# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- Compound 2 FeIPr.CIF' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Nov 11 16:43:59 2010' _audit_creation_method 'PLATON option' _audit_update_record ; ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence 'Richard Layfield' _publ_contact_author_address # address of author for correspondence ; ; _publ_contact_author_email Richard.Layfield@manchester.ac.uk _publ_contact_author_fax ? _publ_contact_author_phone ? # Publication choise FI, CI or EI for Inorganic # FM, CM or EM for Metal-organic # FO, CO or EO for Organic _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Regular Structural Paper in Acta Crystallographica C. ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ; _publ_section_title_footnote ; ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address # author name 'Richard Layfield' ; # author related footnote ; ; # Address of this author ; 'Joseph McDouall' '' '' 'Manfred Scheer' '' '' 'Christoph Schwarzmaier' '' '' 'Floriana Tuna' '' '' #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods (SIR-97) and refined by full-matrix anisotropic least squares (SHELXL97). The H-atoms were calculated geometrically and a riding model was used during refinement process. With the aid of PLATON a solvent accessible area was found, but it was impossible to refine any reasonable molecule from difference Fourier peaks. Therefore the midpoint, the size and the number of electrons in that void were refined and the contribution to the calculated structure factors of the disordered solvent is taken into account by back-Fourier transformation with the program SQUEEZE (Sluis and Spek, 1990). The void is found around (-0.034 0.008 0.000), the size is 326 \%A^3^, and 46 e^-^ were detected. This electron number corresponds roughly to one toluene molecule. ; # Insert blank lines between references _publ_section_references ; ; _publ_section_acknowledgements ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C. Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, R. (1999) J. Appl. Cryst. 32, 115-119. Analytische und numerische Absorptionskorrektur Clark, R. C., Reid, J. S. (1995). Acta Cryst. A51, 887-897. Stickstoffk hlung Cosier, J., Glazer, A.M. (1986). J. Appl. Cryst. 19, 105-107. SXGRAPH L. J. Farrugia, J. Appl. Cryst (1999), 32, 837. XL Sheldrick, G.M. SHELXL97 (1997). Program for crystal structure refinement. University of G\\"ottingen, Germany. SQUEEZE Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201. PLATON Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. TABLES Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. ; #=============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 835631' #TrackingRef '- Compound 2 FeIPr.CIF' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H72 Fe N4 Si4' _chemical_formula_structural ? _chemical_formula_sum 'C39 H72 Fe N4 Si4' _chemical_formula_iupac ? _chemical_formula_weight 765.22 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 10.8510(8) _cell_length_b 11.3172(8) _cell_length_c 22.8051(13) _cell_angle_alpha 76.430(6) _cell_angle_beta 80.054(5) _cell_angle_gamma 66.930(7) _cell_volume 2494.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 9350 _cell_measurement_theta_min 4.0028 _cell_measurement_theta_max 63.5944 _cell_special_details ; ; _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2862 _exptl_crystal_size_mid 0.1423 _exptl_crystal_size_min 0.0853 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.019 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 3.538 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5431 # number of measured reflections (redundant set) _diffrn_reflns_number 15902 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 63.72 _diffrn_reflns_theta_full 63.72 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 7794 # number of observed reflections (> n sig(I)) _reflns_number_gt 7236 _reflns_threshold_expression >2\s(i) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0461P)^2^+0.6646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 7794 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.321 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.044 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Fe1 Fe Uani 1.05252(3) 0.44087(2) 0.26851(1) 1.000 0.0185(1) . . Si1 Si Uani 1.29253(5) 0.17124(5) 0.28349(2) 1.000 0.0264(2) . . Si2 Si Uani 1.20693(5) 0.30286(5) 0.39058(2) 1.000 0.0224(2) . . Si3 Si Uani 1.18101(5) 0.58152(5) 0.14605(2) 1.000 0.0267(2) . . Si4 Si Uani 1.08337(6) 0.70864(5) 0.25465(2) 1.000 0.0285(2) . . N1 N Uani 0.77895(15) 0.46621(16) 0.22094(7) 1.000 0.0252(5) . . N2 N Uani 0.77145(15) 0.40178(15) 0.31680(7) 1.000 0.0235(5) . . N3 N Uani 1.17947(15) 0.29254(14) 0.32024(7) 1.000 0.0225(5) . . N4 N Uani 1.09631(16) 0.58859(15) 0.21682(7) 1.000 0.0254(5) . . C1 C Uani 0.85237(17) 0.43816(16) 0.26902(8) 1.000 0.0194(5) . . C2 C Uani 0.6593(2) 0.4465(2) 0.23889(10) 1.000 0.0407(7) . . C3 C Uani 0.6548(2) 0.4061(2) 0.29847(10) 1.000 0.0391(7) . . C4 C Uani 0.80493(18) 0.51868(19) 0.15764(8) 1.000 0.0242(6) . . C5 C Uani 0.76247(19) 0.65487(19) 0.14012(9) 1.000 0.0261(6) . . C6 C Uani 0.7694(2) 0.7042(2) 0.07847(9) 1.000 0.0298(6) . . C7 C Uani 0.8151(2) 0.6224(2) 0.03641(9) 1.000 0.0304(6) . . C8 C Uani 0.8551(2) 0.48899(19) 0.05504(9) 1.000 0.0288(6) . . C9 C Uani 0.85011(18) 0.43295(18) 0.11635(8) 1.000 0.0252(6) . . C10 C Uani 0.7018(2) 0.7461(2) 0.18569(9) 1.000 0.0340(7) . . C11 C Uani 0.7341(2) 0.8700(2) 0.16673(11) 1.000 0.0429(8) . . C12 C Uani 0.5489(3) 0.7826(3) 0.19569(14) 1.000 0.0585(10) . . C13 C Uani 0.8851(2) 0.28587(19) 0.13556(9) 1.000 0.0321(6) . . C14 C Uani 0.7683(3) 0.2489(3) 0.12651(15) 1.000 0.0564(10) . . C15 C Uani 1.0129(2) 0.20715(19) 0.10059(9) 1.000 0.0333(6) . . C16 C Uani 0.79194(17) 0.36078(18) 0.38070(8) 1.000 0.0223(5) . . C17 C Uani 0.84284(18) 0.22635(18) 0.40374(9) 1.000 0.0263(6) . . C18 C Uani 0.8453(2) 0.1877(2) 0.46625(9) 1.000 0.0312(6) . . C19 C Uani 0.7996(2) 0.2793(2) 0.50377(9) 1.000 0.0318(6) . . C20 C Uani 0.74821(19) 0.41100(19) 0.47999(9) 1.000 0.0289(6) . . C21 C Uani 0.74060(18) 0.45557(18) 0.41784(8) 1.000 0.0242(6) . . C22 C Uani 0.8852(2) 0.1255(2) 0.36286(10) 1.000 0.0327(6) . . C23 C Uani 0.7713(3) 0.0766(3) 0.36401(17) 1.000 0.0654(12) . . C24 C Uani 1.0117(2) 0.0086(2) 0.38116(10) 1.000 0.0352(7) . . C25 C Uani 0.66956(19) 