005(1) 0.004(1) -0.005(1) C22 0.026(2) 0.020(1) 0.025(1) 0.010(1) 0.003(1) -0.0011(10) C23 0.025(2) 0.016(1) 0.023(1) 0.001(1) 0.006(1) -0.0013(9) C24 0.022(1) 0.019(1) 0.019(1) 0.004(1) 0.0026(10) -0.0029(9) C25 0.026(2) 0.019(1) 0.022(1) 0.003(1) 0.008(1) -0.0041(9) C26 0.021(2) 0.045(2) 0.048(2) 0.007(1) 0.002(1) -0.010(1) C27 0.055(2) 0.032(2) 0.029(2) 0.017(2) 0.000(1) 0.005(1) C28 0.030(2) 0.029(2) 0.043(2) -0.002(1) 0.011(1) 0.002(1) C29 0.035(2) 0.035(2) 0.023(1) 0.011(1) -0.005(1) -0.004(1) C30 0.046(2) 0.029(2) 0.035(2) 0.000(1) 0.023(1) 0.001(1) #------------------------------------------------------------------------------ _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 C1 2.068(3) . . yes FE C19 1.757(3) . . yes FE C20 1.747(3) . . yes FE C21 2.111(3) . . yes FE C22 2.112(3) . . yes FE C23 2.107(3) . . yes FE C24 2.136(3) . . yes FE C25 2.115(3) . . yes SI O1 1.655(2) . . yes SI N 1.755(2) . . yes SI C5 1.851(3) . . yes SI C6 1.845(3) . . yes O1 C4 1.444(3) . . yes O2 C19 1.149(4) . . yes O3 C20 1.159(4) . . yes N C7 1.439(3) . . yes N C13 1.414(4) . . yes C1 C2 1.528(4) . . yes C2 C3 1.523(4) . . yes C3 C4 1.517(4) . . yes C7 C8 1.393(4) . . yes C7 C12 1.394(4) . . yes C8 C9 1.383(4) . . yes C9 C10 1.385(4) . . yes C10 C11 1.382(4) . . yes C11 C12 1.388(4) . . yes C13 C14 1.393(4) . . yes C13 C18 1.403(4) . . yes C14 C15 1.386(4) . . yes C15 C16 1.382(5) . . yes C16 C17 1.374(5) . . yes C17 C18 1.389(4) . . yes C21 C22 1.422(4) . . yes C21 C25 1.439(4) . . yes C21 C26 1.503(4) . . yes C22 C23 1.443(4) . . yes C22 C27 1.503(4) . . yes C23 C24 1.429(4) . . yes C23 C28 1.491(4) . . yes C24 C25 1.416(4) . . yes C24 C29 1.497(4) . . yes C25 C30 1.492(4) . . 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 C1 FE C19 89.3(1) . . . yes C1 FE C20 90.4(1) . . . yes C1 FE C21 148.8(1) . . . yes C1 FE C22 141.1(1) . . . yes C1 FE C23 101.5(1) . . . yes C1 FE C24 86.4(1) . . . yes C1 FE C25 109.2(1) . . . yes C19 FE C20 96.0(1) . . . yes C19 FE C21 120.5(1) . . . yes C19 FE C22 92.7(1) . . . yes C19 FE C23 100.7(1) . . . yes C19 FE C24 137.1(1) . . . yes C19 FE C25 158.7(1) . . . yes C20 FE C21 94.8(1) . . . yes C20 FE C22 127.9(1) . . . yes C20 FE C23 159.5(1) . . . yes C20 FE C24 126.7(1) . . . yes C20 FE C25 94.2(1) . . . yes C21 FE C22 39.3(1) . . . yes C21 FE C23 66.5(1) . . . yes C21 FE C24 65.9(1) . . . yes C21 FE C25 39.8(1) . . . yes C22 FE C23 40.0(1) . . . yes C22 FE C24 66.2(1) . . . yes C22 FE C25 66.4(1) . . . yes C23 FE C24 39.4(1) . . . yes C23 FE C25 