Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Drewitt, Mark J.' 'Hascall, Tony' 'O'Hare, Dermot' _publ_contact_author_name 'Prof Dermot O'Hare' _publ_contact_author_address ; Inorganic Chemistry Lab University of Oxford South Parks Rd Oxford Oxon OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'DERMOT.OHARE@CHEM.OX.AC.UK' _publ_section_title ; Silicon-bridged bis(cyclohexadienyl) iron complexes: The first structurally characterised [14]ferrocenophane ; # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-09-23 at 15:31:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : c:\wingx\files\archive.dat # CIF files read : me2si import struct data_me2si _database_code_CSD 170500 _audit_creation_date 2001-09-23T15:31:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H26 Fe1 Si1' _chemical_formula_structural 'C18 H26 SI FE' _chemical_formula_sum 'C18 H26 Fe Si' _chemical_formula_weight 326.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.5115(3) _cell_length_b 8.2107(2) _cell_length_c 16.9607(4) _cell_angle_alpha 90 _cell_angle_beta 103.0030(10) _cell_angle_gamma 90 _cell_volume 1697.66(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3368 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.948 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.569094E-1 _diffrn_orient_matrix_ub_12 -0.362396E-1 _diffrn_orient_matrix_ub_13 0.481149E-1 _diffrn_orient_matrix_ub_21 -0.573729E-1 _diffrn_orient_matrix_ub_22 -0.74482E-2 _diffrn_orient_matrix_ub_23 0.324625E-1 _diffrn_orient_matrix_ub_31 -0.140908E-1 _diffrn_orient_matrix_ub_32 -0.116037 _diffrn_orient_matrix_ub_33 -0.171105E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 6818 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3853 _reflns_number_gt 3422 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0334P)^2^+1.1356P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0052(15) _refine_ls_number_reflns 3853 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.429 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fe Fe 0.762706(18) 0.49179(3) 0.136403(13) 0.01894(10) Uani 1 1 d . . . Si Si 0.95870(4) 0.35509(6) 0.11763(3) 0.02355(13) Uani 1 1 d . . . C1 C 0.96480(17) 0.1791(2) 0.04969(12) 0.0351(4) Uani 1 1 d . . . H1A H 1.0007 0.2127 0.0066 0.053 Uiso 1 1 calc R . . H1B H 0.8902 0.1415 0.0258 0.053 Uiso 1 1 calc R . . H1C H 1.0067 0.0905 0.0809 0.053 Uiso 1 1 calc R . . C2 C 1.09759(15) 0.4233(2) 0.17008(12) 0.0320(4) Uani 1 1 d . . . H2A H 1.1346 0.3357 0.2051 0.048 Uiso 1 1 calc R . . H2B H 1.0916 0.5196 0.203 0.048 Uiso 1 1 calc R . . H2C H 1.1401 0.4507 0.1299 0.048 Uiso 1 1 calc R . . C11 C 0.86692(14) 0.3135(2) 0.19084(10) 0.0230(3) Uani 1 1 d . . . C12 C 0.76157(14) 0.2444(2) 0.15338(11) 0.0248(4) Uani 1 1 d . . . H12 H 0.7578 0.1592 0.115 0.03 Uiso 1 1 calc R . . C13 C 0.66452(14) 0.3007(2) 0.17268(10) 0.0251(4) Uani 1 1 d . . . H13 H 0.5973 0.2924 0.1334 0.03 Uiso 1 1 calc R . . C14 C 0.66457(14) 0.3741(2) 0.25441(10) 0.0234(3) Uani 1 1 d . . . C15 C 0.75816(14) 0.49384(19) 0.26123(10) 0.0223(3) Uani 1 1 d . . . H15 H 0.7481 0.6041 0.275 0.027 Uiso 1 1 calc R . . C16 C 0.86015(14) 0.4435(2) 0.24734(9) 0.0220(3) Uani 1 1 d . . . H16 H 0.9254 0.4957 0.2754 0.026 Uiso 1 1 calc R . . C17 C 0.68583(16) 0.2503(2) 0.32412(11) 0.0308(4) Uani 1 1 d . . . H17A H 0.7579 0.1998 0.3284 0.046 Uiso 1 1 calc R . . H17B H 0.6289 0.166 0.3135 0.046 Uiso 1 1 calc R . . H17C H 0.6843 0.306 0.3749 0.046 Uiso 1 1 