0.60021(19) 0.39260(9) 1.000 0.0300(6) . . C26 C Uani 0.5187(2) 0.6316(2) 0.39452(15) 1.000 0.0565(9) . . C27 C Uani 0.6940(2) 0.6900(2) 0.42632(10) 1.000 0.0406(7) . . C28 C Uani 1.3837(2) 0.0144(2) 0.33457(10) 1.000 0.0408(7) . . C29 C Uani 1.2032(2) 0.1269(2) 0.23361(10) 1.000 0.0384(7) . . C30 C Uani 1.4324(2) 0.2177(2) 0.23632(10) 1.000 0.0391(7) . . C31 C Uani 1.1977(2) 0.1640(2) 0.45280(9) 1.000 0.0327(6) . . C32 C Uani 1.3789(2) 0.3074(2) 0.38990(10) 1.000 0.0351(7) . . C33 C Uani 1.0816(2) 0.4518(2) 0.41802(9) 1.000 0.0305(6) . . C34 C Uani 1.1945(2) 0.4340(2) 0.11833(10) 1.000 0.0361(7) . . C35 C Uani 1.1017(2) 0.7219(2) 0.08459(10) 1.000 0.0384(7) . . C36 C Uani 1.3571(2) 0.5765(2) 0.14457(11) 1.000 0.0419(8) . . C37 C Uani 1.2325(2) 0.6639(2) 0.29806(10) 1.000 0.0389(7) . . C38 C Uani 1.0717(3) 0.8701(2) 0.20502(11) 1.000 0.0452(8) . . C39 C Uani 0.9268(2) 0.7432(2) 0.30799(10) 1.000 0.0368(7) . . H027 H Uiso 0.59410 0.45920 0.21400 1.000 0.0490 calc R H037 H Uiso 0.58600 0.38470 0.32320 1.000 0.0470 calc R H047 H Uiso 0.74290 0.79410 0.06510 1.000 0.0360 calc R H043 H Uiso 0.81880 0.65770 -0.00470 1.000 0.0360 calc R H014 H Uiso 0.88600 0.43530 0.02620 1.000 0.0340 calc R H012 H Uiso 0.73950 0.69930 0.22440 1.000 0.0410 calc R H04J H Uiso 0.69350 0.92410 0.19680 1.000 0.0640 calc R H04K H Uiso 0.69920 0.91690 0.12860 1.000 0.0640 calc R H04L H Uiso 0.82980 0.84720 0.16280 1.000 0.0640 calc R H03O H Uiso 0.51190 0.84000 0.22460 1.000 0.0880 calc R H03P H Uiso 0.52890 0.70480 0.21080 1.000 0.0880 calc R H03Q H Uiso 0.51010 0.82590 0.15800 1.000 0.0880 calc R H021 H Uiso 0.89920 0.26160 0.17870 1.000 0.0390 calc R H04D H Uiso 0.79120 0.15630 0.13930 1.000 0.0850 calc R H04E H Uiso 0.75230 0.27320 0.08450 1.000 0.0850 calc R H04F H Uiso 0.68870 0.29410 0.15020 1.000 0.0850 calc R H02G H Uiso 1.03130 0.11550 0.11460 1.000 0.0500 calc R H02H H Uiso 1.08700 0.22730 0.10700 1.000 0.0500 calc R H02I H Uiso 1.00050 0.22910 0.05820 1.000 0.0500 calc R H031 H Uiso 0.87810 0.09910 0.48310 1.000 0.0370 calc R H026 H Uiso 0.80370 0.25170 0.54540 1.000 0.0380 calc R H033 H Uiso 0.71810 0.47110 0.50580 1.000 0.0350 calc R H017 H Uiso 0.90330 0.16750 0.32130 1.000 0.0390 calc R H04S H Uiso 0.79890 0.01360 0.33800 1.000 0.0980 calc R H04T H Uiso 0.69270 0.14890 0.35020 1.000 0.0980 calc R H04U H Uiso 0.75110 0.03660 0.40460 1.000 0.0980 calc R H04P H Uiso 1.03530 -0.05120 0.35380 1.000 0.0530 calc R H04Q H Uiso 0.99520 -0.03460 0.42160 1.000 0.0530 calc R H04R H Uiso 1.08420 0.03800 0.37960 1.000 0.0530 calc R H028 H Uiso 0.70420 0.61760 0.35010 1.000 0.0360 calc R H05A H Uiso 0.47440 0.72250 0.37840 1.000 0.0850 calc R H05B H Uiso 0.48320 0.61210 0.43570 1.000 0.0850 calc R H05C H Uiso 0.50370 0.57970 0.37070 1.000 0.0850 calc R H03G H Uiso 0.64730 0.77950 0.40870 1.000 0.0610 calc R H03H H Uiso 0.78860 0.67270 0.42330 1.000 0.0610 calc R H03I H Uiso 0.66140 0.67400 0.46820 1.000 0.0610 calc R H01G H Uiso 1.31950 -0.01750 0.36050 1.000 0.0610 calc R H01H H Uiso 1.43790 0.03010 0.35880 1.000 0.0610 calc R H01I H Uiso 1.44030 -0.04930 0.31050 1.000 0.0610 calc R H03A H Uiso 1.15510 0.20380 0.20620 1.000 0.0580 calc R H03B H Uiso 1.14110 0.09010 0.25820 1.000 0.0580 calc R H03C H Uiso 1.26770 0.06400 0.21090 1.000 0.0580 calc R H04G H Uiso 1.39490 0.29770 0.20830 1.000 0.0590 calc R H04H H Uiso 1.48770 0.14960 0.21430 1.000 0.0590 calc R H04I H Uiso 1.48590 0.22960 0.26220 1.000 0.0590 calc R H02D H Uiso 1.25940 0.08290 0.44190 1.000 0.0490 calc R H02E H Uiso 1.10800 0.16400 0.45880 1.000 0.0490 calc R H02F H Uiso 1.22100 0.17420 0.48960 1.000 0.0490 calc R H02A H Uiso 1.44590 0.23220 0.37570 1.000 0.0530 calc R H02B H Uiso 1.39420 0.30700 0.43020 1.000 0.0530 calc R H02C H Uiso 1.38420 0.38530 0.36350 1.000 0.0530 calc R H01A H Uiso 1.07950 0.52790 0.38820 1.000 0.0460 calc R H01B H Uiso 1.10660 0.45790 0.45520 1.000 0.0460 calc R H01C H Uiso 0.99420 0.44600 0.42480 1.000 0.0460 calc R H03L H Uiso 1.10620 0.43290 0.11910 1.000 0.0540 calc R H03M H Uiso 1.24770 0.35680 0.14400 1.000 0.0540 calc R H03N H Uiso 1.23640 0.43650 0.07760 1.000 0.0540 calc R H04M H Uiso 1.01080 0.73010 0.08300 1.000 0.0580 calc R H04N H Uiso 1.15200 0.70620 0.04640 1.000 0.0580 calc R H04O H Uiso 1.10190 0.80110 0.09300 1.000 0.0580 calc R H04A H Uiso 1.40370 0.50600 0.17510 1.000 0.0630 calc R H04B H Uiso 1.35340 0.65760 0.15240 1.000 0.0630 calc R H04C H Uiso 1.40400 0.56330 0.10550 1.000 0.0630 calc R H03D H Uiso 1.24590 0.58150 0.32490 1.000 0.0580 calc R H03E H Uiso 1.21660 0.73000 0.32120 1.000 0.0580 calc R H03F H Uiso 1.31120 0.65720 0.27030 1.000 0.0580 calc R H01D H Uiso 0.99690 0.90090 0.18110 1.000 0.0680 calc R H01E H Uiso 1.15320 0.85950 0.17880 1.000 0.0680 calc R H01F H Uiso 1.05930 0.93240 0.22990 1.000 0.0680 calc R H02J H Uiso 0.85090 0.80060 0.28600 1.000 0.0550 calc R H02K H Uiso 0.93500 0.78400 0.33880 1.000 0.0550 calc R H02L H Uiso 0.91430 0.66280 0.32650 1.000 0.0550 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 Fe1 0.0192(2) 0.0206(2) 0.0174(2) -0.0027(1) -0.0024(1) -0.0090(1) Si1 0.0261(3) 0.0270(3) 0.0229(3) -0.0061(2) -0.0018(2) -0.0057(2) Si2 0.0203(2) 0.0279(3) 0.0194(3) -0.0041(2) -0.0016(2) -0.0096(2) Si3 0.0278(3) 0.0354(3) 0.0221(3) -0.0011(2) -0.0043(2) -0.0185(2) Si4 0.0385(3) 0.0282(3) 0.0264(3) -0.0020(2) -0.0078(2) -0.0201(2) N1 0.0199(8) 0.0388(9) 0.0174(8) -0.0010(7) -0.0032(6) -0.0129(7) N2 0.0185(8) 0.0308(8) 0.0190(8) -0.0004(6) -0.0020(6) -0.0089(6) N3 0.0208(8) 0.0244(8) 0.0207(8) -0.0035(6) -0.0023(6) -0.0067(6) N4 0.0320(9) 0.0263(8) 0.0228(8) -0.0006(6) -0.0051(7) -0.0169(7) C1 0.0197(9) 0.0188(9) 0.0178(9) -0.0032(7) -0.0006(7) -0.0056(7) C2 0.0232(10) 0.0737(16) 0.0272(11) 0.0048(10) -0.0074(8) -0.0258(11) C3 0.0220(10) 0.0665(15) 0.0278(11) 0.0039(10) -0.0025(8) -0.0223(10) C4 0.0188(9) 0.0352(11) 0.0186(9) 0.0007(8) -0.0049(7) -0.0119(8) C5 0.0241(10) 0.0321(10) 0.0248(10) -0.0039(8) -0.0063(8) -0.0124(8) C6 0.0336(11) 0.0306(10) 0.0253(10) -0.0005(8) -0.0074(8) -0.0125(9) C7 0.0357(11) 0.0367(11) 0.0187(10) 0.0012(8) -0.0056(8) -0.0156(9) C8 0.0321(11) 0.0348(11) 0.0213(10) -0.0061(8) -0.0028(8) -0.0136(9) C9 0.0219(9) 0.0302(10) 0.0243(10) -0.0027(8) -0.0038(7) -0.0110(8) C10 0.0387(12) 0.0364(11) 0.0274(11) -0.0082(9) -0.0065(9) -0.0115(9) C11 0.0473(13) 0.0349(12) 0.0476(14) -0.0124(10) -0.0124(11) -0.0101(10) C12 0.0453(15) 0.0727(18) 