Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kawaguchi, Hiroyuki' 'Matsuo, Tsukasa' _publ_contact_author_name 'Prof Hiroyuki Kawaguchi' _publ_contact_author_address ; Coordination Chemistry Laboratories Institute for Molecular Science Myodaiji Okazaki Aichi 444-8585 JAPAN ; _publ_contact_author_email hkawa@ims.ac.jp _publ_contact_author_fax +81-564-55-5245 _publ_contact_author_phone +81-564-55-7290 _publ_contact_letter ; ? ; _publ_requested_journal 'Chemical Communications' _publ_section_title ; Double-stranded binuclear iron(II) complex from a linked-bis(amidenate) ligand: Synthesis and its reaction with carbon monoxide ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 2.00. MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; data_Fe2(L)2 _database_code_CSD 176896 _audit_creation_date 'Thu Mar 7 16:06:07 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C52 H76 Fe2 N8 Si4 ' _chemical_formula_moiety 'C52 H76 Fe2 N8 Si4 ' _chemical_formula_weight 1037.26 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 23.6648(9) _cell_length_b 18.6585(9) _cell_length_c 13.5164(5) _cell_angle_alpha 90 _cell_angle_beta 92.452(1) _cell_angle_gamma 90 _cell_volume 5962.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9478 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.970 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 28006 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 24.78 _diffrn_measured_fraction_theta_max 0.9950 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9927 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _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 7031 _reflns_number_gt 3805 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1110 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6822 _refine_ls_number_parameters 337 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.001Fo^2^ + 0.320\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.79 _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) ; 'N' 'N' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.349 0.972 ;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(1) Fe 0.0000 0.15814(3) 0.2500 0.0359(1) Uani 2.00 d SP . . Fe(2) Fe 0.0000 0.34658(3) 0.2500 0.0360(1) Uani 2.00 d SP . . Si(1) Si 0.13305(3) 0.07480(4) 0.22683(6) 0.0448(2) Uani 1.00 d . . . Si(2) Si -0.11163(3) 0.45074(4) 0.33439(6) 0.0512(2) Uani 1.00 d . . . N(1) N 0.07857(8) 0.1333(1) 0.1978(2) 0.0399(5) Uani 1.00 d . . . N(2) N 0.01150(7) 0.1925(1) 0.1088(1) 0.0360(5) Uani 1.00 d . . . N(3) N -0.05614(7) 0.3169(1) 0.1378(1) 0.0339(5) Uani 1.00 d . . . N(4) N -0.08098(8) 0.3842(1) 0.2666(2) 0.0401(5) Uani 1.00 d . . . C(1) C 0.06419(9) 0.1692(1) 0.1140(2) 0.0353(6) Uani 1.00 d . . . C(2) C -0.09706(9) 0.3502(1) 0.1828(2) 0.0320(5) Uani 1.00 d . . . C(3) C 0.1348(1) 0.0666(2) 0.3639(2) 0.0678(10) Uani 1.00 d . . . C(4) C 0.2046(1) 0.1035(2) 0.1890(3) 0.0709(10) Uani 1.00 d . . . C(5) C 0.1172(2) -0.0142(2) 0.1705(3) 0.0686(10) Uani 1.00 d . . . C(6) C -0.0707(1) 0.4512(2) 0.4555(2) 0.074(1) Uani 1.00 d . . . C(7) C -0.1049(2) 0.5384(2) 0.2721(3) 0.106(1) Uani 1.00 d . . . C(8) C -0.1882(1) 0.4360(2) 0.3583(3) 0.079(1) Uani 1.00 d . . . C(9) C -0.01189(9) 0.2327(1) 0.0236(2) 0.0357(6) Uani 1.00 d . . . C(10) C -0.06593(9) 0.2727(1) 0.0493(2) 0.0333(5) Uani 1.00 d . . . C(11) C -0.0857(1) 0.3167(1) -0.0416(2) 0.0441(7) Uani 1.00 d . . . C(12) C -0.0983(1) 0.2691(2) -0.1316(2) 0.0493(7) Uani 1.00 d . . . C(13) C -0.0471(1) 0.2247(2) -0.1545(2) 0.0538(7) Uani 1.00 d . . . C(14) C -0.0254(1) 0.1830(1) -0.0639(2) 0.0474(7) Uani 1.00 d . . . C(15) C 0.10625(9) 0.1850(1) 0.0369(2) 0.0393(6) Uani 1.00 d . . . C(16) C 0.1326(1) 0.2509(2) 0.0362(2) 0.0503(7) Uani 1.00 d . . . C(17) C 0.1723(1) 0.2656(2) -0.0338(2) 0.0684(10) Uani 1.00 d . . . C(18) C 0.1856(1) 0.2154(2) -0.1025(2) 0.075(1) Uani 1.00 d . . . C(19) C 0.1596(1) 0.1499(2) -0.1023(2) 0.0696(10) Uani 1.00 d . . . C(20) C 0.1201(1) 0.1342(2) -0.0331(2) 0.0530(8) Uani 1.00 d . . . C(21) C -0.15805(9) 