# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jonathan Dilworth' _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK _publ_section_title ; Synthesis, structures and catalytic properties of iron(III) complexes with asymmetric N-capped tripodal NO3 ligands and a pentadentate N2O3 ligand ; loop_ _publ_author_name 'J R Dilworth' 'Sofia I Pascu' 'Lok Tong.' 'Yee-Lok Wong.' # Attachment 'Dalton_Trans_CIFs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 669890' _audit_creation_date 07-11-09 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.14690(10) _cell_length_b 32.0173(3) _cell_length_c 12.68600(10) _cell_angle_alpha 90 _cell_angle_beta 103.5726(4) _cell_angle_gamma 90 _cell_volume 4006.28(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C41 H56 Fe1 N3 O3' _chemical_formula_moiety 'C41 H56 Fe1 N3 O3' _chemical_compound_source ? _chemical_formula_weight 694.76 _cell_measurement_reflns_used 33694 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.34 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 33694 _reflns_number_total 9281 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections with Friedels Law is 9281 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9187 _diffrn_reflns_theta_min 5.121 _diffrn_reflns_theta_max 27.515 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 41 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.36 _refine_diff_density_max 0.36 _refine_ls_number_reflns 5947 _refine_ls_number_restraints 24 _refine_ls_number_parameters 470 #_refine_ls_R_factor_ref 0.0437 _refine_ls_wR_factor_ref 0.0505 _refine_ls_goodness_of_fit_ref 1.0592 #_reflns_number_all 9107 _refine_ls_R_factor_all 0.0809 _refine_ls_wR_factor_all 0.0604 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5947 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_gt 0.0505 _refine_ls_shift/su_max 0.026203 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.31 0.462 2.30 0.461 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.27906(3) 0.333984(9) 0.57319(2) 0.0311 1.0000 Uani . . . . . . O1 O 0.24522(16) 0.27510(5) 0.55296(16) 0.0485 1.0000 Uani . . . . . . O2 O 0.25672(15) 0.36854(5) 0.68778(12) 0.0347 1.0000 Uani . . . . . . O3 O 0.30731(14) 0.36531(5) 0.45698(12) 0.0341 1.0000 Uani . . . . . . N1 N 0.05754(16) 0.33502(5) 0.50258(13) 0.0277 1.0000 Uani . . . . . . N2 N 0.48019(18) 0.31816(6) 0.64544(16) 0.0388 1.0000 Uani . . . . . . N3 N 0.6594(2) 0.27960(7) 0.70933(18) 0.0490 1.0000 Uani . . . . . . C1 C 0.1219(2) 0.26289(7) 0.4982(2) 0.0405 1.0000 Uani . . . . . . C2 C 0.0885(3) 0.22108(8) 0.4728(3) 0.0534 1.0000 Uani . . . . . . C3 C -0.0401(3) 0.21038(8) 0.4154(2) 0.0525 1.0000 Uani . . . . . . C4 C -0.1398(2) 0.24006(8) 0.3802(2) 0.0455 1.0000 Uani . . . . . . C5 C -0.1071(2) 0.28159(7) 0.40601(19) 0.0382 1.0000 Uani . . . . . . C6 C 0.0208(2) 0.29276(6) 0.46440(17) 0.0313 1.0000 Uani . . . . . . C7 C -0.2803(3) 0.22833(10) 0.3163(3) 0.0630 1.0000 Uani . . . . . . C8 C 0.1591(2) 0.39718(7) 0.68795(16) 0.0311 1.0000 Uani . . . . . . C9 C 0.1909(2) 0.43741(7) 0.73496(17) 0.0357 1.0000 Uani . . . . . . C10 C 0.0835(3) 0.46546(7) 0.72549(19) 0.0398 1.0000 Uani . . . . . . C11 C -0.0513(2) 0.45645(7) 0.67398(19) 0.0395 1.0000 Uani . . . . . . C12 C -0.0785(2) 0.41655(7) 0.63387(18) 0.0334 1.0000 Uani . . . . . . C13 C 0.0243(2) 0.38713(6) 0.64104(16) 0.0297 1.0000 Uani . . . . . . C14 C -0.0093(2) 0.34438(6) 0.59380(16) 0.0288 1.0000 Uani . . . . . . C15 C 0.3370(3) 0.45025(8) 0.7879(2) 0.0458 1.0000 Uani . . . . . . C16 C 0.4045(3) 0.41864(10) 0.8748(2) 0.0605 1.0000 Uani . . . . . . C17 C 0.4165(3) 0.45286(10) 0.6994(3) 0.0574 1.0000 Uani . . . . . . C18 C 0.3441(3) 0.49324(10) 0.8420(3) 0.0701 1.0000 Uani . . . . . . C19 C -0.1610(3) 0.49053(8) 0.6613(2) 0.0520 1.0000 Uani . . . . . . C20 C -0.2956(3) 0.47673(9) 0.5883(3) 0.0574 1.0000 Uani . . . . . . C21 C -0.1171(4) 0.52875(10) 0.6046(4) 0.0870 1.0000 Uani . . . . . . C22 C -0.1846(4) 0.50163(15) 0.7714(3) 0.0933 1.0000 Uani . . . . . . C23 C 0.2382(2) 0.36541(7) 0.35202(17) 0.0312 1.0000 Uani . . . . . . C24 C 0.3060(2) 0.36906(8) 0.26745(19) 0.0390 1.0000 Uani . . . . . . C25 C 0.2270(2) 0.37059(10) 0.16249(19) 0.0495 1.0000 Uani D . . . . . C26 C 0.0857(2) 0.36882(10) 0.13601(18) 0.0533 1.0000 Uani D . . . . . C27 C 0.0223(2) 0.36517(9) 0.22123(19) 0.0425 1.0000 Uani D . . . . . C28 C 0.0960(2) 0.36411(7) 0.32823(17) 0.0312 1.0000 Uani . . . . . . C29 C 0.0223(2) 0.36765(6) 0.41744(17) 0.0297 1.0000 Uani . . . . . . C30 C 0.4621(2) 0.37200(9) 0.2921(2) 0.0462 1.0000 Uani . . . . . . C31 C 0.5100(2) 0.41082(9) 0.3606(2) 0.0505 1.0000 Uani . . . . . . C32 C 0.5254(3) 0.33296(10) 0.3525(3) 0.0650 1.0000 Uani . . . . . . C33 C 0.5134(3) 0.37614(14) 0.1879(3) 0.0758 1.0000 Uani . . . . . . C34 C 0.0031(7) 0.3611(2) 0.0178(5) 0.0544 0.472(8) Uani D . P 1 1 . C35 C -0.0265(9) 0.3147(2) -0.0067(5) 0.0825 0.472(8) Uani D . P 1 1 . C36 C 0.0835(9) 0.3793(4) -0.0579(6) 0.1016 0.472(8) Uani D . P 1 1 . C37 C -0.1312(11) 0.3844(4) -0.0009(11) 0.0779 0.472(8) Uani D . P 1 1 . C134 C 0.0051(6) 0.3806(2) 0.0177(5) 0.0593 0.528(8) Uani D . P 1 2 . C135 C 0.0492(8) 0.3494(3) -0.0581(5) 0.0977 0.528(8) Uani D . P 1 2 . C136 C 0.0326(7) 0.4246(3) -0.0201(5) 0.0832 0.528(8) Uani D . P 1 2 . C137 C -0.1462(8) 0.3761(4) 0.0094(8) 0.0803 0.528(8) Uani D . P 1 2 . C38 C 0.5915(2) 0.34379(8) 0.6778(2) 0.0481 1.0000 Uani . . . . . . C39 C 0.7024(2) 0.32017(9) 0.7169(2) 0.0488 1.0000 Uani . . . . . . C40 C 0.5257(2) 0.27977(8) 0.6662(2) 0.0482 1.0000 Uani . . . . . . C41 C 0.7424(3) 0.24224(12) 0.7444(3) 0.0781 1.0000 Uani . . . . . . H21 H 0.1583 0.1988 0.4964 0.0634 1.0000 Uiso . . . . . . H31 H -0.0618 0.1803 0.3987 0.0626 1.0000 Uiso . . . . . . H51 H -0.1772 0.3037 0.3819 0.0453 1.0000 Uiso . . . . . . H71 H -0.2856 0.1974 0.3053 0.0727 1.0000 Uiso . . . . . . H72 H -0.3488 0.2372 0.3571 0.0727 1.0000 Uiso . . . . . . H73 H -0.2995 0.2426 0.2442 0.0727 1.0000 Uiso . . . . . . H101 H 0.1042 0.4939 0.7576 0.0496 1.0000 Uiso . . . . . . H121 H -0.1741 0.4086 0.5989 0.0420 1.0000 Uiso . . . . . . H141 H -0.1098 0.3423 0.5657 0.0346 1.0000 Uiso . . . . . . H142 H 0.0214 0.3232 0.6524 0.0346 1.0000 Uiso . . . . . . H161 H 0.4994 0.4278 0.9080 0.0687 1.0000 Uiso . . . . . . H162 H 0.3520 0.4170 0.9323 0.0687 1.0000 Uiso . . . . . . H163 H 0.4060 0.3905 0.8408 0.0687 1.0000 Uiso . . . . . . H171 H 0.5122 0.4612 0.7325 0.0693 1.0000 Uiso . . . . . . H172 H 0.3736 0.4741 0.6441 0.0693 1.0000 Uiso . . . . . . H173 H 0.4157 0.4250 0.6637 0.0693 1.0000 Uiso . . . . . . H181 H 0.4409 0.5004 0.8754 0.0816 1.0000 Uiso . . . . . . H182 H 0.2916 0.4927 0.8995 0.0816 1.0000 Uiso . . . . . . H183 H 0.3046 0.5147 0.7863 0.0816 1.0000 Uiso . . . . . . H201 H -0.3634 0.4998 0.5825 0.0699 1.0000 Uiso . . . . . . H202 H -0.3293 0.4514 0.6200 0.0699 1.0000 Uiso . . . . . . H203 H -0.2823 0.4699 0.5145 0.0699 1.0000 Uiso . . . . . . H211 H -0.1883 0.5509 0.5962 0.1057 1.0000 Uiso . . . . . . H212 H -0.0294 0.5398 0.6491 0.1057 1.0000 Uiso . . . . . . H213 H -0.1052 0.5204 0.5314 0.1057 1.0000 Uiso . . . . . . H221 H -0.2558 0.5238 0.7629 0.1111 1.0000 Uiso . . . . . . H222 H -0.0983 0.5122 0.8192 0.1111 1.0000 Uiso . . . . . . H223 H -0.2152 0.4762 0.8049 0.1111 1.0000 Uiso . . . . . . H251 H 0.2742 0.3731 0.1019 0.0605 1.0000 Uiso . . . . . . H271 H -0.0789 0.3633 0.2052 0.0507 1.0000 Uiso . . . . . . H291 H 0.0438 0.3955 0.4528 0.0357 1.0000 Uiso . . . . . . H292 H -0.0772 0.3658 0.3843 0.0357 1.0000 Uiso . . . . . . H311 H 0.6112 0.4126 0.3763 0.0606 1.0000 Uiso . . . . . . H312 H 0.4697 0.4363 0.3200 0.0606 1.0000 Uiso . . . . . . H313 H 0.4805 0.4090 0.4303 0.0606 1.0000 Uiso . . . . . . H321 H 0.6264 0.3351 0.3681 0.0785 1.0000 Uiso . . . . . . H322 H 0.4962 0.3304 0.4223 0.0785 1.0000 Uiso . . . . . . H323 H 0.4950 0.3077 0.3068 0.0785 1.0000 Uiso . . . . . . H331 H 0.6146 0.3780 0.2070 0.0936 1.0000 Uiso . . . . . . H332 H 0.4747 0.4020 0.1481 0.0936 1.0000 Uiso . . . . . . H333 H 0.4843 0.3512 0.1408 0.0936 1.0000 Uiso . . . . . . H351 H -0.0796 0.3114 -0.0833 0.0939 0.4724 Uiso . . . 1 1 . H352 H -0.0801 0.3033 0.0437 0.0939 0.4724 Uiso . . . 1 1 . H353 H 0.0609 0.2991 0.0036 0.0939 0.4724 Uiso . . . 1 1 . H361 H 0.0328 0.3749 -0.1347 0.1201 0.4724 Uiso . . . 1 1 . H362 H 0.0969 0.4099 -0.0436 0.1201 0.4724 Uiso . . . 1 1 . H363 H 0.1737 0.3652 -0.0452 0.1201 0.4724 Uiso . . . 1 1 . H371 H -0.1843 0.3794 -0.0769 0.0946 0.4724 Uiso . . . 1 1 . H372 H -0.1137 0.4150 0.0106 0.0946 0.4724 Uiso . . . 1 1 . H373 H -0.1841 0.3740 0.0511 0.0946 0.4724 Uiso . . . 1 1 . H1351 H 0.0007 0.3555 -0.1347 0.1151 0.5276 Uiso . . . 1 2 . H1352 H 0.1492 0.3518 -0.0508 0.1151 0.5276 Uiso . . . 1 2 . H1353 H 0.0268 0.3204 -0.0386 0.1151 0.5276 Uiso . . . 1 2 . H1361 H -0.0226 0.4293 -0.0956 0.0974 0.5276 Uiso . . . 1 2 . H1362 H 0.0072 0.4458 0.0295 0.0974 0.5276 Uiso . . . 1 2 . H1363 H 0.1310 0.4275 -0.0190 0.0974 0.5276 Uiso . . . 1 2 . H1371 H -0.1974 0.3835 -0.0656 0.0922 0.5276 Uiso . . . 1 2 . H1372 H -0.1738 0.3952 0.0628 0.0922 0.5276 Uiso . . . 1 2 . H1373 H -0.1670 0.3466 0.0257 0.0922 0.5276 Uiso . . . 1 2 . H381 H 0.5904 0.3750 0.6730 0.0560 1.0000 Uiso . . . . . . H391 H 0.7972 0.3303 0.7456 0.0569 1.0000 Uiso . . . . . . H401 H 0.4680 0.2541 0.6515 0.0565 1.0000 Uiso . . . . . . H411 H 0.6840 0.2168 0.7289 0.0919 1.0000 Uiso . . . . . . H412 H 0.7837 0.2440 0.8240 0.0919 1.0000 Uiso . . . . . . H413 H 0.8159 0.2405 0.7040 0.0919 1.0000 Uiso . . . . . . 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 0.02432(14) 0.03056(16) 0.03596(16) 0.00086(14) 0.00232(11) 0.00200(12) O1 0.0317(8) 0.0310(8) 0.0754(12) -0.0012(8) -0.0025(8) 0.0046(6) O2 0.0328(8) 0.0353(8) 0.0332(8) -0.0006(6) 0.0021(6) 0.0002(6) O3 0.0249(7) 0.0431(9) 0.0323(8) 0.0010(6) 0.0028(6) -0.0021(6) N1 0.0249(8) 0.0283(8) 0.0299(8) -0.0001(7) 0.0067(6) 0.0024(7) N2 0.0278(9) 0.0438(11) 0.0418(10) 0.0074(9) 0.0022(8) 0.0024(8) N3 0.0301(10) 0.0583(14) 0.0555(13) 0.0169(11) 0.0040(9) 0.0116(9) C1 0.0341(11) 0.0338(12) 0.0526(14) -0.0067(10) 0.0082(10) 0.0006(9) C2 0.0479(14) 0.0322(13) 0.0782(19) -0.0088(12) 0.0109(13) 0.0060(11) C3 0.0511(15) 0.0347(13) 0.0707(18) -0.0175(12) 0.0121(13) -0.0068(11) C4 0.0400(13) 0.0427(13) 0.0522(15) -0.0156(11) 0.0076(11) -0.0093(10) C5 0.0315(11) 0.0373(12) 0.0446(12) -0.0079(10) 0.0066(9) 0.0002(9) C6 0.0294(10) 0.0288(10) 0.0366(11) -0.0055(9) 0.0093(8) -0.0013(8) C7 0.0530(16) 0.0534(17) 0.075(2) -0.0193(15) 0.0009(14) -0.0132(13) C8 0.0386(11) 0.0298(10) 0.0259(10) 0.0017(8) 0.0097(8) -0.0020(8) C9 0.0429(12) 0.0357(11) 0.0306(11) -0.0006(9) 0.0128(9) -0.0085(9) C10 0.0549(14) 0.0267(11) 0.0424(12) -0.0046(9) 0.0210(11) -0.0067(10) C11 0.0488(13) 0.0323(11) 0.0444(13) -0.0005(10) 0.0250(11) -0.0005(10) C12 0.0363(11) 0.0313(11) 0.0375(11) 0.0008(9) 0.0185(9) -0.0006(9) C13 0.0354(11) 0.0304(10) 0.0257(10) 0.0019(8) 0.0121(8) -0.0008(8) C14 0.0278(10) 0.0278(10) 0.0310(10) 0.0006(8) 0.0075(8) -0.0009(7) C15 0.0478(14) 0.0428(13) 0.0445(13) -0.0047(11) 0.0062(11) -0.0141(11) C16 0.0553(16) 0.0667(19) 0.0496(16) 0.0026(14) -0.0073(13) -0.0203(14) C17 0.0447(15) 0.0613(18) 0.0673(18) 0.0051(14) 0.0153(13) -0.0175(13) C18 0.0623(19) 0.0580(19) 0.084(2) -0.0223(16) 0.0044(16) -0.0231(15) C19 0.0534(15) 0.0351(13) 0.0758(19) -0.0088(12) 0.0314(14) 0.0027(11) C20 0.0524(16) 0.0479(16) 0.0745(19) 0.0019(14) 0.0202(14) 0.0139(12) C21 0.066(2) 0.0433(17) 0.155(4) 0.025(2) 0.033(2) 0.0077(15) C22 0.076(2) 0.120(3) 0.081(2) -0.041(2) 0.0141(19) 0.035(2) C23 0.0267(10) 0.0345(11) 0.0312(10) -0.0059(8) 0.0046(8) -0.0019(8) C24 0.0288(11) 0.0517(14) 0.0379(12) -0.0145(10) 0.0107(9) -0.0077(9) C25 0.0383(13) 0.0815(19) 0.0314(12) -0.0145(12) 0.0134(10) -0.0159(12) C26 0.0364(13) 0.094(2) 0.0289(12) -0.0086(13) 0.0063(10) -0.0169(13) C27 0.0270(11) 0.0666(16) 0.0331(11) -0.0047(11) 0.0052(9) -0.0090(10) C28 0.0262(10) 0.0376(11) 0.0302(10) -0.0028(8) 0.0074(8) -0.0013(8) C29 0.0249(9) 0.0328(11) 0.0314(10) 0.0019(8) 0.0067(8) 0.0036(8) C30 0.0270(11) 0.0663(17) 0.0474(14) -0.0178(12) 0.0129(10) -0.0101(11) C31 0.0340(12) 0.0661(17) 0.0514(15) -0.0101(13) 0.0102(11) -0.0149(11) C32 0.0309(12) 0.0689(19) 0.096(2) -0.0187(18) 0.0174(13) 0.0060(13) C33 0.0376(14) 0.138(3) 0.0583(18) -0.032(2) 0.0245(13) -0.0241(17) C34 0.053(4) 0.085(7) 0.022(3) -0.004(3) 0.003(3) -0.028(4) C35 0.102(6) 0.099(6) 0.034(3) -0.007(3) -0.010(3) -0.030(5) C36 0.087(6) 0.182(13) 0.032(4) 0.013(5) 0.005(4) -0.064(7) C37 0.092(9) 0.098(7) 0.047(6) 0.028(5) 0.023(5) 0.016(7) C134 0.040(3) 0.099(7) 0.037(3) -0.022(4) 0.007(2) -0.027(4) C135 0.065(5) 0.184(11) 0.039(4) -0.041(5) 0.001(3) -0.016(5) C136 0.076(4) 0.130(7) 0.038(3) 0.025(4) 0.001(3) -0.022(4) C137 0.042(4) 0.160(11) 0.028(4) 0.022(5) -0.015(3) -0.032(5) C38 0.0342(12) 0.0482(15) 0.0575(15) 0.0057(11) 0.0016(11) -0.0031(10) C39 0.0269(11) 0.0658(17) 0.0496(14) 0.0047(12) 0.0008(10) -0.0020(11) C40 0.0293(11) 0.0457(14) 0.0663(17) 0.0117(12) 0.0047(11) 0.0056(10) C41 0.0488(17) 0.076(2) 0.105(3) 0.035(2) 0.0089(17) 0.0261(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.1772(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 1.9226(17) yes Fe1 . O2 . 1.8823(15) yes Fe1 . O3 . 1.8602(15) yes Fe1 . N1 . 2.2160(16) yes Fe1 . N2 . 2.0938(18) yes O1 . C1 . 1.339(3) yes O2 . C8 . 1.350(3) yes O3 . C23 . 1.351(3) yes N1 . C6 . 1.456(3) yes N1 . C14 . 1.502(3) yes N1 . C29 . 1.485(3) yes N2 . C38 . 1.379(3) yes N2 . C40 . 1.318(3) yes N3 . C39 . 1.366(4) yes N3 . C40 . 1.338(3) yes N3 . C41 . 1.471(4) yes C1 . C2 . 1.400(3) yes C1 . C6 . 1.394(3) yes C2 . C3 . 1.380(4) yes C2 . H21 . 1.000 no C3 . C4 . 1.384(4) yes C3 . H31 . 1.000 no C4 . C5 . 1.391(3) yes C4 . C7 . 1.513(4) yes C5 . C6 . 1.382(3) yes C5 . H51 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . C9 . 1.424(3) yes C8 . C13 . 1.395(3) yes C9 . C10 . 1.396(3) yes C9 . C15 . 1.533(3) yes C10 . C11 . 1.401(4) yes C10 . H101 . 1.000 no C11 . C12 . 1.379(3) yes C11 . C19 . 1.540(3) yes C12 . C13 . 1.393(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.501(3) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.535(4) yes C15 . C17 . 1.531(4) yes C15 . C18 . 1.532(4) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no C19 . C20 . 1.525(4) yes C19 . C21 . 1.537(4) yes C19 . C22 . 1.514(5) yes C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C21 . H211 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . C24 . 1.409(3) yes C23 . C28 . 1.404(3) yes C24 . C25 . 1.385(3) yes C24 . C30 . 1.544(3) yes C25 . C26 . 1.395(3) yes C25 . H251 . 1.000 no C26 . C27 . 1.387(3) yes C26 . C34 . 1.556(6) yes C26 . C134 . 1.577(6) yes C27 . C28 . 1.388(3) yes C27 . H271 . 1.000 no C28 . C29 . 