0.0647(18) -0.0417(15) 0.0148(13) -0.0208(13) C13 0.0364(11) 0.0309(11) 0.0276(11) 0.0003(8) -0.0024(9) -0.0142(9) C14 0.0491(15) 0.0452(14) 0.082(2) -0.0063(13) -0.0025(14) -0.0292(12) C15 0.0420(12) 0.0271(10) 0.0302(11) -0.0032(8) -0.0057(9) -0.0123(9) C16 0.0168(9) 0.0304(10) 0.0175(9) -0.0009(7) 0.0011(7) -0.0094(8) C17 0.0213(9) 0.0288(10) 0.0251(10) -0.0039(8) 0.0000(7) -0.0069(8) C18 0.0297(11) 0.0289(10) 0.0257(10) 0.0012(8) -0.0026(8) -0.0043(9) C19 0.0303(11) 0.0400(12) 0.0167(9) -0.0012(8) 0.0013(8) -0.0077(9) C20 0.0265(10) 0.0350(11) 0.0227(10) -0.0082(8) 0.0028(8) -0.0090(9) C21 0.0185(9) 0.0290(10) 0.0234(10) -0.0028(8) -0.0002(7) -0.0089(8) C22 0.0337(11) 0.0301(11) 0.0288(11) -0.0076(8) -0.0053(9) -0.0038(9) C23 0.0395(14) 0.0571(17) 0.108(3) -0.0448(17) -0.0215(15) -0.0037(12) C24 0.0331(11) 0.0318(11) 0.0367(12) -0.0101(9) -0.0048(9) -0.0048(9) C25 0.0272(10) 0.0282(10) 0.0297(11) -0.0032(8) 0.0022(8) -0.0083(8) C26 0.0298(12) 0.0345(13) 0.088(2) 0.0066(12) -0.0068(12) -0.0033(10) C27 0.0507(14) 0.0312(11) 0.0341(12) -0.0117(9) 0.0063(10) -0.0100(10) C28 0.0410(12) 0.0304(11) 0.0378(12) -0.0068(9) -0.0035(10) 0.0012(9) C29 0.0479(13) 0.0386(12) 0.0328(12) -0.0127(9) -0.0033(10) -0.0168(10) C30 0.0289(11) 0.0484(13) 0.0336(12) -0.0093(10) 0.0020(9) -0.0084(10) C31 0.0386(11) 0.0358(11) 0.0235(10) -0.0021(8) -0.0043(8) -0.0147(9) C32 0.0250(10) 0.0483(13) 0.0357(12) -0.0126(10) -0.0006(9) -0.0156(9) C33 0.0274(10) 0.0383(11) 0.0269(10) -0.0094(8) 0.0002(8) -0.0123(9) C34 0.0406(12) 0.0447(12) 0.0285(11) -0.0091(9) -0.0030(9) -0.0202(10) C35 0.0411(12) 0.0478(13) 0.0256(11) 0.0033(9) -0.0051(9) -0.0205(10) C36 0.0332(12) 0.0563(14) 0.0435(13) -0.0057(11) -0.0050(10) -0.0254(11) C37 0.0450(13) 0.0497(13) 0.0333(12) -0.0053(10) -0.0086(10) -0.0285(11) C38 0.0694(16) 0.0347(12) 0.0440(13) 0.0015(10) -0.0171(12) -0.0323(12) C39 0.0435(12) 0.0341(11) 0.0371(12) -0.0116(9) -0.0050(10) -0.0155(10) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.9816(16) . . yes Fe1 N4 1.9785(17) . . yes Fe1 C1 2.182(2) . . yes Si1 N3 1.7195(16) . . yes Si1 C28 1.881(2) . . yes Si1 C29 1.875(2) . . yes Si1 C30 1.880(2) . . yes Si2 N3 1.7193(16) . . yes Si2 C31 1.876(2) . . yes Si2 C32 1.884(2) . . yes Si2 C33 1.867(2) . . yes Si3 N4 1.7165(17) . . yes Si3 C34 1.866(2) . . yes Si3 C35 1.879(2) . . yes Si3 C36 1.884(2) . . yes Si4 N4 1.7230(17) . . yes Si4 C37 1.879(2) . . yes Si4 C38 1.880(2) . . yes Si4 C39 1.873(2) . . yes N1 C1 1.370(2) . . yes N1 C2 1.380(3) . . yes N1 C4 1.451(2) . . yes N2 C1 1.368(2) . . yes N2 C3 1.380(3) . . yes N2 C16 1.450(2) . . yes C2 C3 1.327(3) . . no C4 C5 1.402(3) . . no C4 C9 1.402(3) . . no C5 C6 1.386(3) . . no C5 C10 1.521(3) . . no C6 C7 1.384(3) . . no C7 C8 1.378(3) . . no C8 C9 1.395(3) . . no C9 C13 1.525(3) . . no C10 C11 1.525(3) . . no C10 C12 1.534(4) . . no C13 C14 1.540(4) . . no C13 C15 1.528(3) . . no C16 C17 1.401(3) . . no C16 C21 1.405(3) . . no C17 C18 1.391(3) . . no C17 C22 1.524(3) . . no C18 C19 1.386(3) . . no C19 C20 1.379(3) . . no C20 C21 1.394(3) . . no C21 C25 1.526(3) . . no C22 C23 1.534(4) . . no C22 C24 1.525(3) . . no C25 C26 1.528(3) . . no C25 C27 1.531(3) . . no C2 H027 0.9300 . . no C3 H037 0.9300 . . no C6 H047 0.9300 . . no C7 H043 0.9300 . . no C8 H014 0.9300 . . no C10 H012 0.9800 . . no C11 H04J 0.9600 . . no C11 H04K 0.9600 . . no C11 H04L 0.9600 . . no C12 H03O 0.9600 . . no C12 H03P 0.9600 . . no C12 H03Q 0.9600 . . no C13 H021 0.9800 . . no C14 H04D 0.9600 . . no C14 H04E 0.9600 . . no C14 H04F 0.9600 . . no C15 H02G 0.9600 . . no C15 H02H 0.9600 . . no C15 H02I 0.9600 . . no C18 H031 0.9300 . . no C19 H026 0.9300 . . no C20 H033 0.9300 . . no C22 H017 0.9800 . . no C23 H04S 0.9600 . . no C23 H04T 0.9600 . . no C23 H04U 0.9600 . . no C24 H04P 0.9600 . . no C24 H04Q 0.9600 . . no C24 H04R 0.9600 . . no C25 H028 0.9800 . . no C26 H05A 0.9600 . . no C26 H05B 0.9600 . . no C26 H05C 0.9600 . . no C27 H03G 0.9600 . . no C27 H03H 0.9600 . . no C27 H03I 0.9600 . . no C28 H01G 0.9600 . . no C28 H01H 0.9600 . . no C28 H01I 0.9600 . . no C29 H03A 0.9600 . . no C29 H03B 0.9600 . . no C29 H03C 0.9600 . . no C30 H04G 0.9600 . . no C30 H04H 0.9600 . . no C30 H04I 0.9600 . . no C31 H02D 0.9600 . . no C31 H02E 0.9600 . . no C31 H02F 0.9600 . . no C32 H02A 0.9600 . . no C32 H02B 0.9600 . . no C32 H02C 0.9600 . . no C33 H01A 0.9600 . . no C33 H01B 0.9600 . . no C33 H01C 0.9600 . . no C34 H03L 0.9600 . . no C34 H03M 0.9600 . . no C34 H03N 0.9600 . . no C35 H04M 0.9600 . . no C35 H04N 0.9600 . . no C35 H04O 0.9600 . . no C36 H04A 0.9600 . . no C36 H04B 0.9600 . . no C36 H04C 0.9600 . . no C37 H03D 0.9600 . . no C37 H03E 0.9600 . . no C37 H03F 0.9600 . . no C38 H01D 0.9600 . . no C38 H01E 0.9600 . . no C38 H01F 0.9600 . . no C39 H02J 0.9600 . . no C39 H02K 0.9600 . . no C39 H02L 0.9600 . . no 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 N3 Fe1 N4 124.30(7) . . . yes N3 Fe1 C1 117.06(7) . . . yes N4 Fe1 C1 118.64(7) . . . yes N3 Si1 C28 114.98(9) . . . yes N3 Si1 C29 109.90(9) . . . yes N3 Si1 C30 113.20(9) . . . yes C28 Si1 C29 105.91(10) . . . yes C28 Si1 C30 103.47(10) . . . yes C29 Si1 C30 108.90(10) . . . yes N3 Si2 C31 115.08(9) . . . yes N3 Si2 C32 111.05(9) . . . yes N3 Si2 C33 112.66(9) . . . yes C31 Si2 C32 105.76(10) . . . yes C31 Si2 C33 104.33(9) . . . yes C32 Si2 C33 107.35(10) . . . yes N4 Si3 C34 111.73(9) . . . yes N4 Si3 C35 115.44(9) . . . yes N4 Si3 C36 112.15(10) . . . yes C34 Si3 C35 104.31(10) . . . yes C34 Si3 C36 107.30(10) . . . yes C35 Si3 C36 105.24(10) . . . yes N4 Si4 C37 112.88(9) . . . yes N4 Si4 C38 115.10(9) . . . yes N4 Si4 C39 109.51(10) . . . yes C37 Si4 C38 103.86(12) . . . yes C37 Si4 C39 109.28(10) . . . yes C38 Si4 C39 105.82(11) . . . yes C1 N1 C2 111.74(16) . . . yes C1 N1 C4 130.14(18) . . . yes C2 N1 C4 118.01(17) . . . yes C1 N2 C3 111.82(16) . . . yes C1 N2 C16 129.79(17) . . . yes C3 N2 C16 118.39(17) . . . yes Fe1 N3 Si1 115.34(8) . . . yes Fe1 N3 Si2 122.22(8) . . . yes Si1 N3 Si2 120.18(10) . . . yes Fe1 N4 Si3 123.25(9) . . . yes Fe1 N4 Si4 114.44(8) . . . yes Si3 N4 Si4 120.28(10) . . . yes Fe1 C1 N1 128.61(13) . . . yes Fe1 C1 N2 128.90(13) . . . yes N1 C1 N2 102.42(16) . . . yes N1 C2 C3 107.0(2) . . . yes N2 C3 C2 107.0(2) . . . yes N1 C4 C5 117.62(17) . . . yes N1 C4 C9 118.10(17) . . . yes C5 C4 C9 123.42(17) . . . no C4 C5 C6 116.86(18) . . . no C4 C5 C10 