0.3487(1) 0.1473(2) 0.0340(5) Uani 1.00 d . . . C(22) C -0.1830(1) 0.4083(1) 0.1019(2) 0.0461(7) Uani 1.00 d . . . C(23) C -0.2393(1) 0.4063(2) 0.0700(2) 0.0540(8) Uani 1.00 d . . . C(24) C -0.2706(1) 0.3457(2) 0.0833(2) 0.0616(8) Uani 1.00 d . . . C(25) C -0.2463(1) 0.2864(2) 0.1287(2) 0.0578(8) Uani 1.00 d . . . C(26) C -0.1900(1) 0.2878(1) 0.1608(2) 0.0429(7) Uani 1.00 d . . . H(1) H 0.0986(1) 0.0482(2) 0.3837(2) 0.080(1) Uiso 1.00 calc . . . H(2) H 0.1646(1) 0.0338(2) 0.3857(2) 0.080(1) Uiso 1.00 calc . . . H(3) H 0.1415(1) 0.1132(2) 0.3939(2) 0.080(1) Uiso 1.00 calc . . . H(4) H 0.2324(1) 0.0675(2) 0.2086(3) 0.083(1) Uiso 1.00 calc . . . H(5) H 0.2039(1) 0.1095(2) 0.1177(3) 0.083(1) Uiso 1.00 calc . . . H(6) H 0.2145(1) 0.1487(2) 0.2208(3) 0.083(1) Uiso 1.00 calc . . . H(7) H 0.0826(2) -0.0326(2) 0.1969(3) 0.081(1) Uiso 1.00 calc . . . H(8) H 0.1125(2) -0.0097(2) 0.0991(3) 0.081(1) Uiso 1.00 calc . . . H(9) H 0.1480(2) -0.0469(2) 0.1868(3) 0.081(1) Uiso 1.00 calc . . . H(10) H -0.0740(1) 0.4048(2) 0.4872(2) 0.087(2) Uiso 1.00 calc . . . H(11) H -0.0312(1) 0.4611(2) 0.4442(2) 0.088(2) Uiso 1.00 calc . . . H(12) H -0.0855(1) 0.4881(2) 0.4980(2) 0.087(2) Uiso 1.00 calc . . . H(13) H -0.0650(2) 0.5486(2) 0.2661(3) 0.116(2) Uiso 1.00 calc . . . H(14) H -0.1234(2) 0.5364(2) 0.2066(3) 0.117(2) Uiso 1.00 calc . . . H(15) H -0.1220(2) 0.5759(2) 0.3105(3) 0.117(2) Uiso 1.00 calc . . . H(16) H -0.2021(1) 0.4758(2) 0.3965(3) 0.091(2) Uiso 1.00 calc . . . H(17) H -0.2097(1) 0.4326(2) 0.2958(3) 0.091(2) Uiso 1.00 calc . . . H(18) H -0.1922(1) 0.3918(2) 0.3952(3) 0.091(2) Uiso 1.00 calc . . . H(19) H 0.01568(9) 0.2678(1) 0.0036(2) 0.042(1) Uiso 1.00 calc . . . H(20) H -0.09484(9) 0.2374(1) 0.0621(2) 0.039(1) Uiso 1.00 calc . . . H(21) H -0.1192(1) 0.3438(1) -0.0264(2) 0.052(1) Uiso 1.00 calc . . . H(22) H -0.0555(1) 0.3495(1) -0.0572(2) 0.052(1) Uiso 1.00 calc . . . H(23) H -0.1288(1) 0.2368(2) -0.1163(2) 0.057(1) Uiso 1.00 calc . . . H(24) H -0.1098(1) 0.2983(2) -0.1885(2) 0.057(1) Uiso 1.00 calc . . . H(25) H -0.0565(1) 0.1919(2) -0.2085(2) 0.062(1) Uiso 1.00 calc . . . H(26) H -0.0174(1) 0.2569(2) -0.1739(2) 0.061(1) Uiso 1.00 calc . . . H(27) H 0.0082(1) 0.1562(1) -0.0792(2) 0.056(1) Uiso 1.00 calc . . . H(28) H -0.0548(1) 0.1500(1) -0.0452(2) 0.056(1) Uiso 1.00 calc . . . H(29) H 0.1229(1) 0.2869(2) 0.0844(2) 0.060(1) Uiso 1.00 calc . . . H(30) H 0.1914(1) 0.3117(2) -0.0332(2) 0.081(1) Uiso 1.00 calc . . . H(31) H 0.2130(1) 0.2261(2) -0.1518(2) 0.086(1) Uiso 1.00 calc . . . H(32) H 0.1690(1) 0.1143(2) -0.1513(2) 0.080(1) Uiso 1.00 calc . . . H(33) H 0.1019(1) 0.0875(2) -0.0327(2) 0.063(1) Uiso 1.00 calc . . . H(34) H -0.1607(1) 0.4513(1) 0.0930(2) 0.054(1) Uiso 1.00 calc . . . H(35) H -0.2566(1) 0.4481(2) 0.0384(2) 0.064(1) Uiso 1.00 calc . . . H(36) H -0.3100(1) 0.3447(2) 0.0601(2) 0.070(1) Uiso 1.00 calc . . . H(37) H -0.2689(1) 0.2438(2) 0.1384(2) 0.066(1) Uiso 1.00 calc . . . H(38) H -0.1727(1) 0.2460(1) 0.1922(2) 0.051(1) 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(1) 0.0339(2) 0.0412(3) 0.0319(3) 0.0000 0.0042(2) 0.0000 Fe(2) 0.0281(2) 0.0440(3) 0.0340(3) 0.0000 -0.0019(2) 0.0000 Si(1) 0.0451(4) 0.0427(4) 0.0463(4) 0.0127(3) -0.0044(3) -0.0049(3) Si(2) 0.0572(4) 0.0485(4) 0.0472(4) 0.0121(3) -0.0005(3) -0.0132(3) N(1) 0.0371(10) 0.042(1) 0.040(1) 0.0095(9) 0.0046(8) 0.0006(8) N(2) 0.0327(9) 0.043(1) 0.0309(10) 0.0055(8) 0.0049(7) 0.0011(8) N(3) 0.0295(9) 0.040(1) 0.0307(10) 0.0028(8) 0.0001(7) -0.0012(8) N(4) 0.0329(9) 0.045(1) 0.041(1) 0.0025(9) -0.0009(8) -0.0098(8) C(1) 0.037(1) 0.036(1) 0.033(1) 0.0040(9) 0.0033(9) -0.0066(9) C(2) 0.0301(10) 0.032(1) 0.034(1) 0.0020(9) 0.0001(8) 0.0019(8) C(3) 0.083(2) 0.065(2) 0.051(2) 0.025(1) -0.016(2) -0.001(2) C(4) 0.044(1) 0.075(2) 0.087(2) 0.016(2) 0.000(1) -0.006(1) C(5) 0.084(2) 0.051(2) 0.067(2) 0.013(1) -0.005(2) -0.009(2) C(6) 0.075(2) 0.087(2) 0.057(2) 0.013(2) -0.009(2) -0.033(2) C(7) 0.154(4) 0.047(2) 0.090(3) 0.004(2) -0.007(3) -0.015(2) C(8) 0.059(2) 0.106(3) 0.062(2) 