calc R . . C18 C 0.55597(15) 0.4614(2) 0.25100(11) 0.0304(4) Uani 1 1 d . . . H18A H 0.5581 0.5152 0.3029 0.046 Uiso 1 1 calc R . . H18B H 0.4959 0.382 0.2402 0.046 Uiso 1 1 calc R . . H18C H 0.5441 0.543 0.2077 0.046 Uiso 1 1 calc R . . C21 C 0.86972(15) 0.5263(2) 0.06346(10) 0.0243(4) Uani 1 1 d . . . C22 C 0.76370(15) 0.4756(2) 0.01644(10) 0.0261(4) Uani 1 1 d . . . H22 H 0.7589 0.3821 -0.0172 0.031 Uiso 1 1 calc R . . C23 C 0.66751(15) 0.5620(2) 0.01951(10) 0.0273(4) Uani 1 1 d . . . H23 H 0.5994 0.5059 0.0108 0.033 Uiso 1 1 calc R . . C24 C 0.67120(15) 0.7424(2) 0.03642(11) 0.0290(4) Uani 1 1 d . . . C25 C 0.76436(15) 0.7483(2) 0.11072(10) 0.0255(4) Uani 1 1 d . . . H25 H 0.7549 0.8058 0.1573 0.031 Uiso 1 1 calc R . . C26 C 0.86494(14) 0.6699(2) 0.11203(10) 0.0241(3) Uani 1 1 d . . . H26 H 0.9306 0.7118 0.1453 0.029 Uiso 1 1 calc R . . C27 C 0.69449(18) 0.8434(3) -0.03443(12) 0.0407(5) Uani 1 1 d . . . H27A H 0.7642 0.8085 -0.0461 0.061 Uiso 1 1 calc R . . H27B H 0.6988 0.9591 -0.0198 0.061 Uiso 1 1 calc R . . H27C H 0.6352 0.8269 -0.0825 0.061 Uiso 1 1 calc R . . C28 C 0.56466(16) 0.8005(3) 0.05685(13) 0.0372(4) Uani 1 1 d . . . H28A H 0.5039 0.7865 0.0095 0.056 Uiso 1 1 calc R . . H28B H 0.5714 0.9158 0.072 0.056 Uiso 1 1 calc R . . H28C H 0.5503 0.7364 0.1021 0.056 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 Fe 0.02395(15) 0.01849(14) 0.01472(14) -0.00112(8) 0.00504(10) -0.00235(8) Si 0.0267(2) 0.0220(2) 0.0241(2) -0.00269(18) 0.01028(19) -0.00100(18) C1 0.0407(11) 0.0315(10) 0.0369(10) -0.0101(8) 0.0171(9) -0.0017(8) C2 0.0286(9) 0.0329(10) 0.0357(10) -0.0035(8) 0.0096(8) -0.0018(8) C11 0.0286(8) 0.0193(8) 0.0223(8) 0.0028(6) 0.0086(7) 0.0013(6) C12 0.0352(9) 0.0164(7) 0.0248(8) -0.0021(6) 0.0110(7) -0.0043(7) C13 0.0289(9) 0.0242(8) 0.0226(8) -0.0022(7) 0.0066(7) -0.0063(7) C14 0.0265(8) 0.0245(8) 0.0210(8) 0.0019(7) 0.0090(7) 0.0006(7) C15 0.0295(9) 0.0215(8) 0.0163(8) 0.0001(6) 0.0064(7) 0.0009(6) C16 0.0263(8) 0.0233(8) 0.0153(7) 0.0021(6) 0.0020(6) -0.0015(6) C17 0.0333(10) 0.0315(9) 0.0302(10) 0.0085(8) 0.0130(8) 0.0014(8) C18 0.0292(9) 0.0347(9) 0.0290(9) 0.0014(8) 0.0100(8) 0.0030(8) C21 0.0294(9) 0.0269(8) 0.0193(8) 0.0014(7) 0.0111(7) -0.0035(7) C22 0.0346(9) 0.0311(9) 0.0133(7) -0.0026(7) 0.0069(7) -0.0029(7) C23 0.0296(9) 0.0330(9) 0.0182(8) 0.0011(7) 0.0034(7) -0.0035(7) C24 0.0324(9) 0.0299(9) 0.0234(9) 0.0070(7) 0.0039(7) 0.0007(7) C25 0.0351(9) 0.0207(8) 0.0209(8) 0.0031(7) 0.0067(7) -0.0006(7) C26 0.0289(9) 0.0219(8) 0.0215(8) 0.0037(7) 0.0059(7) -0.0064(7) C27 0.0464(12) 0.0440(12) 0.0302(10) 0.0156(9) 0.0056(9) 0.0005(9) C28 0.0368(10) 0.0371(11) 0.0359(11) 0.0070(9) 0.0044(8) 0.0075(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C21 2.0368(17) . ? Fe C16 2.0375(16) . ? Fe C11 2.0381(17) . ? Fe C22 2.0417(17) . ? Fe C26 2.0451(16) . ? Fe C12 2.0523(17) . ? Fe C15 2.1307(17) . ? Fe C23 2.1491(17) . ? Fe C25 2.1517(16) . ? Fe C13 2.1656(17) . ? Si C2 1.8518(19) . ? Si C1 1.8602(19) . ? Si C21 1.8973(18) . ? Si C11 1.9023(17) . ? C11 C12 1.444(2) . ? C11 C16 1.450(2) . ? C12 C13 1.405(2) . ? C13 C14 1.512(2) . ? C14 C15 1.513(2) . ? C14 C18 1.526(2) . ? C14 C17 1.537(2) . ? C15 C16 1.411(2) . ? C21 C22 1.447(3) . ? C21 C26 1.447(2) . ? C22 C23 1.408(3) . ? C23 C24 1.507(3) . ? C24 C25 1.513(2) . ? C24 C28 1.527(3) . ? C24 C27 1.541(3) . ? C25 C26 1.409(3) . ? 