66.2(1) . . . yes C24 FE C25 38.9(1) . . . yes O1 SI N 109.5(1) . . . yes O1 SI C5 109.9(1) . . . yes O1 SI C6 105.7(1) . . . yes N SI C5 107.4(1) . . . yes N SI C6 113.2(1) . . . yes C5 SI C6 111.1(1) . . . yes SI O1 C4 118.7(2) . . . yes SI N C7 119.4(2) . . . yes SI N C13 124.4(2) . . . yes C7 N C13 115.7(2) . . . yes FE C1 C2 119.2(2) . . . yes C1 C2 C3 112.0(2) . . . yes C2 C3 C4 113.0(2) . . . yes O1 C4 C3 111.0(2) . . . yes N C7 C8 120.9(2) . . . yes N C7 C12 119.7(2) . . . yes C8 C7 C12 119.5(2) . . . yes C7 C8 C9 119.9(3) . . . yes C8 C9 C10 120.3(3) . . . yes C9 C10 C11 120.3(3) . . . yes C10 C11 C12 119.8(3) . . . yes C7 C12 C11 120.2(3) . . . yes N C13 C14 121.2(2) . . . yes N C13 C18 120.9(3) . . . yes C14 C13 C18 117.9(3) . . . yes C13 C14 C15 120.5(3) . . . yes C14 C15 C16 121.4(3) . . . yes C15 C16 C17 118.4(3) . . . yes C16 C17 C18 121.3(3) . . . yes C13 C18 C17 120.4(3) . . . yes FE C19 O2 179.1(3) . . . yes FE C20 O3 175.8(3) . . . yes FE C21 C22 70.4(2) . . . yes FE C21 C25 70.2(2) . . . yes FE C21 C26 127.7(2) . . . yes C22 C21 C25 108.1(3) . . . yes C22 C21 C26 127.1(3) . . . yes C25 C21 C26 124.8(3) . . . yes FE C22 C21 70.3(2) . . . yes FE C22 C23 69.8(1) . . . yes FE C22 C27 127.9(2) . . . yes C21 C22 C23 107.7(2) . . . yes C21 C22 C27 126.4(3) . . . yes C23 C22 C27 125.8(3) . . . yes FE C23 C22 70.2(2) . . . yes FE C23 C24 71.4(1) . . . yes FE C23 C28 126.9(2) . . . yes C22 C23 C24 107.8(2) . . . yes C22 C23 C28 126.8(3) . . . yes C24 C23 C28 125.3(3) . . . yes FE C24 C23 69.2(1) . . . yes FE C24 C25 69.7(1) . . . yes FE C24 C29 129.0(2) . . . yes C23 C24 C25 108.3(2) . . . yes C23 C24 C29 126.7(3) . . . yes C25 C24 C29 125.0(3) . . . yes FE C25 C21 69.9(2) . . . yes FE C25 C24 71.4(2) . . . yes FE C25 C30 128.2(2) . . . yes C21 C25 C24 108.1(3) . . . yes C21 C25 C30 125.4(3) . . . yes C24 C25 C30 126.3(3) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_of_2-Ph _database_code_CSD 200913 _audit_creation_date 'Mon Jan 27 18:04:18 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C26 H31 Fe N O2 Si ' _chemical_formula_moiety 'C26 H31 Fe N O2 Si ' _chemical_formula_weight 473.47 _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 12.6585(5) _cell_length_b 12.8308(5) _cell_length_c 15.2030(7) _cell_angle_alpha 90 _cell_angle_beta 101.665(2) _cell_angle_gamma 90 _cell_volume 2418.