0.034(2) 0.009(2) -0.014(2) C(9) 0.032(1) 0.045(1) 0.028(1) 0.0020(9) 0.0031(8) 0.0004(9) C(10) 0.0291(10) 0.041(1) 0.028(1) -0.0017(9) 0.0013(8) -0.0007(9) C(11) 0.047(1) 0.051(1) 0.033(1) 0.007(1) -0.003(1) 0.004(1) C(12) 0.051(1) 0.061(2) 0.031(1) -0.005(1) -0.006(1) 0.004(1) C(13) 0.056(2) 0.068(2) 0.029(1) -0.005(1) 0.003(1) -0.006(1) C(14) 0.049(1) 0.055(2) 0.036(1) 0.006(1) 0.004(1) -0.008(1) C(15) 0.032(1) 0.049(1) 0.035(1) 0.006(1) 0.0041(9) -0.0030(10) C(16) 0.042(1) 0.053(1) 0.055(2) -0.001(1) 0.012(1) -0.004(1) C(17) 0.052(2) 0.080(2) 0.070(2) -0.016(2) 0.022(1) -0.001(1) C(18) 0.053(2) 0.104(3) 0.058(2) -0.005(2) 0.026(1) 0.001(2) C(19) 0.056(2) 0.094(2) 0.050(2) 0.007(2) 0.021(1) -0.020(2) C(20) 0.050(1) 0.059(2) 0.050(2) 0.002(1) 0.013(1) -0.013(1) C(21) 0.030(1) 0.038(1) 0.033(1) 0.0043(10) 0.0005(8) -0.0039(9) C(22) 0.037(1) 0.045(1) 0.054(2) 0.003(1) -0.002(1) 0.004(1) C(23) 0.038(1) 0.061(2) 0.060(2) 0.011(1) -0.006(1) 0.012(1) C(24) 0.030(1) 0.075(2) 0.069(2) 0.001(2) -0.006(1) 0.008(1) C(25) 0.034(1) 0.056(2) 0.076(2) -0.009(1) -0.002(1) 0.005(1) C(26) 0.036(1) 0.042(1) 0.049(1) 0.001(1) 0.002(1) 0.003(1) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ORTEP-3 #------------------------------------------------------------------------------ _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(1) N(1) 2.069(2) . . yes Fe(1) N(2) 2.043(2) . . yes Fe(2) N(3) 2.049(2) . . yes Fe(2) N(4) 2.062(2) . . yes Si(1) N(1) 1.722(2) . . yes Si(1) C(3) 1.858(3) . . yes Si(1) C(4) 1.868(3) . . yes Si(1) C(5) 1.859(3) . . yes Si(2) N(4) 1.722(2) . . yes Si(2) C(6) 1.866(3) . . yes Si(2) C(7) 1.850(4) . . yes Si(2) C(8) 1.873(3) . . yes N(1) C(1) 1.346(3) . . yes N(2) C(1) 1.319(3) . . yes N(2) C(9) 1.464(3) . . yes N(3) C(2) 1.321(3) . . yes N(3) C(10) 1.462(3) . . yes N(4) C(2) 1.339(3) . . yes C(1) C(15) 1.501(3) . . yes C(2) C(21) 1.502(3) . . yes C(9) C(10) 1.533(3) . . yes C(9) C(14) 1.526(3) . . yes C(10) C(11) 1.534(3) . . yes C(11) C(12) 1.525(4) . . yes C(12) C(13) 1.511(4) . . yes C(13) C(14) 1.522(4) . . yes C(15) C(16) 1.378(4) . . yes C(15) C(20) 1.389(4) . . yes C(16) C(17) 1.389(4) . . yes C(17) C(18) 1.365(5) . . yes C(18) C(19) 1.368(5) . . yes C(19) C(20) 1.382(4) . . yes C(21) C(22) 1.390(3) . . yes C(21) C(26) 1.381(3) . . yes C(22) C(23) 1.382(3) . . yes C(23) C(24) 1.369(4) . . yes C(24) C(25) 1.380(4) . . yes C(25) C(26) 1.383(3) . . 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 N(1) Fe(1) N(2) 66.03(7) . . . yes N(3) Fe(2) N(4) 66.19(7) . . . yes N(1) Si(1) C(3) 105.3(1) . . . yes N(1) Si(1) C(4) 115.7(1) . . . yes N(1) Si(1) C(5) 109.7(1) . . . yes C(3) Si(1) C(4) 108.4(2) . . . yes C(3) Si(1) C(5) 109.3(1) . . . yes C(4) Si(1) C(5) 108.3(2) . . . yes N(4) Si(2) C(6) 104.8(1) . . . yes N(4) Si(2) C(7) 110.4(2) . . . yes N(4) Si(2) C(8) 114.7(1) . . . yes C(6) Si(2) C(7) 110.1(2) . . . yes C(6) Si(2) C(8) 108.6(1) . . . yes C(7) Si(2) C(8) 108.1(2) . . . yes Fe(1) N(1) Si(1) 137.6(1) . . . yes Fe(1) N(1) C(1) 88.7(1) . . . yes Si(1) N(1) C(1) 131.8(2) . . . yes Fe(1) N(2) C(1) 90.6(1) . . . yes Fe(1) N(2) C(9) 146.6(1) . . . yes C(1) N(2) C(9) 122.4(2) . . . yes Fe(2) N(3) C(2) 89.8(1) . . . yes Fe(2) N(3) C(10) 146.3(1) . . . yes C(2) N(3) C(10) 123.2(2) . . . yes Fe(2) N(4) Si(2) 135.9(1) . . . yes Fe(2) N(4) C(2) 88.8(1) . . . yes Si(2) N(4) C(2) 132.9(2) . . . yes N(1) C(1) N(2) 114.4(2) . . . yes N(1) C(1) C(15) 122.0(2) . . . yes N(2) C(1) C(15) 123.4(2) . . . yes N(3) C(2) N(4) 115.2(2) . . . yes N(3) C(2) C(21) 123.9(2) . . . yes N(4) C(2) C(21) 120.9(2) . . . yes N(2) C(9) C(10) 111.2(2) . . . yes N(2) C(9) C(14) 110.9(2) . . . yes C(10) C(9) C(14) 108.8(2) . . . yes N(3) C(10) C(9) 110.8(2) . . . yes N(3) C(10) C(11) 112.7(2) . . . yes C(9) C(10) C(11) 107.9(2) . . . yes C(10) C(11) C(12) 111.8(2) . . . yes C(11) C(12) C(13) 110.6(2) . . . yes C(12) C(13) C(14) 111.2(2) . . . yes C(9) C(14) C(13) 111.4(2) . . . yes C(1) C(15) C(16) 119.6(2) . . . yes C(1) C(15) C(20) 121.4(2) . . . yes