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 C21 Fe C16 104.44(7) . . ? C21 Fe C11 86.23(7) . . ? C16 Fe C11 41.68(7) . . ? C21 Fe C22 41.55(7) . . ? C16 Fe C22 140.45(7) . . ? C11 Fe C22 104.95(7) . . ? C21 Fe C26 41.52(7) . . ? C16 Fe C26 93.11(7) . . ? C11 Fe C26 103.86(7) . . ? C22 Fe C26 72.59(7) . . ? C21 Fe C12 104.43(7) . . ? C16 Fe C12 72.52(7) . . ? C11 Fe C12 41.35(7) . . ? C22 Fe C12 94.42(7) . . ? C26 Fe C12 139.50(7) . . ? C21 Fe C15 140.40(7) . . ? C16 Fe C15 39.48(7) . . ? C11 Fe C15 73.32(6) . . ? C22 Fe C15 176.52(7) . . ? C26 Fe C15 110.67(7) . . ? C12 Fe C15 82.29(7) . . ? C21 Fe C23 72.90(7) . . ? C16 Fe C23 175.07(7) . . ? C11 Fe C23 140.88(7) . . ? C22 Fe C23 39.16(7) . . ? C26 Fe C23 82.17(7) . . ? C12 Fe C23 112.03(7) . . ? C15 Fe C23 141.38(7) . . ? C21 Fe C25 72.74(7) . . ? C16 Fe C25 110.26(7) . . ? C11 Fe C25 139.50(7) . . ? C22 Fe C25 81.93(7) . . ? C26 Fe C25 39.14(7) . . ? C12 Fe C25 176.35(6) . . ? C15 Fe C25 101.36(6) . . ? C23 Fe C25 65.12(7) . . ? C21 Fe C13 139.98(7) . . ? C16 Fe C13 81.76(7) . . ? C11 Fe C13 72.35(7) . . ? C22 Fe C13 111.52(7) . . ? C26 Fe C13 174.86(7) . . ? C12 Fe C13 38.80(7) . . ? C15 Fe C13 65.15(6) . . ? C23 Fe C13 102.97(7) . . ? C25 Fe C13 143.00(7) . . ? C2 Si C1 111.57(9) . . ? C2 Si C21 113.17(8) . . ? C1 Si C21 112.14(9) . . ? C2 Si C11 112.32(8) . . ? C1 Si C11 112.32(8) . . ? C21 Si C11 94.27(7) . . ? C12 C11 C16 113.39(15) . . ? C12 C11 Si 114.11(12) . . ? C16 C11 Si 115.64(12) . . ? C12 C11 Fe 69.85(9) . . ? C16 C11 Fe 69.14(9) . . ? Si C11 Fe 89.65(7) . . ? C13 C12 C11 121.28(15) . . ? C13 C12 Fe 74.97(10) . . ? C11 C12 Fe 68.80(9) . . ? C12 C13 C14 121.52(16) . . ? C12 C13 Fe 66.24(9) . . ? C14 C13 Fe 95.07(10) . . ? C13 C14 C15 99.78(13) . . ? C13 C14 C18 109.63(14) . . ? C15 C14 C18 111.41(14) . . ? C13 C14 C17 113.96(15) . . ? C15 C14 C17 111.97(14) . . ? C18 C14 C17 109.78(14) . . ? C16 C15 C14 120.70(14) . . ? C16 C15 Fe 66.69(9) . . ? C14 C15 Fe 96.44(10) . . ? C15 C16 C11 121.03(15) . . ? C15 C16 Fe 73.83(10) . . ? C11 C16 Fe 69.18(9) . . ? C22 C21 C26 113.46(16) . . ? C22 C21 Si 114.76(12) . . ? C26 C21 Si 115.01(12) . . ? C22 C21 Fe 69.41(9) . . ? C26 C21 Fe 69.55(9) . . ? Si C21 Fe 89.83(7) . . ? C23 C22 C21 121.31(16) . . ? C23 C22 Fe 74.54(10) . . ? C21 C22 Fe 69.04(9) . . ? C22 C23 C24 120.83(16) . . ? C22 C23 Fe 66.30(9) . . ? C24 C23 Fe 95.81(11) . . ? C23 C24 C25 100.07(14) . . ? C23 C24 C28 111.04(16) . . ? C25 C24 C28 110.45(16) . . ? C23 C24 C27 112.56(16) . . ? C25 C24 C27 112.76(16) . . ? C28 C24 C27 109.67(16) . . ? C26 C25 C24 121.09(16) . . ? C26 C25 Fe 66.34(9) . . ? C24 C25 Fe 95.54(11) . . ? C25 C26 C21 120.96(16) . . ? C25 C26 Fe 74.51(10) . . ? C21 C26 Fe 68.93(9) . . ? # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-08-30 at 15:11:01 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : c:\wingx\files\archive.dat # CIF files read : th168 struct data_th168 _database_code_CSD 170501 _audit_creation_date 2001-08-30T15:11:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H52 Fe2 Si2' _chemical_formula_structural 'C36 H52 FE2 SI2' _chemical_formula_sum 'C36 H52 Fe2 Si2' _chemical_formula_weight 652.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5970(10) _cell_length_b 15.9770(10) _cell_length_c 11.1060(10) _cell_angle_alpha 90 _cell_angle_beta 105.1850(10) _cell_angle_gamma 90 _cell_volume 1643.