122.22(17) . . . no C6 C5 C10 120.77(18) . . . no C5 C6 C7 121.31(19) . . . no C6 C7 C8 120.46(19) . . . no C7 C8 C9 121.18(18) . . . no C4 C9 C8 116.76(17) . . . no C4 C9 C13 123.11(16) . . . no C8 C9 C13 120.04(17) . . . no C5 C10 C11 112.75(18) . . . no C5 C10 C12 110.3(2) . . . no C11 C10 C12 109.6(2) . . . no C9 C13 C14 110.4(2) . . . no C9 C13 C15 112.59(17) . . . no C14 C13 C15 108.81(19) . . . no N2 C16 C17 117.67(16) . . . yes N2 C16 C21 118.58(16) . . . yes C17 C16 C21 122.95(17) . . . no C16 C17 C18 117.31(18) . . . no C16 C17 C22 121.77(18) . . . no C18 C17 C22 120.79(18) . . . no C17 C18 C19 120.89(19) . . . no C18 C19 C20 120.62(19) . . . no C19 C20 C21 121.10(18) . . . no C16 C21 C20 117.05(17) . . . no C16 C21 C25 122.12(16) . . . no C20 C21 C25 120.66(17) . . . no C17 C22 C23 110.2(2) . . . no C17 C22 C24 112.50(18) . . . no C23 C22 C24 108.9(2) . . . no C21 C25 C26 109.72(18) . . . no C21 C25 C27 112.91(17) . . . no C26 C25 C27 109.88(18) . . . no N1 C2 H027 127.00 . . . no C3 C2 H027 126.00 . . . no N2 C3 H037 127.00 . . . no C2 C3 H037 126.00 . . . no C5 C6 H047 119.00 . . . no C7 C6 H047 119.00 . . . no C6 C7 H043 120.00 . . . no C8 C7 H043 120.00 . . . no C7 C8 H014 119.00 . . . no C9 C8 H014 119.00 . . . no C5 C10 H012 108.00 . . . no C11 C10 H012 108.00 . . . no C12 C10 H012 108.00 . . . no C10 C11 H04J 109.00 . . . no C10 C11 H04K 109.00 . . . no C10 C11 H04L 110.00 . . . no H04J C11 H04K 109.00 . . . no H04J C11 H04L 110.00 . . . no H04K C11 H04L 109.00 . . . no C10 C12 H03O 109.00 . . . no C10 C12 H03P 109.00 . . . no C10 C12 H03Q 109.00 . . . no H03O C12 H03P 109.00 . . . no H03O C12 H03Q 109.00 . . . no H03P C12 H03Q 110.00 . . . no C9 C13 H021 108.00 . . . no C14 C13 H021 108.00 . . . no C15 C13 H021 108.00 . . . no C13 C14 H04D 109.00 . . . no C13 C14 H04E 109.00 . . . no C13 C14 H04F 109.00 . . . no H04D C14 H04E 110.00 . . . no H04D C14 H04F 109.00 . . . no H04E C14 H04F 110.00 . . . no C13 C15 H02G 109.00 . . . no C13 C15 H02H 110.00 . . . no C13 C15 H02I 109.00 . . . no H02G C15 H02H 109.00 . . . no H02G C15 H02I 109.00 . . . no H02H C15 H02I 110.00 . . . no C17 C18 H031 120.00 . . . no C19 C18 H031 120.00 . . . no C18 C19 H026 120.00 . . . no C20 C19 H026 120.00 . . . no C19 C20 H033 119.00 . . . no C21 C20 H033 119.00 . . . no C17 C22 H017 108.00 . . . no C23 C22 H017 108.00 . . . no C24 C22 H017 108.00 . . . no C22 C23 H04S 109.00 . . . no C22 C23 H04T 109.00 . . . no C22 C23 H04U 109.00 . . . no H04S C23 H04T 110.00 . . . no H04S C23 H04U 109.00 . . . no H04T C23 H04U 109.00 . . . no C22 C24 H04P 109.00 . . . no C22 C24 H04Q 109.00 . . . no C22 C24 H04R 109.00 . . . no H04P C24 H04Q 109.00 . . . no H04P C24 H04R 109.00 . . . no H04Q C24 H04R 110.00 . . . no C21 C25 H028 108.00 . . . no C26 C25 H028 108.00 . . . no C27 C25 H028 108.00 . . . no C25 C26 H05A 110.00 . . . no C25 C26 H05B 109.00 . . . no C25 C26 H05C 109.00 . . . no H05A C26 H05B 110.00 . . . no H05A C26 H05C 109.00 . . . no H05B C26 H05C 109.00 . . . no C25 C27 H03G 110.00 . . . no C25 C27 H03H 109.00 . . . no C25 C27 H03I 109.00 . . . no H03G C27 H03H 110.00 . . . no H03G C27 H03I 109.00 . . . no H03H C27 H03I 109.00 . . . no Si1 C28 H01G 109.00 . . . no Si1 C28 H01H 109.00 . . . no Si1 C28 H01I 110.00 . . . no H01G C28 H01H 109.00 . . . no H01G C28 H01I 109.00 . . . no H01H C28 H01I 109.00 . . . no Si1 C29 H03A 109.00 . . . no Si1 C29 H03B 109.00 . . . no Si1 C29 H03C 109.00 . . . no H03A C29 H03B 110.00 . . . no H03A C29 H03C 109.00 . . . no H03B C29 H03C 109.00 . . . no Si1 C30 H04G 109.00 . . . no Si1 C30 H04H 109.00 . . . no Si1 C30 H04I 110.00 . . . no H04G C30 H04H 109.00 . . . no H04G C30 H04I 109.00 . . . no H04H C30 H04I 109.00 . . . no Si2 C31 H02D 109.00 . . . no Si2 C31 H02E 109.00 . . . no Si2 C31 H02F 109.00 . . . no H02D C31 H02E 110.00 . . . no H02D C31 H02F 109.00 . . . no H02E C31 H02F 109.00 . . . no Si2 C32 H02A 109.00 . . . no Si2 C32 H02B 109.00 . . . no Si2 C32 H02C 109.00 . . . no H02A C32 H02B 109.00 . . . no H02A C32 H02C 109.00 . . . no H02B C32 H02C 110.00 . . . no Si2 C33 H01A 110.00 . . . no Si2 C33 H01B 109.00 . . . no Si2 C33 H01C 109.00 . . . no H01A C33 H01B 110.00 . . . no H01A C33 H01C 109.00 . . . no H01B C33 H01C 109.00 . . . no Si3 C34 H03L 109.00 . . . no Si3 C34 H03M 109.00 . . . no Si3 C34 H03N 109.00 . . . no H03L C34 H03M 109.00 . . . no H03L C34 H03N 109.00 . . . no H03M C34 H03N 110.00 . . . no Si3 C35 H04M 109.00 . . . no Si3 C35 H04N 109.00 . . . no Si3 C35 H04O 109.00 . . . no H04M C35 H04N 109.00 . . . no H04M C35 H04O 110.00 . . . no H04N C35 H04O 109.00 . . . no Si3 C36 H04A 109.00 . . . no Si3 C36 H04B 109.00 . . . no Si3 C36 H04C 110.00 . . . no H04A C36 H04B 109.00 . . . no H04A C36 H04C 109.00 . . . no H04B C36 H04C 109.00 . . . no Si4 C37 H03D 109.00 . . . no Si4 C37 H03E 110.00 . . . no Si4 C37 H03F 110.00 . . . no H03D C37 H03E 109.00 . . . no H03D C37 H03F 109.00 . . . no H03E C37 H03F 109.00 . . . no Si4 C38 H01D 110.00 . . . no Si4 C38 H01E 109.00 . . . no Si4 C38 H01F 109.00 . . . no H01D C38 H01E 110.00 . . . no H01D C38 H01F 110.00 . . . no H01E C38 H01F 109.00 . . . no Si4 C39 H02J 109.00 . . . no Si4 C39 H02K 109.00 . . . no Si4 C39 H02L 109.00 . . . no H02J C39 H02K 109.00 . . . no H02J C39 H02L 110.00 . . . no H02K C39 H02L 109.00 . . . no 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 N4 Fe1 N3 Si1 -81.47(11) . . . . no C1 Fe1 N3 Si1 98.16(10) . . . . no N4 Fe1 N3 Si2 81.47(12) . . . . no C1 Fe1 N3 Si2 -98.90(11) . . . . no N4 Fe1 C1 N2 -140.12(15) . . . . no C1 Fe1 N4 Si4 98.85(11) . . . . no N3 Fe1 C1 N2 40.24(18) . . . . no C1 Fe1 N4 Si3 -97.36(12) . . . . no N3 Fe1 N4 Si4 -81.53(12) . . . . no N3 Fe1 N4 Si3 82.26(13) . . . . no N4 Fe1 C1 N1 43.58(18) . . . . no N3 Fe1 C1 N1 -136.07(15) . . . . no C28 Si1 N3 Si2 30.71(15) . . . . no C29 Si1 N3 Si2 150.07(11) . . . . no C30 Si1 N3 Fe1 75.38(12) . . . . no C28 Si1 N3 Fe1 -165.98(10) . . . . no C30 Si1 N3 Si2 -87.93(13) . . . . no C29 Si1 N3 Fe1 -46.62(12) . . . . no C32 Si2 N3 Si1 53.38(13) . . . . no C33 Si2 N3 Si1 173.84(11) . . . . no C31 Si2 N3 Fe1 131.14(11) . . . . no C31 Si2 N3 Si1 -66.72(14) . . . . no C32 Si2 N3 Fe1 -108.76(12) . . . . no C33 Si2 N3 Fe1 11.70(15) . . . . no C35 Si3 N4 Fe1 130.60(12) . . . . no C36 Si3 N4 Fe1 -108.88(12) . . . . no C34 Si3 N4 Si4 174.53(11) . . . . no C35 Si3 N4 Si4 -66.51(15) . . . . no C34 Si3 N4 Fe1 