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 22778 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.909 #------------------------------------------------------------------------------ # 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 21562 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.42 _diffrn_measured_fraction_theta_max 0.9978 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.9978 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # 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 5518 _reflns_number_gt 4599 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1661 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5518 _refine_ls_number_parameters 280 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 0.49 _refine_diff_density_min -0.47 _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) ; O O 0.011 0.006 ;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) ; #------------------------------------------------------------------------------ # 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 0.05879(3) 0.15715(3) 0.21953(2) 0.0211(1) Uani 1.00 d . . . Si Si -0.07920(5) 0.08413(6) 0.28081(5) 0.0216(2) Uani 1.00 d . . . O1 O 0.2184(2) 0.1060(2) 0.3788(2) 0.0432(6) Uani 1.00 d . . . O2 O 0.0643(2) -0.0485(2) 0.1427(2) 0.0435(6) Uani 1.00 d . . . N N -0.1411(2) 0.1636(2) 0.3527(1) 0.0225(5) Uani 1.00 d . . . C1 C -0.0366(2) -0.0404(2) 0.3439(2) 0.0375(8) Uani 1.00 d . . . C2 C -0.1944(2) 0.0401(2) 0.1896(2) 0.0308(7) Uani 1.00 d . . . C3 C -0.0841(2) 0.2296(2) 0.4210(2) 0.0231(6) Uani 1.00 d . . . C4 C -0.1322(2) 0.3219(2) 0.4422(2) 0.0265(6) Uani 1.00 d . . . C5 C -0.0802(2) 0.3875(2) 0.5092(2) 0.0314(7) Uani 1.00 d . . . C6 C 0.0232(2) 0.3640(2) 0.5566(2) 0.0340(7) Uani 1.00 d . . . C7 C 0.0718(2) 0.2735(2) 0.5356(2) 0.0320(7) Uani 1.00 d . . . C8 C 0.0194(2) 0.2059(2) 0.4693(2) 0.0267(6) Uani 1.00 d . . . C9 C -0.2493(2) 0.1419(2) 0.3626(2) 0.0233(6) Uani 1.00 d . . . C10 C -0.2661(2) 0.0865(2) 0.4376(2) 0.0291(7) Uani 1.00 d . . . C11 C -0.3703(3) 0.0656(3) 0.4496(2) 0.0394(8) Uani 1.00 d . . . C12 C -0.4583(2) 0.0987(3) 0.3864(2) 0.0420(9) Uani 1.00 d . . . C13 C -0.4420(2) 0.1529(3) 0.3121(2) 0.0421(9) Uani 1.00 d . . . C14 C -0.3381(2) 0.1752(3) 0.3000(2) 0.0331(7) Uani 1.00 d . . . C15 C 0.1513(2) 0.1271(2) 0.3175(2) 0.0295(7) Uani 1.00 d . . . C16 C 0.0606(2) 0.0325(2) 0.1747(2) 0.0287(7) Uani 1.00 d . . . C17 C -0.0203(2) 0.2380(2) 0.1036(2) 0.0258(6) Uani 1.00 d . . . C18 C -0.0278(2) 0.2983(2) 0.1810(2) 0.0258(6) Uani 1.00 d . . . C19 C 0.0789(2) 0.3202(2) 0.2278(2) 0.0295(7) Uani 1.00 d . . . C20 C 0.1533(2) 0.2757(2) 0.1776(2) 0.0294(7) Uani 1.00 d . . . C21 C 0.0920(2) 0.2245(2) 