1.500(3) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C30 . C31 . 1.529(4) yes C30 . C32 . 1.527(4) yes C30 . C33 . 1.535(4) yes C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C32 . H321 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no C34 . C35 . 1.534(7) yes C34 . C36 . 1.515(7) yes C34 . C37 . 1.522(8) yes C34 . C135 . 1.225(10) yes C34 . C137 . 1.568(14) yes C35 . C135 . 1.576(13) yes C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C35 . H1353 . 0.770 no C36 . C134 . 1.383(11) yes C36 . C135 . 1.020(12) yes C36 . C136 . 1.648(14) yes C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C36 . H1352 . 1.097 no C37 . C134 . 1.353(14) yes C37 . H371 . 1.000 no C37 . H372 . 0.999 no C37 . H373 . 1.000 no C37 . H1371 . 0.930 no C37 . H1372 . 1.060 no C134 . C135 . 1.524(7) yes C134 . C136 . 1.537(7) yes C134 . C137 . 1.521(8) yes C135 . H361 . 1.250 no C135 . H1351 . 1.000 no C135 . H1352 . 1.000 no C135 . H1353 . 1.000 no C136 . H362 . 0.910 no C136 . H1361 . 1.000 no C136 . H1362 . 1.000 no C136 . H1363 . 1.000 no C137 . H371 . 1.078 no C137 . H372 . 1.288 no C137 . H373 . 0.726 no C137 . H1371 . 1.000 no C137 . H1372 . 1.000 no C137 . H1373 . 1.000 no C38 . C39 . 1.349(4) yes C38 . H381 . 1.000 no C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . H411 . 1.000 no C41 . H412 . 1.000 no C41 . H413 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 129.00(8) yes O1 . Fe1 . O3 . 118.61(8) yes O2 . Fe1 . O3 . 111.35(7) yes O1 . Fe1 . N1 . 80.11(6) yes O2 . Fe1 . N1 . 90.51(6) yes O3 . Fe1 . N1 . 90.11(6) yes O1 . Fe1 . N2 . 86.92(7) yes O2 . Fe1 . N2 . 94.92(7) yes O3 . Fe1 . N2 . 99.31(7) yes N1 . Fe1 . N2 . 166.55(7) yes Fe1 . O1 . C1 . 118.12(14) yes Fe1 . O2 . C8 . 128.44(13) yes Fe1 . O3 . C23 . 129.89(13) yes Fe1 . N1 . C6 . 106.06(12) yes Fe1 . N1 . C14 . 106.86(11) yes C6 . N1 . C14 . 108.37(15) yes Fe1 . N1 . C29 . 110.65(12) yes C6 . N1 . C29 . 114.38(16) yes C14 . N1 . C29 . 110.17(15) yes Fe1 . N2 . C38 . 129.26(17) yes Fe1 . N2 . C40 . 124.97(16) yes C38 . N2 . C40 . 105.7(2) yes C39 . N3 . C40 . 107.5(2) yes C39 . N3 . C41 . 127.0(2) yes C40 . N3 . C41 . 125.5(3) yes O1 . C1 . C2 . 123.0(2) yes O1 . C1 . C6 . 119.3(2) yes C2 . C1 . C6 . 117.7(2) yes C1 . C2 . C3 . 120.4(2) yes C1 . C2 . H21 . 119.8 no C3 . C2 . H21 . 119.8 no C2 . C3 . C4 . 121.9(2) yes C2 . C3 . H31 . 119.0 no C4 . C3 . H31 . 119.0 no C3 . C4 . C5 . 117.7(2) yes C3 . C4 . C7 . 121.9(2) yes C5 . C4 . C7 . 120.4(2) yes C4 . C5 . C6 . 121.0(2) yes C4 . C5 . H51 . 119.5 no C6 . C5 . H51 . 119.5 no N1 . C6 . C1 . 115.01(18) yes N1 . C6 . C5 . 123.61(19) yes C1 . C6 . C5 . 121.2(2) yes C4 . C7 . H71 . 109.5 no C4 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no C4 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no O2 . C8 . C9 . 121.34(19) yes O2 . C8 . C13 . 119.27(19) yes C9 . C8 . C13 . 119.4(2) yes C8 . C9 . C10 . 116.7(2) yes C8 . C9 . C15 . 121.8(2) yes C10 . C9 . C15 . 121.3(2) yes C9 . C10 . C11 . 124.4(2) yes C9 . C10 . H101 . 117.8 no C11 . C10 . H101 . 117.8 no C10 . C11 . C12 . 116.9(2) yes C10 . C11 . C19 . 120.4(2) yes C12 . C11 . C19 . 122.7(2) yes C11 . C12 . C13 . 121.3(2) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.3 no C8 . C13 . C12 . 121.1(2) yes C8 . C13 . C14 . 119.27(18) yes C12 . C13 . C14 . 119.60(19) yes N1 . C14 . C13 . 112.84(16) yes N1 . C14 . H141 . 108.6 no C13 . C14 . H141 . 108.6 no N1 . C14 . H142 . 108.6 no C13 . C14 . H142 . 108.6 no H141 . C14 . H142 . 109.5 no C9 . C15 . C16 . 111.1(2) yes C9 . C15 . C17 . 108.4(2) yes C16 . C15 . C17 . 109.9(2) yes C9 . C15 . C18 . 112.1(2) yes C16 . C15 . C18 . 107.7(2) yes C17 . C15 . C18 . 107.5(2) yes C15 . C16 . H161 . 109.5 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . H171 . 109.5 no C15 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C15 . C18 . H181 . 109.5 no C15 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no C15 . C18 . H183 . 109.5 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C11 . C19 . C20 . 112.4(2) yes C11 . C19 . C21 . 109.4(2) yes C20 . C19 . C21 . 105.2(3) yes C11 . C19 . C22 . 109.7(3) yes C20 . C19 . C22 . 108.4(2) yes C21 . C19 . C22 . 111.8(3) yes C19 . C20 . H201 . 109.5 no C19 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C19 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C19 . C21 . H211 . 109.5 no C19 . C21 . H212 . 109.5 no H211 . C21 . H212 . 109.5 no C19 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C19 . C22 . H221 . 109.5 no C19 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.5 no C19 . C22 . H223 . 109.5 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no O3 . C23 . C24 . 121.17(18) yes O3 . C23 . C28 . 118.75(18) yes C24 . C23 . C28 . 119.99(19) yes C23 . C24 . C25 . 117.3(2) yes C23 . C24 . C30 . 120.8(2) yes C25 . C24 . C30 . 121.8(2) yes C24 . C25 . C26 . 124.1(2) yes C24 . C25 . H251 . 117.9 no C26 . C25 . H251 . 117.9 no C25 . C26 . C27 . 117.0(2) yes C25 . C26 . C34 . 122.0(3) yes C27 . C26 . C34 . 119.6(3) yes C25 . C26 . C134 . 119.6(3) yes C27 . C26 . C134 . 122.0(3) yes C34 . C26 . C134 . 22.9(3) yes C26 . C27 . C28 . 121.5(2) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 119.3 no C23 . C28 . C27 . 120.02(19) yes C23 . C28 . C29 . 120.32(18) yes C27 . C28 . C29 . 119.11(18) yes C28 . C29 . N1 . 114.73(16) yes C28 . C29 . H291 . 108.1 no N1 . C29 . H291 . 108.1 no C28 . C29 . H292 . 108.1 no N1 . C29 . H292 . 108.1 no H291 . C29 . H292 . 109.5 no C24 . C30 . C31 . 109.8(2) yes C24 . C30 . C32 . 110.0(2) yes C31 . C30 . C32 . 109.9(2) yes C24 . C30 . C33 . 111.7(2) yes C31 . C30 . C33 . 107.0(2) yes C32 . C30 . C33 . 108.4(3) yes C30 . C31 . H311 . 109.5 no C30 . C31 . H312 . 109.5 no H311 . C31 . H312 . 109.5 no C30 . C31 . H313 . 109.5 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C30 . C32 . H321 . 109.5 no C30 . C32 . H322 . 109.5 no H321 . C32 . H322 . 109.5 no C30 . C32 . H323 . 109.5 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C30 . C33 . H331 . 109.5 no C30 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.5 no C30 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C26 . C34 . C35 . 112.6(4) yes C26 . C34 . C36 . 107.5(5) yes C35 . C34 . C36 . 110.7(6) yes C26 . C34 . C37 . 109.5(6) yes C35 . C34 . C37 . 108.5(6) yes C36 . C34 . C37 . 107.9(7) yes C26 . C34 . C135 . 126.0(6) yes C35 . C34 . C135 . 68.6(6) yes C36 . C34 . C135 . 42.1(6) yes C37 . C34 . C135 . 121.4(8) yes C26 . C34 . C137 . 108.1(6) yes C35 . C34 . C137 . 98.1(7) yes C36 . C34 . C137 . 119.7(8) yes C37 . C34 . C137 . 12.8(9) yes C135 . C34 . C137 . 125.6(7) yes C34 . C35 . C135 . 46.4(4) yes C34 . C35 . H351 . 109.5 no C135 . C35 . H351 . 82.8 no C34 . C35 . H352 . 109.5 no C135 . C35 . H352 . 155.8 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 109.5 no C135 . C35 . H353 . 84.4 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C34 . C35 . H1353 . 75.4 no C135 . C35 . H1353 . 31.1 no H351 . C35 . H1353 . 78.3 no H352 . C35 . H1353 . 167.8 no H353 . C35 . H1353 . 58.5 no C34 . C36 . C134 . 24.2(4) yes C34 . C36 . C135 . 53.6(6) yes C134 . C36 . C135 . 77.1(6) yes C34 . C36 . C136 . 84.4(6) yes C134 . C36 . C136 . 60.2(6) yes C135 . C36 . C136 . 134.3(9) yes C34 . C36 . H361 . 109.5 no C134 . C36 . H361 . 115.6 no C135 . C36 . H361 . 76.5 no C136 . C36 . H361 . 106.5 no C34 . C36 . H362 . 109.5 no C134 . C36 . H362 . 85.6 no C135 . C36 . H362 . 162.5 no C136 . C36 . H362 . 28.8 no H361 . C36 . H362 . 109.5 no C34 . C36 . H363 . 109.5 no C134 . C36 . H363 . 123.8 no C135 . C36 . H363 . 82.7 no C136 . C36 . H363 . 133.6 no H361 . C36 . H363 . 109.5 no C34 . C36 . H1352 . 92.6 no C134 . C36 . H1352 . 113.8 no C135 . C36 . H1352 . 56.2 no C136 . C36 . H1352 . 155.5 no H361 . C36 . H1352 . 97.4 no H362 . C36 . H363 . 109.5 no H362 . C36 . H1352 . 135.9 no H363 . C36 . H1352 . 26.7 no C34 . C37 . C134 . 24.1(4) yes C34 . C37 . H371 . 109.4 no C134 . C37 . H371 . 116.8 no C34 . C37 . H372 . 109.5 no C134 . C37 . H372 . 85.6 no H371 . C37 . H372 . 109.5 no C34 . C37 . H373 . 109.5 no C134 . C37 . H373 . 122.6 no H371 . C37 . H373 . 109.4 no H372 . C37 . H373 . 109.5 no C34 . C37 . H1371 . 123.9 no C134 . C37 . H1371 . 130.4 no H371 . C37 . H1371 . 14.5 no H372 . C37 . H1371 . 103.0 no H373 . C37 . H1371 . 100.6 no C34 . C37 . H1372 . 123.4 no C134 . C37 . H1372 . 118.6 no H371 . C37 . H1372 . 124.3 no H372 . C37 . H1372 . 70.1 no H373 . C37 . H1372 . 39.4 no H1371 . C37 . H1372 . 110.1 no C26 . C134 . C36 . 113.5(6) yes C26 . C134 . C37 . 118.0(8) yes C36 . C134 . C37 . 127.8(8) yes C26 . C134 . C135 . 106.3(5) yes C36 . C134 . C135 . 40.7(5) yes C37 . C134 . C135 . 112.9(8) yes C26 . C134 . C136 . 115.1(4) yes C36 . C134 . C136 . 68.5(6) yes C37 . C134 . C136 . 96.6(8) yes C135 . C134 . C136 . 107.6(6) yes C26 . C134 . C137 . 109.5(5) yes C36 . C134 . C137 . 133.3(6) yes C37 . C134 . C137 . 12.2(10) yes C135 . C134 . C137 . 109.6(6) yes C136 . C134 . C137 . 108.6(6) yes C134 . C135 . C35 . 87.5(5) yes C134 . C135 . C34 . 23.0(4) yes C35 . C135 . C34 . 65.0(6) yes C134 . C135 . C36 . 62.2(7) yes C35 . C135 . C36 . 149.4(9) yes C34 . C135 . C36 . 84.4(8) yes C134 . C135 . H361 . 93.3 no C35 . C135 . H361 . 142.5 no C34 . C135 . H361 . 113.9 no C36 . C135 . H361 . 51.1 no C134 . C135 . H1351 . 109.5 no C35 . C135 . H1351 . 111.3 no C34 . C135 . H1351 . 120.7 no C36 . C135 . H1351 . 84.7 no H361 . C135 . H1351 . 34.0 no C134 . C135 . H1352 . 109.5 no C35 . C135 . H1352 . 126.7 no C34 . C135 . H1352 . 118.0 no C36 . C135 . H1352 . 65.8 no H361 . C135 . H1352 . 88.2 no C134 . C135 . H1353 . 109.5 no C35 . C135 . H1353 . 23.4 no C34 . C135 . H1353 . 86.5 no C36 . C135 . H1353 . 165.7 no H361 . C135 . H1353 . 143.3 no H1351 . C135 . H1352 . 109.5 no H1351 . C135 . H1353 . 109.5 no H1352 . C135 . H1353 . 109.5 no C134 . C136 . C36 . 51.3(4) yes C134 . C136 . H362 . 79.9 no C36 . C136 . H362 . 32.0 no C134 . C136 . H1361 . 109.5 no C36 . C136 . H1361 . 89.8 no H362 . C136 . H1361 . 92.7 no C134 . C136 . H1362 . 109.5 no C36 . C136 . H1362 . 157.6 no H362 . C136 . H1362 . 150.2 no H1361 . C136 . H1362 . 109.5 no C134 . C136 . H1363 . 109.5 no C36 . C136 . H1363 . 72.8 no H362 . C136 . H1363 . 42.3 no H1361 . C136 . H1363 . 109.5 no H1362 . C136 . H1363 . 109.5 no C134 . C137 . C34 . 23.2(3) yes C134 . C137 . H371 . 100.1 no C34 . C137 . H371 . 102.1 no C134 . C137 . H372 . 69.8 no C34 . C137 . H372 . 93.0 no H371 . C137 . H372 . 86.8 no C134 . C137 . H373 . 131.0 no C34 . C137 . H373 . 126.2 no H371 . C137 . H373 . 128.7 no H372 . C137 . H373 . 104.9 no C134 . C137 . H1371 . 109.5 no C34 . C137 . H1371 . 114.5 no H371 . C137 . H1371 . 13.4 no H372 . C137 . H1371 . 81.6 no H373 . C137 . H1371 . 118.0 no C134 . C137 . H1372 . 109.5 no C34 . C137 . H1372 . 124.0 no H371 . C137 . H1372 . 122.4 no H372 . C137 . H1372 . 60.8 no H373 . C137 . H1372 . 44.2 no C134 . C137 . H1373 . 109.5 no C34 . C137 . H1373 . 86.9 no H371 . C137 . H1373 . 105.1 no H372 . C137 . H1373 . 167.8 no H373 . C137 . H1373 . 65.9 no H1371 . C137 . H1372 . 109.5 no H1371 . C137 . H1373 . 109.5 no H1372 . C137 . H1373 . 109.5 no N2 . C38 . C39 . 109.3(2) yes N2 . C38 . H381 . 125.4 no C39 . C38 . H381 . 125.4 no N3 . C39 . C38 . 106.4(2) yes N3 . C39 . H391 . 126.8 no C38 . C39 . H391 . 126.8 no N3 . C40 . N2 . 111.1(2) yes N3 . C40 . H401 . 124.5 no N2 . C40 . H401 . 124.5 no N3 . C41 . H411 . 109.5 no N3 . C41 . H412 . 109.5 no H411 . C41 . H412 . 109.5 no N3 . C41 . H413 . 109.5 no H411 . C41 . H413 . 109.5 no H412 . C41 . H413 . 109.5 no #===END ###################################### ## denoted [FeL2(1-Meim)] in text ## ###################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 669891' _audit_creation_date 07-11-09 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.3625(2) _cell_length_b 13.6632(2) _cell_length_c 26.7778(4) _cell_angle_alpha 90 _cell_angle_beta 100.8828(5) _cell_angle_gamma 90 _cell_volume 5160.31(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C50 H77 Fe1 N3 O4.50' _chemical_formula_moiety 'C50 H77 Fe1 N3 O4.50' _chemical_compound_source ? _chemical_formula_weight 848.03 _cell_measurement_reflns_used 39433 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 250 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 250 _diffrn_reflns_number 39433 _reflns_number_total 12027 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 12027 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11862 _diffrn_reflns_theta_min 5.125 _diffrn_reflns_theta_max 27.511 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.43 _refine_diff_density_max 0.66 _refine_ls_number_reflns 6508 _refine_ls_number_restraints 39 _refine_ls_number_parameters 505 #_refine_ls_R_factor_ref 0.0656 _refine_ls_wR_factor_ref 0.0657 _refine_ls_goodness_of_fit_ref 1.1413 #_reflns_number_all 11548 _refine_ls_R_factor_all 0.1315 _refine_ls_wR_factor_all 0.0744 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6508 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_gt 0.0657 _refine_ls_shift/su_max 0.017004 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.67 -0.970 2.45 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.27437(3) 0.18853(3) 0.667902(17) 0.0323 1.0000 Uani . . . . . . O1 O 0.30129(17) 0.20365(18) 0.74043(8) 0.0443 1.0000 Uani . . . . . . O2 O 0.17890(16) 0.25591(17) 0.62439(9) 0.0407 1.0000 Uani . . . . . . O3 O 0.32726(16) 0.08624(17) 0.63657(9) 0.0407 1.0000 Uani . . . . . . N1 N 0.17036(17) 0.08428(19) 0.68884(9) 0.0293 1.0000 Uani . . . . . . C1 C 0.2671(2) 0.1353(3) 0.76775(12) 0.0352 1.0000 Uani . . . . . . C2 C 0.2949(3) 0.1283(3) 0.82066(14) 0.0458 1.0000 Uani . . . . . . C3 C 0.2589(3) 0.0541(3) 0.84695(13) 0.0481 1.0000 Uani . . . . . . C4 C 0.1948(3) -0.0150(3) 0.82257(14) 0.0445 1.0000 Uani . . . . . . C5 C 0.1658(2) -0.0052(3) 0.77001(13) 0.0369 1.0000 Uani . . . . . . C6 C 0.2011(2) 0.0669(2) 0.74338(12) 0.0323 1.0000 Uani . . . . . . C7 C 0.0941(2) 0.2226(2) 0.59998(12) 0.0351 1.0000 Uani . . . . . . C8 C 0.0581(3) 0.2492(3) 0.54871(13) 0.0417 1.0000 Uani . . . . . . C9 C -0.0281(3) 0.2086(3) 0.52596(14) 0.0450 1.0000 Uani . . . . . . C10 C -0.0813(2) 0.1442(3) 0.55003(14) 0.0426 1.0000 Uani . . . . . . C11 C -0.0447(2) 0.1223(3) 0.60046(13) 0.0371 1.0000 Uani . . . . . . C12 C 0.0408(2) 0.1616(2) 0.62542(12) 0.0339 1.0000 Uani . . . . . . C13 C 0.0770(2) 0.1381(2) 0.68037(12) 0.0344 1.0000 Uani . . . . . . C14 C 0.3305(2) -0.0111(3) 0.64340(12) 0.0358 1.0000 Uani . . . . . . C15 C 0.4105(2) -0.0660(3) 0.63631(14) 0.0431 1.0000 Uani . . . . . . C16 C 0.4074(3) -0.1666(3) 0.64280(15) 0.0507 1.0000 Uani . . . . . . C17 C 0.3308(3) -0.2165(3) 0.65560(16) 0.0531 1.0000 Uani D . . . . . C18 C 