11.64(15) . . . . no C36 Si3 N4 Si4 54.01(14) . . . . no C38 Si4 N4 Si3 33.64(18) . . . . no C39 Si4 N4 Si3 152.67(11) . . . . no C37 Si4 N4 Si3 -85.35(13) . . . . no C37 Si4 N4 Fe1 78.97(13) . . . . no C38 Si4 N4 Fe1 -162.05(13) . . . . no C39 Si4 N4 Fe1 -43.02(13) . . . . no C2 N1 C1 Fe1 176.55(14) . . . . no C4 N1 C1 Fe1 -7.5(3) . . . . no C2 N1 C1 N2 -0.5(2) . . . . no C4 N1 C1 N2 175.43(18) . . . . no C2 N1 C4 C5 90.2(2) . . . . no C1 N1 C2 C3 0.2(2) . . . . no C1 N1 C4 C5 -85.5(3) . . . . no C2 N1 C4 C9 -79.5(2) . . . . no C4 N1 C2 C3 -176.32(18) . . . . no C1 N1 C4 C9 104.8(2) . . . . no C16 N2 C1 Fe1 3.2(3) . . . . no C3 N2 C1 Fe1 -176.38(14) . . . . no C1 N2 C3 C2 -0.6(2) . . . . no C1 N2 C16 C21 92.8(2) . . . . no C16 N2 C1 N1 -179.72(18) . . . . no C16 N2 C3 C2 179.73(17) . . . . no C3 N2 C1 N1 0.7(2) . . . . no C1 N2 C16 C17 -97.2(2) . . . . no C3 N2 C16 C17 82.4(2) . . . . no C3 N2 C16 C21 -87.7(2) . . . . no N1 C2 C3 N2 0.3(2) . . . . no N1 C4 C9 C8 170.76(19) . . . . no N1 C4 C9 C13 -5.7(3) . . . . no C5 C4 C9 C8 1.7(3) . . . . no N1 C4 C5 C6 -170.5(2) . . . . no N1 C4 C5 C10 5.1(3) . . . . no C9 C4 C5 C6 -1.4(3) . . . . no C9 C4 C5 C10 174.2(2) . . . . no C5 C4 C9 C13 -174.8(2) . . . . no C4 C5 C10 C12 -89.2(3) . . . . no C6 C5 C10 C12 86.3(3) . . . . no C10 C5 C6 C7 -175.1(2) . . . . no C6 C5 C10 C11 -36.7(3) . . . . no C4 C5 C6 C7 0.5(3) . . . . no C4 C5 C10 C11 147.9(2) . . . . no C5 C6 C7 C8 0.0(4) . . . . no C6 C7 C8 C9 0.3(4) . . . . no C7 C8 C9 C4 -1.1(3) . . . . no C7 C8 C9 C13 175.5(2) . . . . no C4 C9 C13 C15 -138.1(2) . . . . no C8 C9 C13 C14 -76.2(3) . . . . no C8 C9 C13 C15 45.6(3) . . . . no C4 C9 C13 C14 100.1(3) . . . . no N2 C16 C17 C18 -171.59(19) . . . . no N2 C16 C17 C22 4.3(3) . . . . no C21 C16 C17 C18 -2.0(3) . . . . no C21 C16 C17 C22 173.9(2) . . . . no N2 C16 C21 C20 172.75(19) . . . . no N2 C16 C21 C25 -2.6(3) . . . . no C17 C16 C21 C20 3.3(3) . . . . no C17 C16 C21 C25 -172.1(2) . . . . no C16 C17 C18 C19 -0.3(3) . . . . no C22 C17 C18 C19 -176.3(2) . . . . no C16 C17 C22 C23 -97.1(3) . . . . no C16 C17 C22 C24 141.2(2) . . . . no C18 C17 C22 C23 78.7(3) . . . . no C18 C17 C22 C24 -43.0(3) . . . . no C17 C18 C19 C20 1.2(4) . . . . no C18 C19 C20 C21 0.1(4) . . . . no C19 C20 C21 C16 -2.3(3) . . . . no C19 C20 C21 C25 173.2(2) . . . . no C16 C21 C25 C26 90.6(2) . . . . no C16 C21 C25 C27 -146.5(2) . . . . no C20 C21 C25 C26 -84.6(3) . . . . no C20 C21 C25 C27 38.3(3) . . . . no 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 Fe1 H03A 3.0600 . . no Fe1 H01A 3.2000 . . no Fe1 H01C 3.5200 . . no Fe1 H03L 3.3700 . . no Fe1 H03M 3.3300 . . no Fe1 H02L 2.8700 . . no Si1 H04R 3.4100 . . no Si1 H02A 3.2300 . . no Si1 H03M 3.3700 . . no Si2 H01H 3.2700 . . no Si2 H03D 3.3100 . . no Si3 H04G 3.3000 . . no Si3 H01E 3.2900 . . no Si4 H04L 3.3900 . . no Si4 H01A 3.2500 . . no Si4 H04B 3.3600 . . no N1 H012 2.5200 . . no N1 H021 2.5000 . . no N2 H017 2.4600 . . no N2 H028 2.5200 . . no C1 C10 3.454(3) . . no C1 C22 3.599(3) . . no C1 C25 3.589(3) . . no C2 C14 3.541(4) . . no C2 C10 3.505(3) . . no C2 C12 3.457(4) . . no C2 C13 3.374(3) . . no C3 C26 3.470(3) . . no C3 C22 3.369(3) . . no C3 C23 3.476(4) . . no C3 C25 3.474(3) . . no C10 C1 3.454(3) . . no C10 C2 3.505(3) . . no C12 C2 3.457(4) . . no C13 C2 3.374(3) . . no C14 C2 3.541(4) . . no C22 C3 3.369(3) . . no C22 C1 3.599(3) . . no C23 C3 3.476(4) . . no C25 C1 3.589(3) . . no C25 C3 3.474(3) . . no C26 C3 3.470(3) . . no C27 C39 3.479(3) . . no C28 C31 3.434(3) . . no C31 C28 3.434(3) . . no C35 C38 3.448(3) . . no C38 C35 3.448(3) . . no C39 C27 3.479(3) . . no C1 H012 2.7300 . . no C1 H017 2.8800 . . no C1 H021 3.0400 . . no C1 H028 2.8800 . . no C2 H04F 2.8500 . . no C2 H03P 2.6700 . . no C2 H021 2.9800 . . no C3 H017 2.9900 . . no C3 H04T 2.7700 . . no C3 H05C 2.7100 . . no C4 H03L 3.0500 . . no C6 H04M 2.7700 . . no C6 H04L 3.0800 . . no C6 H03Q 3.0800 . . no C6 H04K 2.6900 . . no C7 H03N 3.0200 . 2_765 no C8 H04E 2.9600 . . no C8 H03L 3.0900 . . no C8 H02I 2.7300 . . no C9 H03L 2.7900 . . no C11 H02J 3.0000 . . no C11 H01D 3.0900 . . no C11 H047 2.6300 . . no C15 H03A 3.0600 . . no C15 H014 2.7200 . . no C17 H02E 3.1000 . . no C18 H04U 2.9900 . . no C18 H04Q 2.7300 . . no C18 H02E 2.7400 . . no C19 H05B 3.0300 . 2_666 no C20 H01C 2.8800 . . no C20 H03I 2.7100 . . no C20 H05B 3.0400 . . no C20 H05B 2.9500 . 2_666 no C21 H01C 2.7400 . . no C24 H031 2.7100 . . no C24 H03B 3.0200 . . no C25 H02L 3.0700 . . no C27 H033 2.6500 . . no C27 H02L 2.9800 . . no C28 H02D 2.7100 . . no C28 H05A 3.0200 . 1_645 no C29 H03M 3.0500 . . no C30 H03M 2.8900 . . no C31 H04R 3.0900 . . no C31 H01G 3.0600 . . no C32 H037 2.8000 . 1_655 no C32 H03D 3.0000 . . no C33 H03D 3.0200 . . no C33 H02L 2.9900 . . no C34 H02H 3.0700 . . no C34 H03A 3.0200 . . no C34 H043 3.0500 . 2_765 no C34 H04G 2.9600 . . no C36 H027 2.9400 . 1_655 no C36 H04G 3.0500 . . no C37 H01A 2.9500 . . no C37 H02C 3.0700 . . no C38 H02G 2.9700 . 1_565 no C38 H04O 2.7700 . . no C38 H04L 3.0700 . . no C39 H04S 3.0100 . 1_565 no C39 H03H 2.9000 . . no C39 H01A 2.8000 . . no H027 C36 2.9400 . 1_455 no H027 H03P 2.5700 . . no H027 H04F 2.4300 . . no H027 H04A 2.2100 . 1_455 no H037 C32 2.8000 . 1_455 no H037 H04T 2.4300 . . no H037 H05C 2.4700 . . no H037 H02C 2.2200 . 1_455 no H047 C11 2.6300 . . no H047 H04K 2.1100 . . no H043 C34 3.0500 . 2_765 no H043 H03N 2.4400 . 2_765 no H014 C15 2.7200 . . no H014 H02I 2.1800 . . no H012 N1 2.5200 . . no H012 C1 2.7300 . . no H04J H03O 2.4400 . . no H04K C6 2.6900 . . no H04K H047 2.1100 . . no H04K H03Q 2.5600 . . no H04L Si4 3.3900 . . no H04L C6 3.0800 . . no H04L C38 3.0700 . . no H04L H01D 2.2500 . . no H03O H04J 2.4400 . . no H03O H01I 2.4200 . 1_465 no H03P C2 2.6700 . . no H03P H027 2.5700 . . no H03Q C6 3.0800 . . no H03Q H04K 2.5600 . . no H021 N1 2.5000 . . no H021 C1 3.0400 . . no H021 C2 2.9800 . . no H04D H02G 2.4500 . . no H04E C8 2.9600 . . no H04E H02I 2.5300 . . no H04F C2 2.8500 . . no H04F H027 2.4300 . . no H02G C38 2.9700 . 1_545 no H02G H04D 2.4500 . . no H02H C34 3.0700 . . no H02H H03A 2.4200 . . no H02H H03L 2.5000 . . no H02I C8 2.7300 . . no H02I H014 2.1800 . . no H02I H04E 2.5300 . . no H031 C24 2.7100 . . no H031 H04Q 2.1800 . . no H031 H04Q 2.5800 . 2_756 no H033 C27 2.6500 . . no H033 H03I 2.1300 . . no H017 N2 2.4600 . . no H017 C1 2.8800 . . no H017 C3 2.9900 . . no H04S C39 3.0100 . 