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.979 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 6425 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 3749 _reflns_number_gt 3359 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+3.4439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0016(11) _refine_ls_number_reflns 3749 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.11 _refine_ls_restrained_S_all 1.11 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.583 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 CT01 C 0.305 0.157 -0.004 0 Uiso 0 1 d P . . CT02 C 0.025 0.245 0.036 0 Uiso 0 1 d P . . Fe Fe 0.12576(3) 0.155422(19) 0.01348(3) 0.01183(11) Uani 1 1 d . . . Si Si -0.06223(7) 0.03036(4) 0.19680(6) 0.01346(15) Uani 1 1 d . . . C1 C 0.1079(3) -0.01251(16) 0.3033(2) 0.0228(5) Uani 1 1 d . . . H1A H 0.1641 -0.0413 0.2538 0.034 Uiso 1 1 calc R . . H1B H 0.0834 -0.0521 0.3619 0.034 Uiso 1 1 calc R . . H1C H 0.1651 0.0335 0.3499 0.034 Uiso 1 1 calc R . . C2 C -0.1815(3) 0.06341(16) 0.2978(2) 0.0251(5) Uani 1 1 d . . . H2A H -0.1316 0.1057 0.3576 0.038 Uiso 1 1 calc R . . H2B H -0.2038 0.0147 0.3431 0.038 Uiso 1 1 calc R . . H2C H -0.2712 0.0871 0.2455 0.038 Uiso 1 1 calc R . . C11 C -0.0235(2) 0.12707(14) 0.1153(2) 0.0142(4) Uani 1 1 d . . . C12 C -0.0933(2) 0.15269(14) -0.0094(2) 0.0139(4) Uani 1 1 d . . . H12 H -0.1626 0.117 -0.0616 0.017 Uiso 1 1 calc R . . C13 C -0.0606(2) 0.22992(14) -0.0554(2) 0.0155(4) Uani 1 1 d . . . H13 H -0.0688 0.2367 -0.142 0.019 Uiso 1 1 calc R . . C14 C -0.0119(2) 0.30274(14) 0.0337(2) 0.0157(4) Uani 1 1 d . . . C15 C 0.1108(2) 0.26043(14) 0.1281(2) 0.0156(4) Uani 1 1 d . . . H15 H 0.2039 0.2854 0.1509 0.019 Uiso 1 1 calc R . . C16 C 0.0860(2) 0.18404(14) 0.1819(2) 0.0151(4) Uani 1 1 d . . . H16 H 0.1423 0.1698 0.2632 0.018 Uiso 1 1 calc R . . C17 C 0.0435(3) 0.37549(15) -0.0302(2) 0.0216(5) Uani 1 1 d . . . H17A H 0.0873 0.4177 0.0323 0.032 Uiso 1 1 calc R . . H17B H -0.0372 0.4005 -0.0927 0.032 Uiso 1 1 calc R . . H17C H 0.1158 0.3549 -0.0709 0.032 Uiso 1 1 calc R . . C18 C -0.1320(3) 0.33466(16) 0.0904(2) 0.0239(5) Uani 1 1 d . . . H18A H -0.0949 0.3809 0.1478 0.036 Uiso 1 1 calc R . . H18B H -0.1638 0.2891 0.1359 0.036 Uiso 1 1 calc R . . H18C H -0.2137 0.3544 0.0235 0.036 Uiso 1 1 calc R . . C21 C 0.1659(2) 0.05474(14) -0.0955(2) 0.0137(4) Uani 1 1 d . . . C22 C 0.2510(2) 0.04945(14) 0.0312(2) 0.0147(4) Uani 1 1 d . . . H22 H 0.2459 0.0008 0.0791 0.018 Uiso 1 1 calc R . . C23 C 0.3421(2) 0.11603(14) 0.0848(2) 0.0161(4) Uani 1 1 d . . . H23 H 0.3642 0.1256 0.1722 0.019 Uiso 1 1 calc R . . C24 C 0.4048(2) 0.17239(15) 0.0026(2) 0.0174(5) Uani 1 1 d . . . C25 C 0.2671(2) 0.19733(14) -0.0927(2) 0.0155(4) Uani 1 1 d . . . H25 H 0.2445 0.2546 -0.1107 0.019 Uiso 1 1 calc R . . C26 C 0.1736(2) 0.13425(14) -0.1539(2) 0.0147(4) Uani 1 1 d . . . H26 H 0.1143 0.1442 -0.2356 0.018 Uiso 1 1 calc R . . C27 C 0.4786(3) 0.24847(16) 0.0757(3) 0.0239(5) Uani 1 1 d . . . H27A H 0.5131 0.2858 0.0197 0.036 Uiso 1 1 calc R . . H27B H 0.5605 0.2299 0.1433 0.036 Uiso 1 1 calc R . . H27C H 0.4095 0.2785 0.1111 0.036 Uiso 1 1 calc R . . C28 C 0.5130(3) 0.12696(17) -0.0545(2) 0.0241(5) Uani 1 1 d . . . H28A H 0.4664 0.0781 -0.1015 0.036 Uiso 1 1 calc R . . H28B H 0.5961 0.1087 0.0123 0.036 Uiso 1 1 calc R . . H28C H 0.5458 0.1651 -0.1106 0.036 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 Fe 0.01169(17) 0.01082(17) 0.01306(17) -0.00028(11) 0.00337(12) -0.00009(11) Si 0.0161(3) 0.0118(3) 0.0130(3) -0.0007(2) 0.0049(2) -0.0008(2) C1 0.0240(12) 0.0225(13) 0.0187(12) 0.0030(10) -0.0002(10) -0.0003(10) C2 