C(16) C(15) C(20) 119.0(2) . . . yes C(15) C(16) C(17) 120.0(3) . . . yes C(16) C(17) C(18) 120.6(3) . . . yes C(17) C(18) C(19) 119.7(3) . . . yes C(18) C(19) C(20) 120.6(3) . . . yes C(15) C(20) C(19) 120.1(3) . . . yes C(2) C(21) C(22) 120.7(2) . . . yes C(2) C(21) C(26) 119.8(2) . . . yes C(22) C(21) C(26) 119.5(2) . . . yes C(21) C(22) C(23) 120.1(2) . . . yes C(22) C(23) C(24) 120.1(3) . . . yes C(23) C(24) C(25) 120.2(2) . . . yes C(24) C(25) C(26) 120.1(2) . . . yes C(21) C(26) C(25) 120.0(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe(1) N(1) Si(1) C(3) -34.6(2) . . . . yes Fe(1) N(1) Si(1) C(4) -154.2(2) . . . . yes Fe(1) N(1) Si(1) C(5) 82.9(2) . . . . yes Fe(1) N(1) C(1) N(2) -5.1(2) . . . . yes Fe(1) N(1) C(1) C(15) 171.0(2) . . . . yes Fe(1) N(2) C(1) N(1) 5.2(2) . . . . yes Fe(1) N(2) C(1) C(15) -170.9(2) . . . . yes Fe(1) N(2) C(9) C(10) 8.0(3) . . . . yes Fe(1) N(2) C(9) C(14) -113.2(3) . . . . yes Fe(2) N(3) C(2) N(4) 2.4(2) . . . . yes Fe(2) N(3) C(2) C(21) -175.2(2) . . . . yes Fe(2) N(3) C(10) C(9) -4.1(3) . . . . yes Fe(2) N(3) C(10) C(11) -125.1(2) . . . . yes Fe(2) N(4) Si(2) C(6) -37.1(2) . . . . yes Fe(2) N(4) Si(2) C(7) 81.4(2) . . . . yes Fe(2) N(4) Si(2) C(8) -156.1(2) . . . . yes Fe(2) N(4) C(2) N(3) -2.3(2) . . . . yes Fe(2) N(4) C(2) C(21) 175.3(2) . . . . yes Si(1) N(1) Fe(1) N(2) -161.5(2) . . . . yes Si(1) N(1) C(1) N(2) 161.1(2) . . . . yes Si(1) N(1) C(1) C(15) -22.7(3) . . . . yes Si(2) N(4) Fe(2) N(3) -161.5(2) . . . . yes Si(2) N(4) C(2) N(3) 161.5(2) . . . . yes Si(2) N(4) C(2) C(21) -20.8(3) . . . . yes N(1) Fe(1) N(2) C(1) -3.4(1) . . . . yes N(1) Fe(1) N(2) C(9) -175.1(3) . . . . yes N(1) C(1) N(2) C(9) 179.8(2) . . . . yes N(1) C(1) C(15) C(16) -96.9(3) . . . . yes N(1) C(1) C(15) C(20) 81.9(3) . . . . yes N(2) Fe(1) N(1) C(1) 3.3(1) . . . . yes N(2) C(1) C(15) C(16) 78.9(3) . . . . yes N(2) C(1) C(15) C(20) -102.3(3) . . . . yes N(2) C(9) C(10) N(3) 53.1(2) . . . . yes N(2) C(9) C(10) C(11) 176.8(2) . . . . yes N(2) C(9) C(14) C(13) -177.3(2) . . . . yes N(3) Fe(2) N(4) C(2) 1.5(1) . . . . yes N(3) C(2) C(21) C(22) -105.8(3) . . . . yes N(3) C(2) C(21) C(26) 75.0(3) . . . . yes N(3) C(10) C(9) C(14) 175.5(2) . . . . yes N(3) C(10) C(11) C(12) -177.3(2) . . . . yes N(4) Fe(2) N(3) C(2) -1.5(1) . . . . yes N(4) Fe(2) N(3) C(10) -171.2(3) . . . . yes N(4) C(2) N(3) C(10) 175.6(2) . . . . yes N(4) C(2) C(21) C(22) 76.8(3) . . . . yes N(4) C(2) C(21) C(26) -102.4(3) . . . . yes C(1) N(1) Si(1) C(3) 166.1(2) . . . . yes C(1) N(1) Si(1) C(4) 46.4(3) . . . . yes C(1) N(1) Si(1) C(5) -76.4(2) . . . . yes C(1) N(2) C(9) C(10) -162.2(2) . . . . yes C(1) N(2) C(9) C(14) 76.5(3) . . . . yes C(1) C(15) C(16) C(17) 178.8(2) . . . . yes C(1) C(15) C(20) C(19) -179.0(2) . . . . yes C(2) N(3) C(10) C(9) -171.7(2) . . . . yes C(2) N(3) C(10) C(11) 67.3(3) . . . . yes C(2) N(4) Si(2) C(6) 166.4(2) . . . . yes C(2) N(4) Si(2) C(7) -75.1(3) . . . . yes C(2) N(4) Si(2) C(8) 47.4(3) . . . . yes C(2) C(21) C(22) C(23) -179.7(2) . . . . yes C(2) C(21) C(26) C(25) 179.6(2) . . . . yes C(9) N(2) C(1) C(15) 3.7(3) . . . . yes C(9) C(10) C(11) C(12) 60.1(2) . . . . yes C(9) C(14) C(13) C(12) -56.3(3) . . . . yes C(10) N(3) C(2) C(21) -2.0(3) . . . . yes C(10) C(9) C(14) C(13) 60.1(3) . . . . yes C(10) C(11) C(12) C(13) -56.5(3) . . . . yes C(11) C(10) C(9) C(14) -60.7(2) . . . . yes C(11) C(12) C(13) C(14) 53.4(3) . . . . yes C(15) C(16) C(17) C(18) 0.2(4) . . . . yes C(15) C(20) C(19) C(18) 0.1(4) . . . . yes C(16) C(15) C(20) C(19) -0.2(4) . . . . yes C(16) C(17) C(18) C(19) -0.2(5) . . . . yes C(17) C(16) C(15) C(20) 0.0(4) . . . . yes C(17) C(18) C(19) C(20) 0.0(5) . . . . yes C(21) C(22) C(23) C(24) 0.3(4) . . . . yes C(21) C(26) C(25) C(24) -0.1(4) . . . . yes C(22) C(21) C(26) C(25) 0.5(4) . . . . yes C(22) C(23) C(24) C(25) 0.1(5) . . . . yes C(23) C(22) C(21) C(26) -0.5(4) . . . . yes C(23) C(24) C(25) C(26) -0.2(5) . . . . yes C(23) C(24) C(25) C(26) -0.2(5) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_Fe2(CO)2(L)2 _database_code_CSD 176897 _audit_creation_date 'Thu Mar 7 16:08:54 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H76 Fe2 N8 O2 Si4 ' _chemical_formula_moiety 'C54 H76 Fe2 N8 O2 Si4 ' _chemical_formula_weight 1093.28 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 23.912(4) _cell_length_b 18.384(2) _cell_length_c 13.4886(5) _cell_angle_alpha 90 _cell_angle_beta 92.6946(9) _cell_angle_gamma 90 _cell_volume 5922(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10277 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.000 _exptl_absorpt_correction_T_max 0.