1_545 no H04S H04P 2.4400 . . no H04S H02K 2.4300 . 1_545 no H04T C3 2.7700 . . no H04T H037 2.4300 . . no H04T H02A 2.4800 . 1_455 no H04U C18 2.9900 . . no H04U H04Q 2.5200 . . no H04P H04S 2.4400 . . no H04Q C18 2.7300 . . no H04Q H031 2.1800 . . no H04Q H04U 2.5200 . . no H04Q H031 2.5800 . 2_756 no H04R Si1 3.4100 . . no H04R C31 3.0900 . . no H04R H01G 2.3600 . . no H028 N2 2.5200 . . no H028 C1 2.8800 . . no H028 H02L 2.4700 . . no H05A C28 3.0200 . 1_465 no H05A H03G 2.4500 . . no H05B C20 3.0400 . . no H05B H03I 2.5700 . . no H05B C19 3.0300 . 2_666 no H05B C20 2.9500 . 2_666 no H05C C3 2.7100 . . no H05C H037 2.4700 . . no H03G H05A 2.4500 . . no H03H C39 2.9000 . . no H03H H02L 2.3900 . . no H03I C20 2.7100 . . no H03I H033 2.1300 . . no H03I H05B 2.5700 . . no H03I H02B 2.3300 . 2_766 no H01G C31 3.0600 . . no H01G H04R 2.3600 . . no H01G H02D 2.2700 . . no H01H Si2 3.2700 . . no H01H H02D 2.4600 . . no H01H H02A 2.4400 . . no H01I H03O 2.4200 . 1_645 no H03A Fe1 3.0600 . . no H03A C15 3.0600 . . no H03A C34 3.0200 . . no H03A H02H 2.4200 . . no H03A H03M 2.4000 . . no H03B C24 3.0200 . . no H03B H01F 2.5200 . 1_545 no H04G Si3 3.3000 . . no H04G C34 2.9600 . . no H04G C36 3.0500 . . no H04G H03M 2.1600 . . no H04G H04A 2.3400 . . no H04I H02A 2.5500 . . no H02D C28 2.7100 . . no H02D H01G 2.2700 . . no H02D H01H 2.4600 . . no H02E C17 3.1000 . . no H02E C18 2.7400 . . no H02A Si1 3.2300 . . no H02A H04T 2.4800 . 1_655 no H02A H01H 2.4400 . . no H02A H04I 2.5500 . . no H02B H03I 2.3300 . 2_766 no H02C C37 3.0700 . . no H02C H037 2.2200 . 1_655 no H02C H03D 2.2100 . . no H01A Fe1 3.2000 . . no H01A Si4 3.2500 . . no H01A C37 2.9500 . . no H01A C39 2.8000 . . no H01A H03D 2.2900 . . no H01A H02L 2.2900 . . no H01C Fe1 3.5200 . . no H01C C20 2.8800 . . no H01C C21 2.7400 . . no H03L Fe1 3.3700 . . no H03L C4 3.0500 . . no H03L C8 3.0900 . . no H03L C9 2.7900 . . no H03L H02H 2.5000 . . no H03M Fe1 3.3300 . . no H03M Si1 3.3700 . . no H03M C29 3.0500 . . no H03M C30 2.8900 . . no H03M H03A 2.4000 . . no H03M H04G 2.1600 . . no H03N C7 3.0200 . 2_765 no H03N H043 2.4400 . 2_765 no H04M C6 2.7700 . . no H04O C38 2.7700 . . no H04O H01D 2.4200 . . no H04O H01E 2.4200 . . no H04A H027 2.2100 . 1_655 no H04A H04G 2.3400 . . no H04B Si4 3.3600 . . no H04B H01E 2.5700 . . no H03D Si2 3.3100 . . no H03D C32 3.0000 . . no H03D C33 3.0200 . . no H03D H02C 2.2100 . . no H03D H01A 2.2900 . . no H01D C11 3.0900 . . no H01D H04L 2.2500 . . no H01D H04O 2.4200 . . no H01E Si3 3.2900 . . no H01E H04O 2.4200 . . no H01E H04B 2.5700 . . no H01F H03B 2.5200 . 1_565 no H02J C11 3.0000 . . no H02K H04S 2.4300 . 1_565 no H02L Fe1 2.8700 . . no H02L C25 3.0700 . . no H02L C27 2.9800 . . no H02L C33 2.9900 . . no H02L H028 2.4700 . . no H02L H03H 2.3900 . . no H02L H01A 2.2900 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C10 H012 N1 0.9800 2.5200 2.888(3) 102.00 . yes C13 H021 N1 0.9800 2.5000 2.921(3) 106.00 . yes C22 H017 N2 0.9800 2.4600 2.878(3) 106.00 . yes C25 H028 N2 0.9800 2.5200 2.910(3) 103.00 . yes # start Validation Reply Form _vrf_PLAT602_1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: With the aid of PLATON a solvent accessible area was found, but it was impossible to refine any reasonable molecule from difference Fourier peaks. Therefore the midpoint, the size and the number of electrons in that void were refined and the contribution to the calculated structure factors of the disordered solvent is taken into account by back-Fourier transformation with the program SQUEEZE (Sluis and Spek, 1990). The void is found around (-0.034 0.008 0.000), the size is 326 \%A^3^, and 46 e^-^ were detected. This electron number corresponds roughly to one toluene molecule. ; # end Validation Reply Form #===END # Attachment '- Compound 3 FeIMes.cif' #=============================================================================== data_ralr20 _database_code_depnum_ccdc_archive 'CCDC 835632' #TrackingRef '- Compound 3 FeIMes.cif' _audit_creation_date 'Nov 12 10:27:12 2010' _audit_creation_method 'PLATON
option' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H60 Fe N4 Si4' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C33 H60 Fe N4 Si4' _chemical_formula_sum 'C33 H60 Fe N4 Si4' _chemical_formula_iupac ? _chemical_formula_weight 681.06 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 16.6461(3) _cell_length_b 14.2890(3) _cell_length_c 16.7741(3) _cell_angle_alpha 90 _cell_angle_beta 99.705(2) _cell_angle_gamma 90 _cell_volume 3932.72(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 5173 _cell_measurement_theta_min 4.0986 _cell_measurement_theta_max 70.4559 _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4431 _exptl_crystal_size_mid 0.3543 _exptl_crystal_size_min 0.2560 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.432 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_T_min 0.281 _exptl_absorpt_correction_T_max 0.438 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5431 # number of measured reflections (redundant set) _diffrn_reflns_number 7577 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 70.66 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3675 # number of observed reflections (> n sig(I)) _reflns_number_gt 3554 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0803P)^2^+0.1949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3675 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.736 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.077 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Fe1 Fe Uani 0.00000 0.32165(2) 0.25000 1.000 0.0214(1) . . Si1 Si Uani 0.10285(3) 0.45151(3) 0.15621(3) 1.000 0.0327(2) . . Si2 Si Uani 0.17717(3) 0.39617(3) 0.32654(3) 1.000 0.0280(1) . . N1 N Uani 0.10262(8) 0.38751(9) 0.24306(8) 1.000 0.0246(4) . . N2 N Uani 0.01599(9) 0.10950(9) 0.19102(9) 1.000 0.0268(4) . . C1 C Uani 0.00000 0.16882(15) 0.25000 1.000 0.0245(6) . . C2 C Uani 0.0746(2) 0.57765(16) 0.16689(17) 1.000 0.0757(11) . . C3 C Uani 0.02894(12) 0.40120(13) 0.07087(11) 1.000 0.0327(5) . . C4 C Uani 0.20366(16) 0.4517(3) 0.12030(16) 1.000 0.0871(15) . . C5 C Uani 0.28454(12) 0.38595(17) 0.30489(13) 1.000 0.0430(6) . . C6 C Uani 0.16955(12) 0.29819(15) 0.39897(12) 1.000 0.0386(5) . . C7 C Uani 0.17432(14) 0.51060(15) 0.38111(12) 1.000 0.0419(6) . . C8 C Uani 0.03591(11) 0.13536(11) 0.11362(10) 1.000 