0.1017(2) 0.0275(6) Uani 1.00 d . . . C22 C -0.1116(2) 0.2064(3) 0.0288(2) 0.0348(7) Uani 1.00 d . . . C23 C -0.1289(2) 0.3430(2) 0.2022(2) 0.0313(7) Uani 1.00 d . . . C24 C 0.1086(3) 0.3879(2) 0.3093(2) 0.0419(8) Uani 1.00 d . . . C25 C 0.2734(2) 0.2876(3) 0.1980(3) 0.0484(10) Uani 1.00 d . . . C26 C 0.1341(2) 0.1687(3) 0.0286(2) 0.0373(8) Uani 1.00 d . . . H1 H -0.0975 -0.0607 0.3660 0.0437 Uiso 1.00 calc . . . H2 H -0.0184 -0.0870 0.3080 0.0437 Uiso 1.00 calc . . . H3 H 0.0222 -0.0325 0.4005 0.0437 Uiso 1.00 calc . . . H4 H -0.2293 0.0987 0.1594 0.0398 Uiso 1.00 calc . . . H5 H -0.1678 -0.0066 0.1519 0.0398 Uiso 1.00 calc . . . H6 H -0.2508 0.0085 0.2141 0.0398 Uiso 1.00 calc . . . H7 H -0.1974 0.3443 0.4075 0.0304 Uiso 1.00 calc . . . H8 H -0.1111 0.4545 0.5177 0.0383 Uiso 1.00 calc . . . H9 H 0.0560 0.4138 0.5982 0.0394 Uiso 1.00 calc . . . H10 H 0.1444 0.2505 0.5707 0.0385 Uiso 1.00 calc . . . H11 H 0.0472 0.1476 0.4546 0.0336 Uiso 1.00 calc . . . H12 H -0.2076 0.0637 0.4775 0.0364 Uiso 1.00 calc . . . H13 H -0.3772 0.0228 0.4966 0.0479 Uiso 1.00 calc . . . H14 H -0.5226 0.0814 0.3991 0.0500 Uiso 1.00 calc . . . H15 H -0.5021 0.1710 0.2603 0.0503 Uiso 1.00 calc . . . H16 H -0.3261 0.2168 0.2457 0.0391 Uiso 1.00 calc . . . H17 H -0.1813 0.2019 0.0505 0.0428 Uiso 1.00 calc . . . H18 H -0.1150 0.2448 -0.0194 0.0428 Uiso 1.00 calc . . . H19 H -0.1162 0.1310 0.0098 0.0428 Uiso 1.00 calc . . . H20 H -0.1500 0.3979 0.1727 0.0400 Uiso 1.00 calc . . . H21 H -0.1915 0.2939 0.1817 0.0400 Uiso 1.00 calc . . . H22 H -0.1329 0.3475 0.2612 0.0400 Uiso 1.00 calc . . . H23 H 0.1719 0.3692 0.3442 0.0487 Uiso 1.00 calc . . . H24 H 0.1199 0.4472 0.2974 0.0487 Uiso 1.00 calc . . . H25 H 0.0439 0.3858 0.3500 0.0487 Uiso 1.00 calc . . . H26 H 0.3114 0.2206 0.1730 0.0588 Uiso 1.00 calc . . . H27 H 0.3017 0.3469 0.1683 0.0588 Uiso 1.00 calc . . . H28 H 0.3004 0.2840 0.2608 0.0588 Uiso 1.00 calc . . . H29 H 0.0856 0.1132 0.0051 0.0466 Uiso 1.00 calc . . . H30 H 0.1411 0.2138 -0.0189 0.0466 Uiso 1.00 calc . . . H31 H 0.2071 0.1434 0.0448 0.0466 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 0.0199(2) 0.0235(2) 0.0205(2) 0.0009(1) 0.0052(1) 0.0007(1) Si 0.0226(3) 0.0212(3) 0.0215(4) -0.0005(3) 0.0058(2) 0.0016(3) O1 0.0312(10) 0.058(1) 0.035(1) 0.009(1) -0.0050(9) 0.004(1) O2 0.056(1) 0.034(1) 0.042(1) 0.006(1) 0.015(1) -0.012(1) N 0.0223(10) 0.026(1) 0.020(1) -0.0014(8) 0.0070(8) 0.0002(9) C1 0.045(2) 0.029(1) 0.042(2) 0.004(1) 0.015(1) 0.008(1) C2 0.026(1) 0.035(1) 0.031(1) -0.008(1) 