0.2539(3) -0.1601(3) 0.66254(14) 0.0441 1.0000 Uani . . . . . . C19 C 0.2521(2) -0.0598(2) 0.65608(12) 0.0334 1.0000 Uani . . . . . . C20 C 0.1616(2) -0.0047(3) 0.65670(12) 0.0338 1.0000 Uani . . . . . . C21 C 0.1549(3) -0.0988(3) 0.85085(16) 0.0606 1.0000 Uani . . . . . . C22 C 0.1769(6) -0.1948(4) 0.8294(3) 0.1190 1.0000 Uani . . . . . . C23 C 0.1924(6) -0.0954(5) 0.9078(2) 0.1071 1.0000 Uani . . . . . . C24 C 0.0481(5) -0.0881(5) 0.8438(3) 0.1111 1.0000 Uani . . . . . . C25 C 0.1129(3) 0.3180(3) 0.51939(15) 0.0596 1.0000 Uani . . . . . . C26 C 0.1362(5) 0.4139(4) 0.5484(2) 0.0874 1.0000 Uani . . . . . . C27 C 0.0563(5) 0.3421(5) 0.4664(2) 0.1005 1.0000 Uani . . . . . . C28 C 0.2041(4) 0.2683(4) 0.51177(18) 0.0780 1.0000 Uani . . . . . . C29 C -0.1720(3) 0.0974(3) 0.52031(15) 0.0543 1.0000 Uani . . . . . . C30 C -0.1454(4) 0.0255(5) 0.4823(3) 0.0992 1.0000 Uani . . . . . . C31 C -0.2267(4) 0.0446(8) 0.5545(2) 0.1378 1.0000 Uani . . . . . . C32 C -0.2354(5) 0.1744(5) 0.4899(3) 0.1411 1.0000 Uani . . . . . . C33 C 0.4969(3) -0.0155(3) 0.62112(17) 0.0567 1.0000 Uani . . . . . . C34 C 0.5405(3) 0.0577(4) 0.6621(2) 0.0779 1.0000 Uani . . . . . . C35 C 0.4667(3) 0.0369(4) 0.56972(19) 0.0743 1.0000 Uani . . . . . . C36 C 0.5754(4) -0.0903(4) 0.6156(3) 0.0929 1.0000 Uani . . . . . . C37 C 0.3308(3) -0.3276(3) 0.66160(19) 0.0795 1.0000 Uani D . . . . . C38 C 0.2302(7) -0.3700(9) 0.6598(5) 0.1150(19) 0.537(6) Uiso D . P 2 1 . C39 C 0.3589(9) -0.3748(9) 0.6132(4) 0.1150(19) 0.537(6) Uiso D . P 2 1 . C40 C 0.3996(8) -0.3647(9) 0.7071(4) 0.1150(19) 0.537(6) Uiso D . P 2 1 . C138 C 0.4308(7) -0.3708(10) 0.6640(6) 0.1150(19) 0.463(6) Uiso D . P 2 2 . C139 C 0.2544(9) -0.3766(9) 0.6244(5) 0.1150(19) 0.463(6) Uiso D . P 2 2 . C140 C 0.3138(10) -0.3460(10) 0.7170(4) 0.1150(19) 0.463(6) Uiso D . P 2 2 . N2 N 0.3828(2) 0.2903(2) 0.66526(11) 0.0424 1.0000 Uani . . . . . . N3 N 0.5109(2) 0.3768(2) 0.69201(12) 0.0435 1.0000 Uani . . . . . . C41 C 0.4409(2) 0.3242(3) 0.70501(13) 0.0411 1.0000 Uani . . . . . . C42 C 0.4966(3) 0.3769(4) 0.64038(16) 0.0614 1.0000 Uani . . . . . . C43 C 0.4182(3) 0.3238(4) 0.62411(14) 0.0669 1.0000 Uani . . . . . . C44 C 0.5877(3) 0.4256(4) 0.72623(18) 0.0709 1.0000 Uani . . . . . . O4 O 0.0718(6) 0.3931(7) 0.8146(3) 0.119(2) 0.610(7) Uiso D . P 1 1 . C45 C 0.0658(10) 0.3157(10) 0.8487(4) 0.156(3) 0.610(7) Uiso D . P 1 1 . C46 C 0.0247(11) 0.2275(10) 0.8209(6) 0.127(2) 0.610(7) Uiso D . P 1 1 . C47 C 0.1553(10) 0.3897(10) 0.7951(7) 0.156(3) 0.610(7) Uiso D . P 1 1 . C48 C 0.1675(9) 0.4904(10) 0.7760(5) 0.127(2) 0.610(7) Uiso D . P 1 1 . O104 O 0.0769(8) 0.3395(10) 0.7883(5) 0.119(2) 0.390(7) Uiso D . P 1 2 . C145 C 0.0732(14) 0.2737(17) 0.8279(7) 0.156(3) 0.390(7) Uiso D . P 1 2 . C146 C -0.0097(15) 0.2057(15) 0.8145(9) 0.127(2) 0.390(7) Uiso D . P 1 2 . C147 C 0.1570(16) 0.4009(17) 0.7995(7) 0.156(3) 0.390(7) Uiso D . P 1 2 . C148 C 0.1876(14) 0.4321(16) 0.7512(8) 0.127(2) 0.390(7) Uiso D . P 1 2 . O5 O 0.4820(19) 0.5201(14) 0.4824(8) 0.252(10) 0.5000 Uiso D . . 3 1 . C49 C 0.5292(18) 0.4298(16) 0.4975(14) 0.226(9) 0.5000 Uiso D . . 3 1 . C50 C 0.467(2) 0.3442(16) 0.4762(15) 0.250(10) 0.5000 Uiso D . . 3 1 . C51 C 0.5293(18) 0.6009(15) 0.5091(13) 0.226(9) 0.5000 Uiso D . . 3 1 . C52 C 0.470(2) 0.6927(16) 0.4980(12) 0.250(10) 0.5000 Uiso D . . 3 1 . H21 H 0.3407 0.1768 0.8395 0.0542 1.0000 Uiso . . . . . . H31 H 0.2798 0.0501 0.8847 0.0571 1.0000 Uiso . . . . . . H51 H 0.1181 -0.0521 0.7514 0.0445 1.0000 Uiso . . . . . . H91 H -0.0540 0.2266 0.4898 0.0519 1.0000 Uiso . . . . . . H111 H -0.0806 0.0771 0.6193 0.0437 1.0000 Uiso . . . . . . H131 H 0.0856 0.2007 0.7001 0.0416 1.0000 Uiso . . . . . . H132 H 0.0291 0.0964 0.6930 0.0416 1.0000 Uiso . . . . . . H161 H 0.4639 -0.2058 0.6380 0.0608 1.0000 Uiso . . . . . . H181 H 0.1981 -0.1932 0.6725 0.0530 1.0000 Uiso . . . . . . H201 H 0.1166 -0.0503 0.6692 0.0401 1.0000 Uiso . . . . . . H202 H 0.1345 0.0153 0.6210 0.0401 1.0000 Uiso . . . . . . H221 H 0.1508 -0.2488 0.8479 0.1526 1.0000 Uiso . . . . . . H222 H 0.2471 -0.2025 0.8335 0.1526 1.0000 Uiso . . . . . . H223 H 0.1474 -0.1976 0.7925 0.1526 1.0000 Uiso . . . . . . H231 H 0.1649 -0.1508 0.9247 0.1292 1.0000 Uiso . . . . . . H232 H 0.1740 -0.0319 0.9218 0.1292 1.0000 Uiso . . . . . . H233 H 0.2631 -0.1012 0.9146 0.1292 1.0000 Uiso . . . . . . H241 H 0.0218 -0.1423 0.8620 0.1377 1.0000 Uiso . . . . . . H242 H 0.0323 -0.0237 0.8578 0.1377 1.0000 Uiso . . . . . . H243 H 0.0197 -0.0913 0.8067 0.1377 1.0000 Uiso . . . . . . H261 H 0.1718 0.4579 0.5288 0.1029 1.0000 Uiso . . . . . . H262 H 0.1759 0.4000 0.5825 0.1029 1.0000 Uiso . . . . . . H263 H 0.0760 0.4467 0.5528 0.1029 1.0000 Uiso . . . . . . H271 H 0.0942 0.3870 0.4485 0.1161 1.0000 Uiso . . . . . . H272 H -0.0045 0.3748 0.4698 0.1161 1.0000 Uiso . . . . . . H273 H 0.0422 0.2804 0.4464 0.1161 1.0000 Uiso . . . . . . H281 H 0.2398 0.3132 0.4926 0.0953 1.0000 Uiso . . . . . . H282 H 0.2440 0.2528 0.5456 0.0953 1.0000 Uiso . . . . . . H283 H 0.1884 0.2065 0.4920 0.0953 1.0000 Uiso . . . . . . H301 H -0.2041 -0.0055 0.4627 0.1175 1.0000 Uiso . . . . . . H302 H -0.1031 -0.0263 0.5008 0.1175 1.0000 Uiso . . . . . . H303 H -0.1114 0.0607 0.4584 0.1175 1.0000 Uiso . . . . . . H311 H -0.2851 0.0152 0.5337 0.1635 1.0000 Uiso . . . . . . H312 H -0.2450 0.0918 0.5795 0.1635 1.0000 Uiso . . . . . . H313 H -0.1864 -0.0084 0.5732 0.1635 1.0000 Uiso . . . . . . H321 H -0.2941 0.1424 0.4708 0.1519 1.0000 Uiso . . . . . . H322 H -0.2531 0.2246 0.5136 0.1519 1.0000 Uiso . . . . . . H323 H -0.2006 0.2066 0.4653 0.1519 1.0000 Uiso . . . . . . H341 H 0.5965 0.0900 0.6518 0.0929 1.0000 Uiso . . . . . . H342 H 0.5613 0.0225 0.6951 0.0929 1.0000 Uiso . . . . . . H343 H 0.4923 0.1083 0.6662 0.0929 1.0000 Uiso . . . . . . H351 H 0.5231 0.0696 0.5601 0.0924 1.0000 Uiso . . . . . . H352 H 0.4174 0.0872 0.5727 0.0924 1.0000 Uiso . . . . . . H353 H 0.4401 -0.0120 0.5431 0.0924 1.0000 Uiso . . . . . . H361 H 0.6304 -0.0553 0.6058 0.1160 1.0000 Uiso . . . . . . H362 H 0.5968 -0.1247 0.6488 0.1160 1.0000 Uiso . . . . . . H363 H 0.5497 -0.1393 0.5888 0.1160 1.0000 Uiso . . . . . . H381 H 0.2343 -0.4427 0.6639 0.1380 0.5370 Uiso . . . 2 1 . H382 H 0.2023 -0.3411 0.6880 0.1380 0.5370 Uiso . . . 2 1 . H383 H 0.1891 -0.3536 0.6264 0.1380 0.5370 Uiso . . . 2 1 . H391 H 0.3592 -0.4477 0.6165 0.1380 0.5370 Uiso . . . 2 1 . H392 H 0.4235 -0.3517 0.6098 0.1380 0.5370 Uiso . . . 2 1 . H393 H 0.3119 -0.3551 0.5823 0.1380 0.5370 Uiso . . . 2 1 . H401 H 0.3956 -0.4377 0.7085 0.1380 0.5370 Uiso . . . 2 1 . H402 H 0.3835 -0.3361 0.7388 0.1380 0.5370 Uiso . . . 2 1 . H403 H 0.4655 -0.3450 0.7043 0.1380 0.5370 Uiso . . . 2 1 . H1381 H 0.4283 -0.4435 0.6679 0.1380 0.4630 Uiso . . . 2 2 . H1382 H 0.4753 -0.3423 0.6936 0.1380 0.4630 Uiso . . . 2 2 . H1383 H 0.4535 -0.3546 0.6318 0.1380 0.4630 Uiso . . . 2 2 . H1391 H 0.2577 -0.4490 0.6301 0.1380 0.4630 Uiso . . . 2 2 . H1392 H 0.1911 -0.3519 0.6293 0.1380 0.4630 Uiso . . . 2 2 . H1393 H 0.2630 -0.3618 0.5890 0.1380 0.4630 Uiso . . . 2 2 . H1401 H 0.3130 -0.4180 0.7235 0.1380 0.4630 Uiso . . . 2 2 . H1402 H 0.3660 -0.3148 0.7419 0.1380 0.4630 Uiso . . . 2 2 . H1403 H 0.2517 -0.3168 0.7207 0.1380 0.4630 Uiso . . . 2 2 . H411 H 0.4337 0.3122 0.7409 0.0492 1.0000 Uiso . . . . . . H421 H 0.5367 0.4101 0.6187 0.0739 1.0000 Uiso . . . . . . H431 H 0.3899 0.3105 0.5877 0.0793 1.0000 Uiso . . . . . . H441 H 0.6298 0.4594 0.7059 0.0833 1.0000 Uiso . . . . . . H442 H 0.5607 0.4747 0.7472 0.0833 1.0000 Uiso . . . . . . H443 H 0.6254 0.3760 0.7491 0.0833 1.0000 Uiso . . . . . . H451 H 0.0247 0.3361 0.8731 0.1874 0.6100 Uiso . . . 1 1 . H452 H 0.1308 0.2999 0.8678 0.1874 0.6100 Uiso . . . 1 1 . H461 H 0.0211 0.1735 0.8456 0.1520 0.6100 Uiso . . . 1 1 . H462 H -0.0404 0.2429 0.8017 0.1520 0.6100 Uiso . . . 1 1 . H463 H 0.0657 0.2067 0.7965 0.1520 0.6100 Uiso . . . 1 1 . H471 H 0.2102 0.3717 0.8224 0.1874 0.6100 Uiso . . . 1 1 . H472 H 0.1494 0.3411 0.7668 0.1874 0.6100 Uiso . . . 1 1 . H481 H 0.2266 0.4932 0.7614 0.1520 0.6100 Uiso . . . 1 1 . H482 H 0.1725 0.5380 0.8048 0.1520 0.6100 Uiso . . . 1 1 . H483 H 0.1117 0.5075 0.7491 0.1520 0.6100 Uiso . . . 1 1 . H1451 H 0.0670 0.3113 0.8592 0.1874 0.3900 Uiso . . . 1 2 . H1452 H 0.1331 0.2345 0.8347 0.1874 0.3900 Uiso . . . 1 2 . H1461 H -0.0108 0.1596 0.8433 0.1520 0.3900 Uiso . . . 1 2 . H1462 H -0.0698 0.2446 0.8078 0.1520 0.3900 Uiso . . . 1 2 . H1463 H -0.0037 0.1677 0.7833 0.1520 0.3900 Uiso . . . 1 2 . H1471 H 0.1408 0.4602 0.8180 0.1874 0.3900 Uiso . . . 1 2 . H1472 H 0.2101 0.3647 0.8214 0.1874 0.3900 Uiso . . . 1 2 . H1481 H 0.2444 0.4756 0.7596 0.1520 0.3900 Uiso . . . 1 2 . H1482 H 0.1347 0.4684 0.7293 0.1520 0.3900 Uiso . . . 1 2 . H1483 H 0.2040 0.3729 0.7327 0.1520 0.3900 Uiso . . . 1 2 . H491 H 0.5430 0.4256 0.5354 0.2711 0.5000 Uiso . . . . . . H492 H 0.5899 0.4272 0.4844 0.2711 0.5000 Uiso . . . . . . H501 H 0.5010 0.2815 0.4870 0.3003 0.5000 Uiso . . . . . . H502 H 0.4064 0.3465 0.4892 0.3003 0.5000 Uiso . . . . . . H503 H 0.4533 0.3480 0.4382 0.3003 0.5000 Uiso . . . . . . H511 H 0.5405 0.5872 0.5464 0.2711 0.5000 Uiso . . . . . . H512 H 0.5915 0.6111 0.4982 0.2711 0.5000 Uiso . . . . . . H521 H 0.5040 0.7491 0.5171 0.3003 0.5000 Uiso . . . . . . H522 H 0.4077 0.6829 0.5089 0.3003 0.5000 Uiso . . . . . . H523 H 0.4587 0.7068 0.4607 0.3003 0.5000 Uiso . . . . . . 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 0.0315(2) 0.0324(2) 0.0320(2) 0.0010(2) 0.00344(16) -0.0051(2) O1 0.0494(14) 0.0470(16) 0.0345(12) -0.0020(11) 0.0030(10) -0.0182(12) O2 0.0415(13) 0.0346(13) 0.0430(13) 0.0051(11) 0.0005(11) -0.0035(10) O3 0.0392(13) 0.0369(13) 0.0493(14) -0.0013(11) 0.0168(11) -0.0032(11) N1 0.0282(13) 0.0308(14) 0.0282(13) -0.0008(11) 0.0032(10) -0.0014(11) C1 0.0349(17) 0.0375(19) 0.0334(17) 0.0019(15) 0.0068(14) -0.0031(15) C2 0.044(2) 0.053(2) 0.0386(19) -0.0023(17) 0.0032(16) -0.0073(18) C3 0.055(2) 0.056(2) 0.0313(18) 0.0054(18) 0.0043(16) 0.001(2) C4 0.050(2) 0.045(2) 0.041(2) 0.0094(17) 0.0137(16) -0.0002(17) C5 0.0345(17) 0.0368(19) 0.0399(18) 0.0023(15) 0.0083(14) -0.0036(15) C6 0.0276(15) 0.0367(18) 0.0321(16) 0.0015(14) 0.0047(13) 0.0012(14) C7 0.0369(17) 0.0296(16) 0.0359(17) -0.0002(14) -0.0002(14) 0.0049(14) C8 0.049(2) 0.0344(19) 0.0391(19) 0.0014(15) 0.0011(16) 0.0042(16) C9 0.050(2) 0.041(2) 0.0383(18) -0.0016(16) -0.0048(16) 0.0089(17) C10 0.0356(18) 0.044(2) 0.045(2) -0.0077(17) 0.0006(15) 0.0059(16) C11 0.0313(17) 0.0401(19) 0.0379(18) -0.0051(15) 0.0017(14) 0.0062(14) C12 0.0324(16) 0.0333(17) 0.0353(17) -0.0015(14) 0.0048(13) 0.0093(13) C13 0.0293(16) 0.0387(19) 0.0360(17) -0.0017(15) 0.0084(13) 0.0042(14) C14 0.0355(17) 0.0405(19) 0.0303(16) -0.0035(15) 0.0032(13) -0.0018(15) C15 0.0335(18) 0.052(2) 0.044(2) -0.0087(18) 0.0069(15) 0.0037(16) C16 0.045(2) 0.051(2) 0.056(2) -0.0038(19) 0.0092(17) 0.0147(18) C17 0.057(2) 0.041(2) 0.061(2) 0.0086(19) 0.0106(19) 0.0164(18) C18 0.048(2) 0.0397(19) 0.045(2) 0.0039(16) 0.0092(17) 0.0026(16) C19 0.0352(17) 0.0335(17) 0.0308(17) 0.0012(14) 0.0044(13) 0.0035(14) C20 0.0297(16) 0.0379(18) 0.0326(17) -0.0038(14) 0.0030(13) -0.0020(14) C21 0.080(3) 0.056(3) 0.049(2) 0.014(2) 0.019(2) -0.009(2) C22 0.212(8) 0.056(3) 0.113(5) 0.016(3) 0.093(5) -0.007(4) C23 0.169(6) 0.095(4) 0.059(3) 0.029(3) 0.026(4) -0.028(4) C24 0.096(4) 0.113(5) 0.136(6) 0.049(4) 0.050(4) -0.020(4) C25 0.071(3) 0.054(2) 0.049(2) 0.011(2) -0.0002(19) -0.012(2) C26 0.122(5) 0.050(3) 0.085(4) 0.015(3) 0.007(3) -0.019(3) C27 0.125(5) 0.106(5) 0.060(3) 0.045(3) -0.011(3) -0.034(4) C28 0.089(4) 0.091(4) 0.059(3) 0.008(3) 0.025(3) -0.025(3) C29 0.043(2) 0.067(3) 0.047(2) -0.009(2) -0.0059(17) -0.001(2) C30 0.086(4) 0.097(4) 0.110(5) -0.061(4) 0.009(3) -0.024(3) C31 0.071(4) 0.270(10) 0.067(3) -0.021(5) 0.002(3) -0.089(5) C32 0.090(4) 0.101(5) 0.189(8) 0.001(5) -0.085(5) 0.008(4) C33 0.037(2) 0.068(3) 0.067(3) -0.011(2) 0.0184(19) -0.0009(19) C34 0.042(2) 0.101(4) 0.090(4) -0.024(3) 0.009(2) -0.017(3) C35 0.065(3) 0.096(4) 0.070(3) -0.001(3) 0.033(2) -0.017(3) C36 0.053(3) 0.094(4) 0.143(5) -0.019(4) 0.047(3) 0.003(3) C37 0.079(3) 0.050(3) 0.116(4) 0.020(3) 0.036(3) 0.027(2) N2 0.0418(16) 0.0449(18) 0.0391(15) -0.0007(13) 0.0046(13) -0.0136(14) N3 0.0378(16) 0.0458(18) 0.0457(17) 0.0004(14) 0.0051(13) -0.0114(14) C41 0.0407(18) 0.043(2) 0.0391(18) 0.0035(17) 0.0066(14) -0.0098(17) C42 0.065(3) 0.074(3) 0.045(2) 0.005(2) 0.012(2) -0.030(2) C43 0.072(3) 0.092(4) 0.0340(19) 0.003(2) 0.0038(18) -0.041(3) C44 0.059(3) 0.091(4) 0.058(3) -0.001(3) 0.000(2) -0.036(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.8955(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 1.918(2) yes Fe1 . O2 . 1.866(2) yes Fe1 . O3 . 1.864(2) yes Fe1 . N1 . 2.212(3) yes Fe1 . N2 . 2.099(3) yes O1 . C1 . 1.336(4) yes O2 . C7 . 1.347(4) yes O3 . C14 . 1.343(4) yes N1 . C6 . 1.463(4) yes N1 . C13 . 1.509(4) yes N1 . C20 . 1.481(4) yes C1 . C2 . 1.401(5) yes C1 . C6 . 1.401(5) yes C2 . C3 . 1.389(5) yes C2 . H21 . 1.000 no C3 . C4 . 1.392(5) yes C3 . H31 . 1.000 no C4 . C5 . 1.397(5) yes C4 . C21 . 1.542(5) yes C5 . C6 . 1.369(5) yes C5 . H51 . 1.000 no C7 . C8 . 1.420(5) yes C7 . C12 . 1.394(5) yes C8 . C9 . 1.389(5) yes C8 . C25 . 1.533(5) yes C9 . C10 . 1.400(5) yes C9 . H91 . 1.000 no C10 . C11 . 1.386(5) yes C10 . C29 . 1.532(5) yes C11 . C12 . 1.390(5) yes C11 . H111 . 1.000 no C12 . C13 . 1.500(4) yes C13 . H132 . 1.000 no C13 . H131 . 1.000 no C14 . C15 . 1.415(5) yes C14 . C19 . 1.403(5) yes C15 . C16 . 1.387(6) yes C15 . C33 . 1.541(5) yes C16 . C17 . 1.391(6) yes C16 . H161 . 1.000 no C17 . C18 . 1.387(5) yes C17 . C37 . 1.526(6) yes C18 . C19 . 1.382(5) yes C18 . H181 . 1.000 no C19 . C20 . 1.506(4) yes C20 . H202 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.489(8) yes C21 . C23 . 1.520(7) yes C21 . C24 . 1.517(8) yes C22 . H222 . 1.000 no C22 . H223 . 1.000 no C22 . H221 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C23 . H231 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.529(7) yes C25 . C27 . 1.532(6) yes C25 . C28 . 1.523(7) yes C26 . H262 . 1.000 no C26 . H263 . 1.000 no C26 . H261 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C27 . H271 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C28 . H281 . 1.000 no C29 . C30 . 1.514(7) yes C29 . C31 . 1.500(8) yes C29 . C32 . 1.523(7) yes C30 . H302 . 1.000 no C30 . H303 . 1.000 no C30 . H301 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C31 . H311 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C32 . H321 . 1.000 no C33 . C34 . 1.528(6) yes C33 . C35 . 1.539(7) yes C33 . C36 . 1.550(6) yes C34 . H342 . 1.000 no C34 . H343 . 1.000 no C34 . H341 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C35 . H351 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C36 . H361 . 