0.0268(4) . . C9 C Uani -0.02324(11) 0.12559(11) 0.04456(11) 1.000 0.0290(4) . . C10 C Uani -0.00218(12) 0.15325(13) -0.02904(11) 1.000 0.0316(5) . . C11 C Uani 0.07544(13) 0.18473(12) -0.03521(12) 1.000 0.0332(5) . . C12 C Uani 0.13395(12) 0.18787(12) 0.03494(12) 1.000 0.0324(5) . . C13 C Uani 0.11565(11) 0.16445(12) 0.11005(11) 1.000 0.0290(5) . . C14 C Uani 0.17868(12) 0.17211(13) 0.18528(13) 1.000 0.0351(5) . . C15 C Uani 0.09551(15) 0.21453(16) -0.11582(13) 1.000 0.0461(7) . . C16 C Uani -0.10624(11) 0.08410(13) 0.04652(12) 1.000 0.0349(5) . . C17 C Uani 0.01023(12) 0.01654(12) 0.21307(12) 1.000 0.0350(5) . . H1A H Uiso 0.11490 0.60750 0.20850 1.000 0.1140 calc R H1B H Uiso 0.02060 0.58140 0.18250 1.000 0.1140 calc R H1C H Uiso 0.07370 0.60990 0.11520 1.000 0.1140 calc R H2A H Uiso 0.03630 0.33320 0.06930 1.000 0.0490 calc R H2B H Uiso 0.03850 0.42860 0.01980 1.000 0.0490 calc R H2C H Uiso -0.02680 0.41540 0.07880 1.000 0.0490 calc R H3A H Uiso 0.24290 0.48900 0.15740 1.000 0.1310 calc R H3B H Uiso 0.19710 0.47890 0.06590 1.000 0.1310 calc R H3C H Uiso 0.22370 0.38740 0.11880 1.000 0.1310 calc R H4A H Uiso 0.28910 0.32950 0.27280 1.000 0.0640 calc R H4B H Uiso 0.32280 0.38200 0.35600 1.000 0.0640 calc R H4C H Uiso 0.29740 0.44110 0.27460 1.000 0.0640 calc R H5A H Uiso 0.11260 0.29040 0.40580 1.000 0.0580 calc R H5B H Uiso 0.20300 0.31270 0.45140 1.000 0.0580 calc R H5C H Uiso 0.18900 0.24010 0.37760 1.000 0.0580 calc R H6A H Uiso 0.17270 0.56230 0.34240 1.000 0.0630 calc R H6B H Uiso 0.22320 0.51640 0.42260 1.000 0.0630 calc R H6C H Uiso 0.12570 0.51280 0.40680 1.000 0.0630 calc R H10 H Uiso -0.04230 0.15040 -0.07650 1.000 0.0380 calc R H12 H Uiso 0.18790 0.20660 0.03110 1.000 0.0390 calc R H14A H Uiso 0.23250 0.18140 0.17030 1.000 0.0530 calc R H14B H Uiso 0.17890 0.11450 0.21700 1.000 0.0530 calc R H14C H Uiso 0.16570 0.22540 0.21760 1.000 0.0530 calc R H15A H Uiso 0.12330 0.16320 -0.13890 1.000 0.0690 calc R H15B H Uiso 0.13120 0.26950 -0.10840 1.000 0.0690 calc R H15C H Uiso 0.04510 0.23020 -0.15260 1.000 0.0690 calc R H16A H Uiso -0.10570 0.01740 0.03310 1.000 0.0520 calc R H16B H Uiso -0.14700 0.11630 0.00700 1.000 0.0520 calc R H16C H Uiso -0.11990 0.09170 0.10070 1.000 0.0520 calc R H17 H Uiso 0.01910 -0.03680 0.18180 1.000 0.0420 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 Fe1 0.0240(2) 0.0203(2) 0.0199(2) 0.0000 0.0037(1) 0.0000 Si1 0.0363(3) 0.0352(3) 0.0257(3) 0.0079(2) 0.0026(2) -0.0065(2) Si2 0.0284(2) 0.0324(3) 0.0227(2) 0.0011(2) 0.0027(2) -0.0053(2) N1 0.0250(6) 0.0250(6) 0.0235(7) 0.0020(5) 0.0036(5) -0.0012(5) N2 0.0327(7) 0.0224(7) 0.0265(7) -0.0014(5) 0.0082(6) 0.0007(5) C1 0.0267(11) 0.0220(10) 0.0248(11) 0.0000 0.0048(9) 0.0000 C2 0.136(3) 0.0296(11) 0.0480(13) 0.0078(10) -0.0236(15) -0.0081(14) C3 0.0403(9) 0.0328(8) 0.0241(8) 0.0021(7) 0.0033(7) 0.0049(7) C4 0.0428(12) 0.178(4) 0.0408(13) 0.0441(18) 0.0079(11) -0.0216(17) C5 0.0289(9) 0.0651(13) 0.0338(10) 0.0025(9) 0.0022(8) -0.0053(8) C6 0.0390(9) 0.0433(10) 0.0313(9) 0.0097(8) -0.0008(8) -0.0036(8) C7 0.0504(11) 0.0427(11) 0.0340(9) -0.0082(8) 0.0113(8) -0.0154(9) C8 0.0342(8) 0.0211(7) 0.0266(8) -0.0020(6) 0.0091(7) 0.0023(6) C9 0.0331(8) 0.0244(7) 0.0306(8) -0.0061(7) 0.0085(7) 0.0005(6) C10 0.0396(9) 0.0295(8) 0.0258(8) -0.0067(7) 0.0060(7) 0.0023(7) C11 0.0449(10) 0.0259(8) 0.0316(9) -0.0033(6) 0.0147(8) 0.0029(7) C12 0.0349(9) 0.0273(8) 0.0381(10) -0.0038(7) 0.0154(8) 0.0000(6) C13 0.0321(9) 0.0226(7) 0.0331(9) -0.0042(6) 0.0075(7) 0.0037(6) C14 0.0326(9) 0.0349(9) 0.0375(10) -0.0045(7) 0.0054(8) 0.0037(7) C15 0.0619(13) 0.0443(11) 0.0368(10) 0.0003(9) 0.0223(9) 0.0006(10) C16 0.0335(9) 0.0328(9) 0.0388(9) -0.0068(8) 0.0070(7) -0.0033(7) C17 0.0493(10) 0.0203(8) 0.0379(9) -0.0020(7) 0.0146(8) 0.0007(7) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9709(13) . . yes Fe1 C1 2.184(2) . . yes Fe1 N1 1.9709(13) . 2_555 yes Si1 N1 1.7206(14) . . yes Si1 C2 1.879(2) . . yes Si1 C3 1.8671(19) . . yes Si1 C4 1.876(3) . . yes Si2 N1 1.7118(14) . . yes Si2 C5 1.889(2) . . yes Si2 C6 1.872(2) . . yes Si2 C7 1.878(2) . . yes N2 C1 1.3627(19) . . yes N2 C8 1.441(2) . . yes N2 C17 1.387(2) . . yes C8 C9 1.395(3) . . no C8 C13 1.402(3) . . no C9 C10 1.396(3) . . no C9 C16 1.509(3) . . no C10 C11 1.388(3) . . no C11 C12 1.396(3) . . no C11 C15 1.508(3) . . no C12 C13 1.386(3) . . no C13 C14 1.503(3) . . no C17 C17 1.339(3) . 2_555 no C2 H1A 0.9800 . . no C2 H1B 0.9800 . . no C2 H1C 0.9800 . . no C3 H2A 0.9800 . . no C3 H2B 0.9800 . . no C3 H2C 0.9800 . . no C4 H3A 0.9800 . . no C4 H3B 0.9800 . . no C4 H3C 0.9800 . . no C5 H4A 0.9800 . . no C5 H4B 0.9800 . . no C5 H4C 0.9800 . . no C6 H5A 0.9800 . . no C6 H5B 0.9800 . . no C6 H5C 0.9800 . . no C7 H6A 0.9800 . . no C7 H6B 0.9800 . . no C7 H6C 0.9800 . . no C10 H10 0.9500 . . no C12 H12 0.9500 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C14 H14C 0.9800 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C17 H17 0.9500 . . no 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 N1 Fe1 C1 118.52(4) . . . yes N1 Fe1 N1 122.96(6) . . 2_555 yes N1 Fe1 C1 118.52(4) 2_555 . . yes N1 Si1 C2 113.13(10) . . . yes N1 Si1 C3 110.44(8) . . . yes N1 Si1 C4 113.73(11) . . . yes C2 Si1 C3 107.42(11) . . . yes C2 Si1 C4 106.32(17) . . . yes C3 Si1 C4 105.30(11) . . . yes N1 Si2 C5 114.59(8) . . . yes N1 Si2 C6 110.96(8) . . . yes N1 Si2 C7 112.78(8) . . . yes C5 Si2 C6 103.70(10) . . . yes C5 Si2 C7 105.28(10) . . . yes C6 Si2 C7 108.95(9) . . . yes Fe1 N1 Si1 115.43(7) . . . yes Fe1 N1 Si2 120.15(7) . . . yes Si1 N1 Si2 123.33(8) . . . yes C1 N2 C8 126.68(13) . . . yes C1 N2 C17 111.81(15) . . . yes C8 N2 C17 121.51(14) . . . yes Fe1 C1 N2 128.46(9) . . . yes Fe1 C1 N2 128.46(9) . . 2_555 yes N2 C1 N2 103.07(16) . . 2_555 yes N2 C8 C9 119.01(16) . . . yes N2 C8 C13 118.54(15) . . . yes C9 C8 C13 122.35(16) . . . no C8 C9 C10 117.30(17) . . . no C8 C9 C16 122.81(16) . . . no C10 C9 C16 119.86(17) . . . no C9 C10 C11 122.22(18) . . . no C10 C11 C12 118.26(18) . . . no C10 C11 C15 120.53(18) . . . no C12 C11 C15 121.21(19) . . . no C11 C12 C13 121.96(18) . . . no C8 C13 C12 117.72(17) . . . no C8 C13 C14 121.18(16) . . . no C12 C13 C14 121.08(17) . . . no N2 C17 C17 106.66(16) . . 