0.008(1) -0.007(1) C3 0.027(1) 0.027(1) 0.016(1) -0.0018(10) 0.0059(9) 0.005(1) C4 0.026(1) 0.029(1) 0.026(1) 0.000(1) 0.0079(10) 0.001(1) C5 0.034(1) 0.031(1) 0.031(1) -0.005(1) 0.011(1) -0.002(1) C6 0.038(1) 0.037(2) 0.026(1) -0.013(1) 0.005(1) -0.003(1) C7 0.028(1) 0.042(2) 0.025(1) -0.006(1) 0.0006(10) 0.005(1) C8 0.028(1) 0.030(1) 0.022(1) 0.000(1) 0.0035(10) 0.006(1) C9 0.022(1) 0.027(1) 0.021(1) -0.0010(10) 0.0055(9) -0.003(1) C10 0.032(1) 0.030(1) 0.026(1) -0.004(1) 0.008(1) 0.003(1) C11 0.045(2) 0.040(2) 0.040(2) -0.010(1) 0.023(1) -0.002(1) C12 0.030(1) 0.050(2) 0.053(2) -0.012(1) 0.022(1) -0.015(2) C13 0.024(1) 0.061(2) 0.041(2) 0.001(1) 0.005(1) -0.006(2) C14 0.027(1) 0.047(2) 0.026(1) 0.001(1) 0.007(1) 0.002(1) C15 0.026(1) 0.031(1) 0.032(1) 0.001(1) 0.007(1) -0.003(1) C16 0.028(1) 0.032(1) 0.027(1) 0.002(1) 0.0070(10) -0.001(1) C17 0.025(1) 0.031(1) 0.023(1) -0.001(1) 0.0070(9) 0.005(1) C18 0.025(1) 0.027(1) 0.026(1) 0.004(1) 0.0084(10) 0.006(1) C19 0.034(1) 0.024(1) 0.030(1) -0.003(1) 0.007(1) 0.004(1) C20 0.025(1) 0.031(1) 0.033(1) -0.003(1) 0.007(1) 0.006(1) C21 0.028(1) 0.031(1) 0.027(1) 0.000(1) 0.0117(10) 0.005(1) C22 0.026(1) 0.053(2) 0.026(1) 0.001(1) 0.004(1) 0.005(1) C23 0.036(1) 0.032(1) 0.031(1) 0.015(1) 0.016(1) 0.009(1) C24 0.058(2) 0.030(2) 0.037(2) -0.009(1) 0.008(1) -0.005(1) C25 0.027(1) 0.060(2) 0.057(2) -0.013(1) 0.006(1) 0.006(2) C26 0.039(1) 0.047(2) 0.032(2) 0.005(1) 0.021(1) 0.004(1) #------------------------------------------------------------------------------ _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 2.3355(7) . . yes FE C15 1.741(3) . . yes FE C16 1.741(3) . . yes FE C17 2.115(3) . . yes FE C18 2.136(3) . . yes FE C19 2.108(3) . . yes FE C20 2.112(3) . . yes FE C21 2.106(3) . . yes SI N 1.787(2) . . yes SI C1 1.886(3) . . yes SI C2 1.884(3) . . yes O1 C15 1.159(3) . . yes O2 C16 1.151(4) . . yes N C3 1.418(3) . . yes N C9 1.436(3) . . yes C3 C4 1.399(4) . . yes C3 C8 1.400(3) . . yes C4 C5 1.381(4) . . yes C5 C6 1.393(4) . . yes C6 C7 1.381(4) . . yes C7 C8 1.392(4) . . yes C9 C10 1.396(4) . . yes C9 C14 1.385(4) . . yes C10 C11 1.394(4) . . yes C11 C12 1.382(5) . . yes C12 C13 1.378(5) . . yes C13 C14 1.394(4) . . yes C17 C18 1.428(4) . . yes C17 C21 1.439(3) . . yes C17 C22 1.503(4) . . yes C18 C19 1.421(4) . . yes C18 C23 1.496(4) . . yes C19 C20 1.443(4) . . yes C19 C24 1.498(4) . . yes C20 C21 1.416(4) . . yes C20 C25 1.497(4) . . yes C21 C26 1.506(4) . . 