1.000 no C37 . C39 . 1.568(8) yes C37 . C40 . 1.505(8) yes C37 . C139 . 1.495(9) yes C37 . C140 . 1.567(9) yes C37 . C38 . 1.550(8) yes C37 . C138 . 1.543(9) yes C39 . C139 . 1.587(16) yes C40 . C140 . 1.332(16) yes N2 . C41 . 1.306(4) yes N2 . C43 . 1.376(5) yes N3 . C41 . 1.334(4) yes N3 . C42 . 1.359(5) yes N3 . C44 . 1.456(5) yes C41 . H411 . 1.000 no C42 . C43 . 1.341(6) yes C42 . H421 . 1.000 no C43 . H431 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C44 . H441 . 1.000 no O4 . C45 . 1.411(9) yes O4 . C47 . 1.396(9) yes O4 . O104 . 1.029(13) yes O4 . C145 . 1.67(2) yes O4 . C147 . 1.36(2) yes C45 . C46 . 1.479(9) yes C45 . O104 . 1.686(17) yes C45 . C145 . 0.82(3) yes C45 . H452 . 1.000 no C45 . C46 . 1.479(9) yes C45 . O104 . 1.686(17) yes C45 . C145 . 0.82(3) yes C45 . H451 . 1.000 no C46 . C145 . 0.932(19) yes C46 . H462 . 1.000 no C46 . H463 . 1.000 no C46 . H1463 . 1.300 no C46 . C145 . 0.932(19) yes C46 . H461 . 1.000 no C46 . H1461 . 1.266 no C47 . C48 . 1.490(9) yes C47 . O104 . 1.30(2) yes C47 . C148 . 1.46(2) yes C47 . H472 . 1.000 no C47 . H1472 . 1.011 no C47 . C48 . 1.490(9) yes C47 . O104 . 1.30(2) yes C47 . C148 . 1.46(2) yes C47 . H471 . 1.000 no C47 . H1471 . 1.182 no C48 . C147 . 1.40(3) yes C48 . C148 . 1.11(2) yes C48 . H482 . 1.000 no C48 . H483 . 1.000 no C48 . H1482 . 1.287 no C48 . C147 . 1.40(3) yes C48 . C148 . 1.11(2) yes C48 . H481 . 1.000 no C48 . H1481 . 1.279 no O104 . C145 . 1.400(9) yes O104 . C147 . 1.411(10) yes O104 . H472 . 1.282 no C145 . C146 . 1.500(10) yes C145 . H452 . 1.273 no C145 . H463 . 1.236 no C145 . H1452 . 1.000 no C145 . C146 . 1.500(10) yes C145 . H1451 . 1.000 no C146 . H462 . 0.716 no C146 . H463 . 1.266 no C146 . H1462 . 1.000 no C146 . H1463 . 1.000 no C146 . H461 . 0.971 no C146 . H1461 . 1.000 no C147 . C148 . 1.503(10) yes C147 . H472 . 1.189 no C147 . H1472 . 1.000 no C147 . C148 . 1.503(10) yes C147 . H471 . 0.971 no C147 . H1471 . 1.000 no C148 . H1482 . 1.000 no C148 . H1483 . 1.000 no C148 . H481 . 1.014 no C148 . H1481 . 1.000 no O5 . C51 2_666 1.68(4) yes O5 . H491 2_666 0.918 no O5 . O5 2_666 1.13(4) yes O5 . C49 2_666 0.90(4) yes O5 . C49 . 1.429(10) yes O5 . C51 . 1.417(10) yes C49 . C52 2_666 1.68(4) yes C49 . C51 2_666 0.93(4) yes C49 . C50 . 1.515(10) yes C49 . H492 . 1.000 no C49 . C52 2_666 1.68(4) yes C49 . C51 2_666 0.93(4) yes C49 . C50 . 1.515(10) yes C49 . H491 . 1.000 no C50 . C52 2_666 1.15(4) yes C50 . C51 2_666 0.84(4) yes C50 . H502 . 1.000 no C50 . H503 . 1.000 no C50 . H511 2_666 1.110 no C50 . C52 2_666 1.15(4) yes C50 . C51 2_666 0.84(4) yes C50 . H501 . 1.000 no C51 . H502 2_666 1.164 no C51 . C52 . 1.515(10) yes C51 . H512 . 1.001 no C51 . C52 . 1.515(10) yes C51 . H511 . 0.999 no C52 . H522 . 1.000 no C52 . H523 . 1.000 no C52 . H501 2_666 0.630 no C52 . H521 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 124.26(11) yes O1 . Fe1 . O3 . 121.00(11) yes O2 . Fe1 . O3 . 113.74(11) yes O1 . Fe1 . N1 . 80.18(9) yes O2 . Fe1 . N1 . 91.38(10) yes O3 . Fe1 . N1 . 89.05(10) yes O1 . Fe1 . N2 . 87.35(10) yes O2 . Fe1 . N2 . 96.58(11) yes O3 . Fe1 . N2 . 96.52(11) yes N1 . Fe1 . N2 . 167.48(10) yes Fe1 . O1 . C1 . 117.0(2) yes Fe1 . O2 . C7 . 128.8(2) yes Fe1 . O3 . C14 . 133.5(2) yes Fe1 . N1 . C6 . 105.44(18) yes Fe1 . N1 . C13 . 105.77(19) yes C6 . N1 . C13 . 108.7(2) yes Fe1 . N1 . C20 . 111.66(18) yes C6 . N1 . C20 . 115.1(2) yes C13 . N1 . C20 . 109.7(2) yes O1 . C1 . C2 . 122.5(3) yes O1 . C1 . C6 . 119.8(3) yes C2 . C1 . C6 . 117.7(3) yes C1 . C2 . C3 . 120.0(3) yes C1 . C2 . H21 . 120.0 no C3 . C2 . H21 . 120.0 no C2 . C3 . C4 . 122.3(3) yes C2 . C3 . H31 . 118.9 no C4 . C3 . H31 . 118.9 no C3 . C4 . C5 . 116.9(3) yes C3 . C4 . C21 . 123.2(3) yes C5 . C4 . C21 . 119.9(3) yes C4 . C5 . C6 . 121.6(3) yes C4 . C5 . H51 . 119.2 no C6 . C5 . H51 . 119.2 no N1 . C6 . C1 . 114.0(3) yes N1 . C6 . C5 . 124.4(3) yes C1 . C6 . C5 . 121.5(3) yes O2 . C7 . C8 . 120.9(3) yes O2 . C7 . C12 . 119.6(3) yes C8 . C7 . C12 . 119.5(3) yes C7 . C8 . C9 . 117.0(3) yes C7 . C8 . C25 . 121.6(3) yes C9 . C8 . C25 . 121.4(3) yes C8 . C9 . C10 . 124.7(3) yes C8 . C9 . H91 . 117.7 no C10 . C9 . H91 . 117.7 no C9 . C10 . C11 . 116.4(3) yes C9 . C10 . C29 . 120.5(3) yes C11 . C10 . C29 . 123.0(4) yes C10 . C11 . C12 . 121.5(3) yes C10 . C11 . H111 . 119.2 no C12 . C11 . H111 . 119.2 no C7 . C12 . C11 . 120.9(3) yes C7 . C12 . C13 . 119.1(3) yes C11 . C12 . C13 . 120.0(3) yes N1 . C13 . C12 . 112.7(2) yes N1 . C13 . H132 . 108.7 no C12 . C13 . H132 . 108.7 no N1 . C13 . C12 . 112.7(2) yes N1 . C13 . H131 . 108.7 no C12 . C13 . H131 . 108.7 no O3 . C14 . C15 . 121.0(3) yes O3 . C14 . C19 . 119.6(3) yes C15 . C14 . C19 . 119.4(3) yes C14 . C15 . C16 . 117.5(3) yes C14 . C15 . C33 . 120.8(3) yes C16 . C15 . C33 . 121.6(3) yes C15 . C16 . C17 . 124.2(3) yes C15 . C16 . H161 . 117.9 no C17 . C16 . H161 . 117.9 no C16 . C17 . C18 . 116.6(4) yes C16 . C17 . C37 . 121.9(3) yes C18 . C17 . C37 . 121.5(4) yes C17 . C18 . C19 . 122.1(4) yes C17 . C18 . H181 . 119.0 no C19 . C18 . H181 . 119.0 no C14 . C19 . C18 . 120.2(3) yes C14 . C19 . C20 . 120.0(3) yes C18 . C19 . C20 . 119.4(3) yes C19 . C20 . N1 . 115.9(3) yes C19 . C20 . H202 . 107.8 no N1 . C20 . H202 . 107.8 no C19 . C20 . N1 . 115.9(3) yes C19 . C20 . H201 . 107.8 no N1 . C20 . H201 . 107.8 no C4 . C21 . C22 . 109.9(4) yes C4 . C21 . C23 . 112.1(4) yes C22 . C21 . C23 . 110.7(5) yes C4 . C21 . C24 . 109.2(4) yes C22 . C21 . C24 . 108.6(5) yes C23 . C21 . C24 . 106.3(5) yes C21 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C21 . C22 . H221 . 109.5 no C21 . C23 . H232 . 109.5 no C21 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C21 . C23 . H231 . 109.5 no C21 . C24 . H242 . 109.5 no C21 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C21 . C24 . H241 . 109.5 no C8 . C25 . C26 . 110.5(4) yes C8 . C25 . C27 . 111.9(4) yes C26 . C25 . C27 . 108.2(4) yes C8 . C25 . C28 . 109.5(4) yes C26 . C25 . C28 . 109.8(4) yes C27 . C25 . C28 . 106.9(4) yes C25 . C26 . H262 . 109.5 no C25 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C25 . C26 . H261 . 109.5 no C25 . C27 . H272 . 109.5 no C25 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no C25 . C27 . H271 . 109.5 no C25 . C28 . H282 . 109.5 no C25 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no C25 . C28 . H281 . 109.5 no C10 . C29 . C30 . 108.8(4) yes C10 . C29 . C31 . 112.1(4) yes C30 . C29 . C31 . 109.0(5) yes C10 . C29 . C32 . 110.7(4) yes C30 . C29 . C32 . 106.8(5) yes C31 . C29 . C32 . 109.2(6) yes C29 . C30 . H302 . 109.5 no C29 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C29 . C30 . H301 . 109.5 no C29 . C31 . H312 . 109.5 no C29 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C29 . C31 . H311 . 109.5 no C29 . C32 . H322 . 109.5 no C29 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C29 . C32 . H321 . 109.5 no C15 . C33 . C34 . 110.2(3) yes C15 . C33 . C35 . 109.8(3) yes C34 . C33 . C35 . 110.3(4) yes C15 . C33 . C36 . 111.4(4) yes C34 . C33 . C36 . 107.0(4) yes C35 . C33 . C36 . 108.0(4) yes C33 . C34 . H342 . 109.5 no C33 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C33 . C34 . H341 . 109.5 no C33 . C35 . H352 . 109.5 no C33 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C33 . C35 . H351 . 109.5 no C33 . C36 . H362 . 109.5 no C33 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C33 . C36 . H361 . 109.5 no C17 . C37 . C39 . 108.5(5) yes C17 . C37 . C40 . 114.1(5) yes C39 . C37 . C40 . 107.4(6) yes C17 . C37 . C139 . 113.0(6) yes C39 . C37 . C139 . 62.3(7) yes C40 . C37 . C139 . 132.5(7) yes C17 . C37 . C140 . 105.2(6) yes C39 . C37 . C140 . 145.7(7) yes C40 . C37 . C140 . 51.4(6) yes C139 . C37 . C140 . 109.4(7) yes C17 . C37 . C38 . 112.8(5) yes C17 . C37 . C138 . 111.5(6) yes C38 . C37 . C138 . 135.5(7) yes C37 . C39 . C139 . 56.6(5) yes C37 . C40 . C140 . 66.7(6) yes C37 . C139 . C39 . 61.1(5) yes C37 . C140 . C40 . 61.9(6) yes Fe1 . N2 . C41 . 124.8(2) yes Fe1 . N2 . C43 . 129.5(2) yes C41 . N2 . C43 . 105.0(3) yes C41 . N3 . C42 . 106.8(3) yes C41 . N3 . C44 . 127.0(3) yes C42 . N3 . C44 . 126.2(3) yes N3 . C41 . N2 . 112.0(3) yes N3 . C41 . H411 . 124.0 no N2 . C41 . H411 . 124.0 no N3 . C42 . C43 . 106.6(3) yes N3 . C42 . H421 . 126.7 no C43 . C42 . H421 . 126.7 no N2 . C43 . C42 . 109.5(3) yes N2 . C43 . H431 . 125.2 no C42 . C43 . H431 . 125.2 no N3 . C44 . H442 . 109.5 no N3 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no N3 . C44 . H441 . 109.5 no C45 . O4 . C47 . 112.2(7) yes C45 . O4 . O104 . 85.9(10) yes C47 . O4 . O104 . 62.8(11) yes C45 . O4 . C145 . 29.3(9) yes C47 . O4 . C145 . 94.0(11) yes O104 . O4 . C145 . 56.7(9) yes C45 . O4 . C147 . 114.7(14) yes C47 . O4 . C147 . 7.9(12) yes O104 . O4 . C147 . 70.7(11) yes C145 . O4 . C147 . 99.5(14) yes O4 . C45 . C46 . 110.6(8) yes O4 . C45 . O104 . 37.5(6) yes C46 . C45 . O104 . 77.0(8) yes O4 . C45 . C145 . 93.2(15) yes C46 . C45 . C145 . 34.8(15) yes O104 . C45 . C145 . 55.7(12) yes O4 . C45 . H452 . 109.2 no C46 . C45 . H452 . 109.2 no O104 . C45 . H452 . 106.6 no C145 . C45 . H452 . 88.2 no O4 . C45 . C46 . 110.6(8) yes O4 . C45 . O104 . 37.5(6) yes C46 . C45 . O104 . 77.0(8) yes O4 . C45 . C145 . 93.2(15) yes C46 . C45 . C145 . 34.8(15) yes O104 . C45 . C145 . 55.7(12) yes O4 . C45 . H451 . 109.2 no C46 . C45 . H451 . 109.2 no O104 . C45 . H451 . 138.4 no C145 . C45 . H451 . 143.9 no C45 . C46 . C145 . 30.1(19) yes C45 . C46 . H462 . 109.5 no C145 . C46 . H462 . 123.6 no C45 . C46 . H463 . 109.5 no C145 . C46 . H463 . 79.5 no H462 . C46 . H463 . 109.5 no C45 . C46 . H1463 . 159.8 no C145 . C46 . H1463 . 134.2 no H462 . C46 . H1463 . 66.9 no H463 . C46 . H1463 . 56.9 no C45 . C46 . C145 . 30.1(19) yes C45 . C46 . H461 . 109.5 no C145 . C46 . H461 . 119.7 no C45 . C46 . H1461 . 121.1 no C145 . C46 . H1461 . 138.8 no H461 . C46 . H1461 . 21.0 no O4 . C47 . C48 . 105.2(8) yes O4 . C47 . O104 . 44.7(7) yes C48 . C47 . O104 . 126.4(14) yes O4 . C47 . C148 . 135.4(14) yes C48 . C47 . C148 . 44.2(9) yes O104 . C47 . C148 . 119.5(20) yes O4 . C47 . H472 . 110.5 no C48 . C47 . H472 . 110.5 no O104 . C47 . H472 . 66.2 no C148 . C47 . H472 . 69.3 no O4 . C47 . H1472 . 111.2 no C48 . C47 . H1472 . 115.1 no O104 . C47 . H1472 . 117.3 no C148 . C47 . H1472 . 111.8 no H472 . C47 . H1472 . 104.3 no O4 . C47 . C48 . 105.2(8) yes O4 . C47 . O104 . 44.7(7) yes C48 . C47 . O104 . 126.4(14) yes O4 . C47 . C148 . 135.4(14) yes C48 . C47 . C148 . 44.2(9) yes O104 . C47 . C148 . 119.5(20) yes O4 . C47 . H471 . 110.5 no C48 . C47 . H471 . 110.5 no O104 . C47 . H471 . 121.0 no C148 . C47 . H471 . 111.0 no O4 . C47 . H1471 . 62.0 no C48 . C47 . H1471 . 57.9 no O104 . C47 . H1471 . 105.7 no C148 . C47 . H1471 . 102.0 no H471 . C47 . H1471 . 90.8 no C47 . C48 . C147 . 6.7(12) yes C47 . C48 . C148 . 66.6(13) yes C147 . C48 . C148 . 72.7(13) yes C47 . C48 . H482 . 109.5 no C147 . C48 . H482 . 102.8 no C148 . C48 . H482 . 159.9 no C47 . C48 . H483 . 109.5 no C147 . C48 . H483 . 112.9 no C148 . C48 . H483 . 90.0 no H482 . C48 . H483 . 109.5 no C47 . C48 . H1482 . 94.2 no C147 . C48 . H1482 . 100.5 no C148 . C48 . H1482 . 48.6 no H482 . C48 . H1482 . 149.3 no H483 . C48 . H1482 . 42.0 no C47 . C48 . C147 . 6.7(12) yes C47 . C48 . C148 . 66.6(13) yes C147 . C48 . C148 . 72.7(13) yes C47 . C48 . H481 . 109.5 no C147 . C48 . H481 . 112.4 no C148 . C48 . H481 . 57.2 no C47 . C48 . H1481 . 97.9 no C147 . C48 . H1481 . 100.9 no C148 . C48 . H1481 . 48.9 no H481 . C48 . H1481 . 11.6 no C45 . O104 . C47 . 101.7(13) yes C45 . O104 . O4 . 56.6(8) yes C47 . O104 . O4 . 72.5(11) yes C45 . O104 . C145 . 28.9(12) yes C47 . O104 . C145 . 112.8(13) yes O4 . O104 . C145 . 85.4(14) yes C45 . O104 . C147 . 97.5(10) yes C47 . O104 . C147 . 6.7(14) yes O4 . O104 . C147 . 65.8(14) yes C145 . O104 . C147 . 111.5(8) yes C45 . O104 . H472 . 131.8 no C47 . O104 . H472 . 45.5 no O4 . O104 . H472 . 117.6 no C145 . O104 . H472 . 120.2 no C147 . O104 . H472 . 52.1 no O4 . C145 . O104 . 37.9(7) yes O4 . C145 . C46 . 130(2) yes O104 . C145 . C46 . 114.4(19) yes O4 . C145 . C45 . 57.5(14) yes O104 . C145 . C45 . 95.4(19) yes C46 . C145 . C45 . 115(3) yes O4 . C145 . C146 . 125.2(14) yes O104 . C145 . C146 . 110.9(9) yes C46 . C145 . C146 . 4.5(19) yes C45 . C145 . C146 . 113(3) yes O4 . C145 . H452 . 83.4 no O104 . C145 . H452 . 110.2 no C46 . C145 . H452 . 134.7 no C45 . C145 . H452 . 51.8 no C146 . C145 . H452 . 137.4 no O4 . C145 . H463 . 125.6 no O104 . C145 . H463 . 88.2 no C46 . C145 . H463 . 52.7 no C45 . C145 . H463 . 167.3 no C146 . C145 . H463 . 54.1 no O4 . C145 . H1452 . 122.6 no O104 . C145 . H1452 . 109.1 no C46 . C145 . H1452 . 104.9 no C45 . C145 . H1452 . 118.0 no C146 . C145 . H1452 . 109.1 no H452 . C145 . H463 . 137.8 no H452 . C145 . H1452 . 66.4 no H463 . C145 . H1452 . 71.8 no O4 . C145 . O104 . 37.9(7) yes O4 . C145 . C46 . 130(2) yes O104 . C145 . C46 . 114.4(19) yes O4 . C145 . C45 . 57.5(14) yes O104 . C145 . C45 . 95.4(19) yes C46 . C145 . C45 . 115(3) yes O4 . C145 . C146 . 125.2(14) yes O104 . C145 . C146 . 110.9(9) yes C46 . C145 . C146 . 4.5(19) yes C45 . C145 . C146 . 113(3) yes O4 . C145 . H1451 . 71.2 no O104 . C145 . H1451 . 109.1 no C46 . C145 . H1451 . 109.7 no C45 . C145 . H1451 . 14.0 no C146 . C145 . H1451 . 109.1 no C145 . C146 . H462 . 93.7 no C145 . C146 . H463 . 52.3 no H462 . C146 . H463 . 107.7 no C145 . C146 . H1462 . 109.5 no H462 . C146 . H1462 . 26.6 no H463 . C146 . H1462 . 134.2 no C145 . C146 . H1463 . 109.5 no H462 . C146 . H1463 . 96.4 no H463 . C146 . H1463 . 58.2 no H1462 . C146 . H1463 . 109.5 no C145 . C146 . H461 . 82.1 no C145 . C146 . H1461 . 109.5 no H461 . C146 . H1461 . 28.7 no O104 . C147 . C48 . 125.3(18) yes O104 . C147 . O4 . 43.5(8) yes C48 . C147 . O4 . 112(2) yes O104 . C147 . C148 . 110.1(9) yes C48 . C147 . C148 . 44.8(10) yes O4 . C147 . C148 . 134.5(19) yes O104 . C147 . H472 . 58.4 no C48 . C147 . H472 . 105.8 no O4 . C147 . H472 . 101.7 no C148 . C147 . H472 . 63.9 no O104 . C147 . H1472 . 109.3 no C48 . C147 . H1472 . 124.2 no O4 . C147 . H1472 . 114.5 no C148 . C147 . H1472 . 109.3 no H472 . C147 . H1472 . 92.6 no O104 . C147 . C48 . 125.3(18) yes O104 . C147 . O4 . 43.5(8) yes C48 . C147 . O4 . 112(2) yes O104 . C147 . C148 . 110.1(9) yes C48 . C147 . C148 . 44.8(10) yes O4 . C147 . C148 . 134.5(19) yes O104 . C147 . H471 . 113.7 no C48 . C147 . H471 . 120.4 no O4 . C147 . H471 . 115.1 no C148 . C147 . H471 . 109.7 no O104 . C147 . H1471 . 109.3 no C48 . C147 . H1471 . 64.5 no O4 . C147 . H1471 . 67.1 no C148 . C147 . H1471 . 109.3 no H471 . C147 . H1471 . 104.5 no C147 . C148 . C47 . 7.3(12) yes C147 . C148 . C48 . 