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.32 _diffrn_reflns_number 27945 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9825 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9806 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # 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 6890 _reflns_number_gt 2685 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1270 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6690 _refine_ls_number_parameters 355 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.000Fo^2^ + 0.260\s^2^(Fo)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.69 _refine_diff_density_min -1.00 _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) ; 'N' 'N' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.349 0.972 ;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(1) Fe 0.0000 0.38631(4) 0.2500 0.0312(2) Uani 2.00 d SP . . Fe(2) Fe 0.0000 0.14399(4) 0.2500 0.0319(2) Uani 2.00 d SP . . Si(1) Si 0.13969(5) 0.42551(6) 0.25321(8) 0.0420(3) Uani 1.00 d . . . Si(2) Si -0.10875(5) 0.02524(6) 0.17570(9) 0.0476(3) Uani 1.00 d . . . O(1) O -0.0052(2) 0.5036(2) 0.3939(2) 0.078(1) Uani 1.00 d . . . N(1) N 0.0832(1) 0.3708(2) 0.2790(2) 0.0329(8) Uani 1.00 d . . . N(2) N 0.0185(1) 0.3105(1) 0.3566(2) 0.0282(7) Uani 1.00 d . . . N(3) N -0.0540(1) 0.1850(2) 0.3478(2) 0.0295(8) Uani 1.00 d . . . N(4) N -0.0784(1) 0.0953(2) 0.2428(2) 0.0357(8) Uani 1.00 d . . . C(1) C 0.0720(1) 0.3265(2) 0.3548(2) 0.0306(9) Uani 1.00 d . . . C(2) C -0.0946(1) 0.1422(2) 0.3120(2) 0.0289(9) Uani 1.00 d . . . C(3) C 0.1282(2) 0.5196(2) 0.2983(3) 0.060(1) Uani 1.00 d . . . C(4) C 0.1458(2) 0.4294(3) 0.1163(3) 0.061(1) Uani 1.00 d . . . C(5) C 0.2088(2) 0.3928(3) 0.3070(4) 0.062(1) Uani 1.00 d . . . C(6) C -0.1845(2) 0.0382(3) 0.1416(4) 0.075(2) Uani 1.00 d . . . C(7) C -0.1011(3) -0.0621(3) 0.2439(4) 0.090(2) Uani 1.00 d . . . C(8) C -0.0686(2) 0.0206(3) 0.0614(3) 0.072(2) Uani 1.00 d . . . C(9) C -0.0043(1) 0.2781(2) 0.4462(2) 0.0291(9) Uani 1.00 d . . . C(10) C -0.0600(1) 0.2386(2) 0.4262(2) 0.0308(9) Uani 1.00 d . . . C(11) C -0.0772(2) 0.2045(2) 0.5238(3) 0.041(1) Uani 1.00 d . . . C(12) C -0.0825(2) 0.2603(2) 0.6064(3) 0.049(1) Uani 1.00 d . . . C(13) C -0.0282(2) 0.3033(2) 0.6231(3) 0.046(1) Uani 1.00 d . . . C(14) C -0.0105(2) 0.3360(2) 0.5263(2) 0.038(1) Uani 1.00 d . . . C(15) C 0.1150(1) 0.3041(2) 0.4336(3) 0.036(1) Uani 1.00 d . . . C(16) C 0.1341(2) 0.3557(3) 0.5023(3) 0.052(1) Uani 1.00 d . . . C(17) C 0.1722(2) 0.3370(3) 0.5791(3) 0.072(2) Uani 1.00 d . . . C(18) C 0.1900(2) 0.2667(4) 0.5872(4) 0.083(2) Uani 1.00 d . . . C(19) C 0.1716(2) 0.2148(3) 0.5197(4) 0.072(2) Uani 1.00 d . . . C(20) C 0.1339(2) 0.2333(2) 0.4426(3) 0.047(1) Uani 1.00 d . . . C(21) C -0.1537(1) 0.1464(2) 0.3427(2) 0.0330(9) Uani 1.00 d . . . C(22) C -0.1787(2) 0.0879(2) 0.3876(3) 0.041(1) Uani 1.00 d . . . C(23) C -0.2335(2) 0.0934(3) 0.4184(3) 0.057(1) Uani 1.00 d . . . C(24) C -0.2625(2) 0.1569(3) 0.4029(3) 0.069(2) Uani 1.00 d . . . C(25) C -0.2383(2) 0.2149(3) 0.3572(3) 0.059(1) Uani 1.00 d . . . C(26) C -0.1838(2) 0.2104(2) 0.3266(3) 0.042(1) Uani 1.00 d . . . C(27) C -0.0026(2) 0.4558(2) 0.3399(3) 0.043(1) Uani 1.00 d . . . H(1) H 0.1600(2) 0.5500(2) 0.2839(3) 0.071(2) Uiso 1.00 calc . . . H(2) H 0.0946(2) 0.5392(2) 0.2650(3) 0.071(2) Uiso 1.00 calc . . . H(3) H 0.1236(2) 0.5188(2) 0.3694(3) 0.071(2) Uiso 1.00 calc . . . H(4) H 0.1518(2) 