0.0337(14) 0.0231(13) 0.0234(12) -0.0033(10) 0.0161(11) -0.0018(11) C11 0.0149(10) 0.0137(10) 0.0157(10) -0.0008(8) 0.0067(8) 0.0004(8) C12 0.0106(9) 0.0139(10) 0.0177(11) -0.0002(8) 0.0045(8) 0.0003(8) C13 0.0150(10) 0.0162(11) 0.0153(10) 0.0009(9) 0.0042(8) 0.0021(8) C14 0.0169(10) 0.0115(10) 0.0196(11) 0.0002(9) 0.0063(9) -0.0001(8) C15 0.0158(10) 0.0146(11) 0.0165(11) -0.0037(9) 0.0044(9) -0.0018(8) C16 0.0173(10) 0.0156(11) 0.0131(10) -0.0020(8) 0.0054(8) 0.0000(8) C17 0.0272(13) 0.0127(11) 0.0258(12) 0.0016(9) 0.0083(10) -0.0009(9) C18 0.0236(12) 0.0228(13) 0.0269(13) -0.0017(10) 0.0096(10) 0.0053(10) C21 0.0140(10) 0.0129(10) 0.0158(10) -0.0009(8) 0.0066(8) 0.0017(8) C22 0.0152(10) 0.0128(10) 0.0167(11) 0.0006(8) 0.0052(8) 0.0033(8) C23 0.0141(10) 0.0166(11) 0.0166(10) -0.0013(9) 0.0022(8) 0.0020(8) C24 0.0134(10) 0.0183(11) 0.0204(11) -0.0017(9) 0.0042(9) -0.0015(8) C25 0.0162(10) 0.0133(11) 0.0186(11) 0.0017(8) 0.0073(9) 0.0002(8) C26 0.0160(10) 0.0157(11) 0.0135(10) 0.0003(8) 0.0062(8) 0.0010(8) C27 0.0175(11) 0.0214(12) 0.0317(14) -0.0034(10) 0.0043(10) -0.0045(10) C28 0.0170(11) 0.0272(13) 0.0296(13) -0.0002(11) 0.0088(10) 0.0019(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C12 2.051(2) . ? Fe C16 2.056(2) . ? Fe C22 2.056(2) . ? Fe C26 2.057(2) . ? Fe C11 2.094(2) . ? Fe C21 2.108(2) . ? Fe C23 2.115(2) . ? Fe C13 2.117(2) . ? Fe C25 2.125(2) . ? Fe C15 2.133(2) . ? Fe Fe 5.4956(7) 3 ? Si C21 1.876(2) 3 ? Si C2 1.876(2) . ? Si C11 1.876(2) . ? Si C1 1.877(2) . ? C11 C12 1.431(3) . ? C11 C16 1.440(3) . ? C12 C13 1.402(3) . ? C13 C14 1.519(3) . ? C14 C15 1.515(3) . ? C14 C17 1.527(3) . ? C14 C18 1.538(3) . ? C15 C16 1.406(3) . ? C21 C22 1.432(3) . ? C21 C26 1.437(3) . ? C21 Si 1.876(2) 3 ? C22 C23 1.407(3) . ? C23 C24 1.515(3) . ? C24 C25 1.514(3) . ? C24 C27 1.529(3) . ? C24 C28 1.534(3) . ? C25 C26 1.401(3) . ? 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 C12 Fe C16 71.88(9) . . ? C12 Fe C22 123.30(9) . . ? C16 Fe C22 109.84(9) . . ? C12 Fe C26 110.43(9) . . ? C16 Fe C26 176.06(9) . . ? C22 Fe C26 71.79(9) . . ? C12 Fe C11 40.38(8) . . ? C16 Fe C11 40.59(8) . . ? C22 Fe C11 103.63(9) . . ? C26 Fe C11 143.05(9) . . ? C12 Fe C21 104.38(9) . . ? C16 Fe C21 142.87(9) . . ? C22 Fe C21 40.20(8) . . ? C26 Fe C21 40.35(8) . . ? C11 Fe C21 113.50(8) . . ? C12 Fe C23 156.05(9) . . ? C16 Fe C23 97.07(9) . . ? C22 Fe C23 39.38(9) . . ? C26 Fe C23 81.94(9) . . ? C11 Fe C23 118.46(9) . . ? C21 Fe C23 71.27(9) . . ? C12 Fe C13 39.28(9) . . ? C16 Fe C13 82.15(9) . . ? C22 Fe C13 156.18(9) . . ? C26 Fe C13 97.66(9) . . ? C11 Fe C13 71.60(9) . . ? C21 Fe C13 119.05(9) . . ? C23 Fe C13 162.94(9) . . ? C12 Fe C25 136.09(9) . . ? C16 Fe C25 137.07(9) . . ? C22 Fe C25 82.55(9) . . ? C26 Fe C25 39.09(9) . . ? C11 Fe C25 173.80(9) . . ? C21 Fe C25 71.49(8) . . ? C23 Fe C25 66.12(9) . . ? C13 Fe C25 102.92(9) . . ? C12 Fe C15 82.16(9) . . ? C16 Fe C15 39.17(9) . . ? C22 Fe C15 136.03(9) . . ? C26 Fe C15 137.28(9) . . ? C11 Fe C15 71.66(9) . . ? C21 Fe C15 173.46(9) . . ? C23 Fe C15 102.91(9) . . ? C13 Fe C15 65.86(9) . . ? C25 Fe C15 103.65(9) . . ? C12 Fe Fe 63.43(6) . 3 ? C16 Fe Fe 93.85(6) . 3 ? C22 Fe Fe 59.89(6) . 3 ? C26 Fe Fe 90.06(6) . 3 ? C11 Fe Fe 58.74(6) . 3 ? C21 Fe Fe 54.76(6) . 3 ? C23 Fe Fe 97.22(6) . 3 ? C13 Fe Fe 99.85(6) . 3 ? C25 Fe Fe 126.12(6) . 3 ? C15 Fe Fe 130.23(6) . 