62.5(14) yes C47 . C148 . C48 . 69.3(12) yes C147 . C148 . H1482 . 109.5 no C47 . C148 . H1482 . 110.4 no C48 . C148 . H1482 . 75.0 no C147 . C148 . H1483 . 109.5 no C47 . C148 . H1483 . 102.7 no C48 . C148 . H1483 . 171.9 no H1482 . C148 . H1483 . 109.5 no C147 . C148 . C47 . 7.3(12) yes C147 . C148 . C48 . 62.5(14) yes C47 . C148 . C48 . 69.3(12) yes C147 . C148 . H481 . 103.8 no C47 . C148 . H481 . 110.7 no C48 . C148 . H481 . 56.0 no C147 . C148 . H1481 . 109.5 no C47 . C148 . H1481 . 115.1 no C48 . C148 . H1481 . 74.4 no H481 . C148 . H1481 . 20.6 no C51 2_666 O5 . H491 2_666 145.7 no C51 2_666 O5 . O5 2_666 56.5(16) yes H491 2_666 O5 . O5 2_666 154.2 no C51 2_666 O5 . C49 2_666 129(4) yes H491 2_666 O5 . C49 2_666 66.5 no O5 2_666 O5 . C49 2_666 89(3) yes C51 2_666 O5 . C49 . 33.4(13) yes H491 2_666 O5 . C49 . 164.5 no O5 2_666 O5 . C49 . 39(2) yes C49 2_666 O5 . C49 . 128(2) yes C51 2_666 O5 . C51 . 138.3(15) yes H491 2_666 O5 . C51 . 74.8 no O5 2_666 O5 . C51 . 82(2) yes C49 2_666 O5 . C51 . 40(2) yes C49 . O5 . C51 . 111.9(9) yes O5 . C49 . C52 2_666 151.5(15) yes O5 . C49 . C51 2_666 88(2) yes C52 2_666 C49 . C51 2_666 64(2) yes O5 . C49 . O5 2_666 52(2) yes C52 2_666 C49 . O5 2_666 135(4) yes C51 2_666 C49 . O5 2_666 102(4) yes O5 . C49 . C50 . 110.3(9) yes C52 2_666 C49 . C50 . 41.7(14) yes C51 2_666 C49 . C50 . 30(3) yes O5 2_666 C49 . C50 . 131(4) yes O5 . C49 . H492 . 109.2 no C52 2_666 C49 . H492 . 89.7 no C51 2_666 C49 . H492 . 137.5 no O5 2_666 C49 . H492 . 120.0 no C50 . C49 . H492 . 109.3 no O5 . C49 . C52 2_666 151.5(15) yes O5 . C49 . C51 2_666 88(2) yes C52 2_666 C49 . C51 2_666 64(2) yes O5 . C49 . O5 2_666 52(2) yes C52 2_666 C49 . O5 2_666 135(4) yes C51 2_666 C49 . O5 2_666 102(4) yes O5 . C49 . C50 . 110.3(9) yes C52 2_666 C49 . C50 . 41.7(14) yes C51 2_666 C49 . C50 . 30(3) yes O5 2_666 C49 . C50 . 131(4) yes O5 . C49 . H491 . 109.3 no C52 2_666 C49 . H491 . 82.7 no C51 2_666 C49 . H491 . 99.7 no O5 2_666 C49 . H491 . 57.4 no C50 . C49 . H491 . 109.3 no C49 . C50 . C52 2_666 77(2) yes C49 . C50 . C51 2_666 33(3) yes C52 2_666 C50 . C51 2_666 98(4) yes C49 . C50 . H502 . 109.5 no C52 2_666 C50 . H502 . 116.3 no C51 2_666 C50 . H502 . 77.8 no C49 . C50 . H503 . 109.5 no C52 2_666 C50 . H503 . 128.4 no C51 2_666 C50 . H503 . 114.2 no H502 . C50 . H503 . 109.5 no H511 2_666 C50 . C49 . 62.9 no H511 2_666 C50 . C52 2_666 133.4 no C49 . C50 . C52 2_666 77(2) yes H511 2_666 C50 . C51 2_666 59.7 no C49 . C50 . C51 2_666 33(3) yes C52 2_666 C50 . C51 2_666 98(4) yes H511 2_666 C50 . H501 . 151.0 no C49 . C50 . H501 . 109.5 no C52 2_666 C50 . H501 . 33.3 no C51 2_666 C50 . H501 . 130.0 no H502 2_666 C51 . O5 . 143.3 no H502 2_666 C51 . O5 2_666 134.3 no O5 . C51 . O5 2_666 41.7(15) yes H502 2_666 C51 . C49 2_666 166.3 no O5 . C51 . C49 2_666 39(3) yes O5 2_666 C51 . C49 2_666 58.2(19) yes H502 2_666 C51 . C50 2_666 57.1 no O5 . C51 . C50 2_666 155(4) yes O5 2_666 C51 . C50 2_666 144(5) yes C49 2_666 C51 . C50 2_666 118(5) yes H502 2_666 C51 . C52 . 84.8 no O5 . C51 . C52 . 110.3(9) yes O5 2_666 C51 . C52 . 141(2) yes C49 2_666 C51 . C52 . 83(3) yes C50 2_666 C51 . C52 . 49(3) yes H502 2_666 C51 . H512 . 35.0 no O5 . C51 . H512 . 109.2 no O5 2_666 C51 . H512 . 106.9 no C49 2_666 C51 . H512 . 146.6 no C50 2_666 C51 . H512 . 92.0 no C52 . C51 . H512 . 109.2 no O5 . C51 . O5 2_666 41.7(15) yes O5 . C51 . C49 2_666 39(3) yes O5 2_666 C51 . C49 2_666 58.2(19) yes O5 . C51 . C50 2_666 155(4) yes O5 2_666 C51 . C50 2_666 144(5) yes C49 2_666 C51 . C50 2_666 118(5) yes O5 . C51 . C52 . 110.3(9) yes O5 2_666 C51 . C52 . 141(2) yes C49 2_666 C51 . C52 . 83(3) yes C50 2_666 C51 . C52 . 49(3) yes O5 . C51 . H511 . 109.3 no O5 2_666 C51 . H511 . 71.4 no C49 2_666 C51 . H511 . 94.3 no C50 2_666 C51 . H511 . 73.5 no C52 . C51 . H511 . 109.3 no C51 . C52 . C49 2_666 33.2(14) yes C51 . C52 . C50 2_666 34(2) yes C49 2_666 C52 . C50 2_666 61.5(17) yes C51 . C52 . H522 . 109.4 no C49 2_666 C52 . H522 . 80.8 no C50 2_666 C52 . H522 . 114.2 no C51 . C52 . H523 . 109.5 no C49 2_666 C52 . H523 . 105.1 no C50 2_666 C52 . H523 . 130.4 no H522 . C52 . H523 . 109.5 no C51 . C52 . C49 2_666 33.2(14) yes C51 . C52 . C50 2_666 34(2) yes C49 2_666 C52 . C50 2_666 61.5(17) yes C51 . C52 . H501 2_666 93.2 no C49 2_666 C52 . H501 2_666 121.0 no C50 2_666 C52 . H501 2_666 60.5 no C51 . C52 . H521 . 109.5 no C49 2_666 C52 . H521 . 137.3 no C50 2_666 C52 . H521 . 77.0 no H501 2_666 C52 . H521 . 16.5 no #===END ###################################### ## denoted [FeL3(1-Meim)] in text ## ###################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 669892' _audit_creation_date 07-11-09 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.2778(2) _cell_length_b 13.6398(3) _cell_length_c 14.0391(3) _cell_angle_alpha 94.0494(11) _cell_angle_beta 94.7940(11) _cell_angle_gamma 112.5924(11) _cell_volume 1974.47(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C40 H53 Cl1 Fe1 N3 O3 # Dc = 1.20 Fooo = 774.86 Mu = 4.88 M = 715.18 # Found Formula = C40.36 H54.43 Cl1 Fe1 N3 O3.36 # Dc = 1.22 FOOO = 774.86 Mu = 4.90 M = 726.63 _chemical_formula_sum 'C40.36 H54.43 Cl1 Fe1 N3 O3.36' _chemical_formula_moiety 'C40.36 H54.43 Cl1 Fe1 N3 O3.36' _chemical_compound_source ? _chemical_formula_weight 726.63 _cell_measurement_reflns_used 27291 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour darkbrown _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 774.859 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.92 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 27291 _reflns_number_total 8924 _diffrn_reflns_av_R_equivalents 0.041 # Number of reflections with Friedels Law is 8924 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9014 _diffrn_reflns_theta_min 5.124 _diffrn_reflns_theta_max 27.437 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.05 _refine_diff_density_max 1.16 _refine_ls_number_reflns 6725 _refine_ls_number_restraints 1 _refine_ls_number_parameters 442 #_refine_ls_R_factor_ref 0.0461 _refine_ls_wR_factor_ref 0.0655 _refine_ls_goodness_of_fit_ref 1.0417 #_reflns_number_all 8924 _refine_ls_R_factor_all 0.0678 _refine_ls_wR_factor_all 0.0670 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6725 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_gt 0.0655 _refine_ls_shift/su_max 0.003125 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.28 2.13 5.46 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.16885(3) 0.19679(2) 0.31661(2) 0.0215 1.0000 Uani . . . . . . O1 O 0.21757(17) 0.29393(13) 0.43387(11) 0.0329 1.0000 Uani . . . . . . O2 O 0.00090(13) 0.13073(12) 0.24975(11) 0.0252 1.0000 Uani . . . . . . O3 O 0.29844(13) 0.18699(11) 0.24595(11) 0.0251 1.0000 Uani . . . . . . N1 N 0.19235(15) 0.34817(13) 0.25680(12) 0.0214 1.0000 Uani . . . . . . C1 C 0.2718(2) 0.39834(18) 0.42470(16) 0.0288 1.0000 Uani . . . . . . C2 C 0.3380(3) 0.4765(2) 0.50285(17) 0.0405 1.0000 Uani . . . . . . C3 C 0.3960(3) 0.5831(2) 0.48883(19) 0.0438 1.0000 Uani . . . . . . C4 C 0.3891(3) 0.61359(19) 0.39762(19) 0.0393 1.0000 Uani . . . . . . Cl1 Cl 0.46723(10) 0.74742(5) 0.37703(6) 0.0676 1.0000 Uani . . . . . . C5 C 0.3230(2) 0.53895(18) 0.31917(16) 0.0320 1.0000 Uani . . . . . . C6 C 0.26488(19) 0.43240(17) 0.33349(15) 0.0246 1.0000 Uani . . . . . . C7 C -0.05315(17) 0.15510(16) 0.17031(14) 0.0219 1.0000 Uani . . . . . . C8 C -0.14074(17) 0.07445(15) 0.09940(14) 0.0210 1.0000 Uani . . . . . . C9 C -0.19301(18) 0.10767(16) 0.02063(14) 0.0227 1.0000 Uani . . . . . . C10 C -0.16267(19) 0.21435(16) 0.00653(15) 0.0237 1.0000 Uani . . . . . . C11 C -0.07729(19) 0.29169(16) 0.07707(15) 0.0239 1.0000 Uani . . . . . . C12 C -0.02417(18) 0.26299(16) 0.15841(15) 0.0229 1.0000 Uani . . . . . . C13 C 0.06005(19) 0.34843(16) 0.23620(15) 0.0249 1.0000 Uani . . . . . . C14 C 0.40611(18) 0.26990(15) 0.23073(14) 0.0206 1.0000 Uani . . . . . . C15 C 0.53090(18) 0.26971(15) 0.24995(14) 0.0215 1.0000 Uani . . . . . . C16 C 0.63626(19) 0.36196(16) 0.23635(15) 0.0249 1.0000 Uani . . . . . . C17 C 0.6250(2) 0.45272(16) 0.20312(16) 0.0269 1.0000 Uani . . . . . . C18 C 0.5004(2) 0.44759(16) 0.17967(16) 0.0261 1.0000 Uani . . . . . . C19 C 0.39250(19) 0.35878(15) 0.19291(14) 0.0223 1.0000 Uani . . . . . . C20 C 0.25821(19) 0.35513(16) 0.16878(14) 0.0232 1.0000 Uani . . . . . . C21 C -0.17795(19) -0.04446(16) 0.11059(15) 0.0237 1.0000 Uani . . . . . . C22 C -0.0583(2) -0.07244(17) 0.11278(16) 0.0282 1.0000 Uani . . . . . . C23 C -0.2414(2) -0.07008(17) 0.20352(17) 0.0309 1.0000 Uani . . . . . . C24 C -0.2759(2) -0.11728(17) 0.02684(18) 0.0340 1.0000 Uani . . . . . . C25 C -0.2247(2) 0.24358(17) -0.08298(16) 0.0283 1.0000 Uani . . . . . . C26 C -0.2003(2) 0.1888(2) -0.17462(17) 0.0361 1.0000 Uani . . . . . . C27 C -0.3710(2) 0.2068(2) -0.07837(19) 0.0380 1.0000 Uani . . . . . . C28 C -0.1691(3) 0.3639(2) -0.0887(2) 0.0439 1.0000 Uani . . . . . . C29 C 0.55153(19) 0.17025(16) 0.27847(15) 0.0242 1.0000 Uani . . . . . . C30 C 0.4955(3) 0.0833(2) 0.1934(2) 0.0459 1.0000 Uani . . . . . . C31 C 0.4850(3) 0.1277(2) 0.3662(2) 0.0459 1.0000 Uani . . . . . . C32 C 0.6949(2) 0.1913(2) 0.3005(2) 0.0461 1.0000 Uani . . . . . . C33 C 0.7418(2) 0.55488(17) 0.19236(18) 0.0326 1.0000 Uani . . . . . . C34 C 0.8699(2) 0.5458(2) 0.2249(3) 0.0537 1.0000 Uani . . . . . . C35 C 0.7370(3) 0.6503(2) 0.2519(2) 0.0466 1.0000 Uani . . . . . . C36 C 0.7396(3) 0.5762(2) 0.0859(2) 0.0527 1.0000 Uani . . . . . . N2 N 0.14698(17) 0.07172(15) 0.40165(13) 0.0271 1.0000 Uani . . . . . . C37 C 0.0989(2) -0.03167(19) 0.37239(17) 0.0339 1.0000 Uani . . . . . . N3 N 0.1071(2) -0.08842(16) 0.44548(14) 0.0329 1.0000 Uani . . . . . . C38 C 0.1624(3) -0.0173(2) 0.52541(17) 0.0423 1.0000 Uani . . . . . . C39 C 0.1866(3) 0.0813(2) 0.49807(17) 0.0379 1.0000 Uani . . . . . . C40 C 0.0630(3) -0.2047(2) 0.4407(2) 0.0520 1.0000 Uani . . . . . . O4 O -0.0144(15) 0.4823(12) 0.5087(13) 0.116(5) 0.357(10) Uiso . . . . . . C41 C 0.0980(15) 0.5794(12) 0.5298(14) 0.109(6) 0.357(10) Uiso . . . . . . H1 H -0.0532 0.4767 0.4408 0.1397 0.3572 Uiso . U . . . . H21 H 0.3432 0.4547 0.5691 0.0463 1.0000 Uiso . U . . . . H31 H 0.4428 0.6381 0.5447 0.0489 1.0000 Uiso . U . . . . H51 H 0.3175 0.5618 0.2534 0.0357 1.0000 Uiso . U . . . . H91 H -0.2562 0.0515 -0.0288 0.0273 1.0000 Uiso . U . . . . H111 H -0.0536 0.3690 0.0694 0.0289 1.0000 Uiso . U . . . . H131 H 0.0690 0.4195 0.2159 0.0305 1.0000 Uiso . U . . . . H132 H 0.0173 0.3372 0.2964 0.0305 1.0000 Uiso . U . . . . H161 H 0.7251 0.3632 0.2513 0.0300 1.0000 Uiso . U . . . . H181 H 0.4883 0.5095 0.1526 0.0318 1.0000 Uiso . U . . . . H201 H 0.2638 0.4214 0.1398 0.0281 1.0000 Uiso . U . . . . H202 H 0.2073 0.2912 0.1216 0.0281 1.0000 Uiso . U . . . . H221 H -0.0843 -0.1501 0.1201 0.0362 1.0000 Uiso . U . . . . H222 H 0.0065 -0.0288 0.1683 0.0362 1.0000 Uiso . U . . . . H223 H -0.0192 -0.0566 0.0514 0.0362 1.0000 Uiso . . . . . . H231 H -0.2658 -0.1475 0.2110 0.0377 1.0000 Uiso . U . . . . H232 H -0.3207 -0.0537 0.2000 0.0377 1.0000 Uiso . U . . . . H233 H -0.1790 -0.0257 0.2599 0.0377 1.0000 Uiso . . . . . . H241 H -0.2973 -0.1937 0.0371 0.0378 1.0000 Uiso . U . . . . H242 H -0.3565 -0.1028 0.0240 0.0378 1.0000 Uiso . U . . . . H243 H -0.2376 -0.1027 -0.0350 0.0378 1.0000 Uiso . . . . . . H261 H -0.2409 0.2081 -0.2325 0.0438 1.0000 Uiso . U . . . . H262 H -0.1050 0.2131 -0.1772 0.0438 1.0000 Uiso . U . . . . H263 H -0.2391 0.1095 -0.1736 0.0438 1.0000 Uiso . . . . . . H271 H -0.4118 0.2256 -0.1364 0.0469 1.0000 Uiso . U . . . . H272 H -0.3862 0.2432 -0.0191 0.0469 1.0000 Uiso . U . . . . H273 H -0.4100 0.1276 -0.0766 0.0469 1.0000 Uiso . . . . . . H281 H -0.2116 0.3798 -0.1476 0.0515 1.0000 Uiso . U . . . . H282 H -0.1854 0.4011 -0.0304 0.0515 1.0000 Uiso . U . . . . H283 H -0.0738 0.3897 -0.0919 0.0515 1.0000 Uiso . . . . . . H301 H 0.5078 0.0175 0.2102 0.0558 1.0000 Uiso . U . . . . H302 H 0.5409 0.1090 0.1362 0.0558 1.0000 Uiso . U . . . . H303 H 0.4010 0.0664 0.1779 0.0558 1.0000 Uiso . . . . . . H311 H 0.5013 0.0632 0.3818 0.0645 1.0000 Uiso . U . . . . H312 H 0.5204 0.1842 0.4224 0.0645 1.0000 Uiso . U . . . . H313 H 0.3898 0.1079 0.3518 0.0645 1.0000 Uiso . . . . . . H321 H 0.7037 0.1246 0.3186 0.0556 1.0000 Uiso . U . . . . H322 H 0.7353 0.2495 0.3549 0.0556 1.0000 Uiso . U . . . . H323 H 0.7394 0.2136 0.2422 0.0556 1.0000 Uiso . . . . . . H341 H 0.9436 0.6137 0.2169 0.0623 1.0000 Uiso . U . . . . H342 H 0.8729 0.5328 0.2942 0.0623 1.0000 Uiso . U . . . . H343 H 0.8769 0.4850 0.1851 0.0623 1.0000 Uiso . . . . . . H351 H 0.8139 0.7159 0.2439 0.0530 1.0000 Uiso . U . . . . H352 H 0.7380 0.6378 0.3212 0.0530 1.0000 Uiso . U . . . . H353 H 0.6560 0.6601 0.2298 0.0530 1.0000 Uiso . . . . . . H361 H 0.8156 0.6427 0.0786 0.0615 1.0000 Uiso . U . . . . H362 H 0.7439 0.5144 0.0456 0.0615 1.0000 Uiso . U . . . . H363 H 0.6579 0.5851 0.0645 0.0615 1.0000 Uiso . . . . . . H371 H 0.0613 -0.0636 0.3049 0.0394 1.0000 Uiso . U . . . . H381 H 0.1815 -0.0344 0.5916 0.0533 1.0000 Uiso . U . . . . H391 H 0.2270 0.1500 0.5413 0.0462 1.0000 Uiso . U . . . . H401 H 0.0285 -0.2372 0.3729 0.0615 1.0000 Uiso . U . . . . H402 H -0.0067 -0.2326 0.4832 0.0615 1.0000 Uiso . U . . . . H403 H 0.1373 -0.2238 0.4628 0.0615 1.0000 Uiso . . . . . . H411 H 0.1368 0.5849 0.5978 0.1313 0.3572 Uiso . U . . . . H412 H 0.0734 0.6415 0.5215 0.1313 0.3572 Uiso . U . . . . H413 H 0.1626 0.5795 0.4852 0.1313 0.3572 Uiso . . . . . . 