0.3806(3) 0.0915(3) 0.073(2) Uiso 1.00 calc . . . H(5) H 0.1116(2) 0.4491(3) 0.0854(3) 0.073(2) Uiso 1.00 calc . . . H(6) H 0.1771(2) 0.4602(3) 0.1006(3) 0.073(2) Uiso 1.00 calc . . . H(7) H 0.2077(2) 0.3906(3) 0.3788(4) 0.073(2) Uiso 1.00 calc . . . H(8) H 0.2164(2) 0.3447(3) 0.2812(4) 0.073(2) Uiso 1.00 calc . . . H(9) H 0.2382(2) 0.4260(3) 0.2888(4) 0.073(2) Uiso 1.00 calc . . . H(10) H -0.2052(2) 0.0436(3) 0.2014(4) 0.087(2) Uiso 1.00 calc . . . H(11) H -0.1892(2) 0.0816(3) 0.1011(4) 0.087(2) Uiso 1.00 calc . . . H(12) H -0.1986(2) -0.0036(3) 0.1044(4) 0.087(2) Uiso 1.00 calc . . . H(13) H -0.1190(3) -0.0590(3) 0.3069(4) 0.102(2) Uiso 1.00 calc . . . H(14) H -0.1183(3) -0.1008(3) 0.2042(4) 0.102(2) Uiso 1.00 calc . . . H(15) H -0.0616(3) -0.0723(3) 0.2557(4) 0.102(2) Uiso 1.00 calc . . . H(16) H -0.0295(2) 0.0110(3) 0.0795(3) 0.086(2) Uiso 1.00 calc . . . H(17) H -0.0834(2) -0.0183(3) 0.0194(3) 0.086(2) Uiso 1.00 calc . . . H(18) H -0.0717(2) 0.0664(3) 0.0257(3) 0.086(2) Uiso 1.00 calc . . . H(19) H 0.0224(1) 0.2423(2) 0.4721(2) 0.035(1) Uiso 1.00 calc . . . H(20) H -0.0880(1) 0.2741(2) 0.4049(2) 0.037(1) Uiso 1.00 calc . . . H(21) H -0.1127(2) 0.1797(2) 0.5122(3) 0.048(1) Uiso 1.00 calc . . . H(22) H -0.0487(2) 0.1695(2) 0.5446(3) 0.048(1) Uiso 1.00 calc . . . H(23) H -0.1125(2) 0.2939(2) 0.5876(3) 0.057(2) Uiso 1.00 calc . . . H(24) H -0.0912(2) 0.2356(2) 0.6673(3) 0.057(2) Uiso 1.00 calc . . . H(25) H -0.0336(2) 0.3415(2) 0.6713(3) 0.053(2) Uiso 1.00 calc . . . H(26) H 0.0009(2) 0.2705(2) 0.6481(3) 0.053(2) Uiso 1.00 calc . . . H(27) H 0.0248(2) 0.3611(2) 0.5378(2) 0.045(1) Uiso 1.00 calc . . . H(28) H -0.0389(2) 0.3704(2) 0.5029(2) 0.045(1) Uiso 1.00 calc . . . H(29) H 0.1207(2) 0.4054(3) 0.4966(3) 0.062(2) Uiso 1.00 calc . . . H(30) H 0.1859(2) 0.3732(3) 0.6267(3) 0.082(2) Uiso 1.00 calc . . . H(31) H 0.2162(2) 0.2532(4) 0.6413(4) 0.094(2) Uiso 1.00 calc . . . H(32) H 0.1851(2) 0.1652(3) 0.5264(4) 0.086(2) Uiso 1.00 calc . . . H(33) H 0.1204(2) 0.1968(2) 0.3952(3) 0.057(2) Uiso 1.00 calc . . . H(34) H -0.1578(2) 0.0432(2) 0.3985(3) 0.049(1) Uiso 1.00 calc . . . H(35) H -0.2512(2) 0.0525(3) 0.4501(3) 0.066(2) Uiso 1.00 calc . . . H(36) H -0.3004(2) 0.1612(3) 0.4252(3) 0.077(2) Uiso 1.00 calc . . . H(37) H -0.2598(2) 0.2591(3) 0.3451(3) 0.069(2) Uiso 1.00 calc . . . H(38) H -0.1662(2) 0.2515(2) 0.2953(3) 0.050(1) 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(1) 0.0384(4) 0.0277(4) 0.0258(4) 0.0000 -0.0007(3) 0.0000 Fe(2) 0.0282(4) 0.0325(4) 0.0346(4) 0.0000 0.0071(3) 0.0000 Si(1) 0.0436(6) 0.0372(6) 0.0449(6) -0.0145(5) 0.0035(5) -0.0015(5) Si(2) 0.0491(7) 0.0432(7) 0.0503(7) -0.0129(5) 0.0094(5) -0.0163(5) O(1) 0.119(3) 0.036(2) 0.052(2) -0.002(1) 0.005(2) -0.016(2) N(1) 0.038(2) 0.028(2) 0.033(2) -0.006(1) -0.001(1) 0.001(1) N(2) 0.033(2) 0.025(2) 0.026(1) -0.005(1) 0.003(1) 0.000(1) N(3) 0.029(1) 0.028(2) 0.031(1) -0.003(1) 0.004(1) -0.003(1) N(4) 0.030(2) 0.035(2) 0.042(2) -0.004(1) 0.007(1) -0.010(1) C(1) 0.035(2) 0.026(2) 0.030(2) -0.001(1) -0.001(1) -0.003(2) C(2) 0.029(2) 0.029(2) 0.028(2) 0.001(2) 0.003(1) 0.003(2) C(3) 0.068(3) 0.044(3) 0.066(3) -0.021(2) -0.001(2) -0.006(2) C(4) 0.065(3) 0.064(3) 0.053(3) -0.029(2) 0.012(2) -0.001(2) C(5) 0.042(2) 0.064(3) 0.075(3) -0.017(3) 0.000(2) -0.004(2) C(6) 0.056(3) 0.098(4) 0.064(3) -0.035(3) -0.001(2) -0.024(3) C(7) 0.113(5) 0.045(3) 0.097(4) -0.011(3) 0.011(3) -0.016(3) C(8) 0.074(3) 0.076(4) 0.065(3) -0.017(3) 0.019(3) -0.034(3) C(9) 0.034(2) 0.026(2) 0.027(2) 0.003(1) -0.002(1) 0.001(1) C(10) 0.032(2) 0.031(2) 0.030(2) 0.001(2) 0.004(1) -0.004(2) C(11) 0.044(2) 0.044(2) 0.032(2) -0.003(2) 0.009(2) 0.000(2) C(12) 0.057(2) 0.053(3) 0.034(2) 0.004(2) 0.013(2) -0.001(2) C(13) 0.056(2) 0.046(2) 0.032(2) 0.008(2) 0.003(2) -0.007(2) C(14) 0.046(2) 0.033(2) 0.032(2) -0.002(2) -0.001(2) -0.006(2) C(15) 0.034(2) 0.039(2) 0.034(2) 0.000(2) -0.001(2) -0.001(2) C(16) 0.045(2) 0.056(3) 0.053(2) 0.001(2) -0.011(2) -0.010(2) C(17) 0.055(3) 0.098(4) 0.053(3) 0.007(3) -0.019(2) -0.019(3) C(18) 