3 ? C21 Si C2 104.59(11) 3 . ? C21 Si C11 116.65(10) 3 . ? C2 Si C11 106.60(11) . . ? C21 Si C1 110.54(11) 3 . ? C2 Si C1 106.98(12) . . ? C11 Si C1 110.78(11) . . ? C12 C11 C16 114.19(19) . . ? C12 C11 Si 126.92(17) . . ? C16 C11 Si 118.89(16) . . ? C12 C11 Fe 68.19(12) . . ? C16 C11 Fe 68.28(12) . . ? Si C11 Fe 133.53(12) . . ? C13 C12 C11 120.8(2) . . ? C13 C12 Fe 72.92(13) . . ? C11 C12 Fe 71.43(12) . . ? C12 C13 C14 119.8(2) . . ? C12 C13 Fe 67.80(12) . . ? C14 C13 Fe 96.24(14) . . ? C15 C14 C13 99.19(17) . . ? C15 C14 C17 111.05(19) . . ? C13 C14 C17 111.45(19) . . ? C15 C14 C18 113.20(19) . . ? C13 C14 C18 112.64(19) . . ? C17 C14 C18 109.07(19) . . ? C16 C15 C14 119.6(2) . . ? C16 C15 Fe 67.43(12) . . ? C14 C15 Fe 95.70(14) . . ? C15 C16 C11 120.8(2) . . ? C15 C16 Fe 73.40(13) . . ? C11 C16 Fe 71.13(12) . . ? C22 C21 C26 114.3(2) . . ? C22 C21 Si 128.53(17) . 3 ? C26 C21 Si 116.86(16) . 3 ? C22 C21 Fe 67.92(12) . . ? C26 C21 Fe 67.89(12) . . ? Si C21 Fe 138.53(12) 3 . ? C23 C22 C21 120.2(2) . . ? C23 C22 Fe 72.58(13) . . ? C21 C22 Fe 71.88(12) . . ? C22 C23 C24 119.7(2) . . ? C22 C23 Fe 68.04(12) . . ? C24 C23 Fe 95.91(14) . . ? C25 C24 C23 99.57(17) . . ? C25 C24 C27 111.1(2) . . ? C23 C24 C27 110.72(19) . . ? C25 C24 C28 113.4(2) . . ? C23 C24 C28 112.7(2) . . ? C27 C24 C28 109.02(19) . . ? C26 C25 C24 118.7(2) . . ? C26 C25 Fe 67.81(12) . . ? C24 C25 Fe 95.52(14) . . ? C25 C26 C21 121.3(2) . . ? C25 C26 Fe 73.10(13) . . ? C21 C26 Fe 71.76(12) . . ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-07-09 at 14:56:38 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : c:\wingx\files\archive.dat # CIF files read : th159 struct data_th159 _database_code_CSD 170502 _audit_creation_date 2001-07-09T14:56:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H26 Fe1 Si1' _chemical_formula_structural 'C18 H26 FE1 SI1' _chemical_formula_sum 'C72 H104 Fe4 Si4' _chemical_formula_weight 1305.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n' _symmetry_space_group_name_Hall 'P 4ab -1ab' _symmetry_Int_Tables_number 85 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 19.2430(10) _cell_length_b 19.2430(10) _cell_length_c 9.6490(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3573.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.901 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 4072 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0484 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 4072 _reflns_number_gt 2998 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0318P)^2^+2.0182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0002(5) _refine_ls_number_reflns 4072 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.06 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.379 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fe Fe 0.030844(14) 0.326878(14) -0.16263(3) 0.01740(10) Uani 1 1 d . . . Si Si 0.15954(3) 0.43296(3) -0.33505(6) 0.02026(14) Uani 1 1 d . . . C1 C 0.09919(12) 0.49441(14) -0.4249(3) 0.0404(6) Uani 1 1 d . . . H1A H 0.0873 0.5327 -0.3622 0.061 Uiso 1 1 calc R . . H1B H 0.0568 0.4697 -0.4518 0.061 Uiso 1 1 calc R . . H1C H 0.1219 0.5131 -0.5079 0.061 Uiso 1 1 calc R . . C2 C 0.18773(12) 0.36529(13) -0.4603(2) 0.0324(5) Uani 1 1 d . . . H2A H 0.2168 0.3866 -0.532 0.049 Uiso 1 1 calc R . . H2B H 0.1468 0.3441 -0.5034 0.049 Uiso 1 1 calc R . . H2C H 0.2145 0.3295 -0.4115 0.049 Uiso 1 1 calc R . . C11 C 0.11496(10) 0.39499(10) -0.1805(2) 0.0191(4) Uani 1 1 d . . . C12 C 0.13502(10) 0.33113(10) -0.1155(2) 