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 0.01830(15) 0.02312(16) 0.02318(16) 0.00631(10) 0.00249(10) 0.00745(11) O1 0.0421(9) 0.0280(8) 0.0246(7) 0.0050(6) 0.0013(6) 0.0095(7) O2 0.0205(6) 0.0252(7) 0.0284(7) 0.0078(6) 0.0001(5) 0.0070(6) O3 0.0210(6) 0.0190(7) 0.0349(8) 0.0062(6) 0.0085(6) 0.0060(5) N1 0.0185(7) 0.0220(8) 0.0234(8) 0.0028(6) 0.0002(6) 0.0080(6) C1 0.0294(10) 0.0289(10) 0.0259(10) 0.0022(8) 0.0030(8) 0.0093(9) C2 0.0529(15) 0.0378(13) 0.0250(11) 0.0030(9) -0.0045(10) 0.0134(11) C3 0.0562(16) 0.0344(12) 0.0317(12) -0.0059(10) -0.0101(11) 0.0125(12) C4 0.0469(14) 0.0252(11) 0.0363(12) 0.0003(9) -0.0051(10) 0.0065(10) Cl1 0.1000(7) 0.0267(3) 0.0450(4) 0.0003(3) -0.0165(4) -0.0036(4) C5 0.0367(11) 0.0253(10) 0.0273(10) 0.0019(8) -0.0036(9) 0.0066(9) C6 0.0229(9) 0.0249(10) 0.0260(10) 0.0016(8) -0.0004(7) 0.0101(8) C7 0.0158(8) 0.0259(9) 0.0246(9) 0.0059(7) 0.0035(7) 0.0082(7) C8 0.0161(8) 0.0216(9) 0.0255(9) 0.0052(7) 0.0061(7) 0.0068(7) C9 0.0190(8) 0.0239(9) 0.0254(9) 0.0019(7) 0.0020(7) 0.0089(7) C10 0.0194(8) 0.0259(10) 0.0272(10) 0.0063(8) 0.0015(7) 0.0102(8) C11 0.0187(8) 0.0214(9) 0.0320(10) 0.0047(8) 0.0025(7) 0.0083(7) C12 0.0171(8) 0.0221(9) 0.0287(10) 0.0022(7) 0.0008(7) 0.0073(7) C13 0.0210(9) 0.0246(9) 0.0305(10) 0.0020(8) 0.0005(7) 0.0113(8) C14 0.0189(8) 0.0185(9) 0.0229(9) 0.0044(7) 0.0053(7) 0.0047(7) C15 0.0194(8) 0.0214(9) 0.0236(9) 0.0033(7) 0.0042(7) 0.0074(7) C16 0.0205(9) 0.0231(9) 0.0314(10) 0.0054(8) 0.0050(7) 0.0081(8) C17 0.0243(9) 0.0207(9) 0.0345(11) 0.0083(8) 0.0095(8) 0.0052(8) C18 0.0267(10) 0.0213(9) 0.0317(10) 0.0088(8) 0.0061(8) 0.0093(8) C19 0.0220(9) 0.0218(9) 0.0248(9) 0.0057(7) 0.0061(7) 0.0092(7) C20 0.0236(9) 0.0254(9) 0.0214(9) 0.0062(7) 0.0012(7) 0.0100(8) C21 0.0228(9) 0.0219(9) 0.0274(10) 0.0055(7) 0.0043(7) 0.0093(7) C22 0.0300(10) 0.0271(10) 0.0334(11) 0.0097(8) 0.0107(8) 0.0153(8) C23 0.0310(11) 0.0264(10) 0.0370(12) 0.0099(9) 0.0134(9) 0.0099(9) C24 0.0337(11) 0.0210(10) 0.0397(12) 0.0022(9) -0.0023(9) 0.0041(9) C25 0.0258(10) 0.0288(10) 0.0298(10) 0.0081(8) -0.0032(8) 0.0107(8) C26 0.0394(12) 0.0429(13) 0.0273(11) 0.0100(9) 0.0031(9) 0.0168(10) C27 0.0267(11) 0.0498(14) 0.0406(13) 0.0064(10) -0.0040(9) 0.0199(10) C28 0.0524(15) 0.0311(12) 0.0453(14) 0.0109(10) -0.0101(12) 0.0154(11) C29 0.0227(9) 0.0201(9) 0.0306(10) 0.0048(7) 0.0038(7) 0.0088(7) C30 0.0571(16) 0.0327(13) 0.0497(15) -0.0068(11) -0.0113(12) 0.0252(12) C31 0.0649(17) 0.0461(14) 0.0503(15) 0.0294(12) 0.0278(13) 0.0393(14) C32 0.0258(11) 0.0317(12) 0.082(2) 0.0156(13) -0.0033(12) 0.0126(10) C33 0.0265(10) 0.0249(10) 0.0445(13) 0.0122(9) 0.0111(9) 0.0051(8) C34 0.0228(11) 0.0349(13) 0.098(2) 0.0223(15) 0.0123(13) 0.0018(10) C35 0.0456(14) 0.0226(11) 0.0642(17) 0.0103(11) 0.0194(13) 0.0018(10) C36 0.0544(17) 0.0449(15) 0.0544(17) 0.0216(13) 0.0267(14) 0.0080(13) N2 0.0227(8) 0.0308(9) 0.0269(9) 0.0110(7) 0.0050(7) 0.0076(7) C37 0.0403(12) 0.0304(11) 0.0279(11) 0.0114(9) 0.0028(9) 0.0092(9) N3 0.0373(10) 0.0304(10) 0.0321(10) 0.0130(8) 0.0072(8) 0.0122(8) C38 0.0636(17) 0.0445(14) 0.0251(11) 0.0083(10) -0.0031(11) 0.0290(13) C39 0.0501(14) 0.0372(13) 0.0281(11) 0.0041(9) -0.0056(10) 0.0211(11) C40 0.071(2) 0.0328(13) 0.0504(16) 0.0168(12) 0.0088(14) 0.0156(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.389(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 1.9362(16) yes Fe1 . O2 . 1.8848(14) yes Fe1 . O3 . 1.8740(14) yes Fe1 . N1 . 2.2137(17) yes Fe1 . N2 . 2.1000(18) yes O1 . C1 . 1.337(3) yes O2 . C7 . 1.349(2) yes O3 . C14 . 1.350(2) yes N1 . C6 . 1.451(3) yes N1 . C13 . 1.497(2) yes N1 . C20 . 1.484(3) yes C1 . C2 . 1.409(3) yes C1 . C6 . 1.399(3) yes C2 . C3 . 1.383(4) yes C2 . H21 . 1.000 no C3 . C4 . 1.379(4) yes C3 . H31 . 1.000 no C4 . Cl1 . 1.753(3) yes C4 . C5 . 1.388(3) yes C5 . C6 . 1.383(3) yes C5 . H51 . 1.000 no C7 . C8 . 1.422(3) yes C7 . C12 . 1.405(3) yes C8 . C9 . 1.394(3) yes C8 . C21 . 1.535(3) yes C9 . C10 . 1.394(3) yes C9 . H91 . 1.000 no C10 . C11 . 1.390(3) yes C10 . C25 . 1.538(3) yes C11 . C12 . 1.395(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.500(3) yes C13 . H132 . 1.000 no C13 . H131 . 1.000 no C14 . C15 . 1.412(3) yes C14 . C19 . 1.413(3) yes C15 . C16 . 1.398(3) yes C15 . C29 . 1.536(3) yes C16 . C17 . 1.400(3) yes C16 . H161 . 1.000 no C17 . C18 . 1.390(3) yes C17 . C33 . 1.534(3) yes C18 . C19 . 1.386(3) yes C18 . H181 . 1.000 no C19 . C20 . 1.505(3) yes C20 . H202 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.535(3) yes C21 . C23 . 1.538(3) yes C21 . C24 . 1.538(3) yes C22 . H222 . 1.000 no C22 . H223 . 1.000 no C22 . H221 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C23 . H231 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.540(3) yes C25 . C27 . 1.537(3) yes C25 . C28 . 1.527(3) yes C26 . H262 . 1.000 no C26 . H263 . 1.000 no C26 . H261 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C27 . H271 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C28 . H281 . 1.000 no C29 . C30 . 1.527(3) yes C29 . C31 . 1.529(3) yes C29 . C32 . 1.530(3) yes C30 . H302 . 1.000 no C30 . H303 . 1.000 no C30 . H301 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C31 . H311 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C32 . H321 . 1.000 no C33 . C34 . 1.532(4) yes C33 . C35 . 1.518(4) yes C33 . C36 . 1.542(4) yes C34 . H342 . 1.000 no C34 . H343 . 1.000 no C34 . H341 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C35 . H351 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C36 . H361 . 1.000 no N2 . C37 . 1.321(3) yes N2 . C39 . 1.371(3) yes C37 . N3 . 1.346(3) yes C37 . H371 . 1.000 no N3 . C38 . 1.362(3) yes N3 . C40 . 1.463(3) yes C38 . C39 . 1.356(4) yes C38 . H381 . 1.000 no C39 . H391 . 1.000 no C40 . H402 . 1.000 no C40 . H403 . 1.000 no C40 . H401 . 1.000 no O4 . H1 2_566 0.960 no O4 . C41 2_566 1.06(2) yes O4 . C41 . 1.429(10) yes O4 . H1 . 1.000 no C41 . H412 . 1.000 no C41 . H413 . 1.000 no C41 . H1 2_566 0.890 no C41 . H411 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 125.69(7) yes O1 . Fe1 . O3 . 119.20(7) yes O2 . Fe1 . O3 . 113.74(7) yes O1 . Fe1 . N1 . 79.66(6) yes O2 . Fe1 . N1 . 90.12(6) yes O3 . Fe1 . N1 . 89.17(6) yes O1 . Fe1 . N2 . 88.30(7) yes O2 . Fe1 . N2 . 94.50(7) yes O3 . Fe1 . N2 . 99.45(7) yes N1 . Fe1 . N2 . 167.58(7) yes Fe1 . O1 . C1 . 116.80(13) yes Fe1 . O2 . C7 . 130.74(12) yes Fe1 . O3 . C14 . 125.45(12) yes Fe1 . N1 . C6 . 105.60(12) yes Fe1 . N1 . C13 . 107.23(12) yes C6 . N1 . C13 . 108.61(15) yes Fe1 . N1 . C20 . 109.50(12) yes C6 . N1 . C20 . 113.57(16) yes C13 . N1 . C20 . 111.96(15) yes O1 . C1 . C2 . 123.0(2) yes O1 . C1 . C6 . 119.10(19) yes C2 . C1 . C6 . 117.9(2) yes C1 . C2 . C3 . 120.6(2) yes C1 . C2 . H21 . 119.7 no C3 . C2 . H21 . 119.7 no C2 . C3 . C4 . 119.9(2) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 120.1 no C3 . C4 . Cl1 . 120.85(19) yes C3 . C4 . C5 . 121.1(2) yes Cl1 . C4 . C5 . 118.08(19) yes C4 . C5 . C6 . 118.9(2) yes C4 . C5 . H51 . 120.6 no C6 . C5 . H51 . 120.6 no N1 . C6 . C1 . 114.99(18) yes N1 . C6 . C5 . 123.37(19) yes C1 . C6 . C5 . 121.6(2) yes O2 . C7 . C8 . 121.73(17) yes O2 . C7 . C12 . 119.06(17) yes C8 . C7 . C12 . 119.20(18) yes C7 . C8 . C9 . 117.43(18) yes C7 . C8 . C21 . 121.05(17) yes C9 . C8 . C21 . 121.51(17) yes C8 . C9 . C10 . 124.06(18) yes C8 . C9 . H91 . 118.0 no C10 . C9 . H91 . 118.0 no C9 . C10 . C11 . 117.41(18) yes C9 . C10 . C25 . 120.46(18) yes C11 . C10 . C25 . 122.12(18) yes C10 . C11 . C12 . 120.97(18) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 119.5 no C7 . C12 . C11 . 120.91(18) yes C7 . C12 . C13 . 119.67(18) yes C11 . C12 . C13 . 119.36(18) yes C12 . C13 . N1 . 113.05(16) yes C12 . C13 . H132 . 108.6 no N1 . C13 . H132 . 108.6 no C12 . C13 . N1 . 113.05(16) yes C12 . C13 . H131 . 108.6 no N1 . C13 . H131 . 108.6 no O3 . C14 . C15 . 122.17(17) yes O3 . C14 . C19 . 118.54(17) yes C15 . C14 . C19 . 119.28(17) yes C14 . C15 . C16 . 117.45(17) yes C14 . C15 . C29 . 121.92(17) yes C16 . C15 . C29 . 120.51(17) yes C15 . C16 . C17 . 124.01(18) yes C15 . C16 . H161 . 118.0 no C17 . C16 . H161 . 118.0 no C16 . C17 . C18 . 116.86(18) yes C16 . C17 . C33 . 123.29(19) yes C18 . C17 . C33 . 119.85(19) yes C17 . C18 . C19 . 121.56(18) yes C17 . C18 . H181 . 119.2 no C19 . C18 . H181 . 119.2 no C14 . C19 . C18 . 120.66(18) yes C14 . C19 . C20 . 118.37(17) yes C18 . C19 . C20 . 120.97(17) yes C19 . C20 . N1 . 110.41(15) yes C19 . C20 . H202 . 109.2 no N1 . C20 . H202 . 109.2 no C19 . C20 . N1 . 110.41(15) yes C19 . C20 . H201 . 109.2 no N1 . C20 . H201 . 109.2 no C8 . C21 . C22 . 110.57(16) yes C8 . C21 . C23 . 109.26(16) yes C22 . C21 . C23 . 110.46(17) yes C8 . C21 . C24 . 112.18(17) yes C22 . C21 . C24 . 106.96(18) yes C23 . C21 . C24 . 107.35(18) yes C21 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C21 . C22 . H221 . 109.5 no C21 . C23 . H232 . 109.5 no C21 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C21 . C23 . H231 . 109.5 no C21 . C24 . H242 . 109.5 no C21 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C21 . C24 . H241 . 109.5 no C10 . C25 . C26 . 109.90(17) yes C10 . C25 . C27 . 109.12(18) yes C26 . C25 . C27 . 109.86(19) yes C10 . C25 . C28 . 111.76(18) yes C26 . C25 . C28 . 108.1(2) yes C27 . C25 . C28 . 108.1(2) yes C25 . C26 . H262 . 109.5 no C25 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C25 . C26 . H261 . 109.5 no C25 . C27 . H272 . 109.5 no C25 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no C25 . C27 . H271 . 109.5 no C25 . C28 . H282 . 109.5 no C25 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no C25 . C28 . H281 . 109.5 no C15 . C29 . C30 . 107.97(17) yes C15 . C29 . C31 . 112.60(17) yes C30 . C29 . C31 . 108.7(2) yes C15 . C29 . C32 . 112.23(17) yes C30 . C29 . C32 . 107.4(2) yes C31 . C29 . C32 . 107.8(2) yes C29 . C30 . H302 . 109.5 no C29 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C29 . C30 . H301 . 109.5 no C29 . C31 . H312 . 109.5 no C29 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C29 . C31 . H311 . 109.5 no C29 . C32 . H322 . 109.5 no C29 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C29 . C32 . H321 . 109.5 no C17 . C33 . C34 . 111.80(19) yes C17 . C33 . C35 . 110.78(19) yes C34 . C33 . C35 . 107.9(2) yes C17 . C33 . C36 . 109.2(2) yes C34 . C33 . C36 . 108.7(2) yes C35 . C33 . C36 . 108.3(2) yes C33 . C34 . H342 . 109.5 no C33 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C33 . C34 . H341 . 109.5 no C33 . C35 . H352 . 109.5 no C33 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C33 . C35 . H351 . 109.5 no C33 . C36 . H362 . 109.5 no C33 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C33 . C36 . H361 . 109.5 no Fe1 . N2 . C37 . 127.15(15) yes Fe1 . N2 . C39 . 126.78(16) yes C37 . N2 . C39 . 105.98(19) yes N2 . C37 . N3 . 111.0(2) yes N2 . C37 . H371 . 124.5 no N3 . C37 . H371 . 124.5 no C37 . N3 . C38 . 107.1(2) yes C37 . N3 . C40 . 126.7(2) yes C38 . N3 . C40 . 126.3(2) yes N3 . C38 . C39 . 106.8(2) yes N3 . C38 . H381 . 126.6 no C39 . C38 . H381 . 126.6 no N2 . C39 . C38 . 109.1(2) yes N2 . C39 . H391 . 125.5 no C38 . C39 . H391 . 125.5 no N3 . C40 . H402 . 109.5 no N3 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no N3 . C40 . H401 . 109.5 no H1 2_566 O4 . C41 2_566 161.8 no H1 2_566 O4 . C41 . 37.7 no C41 2_566 O4 . C41 . 160.5(17) yes H1 2_566 O4 . H1 . 147.2 no C41 2_566 O4 . H1 . 51.0 no C41 . O4 . H1 . 109.5 no O4 . C41 . O4 2_566 19.5(17) yes O4 . C41 . H412 . 109.5 no O4 2_566 C41 . H412 . 99.0 no O4 . C41 . H413 . 109.5 no O4 2_566 C41 . H413 . 99.0 no H412 . C41 . H413 . 109.5 no O4 . C41 . H1 2_566 41.3 no O4 . C41 . O4 2_566 19.5(17) yes H1 2_566 C41 . O4 2_566 60.8 no O4 . C41 . H411 . 109.5 no H1 2_566 C41 . H411 . 68.2 no O4 2_566 C41 . H411 . 129.0 no #===END ###################################### ## denoted [FeL5]in text ## ###################################### data_5 _database_code_depnum_ccdc_archive 'CCDC 669893' _audit_creation_date 07-11-09 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.4928(3) _cell_length_b 19.4211(4) _cell_length_c 16.9802(4) _cell_angle_alpha 90 _cell_angle_beta 115.7166(7) _cell_angle_gamma 90 _cell_volume 4603.07(17) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C47 H70 Fe1 N2 O3 # Dc = 1.11 Fooo = 1700.00 Mu = 3.66 M = 766.93 # Found Formula = C48 H73 Fe1 N2 O3 # Dc = 1.13 FOOO = 1700.00 Mu = 3.67 M = 781.97 _chemical_formula_sum 'C48 H73 Fe1 N2 O3' _chemical_formula_moiety 'C48 H73 Fe1 N2 O3' _chemical_compound_source ? _chemical_formula_weight 781.97 _cell_measurement_reflns_used 40111 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description fragment _exptl_crystal_colour brown _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 40111 _reflns_number_total 10776 _diffrn_reflns_av_R_equivalents 0.053 # Number of reflections with Friedels Law is 10776 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10567 _diffrn_reflns_theta_min 5.103 _diffrn_reflns_theta_max 27.493 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -20 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.46 _refine_diff_density_max 0.43 _refine_ls_number_reflns 7378 _refine_ls_number_restraints 0 _refine_ls_number_parameters 487 #_refine_ls_R_factor_ref 0.0390 _refine_ls_wR_factor_ref 0.0453 _refine_ls_goodness_of_fit_ref 1.0735 #_reflns_number_all 10467 _refine_ls_R_factor_all 0.0690 _refine_ls_wR_factor_all 0.0474 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7378 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_gt 0.0453 _refine_ls_shift/su_max 0.000515 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.45 -0.465 2.82 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.409320(16) 0.146346(12) 0.413239(15) 0.0181 1.0000 Uani . . . . . . O1 O 0.46400(9) 0.14015(7) 0.33453(8) 0.0258 1.0000 Uani . . . . . . O2 O 0.30594(8) 0.20752(6) 0.37927(8) 0.0240 1.0000 Uani . . . . . . O3 O 0.35689(8) 0.05693(6) 0.38445(8) 0.0239 1.0000 Uani . . . . . . N1 N 0.51494(10) 0.23036(7) 0.48041(9) 0.0201 1.0000 Uani . . . . . . N2 N 0.45079(10) 0.12169(7) 0.55259(9) 0.0196 1.0000 Uani . . . . . . C1 C 0.51270(12) 0.18304(9) 0.30672(11) 0.0216 1.0000 Uani . . . . . . C2 C 0.49933(12) 0.18243(9) 0.21853(11) 0.0221 1.0000 Uani . . . . . . C3 C 0.55570(12) 0.22687(9) 0.19645(11) 0.0232 1.0000 Uani . . . . . . C4 C 0.62431(12) 0.27179(9) 0.25554(11) 0.0228 1.0000 Uani . . . . . . C5 C 0.63328(12) 0.27227(9) 0.34049(11) 0.0220 1.0000 Uani . . . . . . C6 C 0.57945(12) 0.22808(9) 0.36663(11) 0.0216 1.0000 Uani . . . . . . C7 C 0.60045(12) 0.22346(9) 0.46145(11) 0.0230 1.0000 Uani . . . . . . C8 C 0.29886(12) 0.26367(9) 0.42237(11) 0.0216 1.0000 Uani . . . . . . C9 C 0.21400(12) 0.27831(9) 0.43128(11) 0.0234 1.0000 Uani . . . . . . C10 C 0.21496(12) 0.33541(9) 0.48178(12) 0.0247 1.0000 Uani . . . . . . C11 C 0.29375(13) 0.37844(9) 0.52362(12) 0.0256 1.0000 Uani . . . . . . C12 C 0.37510(12) 0.36411(9) 0.51079(12) 0.0253 1.0000 Uani . . . . . . C13 C 0.37828(12) 0.30859(9) 0.46065(11) 0.0229 1.0000 Uani . . . . . . C14 C 0.46588(12) 0.29715(9) 0.44501(12) 0.0234 1.0000 Uani . . . . . . C15 C 0.31693(12) 0.01629(8) 0.42341(11) 0.0213 1.0000 Uani . . . . . . C16 C 0.23171(12) -0.02154(9) 0.37347(11) 0.0228 1.0000 Uani . . . . . . C17 C 0.19275(12) -0.05939(9) 0.42016(12) 0.0250 1.0000 Uani . . . . . . C18 C 0.23307(12) -0.06355(9) 0.51169(12) 0.0242 1.0000 Uani . . . . . . C19 C 0.31969(12) -0.02952(9) 0.55777(11) 0.0235 1.0000 Uani . . . . . . C20 C 0.36157(12) 0.00970(8) 0.51502(11) 0.0215 1.0000 Uani . . . . . . C21 C 0.45571(12) 0.04574(9) 0.56688(11) 0.0224 1.0000 Uani . . . . . . C22 C 0.54913(12) 0.22546(9) 0.57661(11) 0.0224 1.0000 Uani . . . . . . C23 C 0.54871(11) 0.15041(9) 0.60072(10) 0.0217 1.0000 Uani . . . . . . C24 C 0.38570(12) 0.15094(9) 0.58702(11) 0.0237 1.0000 Uani . . . . . . C25 C 0.42597(13) 0.13362(9) 0.15158(11) 0.0260 1.0000 Uani . . . . . . C26 C 0.32493(14) 0.15294(12) 0.14093(14) 0.0377 1.0000 Uani . . . . . . C27 C 0.44911(16) 0.05849(10) 