0.064(3) 0.115(5) 0.057(3) 0.033(3) -0.029(2) -0.008(3) C(19) 0.068(3) 0.081(4) 0.065(3) 0.032(3) -0.013(2) 0.005(3) C(20) 0.042(2) 0.051(2) 0.048(2) 0.010(2) -0.005(2) -0.001(2) C(21) 0.028(2) 0.040(2) 0.030(2) -0.002(2) 0.002(1) -0.001(2) C(22) 0.034(2) 0.046(2) 0.043(2) -0.003(2) 0.005(2) 0.005(2) C(23) 0.035(2) 0.076(3) 0.053(3) -0.014(2) 0.009(2) 0.013(2) C(24) 0.033(2) 0.093(4) 0.067(3) 0.006(3) 0.014(2) 0.007(2) C(25) 0.040(2) 0.066(3) 0.067(3) 0.015(2) 0.005(2) 0.001(2) C(26) 0.036(2) 0.045(2) 0.044(2) 0.000(2) 0.003(2) 0.001(2) C(27) 0.058(3) 0.032(2) 0.034(2) 0.001(2) -0.003(2) 0.005(2) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ORTEP-3 #------------------------------------------------------------------------------ _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(1) N(1) 2.029(3) . . yes Fe(1) N(2) 2.036(3) . . yes Fe(1) C(27) 1.764(4) . . yes Fe(2) N(3) 2.034(3) . . yes Fe(2) N(4) 2.076(3) . . yes Si(1) N(1) 1.732(3) . . yes Si(1) C(3) 1.859(4) . . yes Si(1) C(4) 1.860(4) . . yes Si(1) C(5) 1.873(4) . . yes Si(2) N(4) 1.716(3) . . yes Si(2) C(6) 1.863(4) . . yes Si(2) C(7) 1.855(5) . . yes Si(2) C(8) 1.856(5) . . yes O(1) C(27) 1.146(5) . . yes N(1) C(1) 1.344(4) . . yes N(2) C(1) 1.314(4) . . yes N(2) C(9) 1.474(4) . . yes N(3) C(2) 1.322(4) . . yes N(3) C(10) 1.458(4) . . yes N(4) C(2) 1.340(4) . . yes C(1) C(15) 1.503(5) . . yes C(2) C(21) 1.495(4) . . yes C(9) C(10) 1.529(4) . . yes C(9) C(14) 1.529(5) . . yes C(10) C(11) 1.531(5) . . yes C(11) C(12) 1.525(5) . . yes C(12) C(13) 1.526(6) . . yes C(13) C(14) 1.516(5) . . yes C(15) C(16) 1.388(6) . . yes C(15) C(20) 1.381(6) . . yes C(16) C(17) 1.390(6) . . yes C(17) C(18) 1.363(9) . . yes C(18) C(19) 1.377(8) . . yes C(19) C(20) 1.388(6) . . yes C(21) C(22) 1.384(5) . . yes C(21) C(26) 1.390(5) . . yes C(22) C(23) 1.395(5) . . yes C(23) C(24) 1.371(7) . . yes C(24) C(25) 1.372(7) . . yes C(25) C(26) 1.389(6) . . 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 N(1) Fe(1) N(2) 65.8(1) . . . yes N(1) Fe(1) C(27) 92.0(2) . . . yes N(2) Fe(1) C(27) 91.4(1) . . . yes N(3) Fe(2) N(4) 65.8(1) . . . yes N(1) Si(1) C(3) 110.2(2) . . . yes N(1) Si(1) C(4) 108.6(2) . . . yes N(1) Si(1) C(5) 114.7(2) . . . yes C(3) Si(1) C(4) 108.0(2) . . . yes C(3) Si(1) C(5) 108.3(2) . . . yes C(4) Si(1) C(5) 106.8(2) . . . yes N(4) Si(2) C(6) 114.6(2) . . . yes N(4) Si(2) C(7) 111.0(2) . . . yes N(4) Si(2) C(8) 104.5(2) . . . yes C(6) Si(2) C(7) 107.8(3) . . . yes C(6) Si(2) C(8) 109.6(2) . . . yes C(7) Si(2) C(8) 109.2(2) . . . yes Fe(1) N(1) Si(1) 130.3(2) . . . yes Fe(1) N(1) C(1) 90.1(2) . . . yes Si(1) N(1) C(1) 133.6(2) . . . yes Fe(1) N(2) C(1) 90.7(2) . . . yes Fe(1) N(2) C(9) 141.2(2) . . . yes C(1) N(2) C(9) 120.3(3) . . . yes Fe(2) N(3) C(2) 91.1(2) . . . yes Fe(2) N(3) C(10) 143.9(2) . . . yes C(2) N(3) C(10) 124.9(3) . . . yes Fe(2) N(4) Si(2) 135.0(2) . . . yes Fe(2) N(4) C(2) 88.8(2) . . . yes Si(2) N(4) C(2) 136.2(2) . . . yes N(1) C(1) N(2) 112.3(3) . . . yes N(1) C(1) C(15) 123.3(3) . . . yes N(2) C(1) C(15) 124.1(3) . . . yes N(3) C(2) N(4) 114.0(3) . . . yes N(3) C(2) C(21) 123.7(3) . . . yes N(4) C(2) C(21) 122.3(3) . . . yes N(2) C(9) C(10) 113.6(2) . . . yes N(2) C(9) C(14) 110.5(3) . . . yes C(10) C(9) C(14) 110.0(3) . . . yes N(3) C(10) C(9) 109.5(3) . . . yes N(3) C(10) C(11) 112.7(3) . . . yes C(9) C(10) C(11) 108.1(3) . . . yes C(10) C(11) C(12) 112.8(3) . . . yes C(11) C(12) C(13) 110.9(3) . . . yes C(12) C(13) C(14) 110.4(3) . . . yes C(9) C(14) C(13) 111.9(3) . . . yes C(1) C(15) C(16) 118.6(3) . . . yes C(1) C(15) C(20) 122.0(3) . . . yes C(16) C(15) C(20) 119.4(3) . . . yes C(15) C(16) C(17) 120.8(4) . . . yes C(16) C(17) C(18) 119.0(5) . . . yes C(17) C(18) C(19) 121.0(4) . . . yes C(18) C(19) C(20) 120.2(5) . . . yes C(15) C(20) C(19) 119.7(4) . . . yes C(2) C(21) C(22) 121.0(3) . . . yes C(2) C(21) C(26) 119.3(3) . . . yes C(22) C(21) C(26) 119.7(3) . . . yes C(21) C(22) C(23) 120.3(4) . . . yes C(22) C(23) C(24) 119.4(4) . . . yes