0.0193(4) Uani 1 1 d . . . H12 H 0.1717 0.3043 -0.1539 0.023 Uiso 1 1 calc R . . C13 C 0.10091(11) 0.30781(11) 0.0043(2) 0.0235(4) Uani 1 1 d . . . H13 H 0.0986 0.2595 0.0241 0.028 Uiso 1 1 calc R . . C14 C 0.06775(13) 0.35969(12) 0.1020(2) 0.0312(5) Uani 1 1 d . . . C15 C 0.02457(12) 0.40130(11) 0.0005(2) 0.0285(5) Uani 1 1 d . . . H15 H -0.0234 0.4091 0.0179 0.034 Uiso 1 1 calc R . . C16 C 0.05549(11) 0.42827(11) -0.1192(2) 0.0242(5) Uani 1 1 d . . . H16 H 0.037 0.4691 -0.1605 0.029 Uiso 1 1 calc R . . C17 C 0.02179(16) 0.32186(14) 0.2080(3) 0.0444(7) Uani 1 1 d . . . H17A H 0.051 0.2932 0.2685 0.067 Uiso 1 1 calc R . . H17B H -0.0115 0.2921 0.1591 0.067 Uiso 1 1 calc R . . H17C H -0.0034 0.3561 0.2639 0.067 Uiso 1 1 calc R . . C18 C 0.12046(15) 0.40513(14) 0.1787(3) 0.0424(6) Uani 1 1 d . . . H18A H 0.1522 0.3755 0.2318 0.064 Uiso 1 1 calc R . . H18B H 0.0959 0.4365 0.2419 0.064 Uiso 1 1 calc R . . H18C H 0.1471 0.4325 0.1114 0.064 Uiso 1 1 calc R . . C21 C 0.01441(10) 0.23625(10) -0.2778(2) 0.0203(4) Uani 1 1 d . . . C22 C -0.02314(10) 0.23480(11) -0.1500(2) 0.0243(5) Uani 1 1 d . . . H22 H -0.0158 0.1978 -0.0865 0.029 Uiso 1 1 calc R . . C23 C -0.07061(11) 0.28749(12) -0.1175(3) 0.0303(5) Uani 1 1 d . . . H23 H -0.0804 0.2985 -0.0236 0.036 Uiso 1 1 calc R . . C24 C -0.10630(11) 0.32681(13) -0.2338(3) 0.0370(6) Uani 1 1 d . . . C25 C -0.04389(10) 0.34812(11) -0.3186(2) 0.0261(5) Uani 1 1 d . . . H25 H -0.0373 0.3954 -0.3434 0.031 Uiso 1 1 calc R . . C26 C 0.00426(10) 0.29752(10) -0.3605(2) 0.0212(4) Uani 1 1 d . . . H26 H 0.0301 0.3038 -0.4435 0.025 Uiso 1 1 calc R . . C27 C -0.14457(14) 0.39074(15) -0.1774(4) 0.0549(8) Uani 1 1 d . . . H27A H -0.1801 0.3759 -0.111 0.082 Uiso 1 1 calc R . . H27B H -0.1667 0.4157 -0.2541 0.082 Uiso 1 1 calc R . . H27C H -0.1113 0.4215 -0.1309 0.082 Uiso 1 1 calc R . . C28 C -0.15694(14) 0.28042(18) -0.3148(4) 0.0606(9) Uani 1 1 d . . . H28A H -0.194 0.2644 -0.2529 0.091 Uiso 1 1 calc R . . H28B H -0.1319 0.2402 -0.352 0.091 Uiso 1 1 calc R . . H28C H -0.1773 0.307 -0.3914 0.091 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 Fe 0.01532(16) 0.01609(16) 0.02077(16) -0.00095(12) 0.00236(12) 0.00094(10) Si 0.0175(3) 0.0234(3) 0.0199(3) 0.0047(2) -0.0034(2) -0.0019(2) C1 0.0272(12) 0.0501(16) 0.0440(16) 0.0210(13) -0.0077(11) 0.0017(11) C2 0.0310(12) 0.0416(14) 0.0246(12) -0.0062(10) 0.0023(10) -0.0124(10) C11 0.0180(9) 0.0188(10) 0.0206(11) -0.0005(8) -0.0017(8) -0.0026(7) C12 0.0167(9) 0.0225(10) 0.0187(10) -0.0017(8) -0.0029(8) 0.0002(8) C13 0.0285(11) 0.0221(10) 0.0199(10) 0.0006(8) -0.0026(9) -0.0033(8) C14 0.0412(14) 0.0310(12) 0.0215(12) -0.0043(9) 0.0078(10) -0.0053(10) C15 0.0320(12) 0.0229(11) 0.0304(13) -0.0090(9) 0.0096(10) -0.0006(9) C16 0.0279(11) 0.0154(10) 0.0295(12) -0.0044(8) 0.0016(9) -0.0004(8) C17 0.0604(18) 0.0477(16) 0.0250(12) 0.0009(12) 0.0155(12) -0.0040(13) C18 0.0594(17) 0.0458(15) 0.0219(13) -0.0085(11) 0.0007(12) -0.0063(13) C21 0.0158(9) 0.0196(10) 0.0255(11) -0.0030(8) -0.0041(8) -0.0018(7) C22 0.0190(10) 0.0194(10) 0.0345(12) 0.0012(9) 0.0030(9) -0.0052(8) C23 0.0203(11) 0.0286(12) 0.0420(14) -0.0014(10) 0.0107(10) -0.0030(9) C24 0.0167(11) 0.0367(13) 0.0577(17) 0.0045(12) 0.0038(11) 0.0050(9) C25 0.0173(10) 0.0244(11) 0.0367(13) 0.0009(9) -0.0062(9) 0.0035(8) C26 0.0174(10) 0.0237(10) 0.0223(11) -0.0009(8) -0.0065(8) 0.0000(8) C27 0.0287(13) 0.0541(18) 0.082(2) 0.0083(16) 0.0164(15) 0.0206(12) C28 0.0220(13) 0.072(2) 