0.18191(13) 0.0338 1.0000 Uani . . . . . . C28 C 0.42548(16) 0.13894(11) 0.06108(12) 0.0353 1.0000 Uani . . . . . . C29 C 0.68636(13) 0.31636(9) 0.22562(12) 0.0273 1.0000 Uani . . . . . . C30 C 0.73730(16) 0.26954(11) 0.18568(15) 0.0397 1.0000 Uani . . . . . . C31 C 0.62384(18) 0.36750(12) 0.15664(18) 0.0490 1.0000 Uani . . . . . . C32 C 0.76509(18) 0.35436(13) 0.30147(16) 0.0476 1.0000 Uani . . . . . . C33 C 0.12308(12) 0.23400(9) 0.38599(12) 0.0257 1.0000 Uani . . . . . . C34 C 0.09322(14) 0.23323(11) 0.28677(13) 0.0330 1.0000 Uani . . . . . . C35 C 0.03831(14) 0.26245(12) 0.39938(15) 0.0374 1.0000 Uani . . . . . . C36 C 0.14055(14) 0.15989(10) 0.42086(12) 0.0303 1.0000 Uani . . . . . . C37 C 0.29497(14) 0.43896(10) 0.58199(13) 0.0307 1.0000 Uani . . . . . . C38 C 0.32064(18) 0.50539(11) 0.54776(17) 0.0438 1.0000 Uani . . . . . . C39 C 0.37041(16) 0.42489(12) 0.67563(14) 0.0391 1.0000 Uani . . . . . . C40 C 0.19775(16) 0.44899(12) 0.58438(17) 0.0454 1.0000 Uani . . . . . . C41 C 0.18461(13) -0.02050(9) 0.27282(12) 0.0270 1.0000 Uani . . . . . . C42 C 0.15584(14) 0.05340(11) 0.23911(13) 0.0343 1.0000 Uani . . . . . . C43 C 0.25489(15) -0.04873(12) 0.23869(13) 0.0376 1.0000 Uani . . . . . . C44 C 0.09385(15) -0.06500(11) 0.23363(13) 0.0389 1.0000 Uani . . . . . . C45 C 0.17964(13) -0.10086(9) 0.55649(13) 0.0269 1.0000 Uani . . . . . . C46 C 0.08813(14) -0.05990(11) 0.53898(15) 0.0365 1.0000 Uani . . . . . . C47 C 0.23913(15) -0.10623(10) 0.65545(13) 0.0330 1.0000 Uani . . . . . . C48 C 0.15138(14) -0.17386(10) 0.51904(14) 0.0313 1.0000 Uani . . . . . . H31 H 0.5468 0.2269 0.1345 0.0291 1.0000 Uiso . . . . . . H51 H 0.6793 0.3050 0.3839 0.0276 1.0000 Uiso . . . . . . H71 H 0.6466 0.2610 0.4934 0.0290 1.0000 Uiso . . . . . . H72 H 0.6307 0.1777 0.4839 0.0290 1.0000 Uiso . . . . . . H101 H 0.1552 0.3461 0.4883 0.0305 1.0000 Uiso . . . . . . H121 H 0.4325 0.3946 0.5384 0.0311 1.0000 Uiso . . . . . . H141 H 0.5122 0.3354 0.4736 0.0302 1.0000 Uiso . . . . . . H142 H 0.4460 0.2980 0.3806 0.0302 1.0000 Uiso . . . . . . H171 H 0.1320 -0.0853 0.3861 0.0298 1.0000 Uiso . . . . . . H191 H 0.3525 -0.0333 0.6229 0.0289 1.0000 Uiso . . . . . . H211 H 0.4757 0.0368 0.6304 0.0261 1.0000 Uiso . . . . . . H212 H 0.5047 0.0263 0.5495 0.0261 1.0000 Uiso . . . . . . H221 H 0.6157 0.2443 0.6068 0.0274 1.0000 Uiso . . . . . . H222 H 0.5056 0.2524 0.5947 0.0274 1.0000 Uiso . . . . . . H231 H 0.5689 0.1465 0.6650 0.0258 1.0000 Uiso . . . . . . H232 H 0.5944 0.1241 0.5848 0.0258 1.0000 Uiso . . . . . . H241 H 0.3813 0.2020 0.5781 0.0304 1.0000 Uiso . . . . . . H242 H 0.4112 0.1405 0.6508 0.0304 1.0000 Uiso . . . . . . H243 H 0.3206 0.1301 0.5553 0.0304 1.0000 Uiso . . . . . . H261 H 0.2767 0.1214 0.0974 0.0432 1.0000 Uiso . . . . . . H262 H 0.3103 0.2016 0.1199 0.0432 1.0000 Uiso . . . . . . H263 H 0.3223 0.1484 0.1985 0.0432 1.0000 Uiso . . . . . . H271 H 0.4009 0.0273 0.1378 0.0406 1.0000 Uiso . . . . . . H272 H 0.5146 0.0466 0.1881 0.0406 1.0000 Uiso . . . . . . H273 H 0.4469 0.0527 0.2395 0.0406 1.0000 Uiso . . . . . . H281 H 0.3769 0.1064 0.0198 0.0416 1.0000 Uiso . . . . . . H282 H 0.4903 0.1268 0.0659 0.0416 1.0000 Uiso . . . . . . H283 H 0.4089 0.1871 0.0386 0.0416 1.0000 Uiso . . . . . . H301 H 0.7779 0.2983 0.1660 0.0537 1.0000 Uiso . . . . . . H302 H 0.7787 0.2357 0.2306 0.0537 1.0000 Uiso . . . . . . H303 H 0.6884 0.2442 0.1345 0.0537 1.0000 Uiso . . . . . . H311 H 0.6648 0.3963 0.1375 0.0607 1.0000 Uiso . . . . . . H312 H 0.5900 0.3979 0.1818 0.0607 1.0000 Uiso . . . . . . H313 H 0.5756 0.3420 0.1052 0.0607 1.0000 Uiso . . . . . . H321 H 0.8035 0.3826 0.2789 0.0604 1.0000 Uiso . . . . . . H322 H 0.8078 0.3202 0.3450 0.0604 1.0000 Uiso . . . . . . H323 H 0.7355 0.3852 0.3302 0.0604 1.0000 Uiso . . . . . . H341 H 0.0342 0.2046 0.2570 0.0380 1.0000 Uiso . . . . . . H342 H 0.0798 0.2813 0.2636 0.0380 1.0000 Uiso . . . . . . H343 H 0.1462 0.2133 0.2754 0.0380 1.0000 Uiso . . . . . . H351 H -0.0187 0.2321 0.3689 0.0458 1.0000 Uiso . . . . . . H352 H 0.0552 0.2638 0.4633 0.0458 1.0000 Uiso . . . . . . H353 H 0.0231 0.3100 0.3747 0.0458 1.0000 Uiso . . . . . . H361 H 0.0806 0.1324 0.3904 0.0367 1.0000 Uiso . . . . . . H362 H 0.1594 0.1603 0.4851 0.0367 1.0000 Uiso . . . . . . H363 H 0.1931 0.1388 0.4097 0.0367 1.0000 Uiso . . . . . . H381 H 0.3215 0.5449 0.5858 0.0559 1.0000 Uiso . . . . . . H382 H 0.3853 0.5003 0.5487 0.0559 1.0000 Uiso . . . . . . H383 H 0.2718 0.5141 0.4865 0.0559 1.0000 Uiso . . . . . . H391 H 0.3717 0.4642 0.7142 0.0476 1.0000 Uiso . . . . . . H392 H 0.4348 0.4199 0.6760 0.0476 1.0000 Uiso . . . . . . H393 H 0.3538 0.3815 0.6976 0.0476 1.0000 Uiso . . . . . . H401 H 0.2018 0.4889 0.6231 0.0578 1.0000 Uiso . . . . . . H402 H 0.1809 0.4064 0.6077 0.0578 1.0000 Uiso . . . . . . H403 H 0.1474 0.4583 0.5239 0.0578 1.0000 Uiso . . . . . . H421 H 0.1254 0.0534 0.1737 0.0370 1.0000 Uiso . . . . . . H422 H 0.2141 0.0833 0.2613 0.0370 1.0000 Uiso . . . . . . H423 H 0.1093 0.0716 0.2603 0.0370 1.0000 Uiso . . . . . . H431 H 0.2238 -0.0479 0.1733 0.0431 1.0000 Uiso . . . . . . H432 H 0.3139 -0.0195 0.2611 0.0431 1.0000 Uiso . . . . . . H433 H 0.2727 -0.0971 0.2595 0.0431 1.0000 Uiso . . . . . . H441 H 0.0657 -0.0628 0.1684 0.0418 1.0000 Uiso . . . . . . H442 H 0.1105 -0.1138 0.2532 0.0418 1.0000 Uiso . . . . . . H443 H 0.0461 -0.0474 0.2538 0.0418 1.0000 Uiso . . . . . . H461 H 0.0520 -0.0835 0.5678 0.0460 1.0000 Uiso . . . . . . H462 H 0.1058 -0.0123 0.5632 0.0460 1.0000 Uiso . . . . . . H463 H 0.0471 -0.0573 0.4746 0.0460 1.0000 Uiso . . . . . . H471 H 0.2013 -0.1309 0.6818 0.0427 1.0000 Uiso . . . . . . H472 H 0.2994 -0.1323 0.6682 0.0427 1.0000 Uiso . . . . . . H473 H 0.2555 -0.0590 0.6811 0.0427 1.0000 Uiso . . . . . . H481 H 0.1165 -0.1975 0.5490 0.0394 1.0000 Uiso . . . . . . H482 H 0.2104 -0.2005 0.5288 0.0394 1.0000 Uiso . . . . . . H483 H 0.1088 -0.1710 0.4549 0.0394 1.0000 Uiso . . . . . . 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 0.01830(11) 0.02084(11) 0.01693(11) -0.00116(9) 0.00934(8) -0.00138(9) O1 0.0279(6) 0.0307(6) 0.0242(6) -0.0061(5) 0.0163(5) -0.0084(5) O2 0.0229(6) 0.0259(6) 0.0231(6) -0.0029(5) 0.0100(5) 0.0010(5) O3 0.0263(6) 0.0243(6) 0.0210(6) 0.0000(5) 0.0102(5) -0.0034(5) N1 0.0195(6) 0.0251(7) 0.0182(6) -0.0022(5) 0.0105(5) -0.0018(5) N2 0.0199(7) 0.0214(6) 0.0189(7) -0.0017(5) 0.0098(5) 0.0000(5) C1 0.0205(7) 0.0260(8) 0.0235(8) -0.0015(7) 0.0143(7) -0.0009(6) C2 0.0212(8) 0.0243(8) 0.0213(8) -0.0025(6) 0.0096(6) 0.0004(6) C3 0.0251(8) 0.0270(8) 0.0206(8) -0.0005(7) 0.0127(7) 0.0012(7) C4 0.0236(8) 0.0237(8) 0.0239(8) 0.0002(7) 0.0127(7) -0.0003(6) C5 0.0196(7) 0.0234(8) 0.0260(8) -0.0029(7) 0.0126(7) -0.0010(6) C6 0.0192(7) 0.0280(8) 0.0203(8) -0.0026(6) 0.0109(6) 0.0002(6) C7 0.0193(8) 0.0307(9) 0.0224(8) -0.0046(7) 0.0123(7) -0.0026(6) C8 0.0232(8) 0.0215(8) 0.0207(8) 0.0032(6) 0.0101(7) 0.0026(6) C9 0.0232(8) 0.0259(8) 0.0224(8) 0.0044(7) 0.0111(7) 0.0032(7) C10 0.0238(8) 0.0267(8) 0.0257(8) 0.0037(7) 0.0126(7) 0.0055(7) C11 0.0280(9) 0.0253(8) 0.0256(8) 0.0023(7) 0.0137(7) 0.0046(7) C12 0.0245(8) 0.0235(9) 0.0299(9) 0.0006(7) 0.0135(7) 0.0005(7) C13 0.0239(8) 0.0234(8) 0.0255(8) 0.0035(7) 0.0145(7) 0.0013(6) C14 0.0258(8) 0.0215(8) 0.0281(9) -0.0009(7) 0.0165(7) -0.0009(7) C15 0.0232(8) 0.0190(7) 0.0223(8) 0.0006(6) 0.0106(7) 0.0003(6) C16 0.0216(8) 0.0214(8) 0.0220(8) -0.0018(6) 0.0062(7) 0.0002(6) C17 0.0239(8) 0.0212(8) 0.0295(9) -0.0010(7) 0.0111(7) -0.0024(7) C18 0.0264(8) 0.0191(8) 0.0292(9) 0.0022(7) 0.0141(7) 0.0033(7) C19 0.0265(8) 0.0216(8) 0.0242(8) 0.0027(6) 0.0127(7) 0.0039(6) C20 0.0218(8) 0.0202(8) 0.0220(8) -0.0008(6) 0.0089(7) 0.0025(6) C21 0.0222(8) 0.0229(8) 0.0201(8) 0.0018(6) 0.0073(6) 0.0026(6) C22 0.0241(8) 0.0259(8) 0.0184(8) -0.0050(6) 0.0105(6) -0.0043(7) C23 0.0204(7) 0.0264(8) 0.0176(7) -0.0030(7) 0.0076(6) -0.0006(7) C24 0.0255(8) 0.0252(8) 0.0254(8) 0.0016(7) 0.0158(7) 0.0041(7) C25 0.0274(9) 0.0276(9) 0.0224(8) -0.0039(7) 0.0101(7) -0.0045(7) C26 0.0261(9) 0.0476(12) 0.0343(10) -0.0078(9) 0.0084(8) -0.0047(9) C27 0.0472(11) 0.0267(9) 0.0275(9) -0.0046(7) 0.0162(8) -0.0040(8) C28 0.0459(11) 0.0363(11) 0.0218(9) -0.0049(8) 0.0129(8) -0.0090(9) C29 0.0297(9) 0.0285(9) 0.0274(9) 0.0006(7) 0.0159(7) -0.0041(7) C30 0.0455(12) 0.0396(11) 0.0490(12) -0.0014(10) 0.0347(11) -0.0049(9) C31 0.0489(13) 0.0416(13) 0.0613(15) 0.0208(11) 0.0285(12) 0.0071(10) C32 0.0520(13) 0.0565(14) 0.0424(12) -0.0120(11) 0.0281(11) -0.0284(12) C33 0.0220(8) 0.0303(9) 0.0247(8) 0.0031(7) 0.0101(7) 0.0013(7) C34 0.0293(9) 0.0402(11) 0.0254(9) 0.0060(8) 0.0079(7) 0.0001(8) C35 0.0240(9) 0.0449(12) 0.0454(12) -0.0036(9) 0.0172(8) -0.0006(8) C36 0.0295(9) 0.0338(10) 0.0285(9) 0.0047(7) 0.0134(7) -0.0041(7) C37 0.0315(9) 0.0294(9) 0.0356(10) -0.0052(8) 0.0186(8) 0.0028(8) C38 0.0563(14) 0.0267(10) 0.0566(14) -0.0021(9) 0.0321(12) 0.0035(9) C39 0.0414(11) 0.0436(12) 0.0339(11) -0.0084(9) 0.0179(9) -0.0013(9) C40 0.0416(12) 0.0420(12) 0.0609(15) -0.0180(11) 0.0301(11) 0.0023(10) C41 0.0258(8) 0.0260(9) 0.0243(9) -0.0022(7) 0.0062(7) -0.0016(7) C42 0.0329(10) 0.0350(10) 0.0245(9) 0.0025(8) 0.0027(8) -0.0001(8) C43 0.0354(10) 0.0468(12) 0.0255(10) -0.0064(8) 0.0083(8) 0.0046(9) C44 0.0357(10) 0.0384(11) 0.0304(10) -0.0049(9) 0.0029(8) -0.0087(9) C45 0.0282(9) 0.0215(8) 0.0349(10) 0.0031(7) 0.0174(8) 0.0005(7) C46 0.0310(10) 0.0314(10) 0.0525(13) -0.0002(9) 0.0233(9) 0.0028(8) C47 0.0400(10) 0.0330(10) 0.0339(10) 0.0041(8) 0.0233(9) -0.0023(8) C48 0.0313(9) 0.0229(8) 0.0443(11) 0.0022(8) 0.0207(9) -0.0005(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7962(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 1.8712(12) yes Fe1 . O2 . 1.8728(12) yes Fe1 . O3 . 1.8895(12) yes Fe1 . N1 . 2.2407(14) yes Fe1 . N2 . 2.2185(14) yes O1 . C1 . 1.340(2) yes O2 . C8 . 1.344(2) yes O3 . C15 . 1.341(2) yes N1 . C7 . 1.499(2) yes N1 . C14 . 1.492(2) yes N1 . C22 . 1.486(2) yes N2 . C21 . 1.491(2) yes N2 . C23 . 1.485(2) yes N2 . C24 . 1.481(2) yes C1 . C2 . 1.420(2) yes C1 . C6 . 1.399(2) yes C2 . C3 . 1.390(2) yes C2 . C25 . 1.537(2) yes C3 . C4 . 1.404(2) yes C3 . H31 . 1.000 no C4 . C5 . 1.388(2) yes C4 . C29 . 1.535(2) yes C5 . C6 . 1.397(2) yes C5 . H51 . 1.000 no C6 . C7 . 1.500(2) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . C9 . 1.416(2) yes C8 . C13 . 1.415(2) yes C9 . C10 . 1.398(2) yes C9 . C33 . 1.541(2) yes C10 . C11 . 1.393(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.397(2) yes C11 . C37 . 1.532(3) yes C12 . C13 . 1.388(2) yes C12 . H121 . 1.000 no C13 . C14 . 1.508(2) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.425(2) yes C15 . C20 . 1.407(2) yes C16 . C17 . 1.396(2) yes C16 . C41 . 1.540(2) yes C17 . C18 . 1.404(3) yes C17 . H171 . 1.000 no C18 . C19 . 1.392(2) yes C18 . C45 . 1.528(2) yes C19 . C20 . 1.392(2) yes C19 . H191 . 1.000 no C20 . C21 . 1.509(2) yes C21 . H211 . 1.000 no C21 . H212 . 1.000 no C22 . C23 . 1.515(2) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C25 . C26 . 1.542(3) yes C25 . C27 . 1.537(3) yes C25 . C28 . 1.537(2) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . C30 . 1.541(3) yes C29 . C31 . 1.520(3) yes C29 . C32 . 1.526(3) yes C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 no C31 . H311 . 1.000 no C31 . H312 . 1.000 no C31 . H313 . 1.000 no C32 . H321 . 1.000 no C32 . H322 . 1.000 no C32 . H323 . 1.000 no C33 . C34 . 1.541(3) yes C33 . C35 . 1.530(3) yes C33 . C36 . 1.535(3) yes C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no C35 . H351 . 1.000 no C35 . H352 . 1.000 no C35 . H353 . 1.000 no C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C37 . C38 . 1.537(3) yes C37 . C39 . 1.535(3) yes C37 . C40 . 1.537(3) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no C38 . H383 . 1.000 no C39 . H391 . 1.000 no C39 . H392 . 1.000 no C39 . H393 . 1.000 no C40 . H401 . 1.000 no C40 . H402 . 1.000 no C40 . H403 . 1.000 no C41 . C42 . 1.538(3) yes C41 . C43 . 1.539(3) yes C41 . C44 . 1.535(3) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C42 . H423 . 1.000 no C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 1.000 no C44 . H441 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C45 . C46 . 1.538(3) yes C45 . C47 . 1.530(3) yes C45 . C48 . 1.538(3) yes C46 . H461 . 1.000 no C46 . H462 . 1.000 no C46 . H463 . 1.000 no C47 . H471 . 1.000 no C47 . H472 . 1.000 no C47 . H473 . 1.000 no C48 . H481 . 1.000 no C48 . H482 . 1.000 no C48 . H483 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 114.36(6) yes O1 . Fe1 . O3 . 91.90(5) yes O2 . Fe1 . O3 . 106.81(5) yes O1 . Fe1 . N1 . 87.33(5) yes O2 . Fe1 . N1 . 91.89(5) yes O3 . Fe1 . N1 . 159.71(5) yes O1 . Fe1 . N2 . 137.45(5) yes O2 . Fe1 . N2 . 106.17(5) yes O3 . Fe1 . N2 . 88.32(5) yes N1 . Fe1 . N2 . 78.74(5) yes Fe1 . O1 . C1 . 135.27(11) yes Fe1 . O2 . C8 . 127.44(11) yes Fe1 . O3 . C15 . 130.68(11) yes Fe1 . N1 . C7 . 110.11(10) yes Fe1 . N1 . C14 . 107.23(10) yes C7 . N1 . C14 . 109.53(13) yes Fe1 . N1 . C22 . 110.26(10) yes C7 . N1 . C22 . 107.69(12) yes C14 . N1 . C22 . 112.02(13) yes Fe1 . N2 . C21 . 110.96(10) yes Fe1 . N2 . C23 . 105.06(9) yes C21 . N2 . C23 . 108.30(13) yes Fe1 . N2 . C24 . 113.99(10) yes C21 . N2 . C24 . 108.10(13) yes C23 . N2 . C24 . 110.30(13) yes O1 . C1 . C2 . 121.30(15) yes O1 . C1 . C6 . 118.96(15) yes C2 . C1 . C6 . 119.72(15) yes C1 . C2 . C3 . 117.25(15) yes C1 . C2 . C25 . 120.53(15) yes C3 . C2 . C25 . 122.22(15) yes C2 . C3 . C4 . 124.23(15) yes C2 . C3 . H31 . 117.9 no C4 . C3 . H31 . 117.9 no C3 . C4 . C5 . 116.75(15) yes C3 . C4 . C29 . 120.17(15) yes C5 . C4 . C29 . 123.07(15) yes C4 . C5 . C6 . 121.46(16) yes C4 . C5 . H51 . 119.3 no C6 . C5 . H51 . 119.3 no C1 . C6 . C5 . 120.54(15) yes C1 . C6 . C7 . 119.39(15) yes C5 . C6 . C7 . 119.76(15) yes C6 . C7 . N1 . 115.14(13) yes C6 . C7 . H71 . 108.0 no N1 . C7 . H71 . 108.0 no C6 . C7 . H72 . 108.0 no N1 . C7 . H72 . 108.0 no H71 . C7 . H72 . 109.5 no O2 . C8 . C9 . 121.33(15) yes O2 . C8 . C13 . 119.34(14) yes C9 . C8 . C13 . 119.32(16) yes C8 . C9 . C10 . 117.49(16) yes C8 . C9 . C33 . 121.63(15) yes C10 . C9 . C33 . 120.87(15) yes C9 . C10 . C11 . 124.23(16) yes C9 . C10 . H101 . 117.9 no C11 . C10 . H101 . 117.9 no C10 . C11 . C12 . 116.82(16) yes C10 . C11 . C37 . 123.52(16) yes C12 . C11 . C37 . 119.67(16) yes C11 . C12 . C13 . 121.67(16) yes C11 . C12 . H121 . 119.2 no C13 . C12 . H121 . 119.2 no C8 . C13 . C12 . 120.35(15) yes C8 . C13 . C14 . 119.85(15) yes C12 . C13 . C14 . 119.78(15) yes C13 . C14 . N1 . 113.41(13) yes C13 . C14 . H141 . 108.5 no N1 . C14 . H141 . 108.5 no C13 . C14 . H142 . 108.5 no N1 . C14 . H142 . 108.5 no H141 . C14 . H142 . 109.5 no O3 . C15 . C16 . 121.10(15) yes O3 . C15 . C20 . 119.21(15) yes C16 . C15 . C20 . 