C(23) C(24) C(25) 120.6(4) . . . yes C(24) C(25) C(26) 120.6(4) . . . yes C(21) C(26) C(25) 119.3(4) . . . yes Fe(1) C(27) O(1) 176.1(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe(1) N(1) Si(1) C(3) 51.1(3) . . . . yes Fe(1) N(1) Si(1) C(4) -67.1(3) . . . . yes Fe(1) N(1) Si(1) C(5) 173.6(2) . . . . yes Fe(1) N(1) C(1) N(2) 9.6(3) . . . . yes Fe(1) N(1) C(1) C(15) -164.8(3) . . . . yes Fe(1) N(2) C(1) N(1) -9.5(3) . . . . yes Fe(1) N(2) C(1) C(15) 164.8(3) . . . . yes Fe(1) N(2) C(9) C(10) 62.0(4) . . . . yes Fe(1) N(2) C(9) C(14) -62.1(4) . . . . yes Fe(2) N(3) C(2) N(4) 4.7(3) . . . . yes Fe(2) N(3) C(2) C(21) -173.5(3) . . . . yes Fe(2) N(3) C(10) C(9) -2.9(5) . . . . yes Fe(2) N(3) C(10) C(11) -123.3(3) . . . . yes Fe(2) N(4) Si(2) C(6) -145.1(2) . . . . yes Fe(2) N(4) Si(2) C(7) 92.5(3) . . . . yes Fe(2) N(4) Si(2) C(8) -25.2(3) . . . . yes Fe(2) N(4) C(2) N(3) -4.6(3) . . . . yes Fe(2) N(4) C(2) C(21) 173.6(3) . . . . yes Si(1) N(1) Fe(1) N(2) -161.3(2) . . . . yes Si(1) N(1) Fe(1) C(27) -70.7(2) . . . . yes Si(1) N(1) C(1) N(2) 163.2(3) . . . . yes Si(1) N(1) C(1) C(15) -11.2(5) . . . . yes Si(2) N(4) Fe(2) N(3) -177.3(3) . . . . yes Si(2) N(4) C(2) N(3) 175.7(3) . . . . yes Si(2) N(4) C(2) C(21) -6.1(5) . . . . yes O(1) C(27) Fe(1) N(1) 116(5) . . . . yes O(1) C(27) Fe(1) N(2) -177(5) . . . . yes N(1) Fe(1) N(2) C(1) 6.4(2) . . . . yes N(1) Fe(1) N(2) C(9) 151.4(3) . . . . yes N(1) C(1) N(2) C(9) -164.9(3) . . . . yes N(1) C(1) C(15) C(16) 70.9(5) . . . . yes N(1) C(1) C(15) C(20) -112.5(4) . . . . yes N(2) Fe(1) N(1) C(1) -6.2(2) . . . . yes N(2) C(1) C(15) C(16) -102.9(4) . . . . yes N(2) C(1) C(15) C(20) 73.8(5) . . . . yes N(2) C(9) C(10) N(3) 54.0(3) . . . . yes N(2) C(9) C(10) C(11) 177.1(3) . . . . yes N(2) C(9) C(14) C(13) -174.2(3) . . . . yes N(3) Fe(2) N(4) C(2) 3.0(2) . . . . yes N(3) C(2) C(21) C(22) -118.7(4) . . . . yes N(3) C(2) C(21) C(26) 60.8(4) . . . . yes N(3) C(10) C(9) C(14) 178.4(3) . . . . yes N(3) C(10) C(11) C(12) 179.0(3) . . . . yes N(4) Fe(2) N(3) C(2) -3.0(2) . . . . yes N(4) Fe(2) N(3) C(10) -180.0(4) . . . . yes N(4) C(2) N(3) C(10) -177.5(3) . . . . yes N(4) C(2) C(21) C(22) 63.3(4) . . . . yes N(4) C(2) C(21) C(26) -117.2(4) . . . . yes C(1) N(1) Fe(1) C(27) 84.3(2) . . . . yes C(1) N(1) Si(1) C(3) -93.3(4) . . . . yes C(1) N(1) Si(1) C(4) 148.6(3) . . . . yes C(1) N(1) Si(1) C(5) 29.2(4) . . . . yes C(1) N(2) Fe(1) C(27) -85.2(2) . . . . yes C(1) N(2) C(9) C(10) -159.6(3) . . . . yes C(1) N(2) C(9) C(14) 76.3(4) . . . . yes C(1) C(15) C(16) C(17) 177.4(4) . . . . yes C(1) C(15) C(20) C(19) -176.8(4) . . . . yes C(2) N(3) C(10) C(9) -179.2(3) . . . . yes C(2) N(3) C(10) C(11) 60.4(4) . . . . yes C(2) N(4) Si(2) C(6) 34.4(4) . . . . yes C(2) N(4) Si(2) C(7) -87.9(4) . . . . yes C(2) N(4) Si(2) C(8) 154.4(4) . . . . yes C(2) C(21) C(22) C(23) 178.2(3) . . . . yes C(2) C(21) C(26) C(25) -178.6(3) . . . . yes C(9) N(2) Fe(1) C(27) 59.8(3) . . . . yes C(9) N(2) C(1) C(15) 9.4(5) . . . . yes C(9) C(10) C(11) C(12) 57.8(4) . . . . yes C(9) C(14) C(13) C(12) -56.2(4) . . . . yes C(10) N(3) C(2) C(21) 4.3(5) . . . . yes C(10) C(9) C(14) C(13) 59.7(4) . . . . yes C(10) C(11) C(12) C(13) -55.8(4) . . . . yes C(11) C(10) C(9) C(14) -58.5(3) . . . . yes C(11) C(12) C(13) C(14) 53.4(4) . . . . yes C(15) C(16) C(17) C(18) -1.1(7) . . . . yes C(15) C(20) C(19) C(18) 0.3(7) . . . . yes C(16) C(15) C(20) C(19) -0.2(6) . . . . yes C(16) C(17) C(18) C(19) 1.2(7) . . . . yes C(17) C(16) C(15) C(20) 0.6(6) . . . . yes C(17) C(18) C(19) C(20) -0.8(7) . . . . yes C(21) C(22) C(23) C(24) 0.8(6) . . . . yes C(21) C(26) C(25) C(24) 0.0(6) . . . . yes C(22) C(21) C(26) C(25) 0.9(5) . . . . yes C(22) C(23) C(24) C(25) 0.1(7) . . . . yes C(23) C(22) C(21) C(26) -1.3(5) . . . . yes C(23) C(24) C(25) C(26) -0.5(7) . . . . yes C(23) C(24) C(25) C(26) -0.5(7) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(1) 2.864(6) . 2_566 ? O(1) C(14) 3.155(4) . 2_566 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------