0.088(3) 0.0096(18) -0.0127(15) -0.0107(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C16 2.051(2) . ? Fe C26 2.056(2) . ? Fe C12 2.057(2) . ? Fe C22 2.057(2) . ? Fe C11 2.0898(19) . ? Fe C21 2.092(2) . ? Fe C25 2.121(2) . ? Fe C15 2.131(2) . ? Fe C13 2.132(2) . ? Fe C23 2.139(2) . ? Si C2 1.857(2) . ? Si C11 1.870(2) . ? Si C1 1.871(2) . ? Si C21 1.873(2) 4 ? C11 C12 1.432(3) . ? C11 C16 1.438(3) . ? C12 C13 1.403(3) . ? C13 C14 1.514(3) . ? C14 C15 1.514(3) . ? C14 C18 1.530(3) . ? C14 C17 1.535(3) . ? C15 C16 1.398(3) . ? C21 C22 1.429(3) . ? C21 C26 1.437(3) . ? C21 Si 1.873(2) 3 ? C22 C23 1.400(3) . ? C23 C24 1.517(4) . ? C24 C25 1.510(3) . ? C24 C27 1.534(3) . ? C24 C28 1.536(4) . ? C25 C26 1.404(3) . ? 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 C16 Fe C26 120.59(9) . . ? C16 Fe C12 72.04(8) . . ? C26 Fe C12 117.30(8) . . ? C16 Fe C22 157.47(9) . . ? C26 Fe C22 72.11(9) . . ? C12 Fe C22 120.87(8) . . ? C16 Fe C11 40.64(8) . . ? C26 Fe C11 106.78(8) . . ? C12 Fe C11 40.40(8) . . ? C22 Fe C11 159.39(8) . . ? C16 Fe C21 159.48(9) . . ? C26 Fe C21 40.54(8) . . ? C12 Fe C21 107.32(8) . . ? C22 Fe C21 40.29(8) . . ? C11 Fe C21 126.61(8) . . ? C16 Fe C25 96.81(9) . . ? C26 Fe C25 39.23(8) . . ? C12 Fe C25 144.07(9) . . ? C22 Fe C25 82.28(9) . . ? C11 Fe C25 110.24(8) . . ? C21 Fe C25 71.42(8) . . ? C16 Fe C15 39.01(8) . . ? C26 Fe C15 148.91(9) . . ? C12 Fe C15 82.26(9) . . ? C22 Fe C15 120.41(9) . . ? C11 Fe C15 71.53(8) . . ? C21 Fe C15 160.70(9) . . ? C25 Fe C15 110.85(9) . . ? C16 Fe C13 82.13(8) . . ? C26 Fe C13 144.25(8) . . ? C12 Fe C13 39.08(8) . . ? C22 Fe C13 97.25(8) . . ? C11 Fe C13 71.35(8) . . ? C21 Fe C13 110.69(8) . . ? C25 Fe C13 176.11(9) . . ? C15 Fe C13 66.03(9) . . ? C16 Fe C23 120.43(9) . . ? C26 Fe C23 82.21(9) . . ? C12 Fe C23 149.15(9) . . ? C22 Fe C23 38.92(8) . . ? C11 Fe C23 161.06(8) . . ? C21 Fe C23 71.01(8) . . ? C25 Fe C23 66.04(9) . . ? C15 Fe C23 92.07(9) . . ? C13 Fe C23 111.25(9) . . ? C2 Si C11 112.28(10) . . ? C2 Si C1 108.84(13) . . ? C11 Si C1 109.39(11) . . ? C2 Si C21 109.92(10) . 4 ? C11 Si C21 109.72(9) . 4 ? C1 Si C21 106.52(11) . 4 ? C12 C11 C16 114.62(18) . . ? C12 C11 Si 124.10(15) . . ? C16 C11 Si 121.27(15) . . ? C12 C11 Fe 68.57(11) . . ? C16 C11 Fe 68.24(11) . . ? Si C11 Fe 131.78(11) . . ? C13 C12 C11 120.57(19) . . ? C13 C12 Fe 73.35(12) . . ? C11 C12 Fe 71.02(11) . . ? C12 C13 C14 119.97(19) . . ? C12 C13 Fe 67.57(11) . . ? C14 C13 Fe 95.20(14) . . ? C15 C14 C13 100.18(18) . . ? C15 C14 C18 112.0(2) . . ? C13 C14 C18 113.5(2) . . ? C15 C14 C17 111.4(2) . . ? C13 C14 C17 110.2(2) . . ? C18 C14 C17 109.3(2) . . ? C16 C15 C14 119.8(2) . . ? C16 C15 Fe 67.41(12) . . ? C14 C15 Fe 95.25(13) . . ? C15 C16 C11 120.8(2) . . ? C15 C16 Fe 73.58(12) . . ? C11 C16 Fe 71.12(11) . . ? C22 C21 C26 115.25(18) . . ? C22 C21 Si 120.83(15) . 3 ? C26 C21 Si 123.76(16) . 3 ? C22 C21 Fe 68.57(11) . . ? C26 C21 Fe 68.40(11) . . ? Si C21 Fe 137.05(11) 3 . ? C23 C22 C21 120.6(2) . . ? C23 C22 Fe 73.69(12) . . ? C21 C22 Fe 71.14(11) . . ? C22 C23 C24 119.4(2) . . ? C22 C23 Fe 67.39(11) . . ? C24 C23 Fe 94.93(14) . . ? C25 C24 C23 100.14(17) . . ? C25 C24 C27 110.9(2) . . ? C23 C24 C27 110.8(2) . . ? C25 C24 C28 112.7(2) . . ? C23 C24 C28 112.0(2) . . ? C27 C24 C28 110.0(2) . . ? C26 C25 C24 119.5(2) . . ? C26 C25 Fe 67.88(12) . . ? C24 C25 Fe 95.87(15) . . ? C25 C26 C21 119.9(2) . . ? C25 C26 Fe 72.89(13) . . ? C21 C26 Fe 71.06(12) . . ?