2_555 yes Si1 C2 H1A 109.00 . . . no Si1 C2 H1B 109.00 . . . no Si1 C2 H1C 109.00 . . . no H1A C2 H1B 110.00 . . . no H1A C2 H1C 109.00 . . . no H1B C2 H1C 109.00 . . . no Si1 C3 H2A 109.00 . . . no Si1 C3 H2B 109.00 . . . no Si1 C3 H2C 109.00 . . . no H2A C3 H2B 109.00 . . . no H2A C3 H2C 110.00 . . . no H2B C3 H2C 109.00 . . . no Si1 C4 H3A 109.00 . . . no Si1 C4 H3B 110.00 . . . no Si1 C4 H3C 110.00 . . . no H3A C4 H3B 109.00 . . . no H3A C4 H3C 109.00 . . . no H3B C4 H3C 109.00 . . . no Si2 C5 H4A 109.00 . . . no Si2 C5 H4B 109.00 . . . no Si2 C5 H4C 110.00 . . . no H4A C5 H4B 110.00 . . . no H4A C5 H4C 109.00 . . . no H4B C5 H4C 109.00 . . . no Si2 C6 H5A 109.00 . . . no Si2 C6 H5B 109.00 . . . no Si2 C6 H5C 109.00 . . . no H5A C6 H5B 109.00 . . . no H5A C6 H5C 109.00 . . . no H5B C6 H5C 110.00 . . . no Si2 C7 H6A 109.00 . . . no Si2 C7 H6B 109.00 . . . no Si2 C7 H6C 109.00 . . . no H6A C7 H6B 109.00 . . . no H6A C7 H6C 110.00 . . . no H6B C7 H6C 109.00 . . . no C9 C10 H10 119.00 . . . no C11 C10 H10 119.00 . . . no C11 C12 H12 119.00 . . . no C13 C12 H12 119.00 . . . no C13 C14 H14A 109.00 . . . no C13 C14 H14B 109.00 . . . no C13 C14 H14C 109.00 . . . no H14A C14 H14B 109.00 . . . no H14A C14 H14C 109.00 . . . no H14B C14 H14C 109.00 . . . no C11 C15 H15A 109.00 . . . no C11 C15 H15B 109.00 . . . no C11 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 109.00 . . . no H15B C15 H15C 109.00 . . . no C9 C16 H16A 109.00 . . . no C9 C16 H16B 109.00 . . . no C9 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no N2 C17 H17 127.00 . . . no C17 C17 H17 127.00 2_555 . . no 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 C1 Fe1 N1 Si1 114.29(6) . . . . no C1 Fe1 N1 Si2 -77.26(8) . . . . no N1 Fe1 N1 Si1 -65.71(9) 2_555 . . . no N1 Fe1 N1 Si2 102.74(9) 2_555 . . . no N1 Fe1 C1 N2 117.74(9) . . . 2_555 no N1 Fe1 C1 N2 -62.26(9) . . . . no N1 Fe1 C1 N2 117.74(9) 2_555 . . . no C3 Si1 N1 Fe1 -26.96(10) . . . . no C3 Si1 N1 Si2 165.01(9) . . . . no C4 Si1 N1 Fe1 -145.09(14) . . . . no C2 Si1 N1 Si2 -74.56(14) . . . . no C2 Si1 N1 Fe1 93.48(13) . . . . no C4 Si1 N1 Si2 46.88(16) . . . . no C7 Si2 N1 Fe1 -97.14(10) . . . . no C6 Si2 N1 Si1 -167.09(10) . . . . no C7 Si2 N1 Si1 70.36(12) . . . . no C5 Si2 N1 Si1 -50.07(13) . . . . no C5 Si2 N1 Fe1 142.43(10) . . . . no C6 Si2 N1 Fe1 25.41(11) . . . . no C8 N2 C1 Fe1 -0.8(2) . . . . no C17 N2 C1 Fe1 179.85(10) . . . . no C8 N2 C1 N2 179.20(16) . . . 2_555 no C17 N2 C1 N2 -0.15(15) . . . 2_555 no C1 N2 C8 C9 -104.75(18) . . . . no C17 N2 C8 C9 74.5(2) . . . . no C1 N2 C8 C13 78.8(2) . . . . no C17 N2 C8 C13 -101.9(2) . . . . no C1 N2 C17 C17 0.4(2) . . . 2_555 no C8 N2 C17 C17 -178.99(17) . . . 2_555 no N2 C8 C9 C10 178.67(15) . . . . no C13 C8 C9 C16 172.91(16) . . . . no N2 C8 C13 C12 179.17(15) . . . . no N2 C8 C13 C14 -2.2(2) . . . . no C9 C8 C13 C12 2.9(3) . . . . no C9 C8 C13 C14 -178.50(16) . . . . no N2 C8 C9 C16 -3.4(2) . . . . no C13 C8 C9 C10 -5.0(2) . . . . no C8 C9 C10 C11 3.3(3) . . . . no C16 C9 C10 C11 -174.68(17) . . . . no C9 C10 C11 C15 -179.61(18) . . . . no C9 C10 C11 C12 0.4(3) . . . . no C10 C11 C12 C13 -2.8(3) . . . . no C15 C11 C12 C13 177.27(18) . . . . no C11 C12 C13 C14 -177.46(17) . . . . no C11 C12 C13 C8 1.2(3) . . . . no N2 C17 C17 N2 -0.5(2) . . 2_555 2_555 no 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 Fe1 C13 3.9732(18) . . no Fe1 C14 3.960(2) . . no Fe1 C13 3.9732(18) . 2_555 no Fe1 C14 3.960(2) . 2_555 no Fe1 H2A 3.1900 . . no Fe1 H14C 3.2100 . . no Fe1 H2C 3.1300 . . no Fe1 H5A 2.9800 . . no Fe1 H2A 3.1900 . 2_555 no Fe1 H2C 3.1300 . 2_555 no Fe1 H5A 2.9800 . 2_555 no Fe1 H14C 3.2100 . 2_555 no Si2 C14 3.986(2) . . no Si1 H14C 3.5000 . . no Si2 H3A 3.4700 . . no Si2 H14C 3.0400 . . no Si2 H2C 3.1900 . 2_555 no N1 H14C 2.6100 . . no N2 H14B 2.6700 . . no N2 H16C 2.5100 . . no C4 C5 3.298(4) . . no C5 C4 3.298(4) . . no C6 C16 3.410(3) . 2_555 no C1 C14 3.334(2) . 2_555 no C1 C14 3.334(2) . . no C13 Fe1 3.9732(18) . . no C14 Fe1 3.960(2) . . no C14 C1 3.334(2) . . no C14 Si2 3.986(2) . . no C16 C6 3.410(3) . 2_555 no C16 C17 3.266(3) . . no C17 C16 3.266(3) . . no C3 H5A 2.9200 . 2_555 no C3 H2B 2.9900 . 3_565 no C4 H4C 2.7900 . . no C5 H3A 2.8600 . . no C6 H16B 3.1000 . 2_555 no C6 H16C 3.0600 . 2_555 no C6 H2C 2.9800 . 2_555 no C7 H3B 3.0600 . 4_565 no C7 H2C 2.9800 . 2_555 no C7 H14A 3.0900 . 6_555 no C1 H14C 3.0100 . . no C1 H14C 3.0100 . 2_555 no C8 H2A 2.9200 . . no C9 H5A 2.9800 . 2_555 no C10 H2A 3.0600 . . no C10 H16A 3.0400 . 3_555 no C10 H17 3.0300 . 3_555 no C11 H16A 2.9300 . 3_555 no C11 H2A 2.9000 . . no C12 H2A 2.7600 . . no C13 H2A 2.7800 . . no C14 H6A 3.0300 . 6_545 no C16 H5A 3.0600 . 2_555 no C16 H5C 3.0100 . 2_555 no C17 H16C 2.8300 . . no H1A H6A 2.3800 . . no H1B H1B 2.4700 . 2_555 no H2A Fe1 3.1900 . . no H2A C8 2.9200 . . no H2A C10 3.0600 . . no H2A C11 2.9000 . . no H2A C12 2.7600 . . no H2A C13 2.7800 . . no H2B C3 2.9900 . 3_565 no H2B H2B 2.4400 . 3_565 no H2C Fe1 3.1300 . . no H2C Si2 3.1900 . 2_555 no H2C C6 2.9800 . 2_555 no H2C C7 2.9800 . 2_555 no H2C H5A 2.3300 . 2_555 no H2C H6C 2.2000 . 2_555 no H3A Si2 3.4700 . . no H3A C5 2.8600 . . no H3A H4C 2.1300 . . no H3B C7 3.0600 . 4_564 no H3B H6B 2.5100 . 4_564 no H4A H14C 2.5800 . . no H4B H10 2.3800 . 8_555 no H4B H16B 2.5000 . 8_555 no H4C C4 2.7900 . . no H4C H3A 2.1300 . . no H4C H14B 2.5100 . 6_555 no H5A Fe1 2.9800 . . no H5A C3 2.9200 . 2_555 no H5A C9 2.9800 . 2_555 no H5A C16 3.0600 . 2_555 no H5A H2C 2.3300 . 2_555 no H5C C16 3.0100 . 2_555 no H5C H16C 2.4700 . 2_555 no H6A H1A 2.3800 . . no H6A C14 3.0300 . 6_555 no H6A H14A 2.3500 . 6_555 no H6B H3B 2.5100 . 4_565 no H6C H2C 2.2000 . 2_555 no H10 H15C 2.3800 . . no H10 H16B 2.4600 . . no H10 H17 2.4800 . 3_555 no H10 H4B 2.3800 . 8_454 no H12 H14A 2.3600 . . no H12 H15B 2.5400 . . no H14A H12 2.3600 . . no H14A C7 3.0900 . 6_545 no H14A H6A 2.3500 . 6_545 no H14B N2 2.6700 . . no H14B H4C 2.5100 . 6_545 no H14C Fe1 3.2100 . . no H14C Si1 3.5000 . . no H14C Si2 3.0400 . . no H14C N1 2.6100 . . no H14C C1 3.0100 . . no H14C H4A 2.5800 . . no H15B H12 2.5400 . . no H15C H10 2.3800 . . no H16A C10 3.0400 . 3_555 no H16A C11 2.9300 . 3_555 no H16B H10 2.4600 . . no H16B C6 3.1000 . 2_555 no H16B H4B 2.5000 . 8_454 no H16C N2 2.5100 . . no H16C C17 2.8300 . . no H16C C6 3.0600 . 2_555 no H16C H5C 2.4700 . 2_555 no H17 C10 3.0300 . 3_555 no H17 H10 2.4800 . 3_555 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C14 H14C N1 0.9800 2.6100 3.526(2) 156.00 . yes C16 H16C N2 0.9800 2.5100 2.913(2) 104.00 . yes #===END