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 C15 89.89(9) . . . yes SI FE C16 81.83(9) . . . yes SI FE C17 105.25(7) . . . yes SI FE C18 93.78(7) . . . yes SI FE C19 117.74(8) . . . yes SI FE C20 157.56(8) . . . yes SI FE C21 142.93(7) . . . yes C15 FE C16 94.1(1) . . . yes C15 FE C17 160.8(1) . . . yes C15 FE C18 129.9(1) . . . yes C15 FE C19 96.7(1) . . . yes C15 FE C20 95.4(1) . . . yes C15 FE C21 127.1(1) . . . yes C16 FE C17 99.6(1) . . . yes C16 FE C18 135.9(1) . . . yes C16 FE C19 157.5(1) . . . yes C16 FE C20 119.4(1) . . . yes C16 FE C21 91.3(1) . . . yes C17 FE C18 39.2(1) . . . yes C17 FE C19 66.0(1) . . . yes C17 FE C20 66.22(10) . . . yes C17 FE C21 39.85(9) . . . yes C18 FE C19 39.11(10) . . . yes C18 FE C20 66.24(10) . . . yes C18 FE C21 66.4(1) . . . yes C19 FE C20 40.0(1) . . . yes C19 FE C21 66.5(1) . . . yes C20 FE C21 39.2(1) . . . yes FE SI N 118.07(8) . . . yes FE SI C1 112.52(10) . . . yes FE SI C2 110.89(9) . . . yes N SI C1 106.7(1) . . . yes N SI C2 104.6(1) . . . yes C1 SI C2 102.7(1) . . . yes SI N C3 124.6(2) . . . yes SI N C9 119.9(2) . . . yes C3 N C9 113.2(2) . . . yes N C3 C4 119.6(2) . . . yes N C3 C8 122.5(2) . . . yes C4 C3 C8 117.9(2) . . . yes C3 C4 C5 121.4(2) . . . yes C4 C5 C6 120.5(3) . . . yes C5 C6 C7 118.6(3) . . . yes C6 C7 C8 121.5(2) . . . yes C3 C8 C7 120.1(3) . . . yes N C9 C10 119.3(2) . . . yes N C9 C14 121.8(2) . . . yes C10 C9 C14 118.8(2) . . . yes C9 C10 C11 120.6(3) . . . yes C10 C11 C12 120.1(3) . . . yes C11 C12 C13 119.4(3) . . . yes C12 C13 C14 120.9(3) . . . yes C9 C14 C13 120.1(3) . . . yes FE C15 O1 175.0(3) . . . yes FE C16 O2 177.3(3) . . . yes FE C17 C18 71.2(1) . . . yes FE C17 C21 69.8(1) . . . yes FE C17 C22 131.3(2) . . . yes C18 C17 C21 108.2(2) . . . yes C18 C17 C22 126.9(2) . . . yes C21 C17 C22 124.3(3) . . . yes FE C18 C17 69.6(1) . . . yes FE C18 C19 69.4(2) . . . yes FE C18 C23 132.8(2) . . . yes C17 C18 C19 107.7(2) . . . yes C17 C18 C23 126.0(2) . . . yes C19 C18 C23 125.8(3) . . . yes FE C19 C18 71.5(2) . . . yes FE C19 C20 70.2(2) . . . yes FE C19 C24 129.2(2) . . . yes C18 C19 C20 108.3(2) . . . yes C18 C19 C24 125.6(3) . . . yes C20 C19 C24 125.8(3) . . . yes FE C20 C19 69.8(2) . . . yes FE C20 C21 70.2(1) . . . yes FE C20 C25 128.6(2) . . . yes C19 C20 C21 107.8(2) . . . yes C19 C20 C25 126.5(3) . . . yes C21 C20 C25 125.6(3) . . . yes FE C21 C17 70.4(1) . . . yes FE C21 C20 70.6(2) . . . yes FE C21 C26 126.4(2) . . . yes C17 C21 C20 108.0(2) . . . yes C17 C21 C26 124.8(3) . . . yes C20 C21 C26 127.2(2) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------