119.67(15) yes C15 . C16 . C17 . 116.80(15) yes C15 . C16 . C41 . 121.62(15) yes C17 . C16 . C41 . 121.59(15) yes C16 . C17 . C18 . 124.39(16) yes C16 . C17 . H171 . 117.8 no C18 . C17 . H171 . 117.8 no C17 . C18 . C19 . 116.89(15) yes C17 . C18 . C45 . 120.10(15) yes C19 . C18 . C45 . 122.92(16) yes C18 . C19 . C20 . 121.36(16) yes C18 . C19 . H191 . 119.3 no C20 . C19 . H191 . 119.3 no C15 . C20 . C19 . 120.63(15) yes C15 . C20 . C21 . 119.32(15) yes C19 . C20 . C21 . 120.05(15) yes C20 . C21 . N2 . 113.30(13) yes C20 . C21 . H211 . 108.5 no N2 . C21 . H211 . 108.5 no C20 . C21 . H212 . 108.5 no N2 . C21 . H212 . 108.5 no H211 . C21 . H212 . 109.5 no N1 . C22 . C23 . 108.51(13) yes N1 . C22 . H221 . 109.7 no C23 . C22 . H221 . 109.7 no N1 . C22 . H222 . 109.7 no C23 . C22 . H222 . 109.7 no H221 . C22 . H222 . 109.5 no C22 . C23 . N2 . 109.63(13) yes C22 . C23 . H231 . 109.4 no N2 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.4 no N2 . C23 . H232 . 109.4 no H231 . C23 . H232 . 109.5 no N2 . C24 . H241 . 109.5 no N2 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.5 no N2 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C2 . C25 . C26 . 108.90(15) yes C2 . C25 . C27 . 110.35(15) yes C26 . C25 . C27 . 110.34(16) yes C2 . C25 . C28 . 112.29(15) yes C26 . C25 . C28 . 107.58(16) yes C27 . C25 . C28 . 107.34(15) yes C25 . C26 . H261 . 109.5 no C25 . C26 . H262 . 109.5 no H261 . C26 . H262 . 109.5 no C25 . C26 . H263 . 109.5 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C25 . C27 . H271 . 109.5 no C25 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.5 no C25 . C27 . H273 . 109.5 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no C25 . C28 . H281 . 109.5 no C25 . C28 . H282 . 109.5 no H281 . C28 . H282 . 109.5 no C25 . C28 . H283 . 109.5 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no C4 . C29 . C30 . 109.07(15) yes C4 . C29 . C31 . 110.02(16) yes C30 . C29 . C31 . 108.86(17) yes C4 . C29 . C32 . 112.30(15) yes C30 . C29 . C32 . 106.41(17) yes C31 . C29 . C32 . 110.07(19) yes C29 . C30 . H301 . 109.5 no C29 . C30 . H302 . 109.5 no H301 . C30 . H302 . 109.5 no C29 . C30 . H303 . 109.5 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C29 . C31 . H311 . 109.5 no C29 . C31 . H312 . 109.5 no H311 . C31 . H312 . 109.5 no C29 . C31 . H313 . 109.5 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no C29 . C32 . H321 . 109.5 no C29 . C32 . H322 . 109.5 no H321 . C32 . H322 . 109.5 no C29 . C32 . H323 . 109.5 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C9 . C33 . C34 . 109.07(14) yes C9 . C33 . C35 . 112.44(15) yes C34 . C33 . C35 . 107.22(16) yes C9 . C33 . C36 . 111.16(14) yes C34 . C33 . C36 . 109.36(15) yes C35 . C33 . C36 . 107.47(15) yes C33 . C34 . H341 . 109.5 no C33 . C34 . H342 . 109.5 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C33 . C35 . H351 . 109.5 no C33 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.5 no C33 . C35 . H353 . 109.5 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C33 . C36 . H361 . 109.5 no C33 . C36 . H362 . 109.5 no H361 . C36 . H362 . 109.5 no C33 . C36 . H363 . 109.5 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C11 . C37 . C38 . 109.39(16) yes C11 . C37 . C39 . 108.88(16) yes C38 . C37 . C39 . 109.61(18) yes C11 . C37 . C40 . 112.16(16) yes C38 . C37 . C40 . 108.73(17) yes C39 . C37 . C40 . 108.04(17) yes C37 . C38 . H381 . 109.5 no C37 . C38 . H382 . 109.5 no H381 . C38 . H382 . 109.5 no C37 . C38 . H383 . 109.5 no H381 . C38 . H383 . 109.5 no H382 . C38 . H383 . 109.5 no C37 . C39 . H391 . 109.5 no C37 . C39 . H392 . 109.5 no H391 . C39 . H392 . 109.5 no C37 . C39 . H393 . 109.5 no H391 . C39 . H393 . 109.5 no H392 . C39 . H393 . 109.5 no C37 . C40 . H401 . 109.5 no C37 . C40 . H402 . 109.5 no H401 . C40 . H402 . 109.5 no C37 . C40 . H403 . 109.5 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no C16 . C41 . C42 . 110.28(15) yes C16 . C41 . C43 . 109.95(15) yes C42 . C41 . C43 . 109.30(16) yes C16 . C41 . C44 . 112.18(16) yes C42 . C41 . C44 . 107.53(16) yes C43 . C41 . C44 . 107.51(16) yes C41 . C42 . H421 . 109.5 no C41 . C42 . H422 . 109.5 no H421 . C42 . H422 . 109.5 no C41 . C42 . H423 . 109.5 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no C41 . C43 . H431 . 109.5 no C41 . C43 . H432 . 109.5 no H431 . C43 . H432 . 109.5 no C41 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no C41 . C44 . H441 . 109.5 no C41 . C44 . H442 . 109.5 no H441 . C44 . H442 . 109.5 no C41 . C44 . H443 . 109.5 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C18 . C45 . C46 . 108.15(15) yes C18 . C45 . C47 . 112.38(15) yes C46 . C45 . C47 . 108.24(16) yes C18 . C45 . C48 . 110.48(15) yes C46 . C45 . C48 . 108.90(15) yes C47 . C45 . C48 . 108.61(15) yes C45 . C46 . H461 . 109.5 no C45 . C46 . H462 . 109.5 no H461 . C46 . H462 . 109.5 no C45 . C46 . H463 . 109.5 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no C45 . C47 . H471 . 109.5 no C45 . C47 . H472 . 109.5 no H471 . C47 . H472 . 109.5 no C45 . C47 . H473 . 109.5 no H471 . C47 . H473 . 109.5 no H472 . C47 . H473 . 109.5 no C45 . C48 . H481 . 109.5 no C45 . C48 . H482 . 109.5 no H481 . C48 . H482 . 109.5 no C45 . C48 . H483 . 109.5 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no #===END #===END ###################################### ## denoted [FeL4(1-Meim)]in text ## ###################################### data_4 _database_code_depnum_ccdc_archive 'CCDC 670101' _audit_creation_date 07-11-09 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.3141(2) _cell_length_b 10.76380(10) _cell_length_c 22.3380(3) _cell_angle_alpha 90 _cell_angle_beta 102.1568(6) _cell_angle_gamma 90 _cell_volume 3129.48(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C31 H31 Fe1 N3 O3 # Dc = 1.17 Fooo = 1236.00 Mu = 5.14 M = 549.45 # Found Formula = C33 H40 Fe1 N3 O3 # Dc = 1.24 FOOO = 1236.00 Mu = 5.18 M = 582.55 _chemical_formula_sum 'C33 H40 Fe1 N3 O3' _chemical_formula_moiety 'C33 H40 Fe1 N3 O3' _chemical_compound_source ? _chemical_formula_weight 582.55 _cell_measurement_reflns_used 41442 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK(Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 41442 _reflns_number_total 7470 _diffrn_reflns_av_R_equivalents 0.057 # Number of reflections with Friedels Law is 7470 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7169 _diffrn_reflns_theta_min 5.125 _diffrn_reflns_theta_max 27.479 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.655 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.41 _refine_diff_density_max 0.35 _refine_ls_number_reflns 4882 _refine_ls_number_restraints 0 _refine_ls_number_parameters 361 #_refine_ls_R_factor_ref 0.0380 _refine_ls_wR_factor_ref 0.0490 _refine_ls_goodness_of_fit_ref 1.0218 #_reflns_number_all 7101 _refine_ls_R_factor_all 0.0738 _refine_ls_wR_factor_all 0.0790 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4882 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_gt 0.0490 _refine_ls_shift/su_max 0.000465 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.41 0.964 2.92 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.239542(19) 0.01787(2) 0.431421(11) 0.0169 1.0000 Uani . . . . . . O1 O 0.32422(11) 0.08115(13) 0.50549(6) 0.0256 1.0000 Uani . . . . . . O2 O 0.11855(10) -0.07415(13) 0.41880(6) 0.0234 1.0000 Uani . . . . . . O3 O 0.26652(10) 0.07559(12) 0.35750(6) 0.0221 1.0000 Uani . . . . . . N1 N 0.15438(11) 0.18927(14) 0.44124(7) 0.0194 1.0000 Uani . . . . . . N2 N 0.33121(12) -0.14220(15) 0.44312(7) 0.0221 1.0000 Uani . . . . . . N3 N 0.43507(13) -0.28389(15) 0.49211(8) 0.0247 1.0000 Uani . . . . . . C1 C 0.30590(15) 0.19665(18) 0.52190(8) 0.0231 1.0000 Uani . . . . . . C2 C 0.36856(17) 0.2572(2) 0.57167(9) 0.0284 1.0000 Uani . . . . . . C3 C 0.34834(18) 0.3795(2) 0.58521(9) 0.0310 1.0000 Uani . . . . . . C4 C 0.26543(18) 0.4454(2) 0.55115(9) 0.0310 1.0000 Uani . . . . . . C5 C 0.20167(17) 0.38406(19) 0.50212(9) 0.0269 1.0000 Uani . . . . . . C6 C 0.22155(15) 0.26217(18) 0.48816(8) 0.0216 1.0000 Uani . . . . . . C7 C 0.2426(2) 0.5771(2) 0.56743(11) 0.0431 1.0000 Uani . . . . . . C8 C 0.01859(14) -0.04397(19) 0.40409(8) 0.0227 1.0000 Uani . . . . . . C9 C -0.05405(15) -0.1275(2) 0.36969(9) 0.0261 1.0000 Uani . . . . . . C10 C -0.15735(16) -0.0919(2) 0.35834(11) 0.0371 1.0000 Uani . . . . . . C11 C -0.18916(17) 0.0206(3) 0.37865(13) 0.0446 1.0000 Uani . . . . . . C12 C -0.11757(17) 0.1008(2) 0.41154(12) 0.0367 1.0000 Uani . . . . . . C13 C -0.01377(15) 0.06975(19) 0.42492(9) 0.0261 1.0000 Uani . . . . . . C14 C 0.06159(15) 0.15216(18) 0.46595(9) 0.0247 1.0000 Uani . . . . . . C15 C -0.01993(16) -0.2510(2) 0.34687(9) 0.0306 1.0000 Uani . . . . . . C16 C 0.03690(16) -0.3302(2) 0.40074(10) 0.0306 1.0000 Uani . . . . . . C17 C 0.04932(18) -0.2264(2) 0.30104(10) 0.0374 1.0000 Uani . . . . . . C18 C -0.11182(19) -0.3294(3) 0.31373(12) 0.0452 1.0000 Uani . . . . . . C19 C 0.28063(13) 0.19269(17) 0.34079(8) 0.0192 1.0000 Uani . . . . . . C20 C 0.35918(14) 0.22153(18) 0.30848(8) 0.0206 1.0000 Uani . . . . . . C21 C 0.36980(15) 0.3458(2) 0.29302(9) 0.0267 1.0000 Uani . . . . . . C22 C 0.30731(18) 0.4387(2) 0.30761(10) 0.0310 1.0000 Uani . . . . . . C23 C 0.22942(16) 0.40874(19) 0.33757(9) 0.0269 1.0000 Uani . . . . . . C24 C 0.21466(14) 0.28676(17) 0.35395(8) 0.0195 1.0000 Uani . . . . . . C25 C 0.12411(14) 0.25217(18) 0.38101(8) 0.0212 1.0000 Uani . . . . . . C26 C 0.42616(15) 0.11836(19) 0.28976(8) 0.0239 1.0000 Uani . . . . . . C27 C 0.49216(17) 0.0561(2) 0.34664(10) 0.0336 1.0000 Uani . . . . . . C28 C 0.35846(17) 0.0202(2) 0.25072(9) 0.0291 1.0000 Uani . . . . . . C29 C 0.50045(18) 0.1701(2) 0.25174(11) 0.0349 1.0000 Uani . . . . . . C30 C 0.31628(17) -0.2505(2) 0.41024(10) 0.0314 1.0000 Uani . . . . . . C31 C 0.38001(17) -0.3388(2) 0.44035(10) 0.0336 1.0000 Uani . . . . . . C32 C 0.40313(14) -0.16596(18) 0.49181(8) 0.0227 1.0000 Uani . . . . . . C33 C 0.51236(17) -0.3428(2) 0.54011(10) 0.0316 1.0000 Uani . . . . . . H21 H 0.4279 0.2123 0.5974 0.0336 1.0000 Uiso . . . . . . H31 H 0.3946 0.4214 0.6205 0.0378 1.0000 Uiso . . . . . . H51 H 0.1413 0.4286 0.4771 0.0331 1.0000 Uiso . . . . . . H71 H 0.2958 0.6053 0.6034 0.0527 1.0000 Uiso . . . . . . H72 H 0.1732 0.5803 0.5781 0.0527 1.0000 Uiso . . . . . . H73 H 0.2432 0.6328 0.5317 0.0527 1.0000 Uiso . . . . . . H101 H -0.2102 -0.1492 0.3347 0.0434 1.0000 Uiso . . . . . . H111 H -0.2636 0.0431 0.3695 0.0529 1.0000 Uiso . . . . . . H121 H -0.1404 0.1821 0.4259 0.0451 1.0000 Uiso . . . . . . H141 H 0.0862 0.1075 0.5056 0.0314 1.0000 Uiso . . . . . . H142 H 0.0247 0.2298 0.4735 0.0314 1.0000 Uiso . . . . . . H161 H 0.0586 -0.4106 0.3849 0.0367 1.0000 Uiso . . . . . . H162 H -0.0100 -0.3473 0.4294 0.0367 1.0000 Uiso . . . . . . H163 H 0.0989 -0.2843 0.4230 0.0367 1.0000 Uiso . . . . . . H171 H 0.0717 -0.3073 0.2861 0.0452 1.0000 Uiso . . . . . . H172 H 0.1111 -0.1780 0.3217 0.0452 1.0000 Uiso . . . . . . H173 H 0.0102 -0.1777 0.2655 0.0452 1.0000 Uiso . . . . . . H181 H -0.0862 -0.4092 0.2995 0.0528 1.0000 Uiso . . . . . . H182 H -0.1582 -0.3474 0.3425 0.0528 1.0000 Uiso . . . . . . H183 H -0.1506 -0.2821 0.2776 0.0528 1.0000 Uiso . . . . . . H211 H 0.4247 0.3684 0.2706 0.0330 1.0000 Uiso . . . . . . H221 H 0.3183 0.5270 0.2966 0.0389 1.0000 Uiso . . . . . . H231 H 0.1834 0.4756 0.3475 0.0332 1.0000 Uiso . . . . . . H251 H 0.0854 0.3296 0.3864 0.0258 1.0000 Uiso . . . . . . H252 H 0.0786 0.1951 0.3520 0.0258 1.0000 Uiso . . . . . . H271 H 0.5351 -0.0107 0.3335 0.0407 1.0000 Uiso . . . . . . H272 H 0.5379 0.1196 0.3713 0.0407 1.0000 Uiso . . . . . . H273 H 0.4464 0.0189 0.3721 0.0407 1.0000 Uiso . . . . . . H281 H 0.4029 -0.0463 0.2389 0.0358 1.0000 Uiso . . . . . . H282 H 0.3108 -0.0172 0.2749 0.0358 1.0000 Uiso . . . . . . H283 H 0.3175 0.0602 0.2130 0.0358 1.0000 Uiso . . . . . . H291 H 0.5429 0.1007 0.2403 0.0447 1.0000 Uiso . . . . . . H292 H 0.5466 0.2332 0.2764 0.0447 1.0000 Uiso . . . . . . H293 H 0.4604 0.2099 0.2137 0.0447 1.0000 Uiso . . . . . . H301 H 0.2663 -0.2625 0.3704 0.0355 1.0000 Uiso . . . . . . H311 H 0.3858 -0.4269 0.4272 0.0381 1.0000 Uiso . . . . . . H321 H 0.4306 -0.1037 0.5245 0.0270 1.0000 Uiso . . . . . . H331 H 0.5399 -0.2803 0.5725 0.0361 1.0000 Uiso . . . . . . H332 H 0.4802 -0.4130 0.5586 0.0361 1.0000 Uiso . . . . . . H333 H 0.5697 -0.3752 0.5219 0.0361 1.0000 Uiso . . . . . . 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 0.01693(14) 0.01559(14) 0.01866(14) 0.00169(10) 0.00476(9) 0.00200(10) O1 0.0279(7) 0.0205(7) 0.0258(7) -0.0013(5) 0.0001(5) 0.0056(5) O2 0.0177(6) 0.0217(7) 0.0310(7) 0.0019(5) 0.0055(5) 0.0021(5) O3 0.0265(7) 0.0185(6) 0.0232(6) 0.0023(5) 0.0101(5) 0.0037(5) N1 0.0209(7) 0.0180(8) 0.0211(7) 0.0022(6) 0.0084(6) 0.0044(6) N2 0.0207(7) 0.0203(8) 0.0246(8) 0.0005(6) 0.0030(6) 0.0044(6) N3 0.0242(8) 0.0199(8) 0.0277(8) 0.0005(6) 0.0003(7) 0.0048(6) C1 0.0300(10) 0.0201(9) 0.0208(8) -0.0004(7) 0.0089(7) -0.0039(7) C2 0.0372(11) 0.0252(10) 0.0220(9) 0.0010(8) 0.0047(8) -0.0029(8) C3 0.0462(12) 0.0263(11) 0.0228(9) -0.0043(8) 0.0124(8) -0.0083(9) C4 0.0481(13) 0.0214(10) 0.0266(9) -0.0019(8) 0.0146(9) -0.0010(9) C5 0.0367(11) 0.0218(10) 0.0246(9) 0.0024(7) 0.0116(8) 0.0042(8) C6 0.0268(9) 0.0193(9) 0.0214(8) 0.0012(7) 0.0114(7) 0.0015(7) C7 0.0635(16) 0.0245(12) 0.0437(13) -0.0080(10) 0.0171(12) 0.0037(10) C8 0.0186(9) 0.0286(11) 0.0220(8) 0.0085(7) 0.0067(7) 0.0016(7) C9 0.0223(9) 0.0301(11) 0.0256(9) 0.0043(8) 0.0044(7) -0.0014(8) C10 0.0201(10) 0.0462(14) 0.0423(12) 0.0053(10) 0.0003(9) -0.0014(9) C11 0.0195(11) 0.0505(15) 0.0632(16) 0.0137(12) 0.0078(10) 0.0081(10) C12 0.0270(11) 0.0308(11) 0.0552(14) 0.0095(10) 0.0154(10) 0.0073(9) C13 0.0248(10) 0.0253(10) 0.0314(10) 0.0090(8) 0.0137(8) 0.0028(7) C14 0.0256(9) 0.0223(9) 0.0310(10) 0.0010(8) 0.0169(8) 0.0010(7) C15 0.0245(10) 0.0382(12) 0.0278(10) -0.0050(9) 0.0027(8) -0.0055(9) C16 0.0315(11) 0.0266(11) 0.0338(11) -0.0037(8) 0.0072(9) -0.0005(8) C17 0.0350(12) 0.0494(14) 0.0283(10) -0.0058(10) 0.0080(9) -0.0044(10) C18 0.0359(13) 0.0515(16) 0.0447(13) -0.0132(12) 0.0005(10) -0.0137(11) C19 0.0184(8) 0.0221(9) 0.0170(8) 0.0014(7) 0.0034(7) 0.0016(7) C20 0.0202(9) 0.0236(10) 0.0190(8) 0.0017(7) 0.0062(7) 0.0017(7) C21 0.0260(10) 0.0281(11) 0.0289(10) 0.0021(8) 0.0124(8) -0.0016(8) C22 0.0393(12) 0.0202(9) 0.0383(11) 0.0039(8) 0.0193(9) -0.0019(8) C23 0.0307(10) 0.0225(10) 0.0307(10) 0.0023(8) 0.0135(8) 0.0049(8) C24 0.0208(9) 0.0224(9) 0.0156(8) 0.0025(7) 0.0049(7) 0.0034(7) C25 0.0207(9) 0.0230(10) 0.0217(8) 0.0050(7) 0.0085(7) 0.0067(7) C26 0.0225(9) 0.0285(10) 0.0231(9) 0.0016(7) 0.0101(7) 0.0066(8) C27 0.0287(11) 0.0415(13) 0.0313(10) 0.0045(9) 0.0082(8) 0.0131(9) C28 0.0318(11) 0.0289(10) 0.0293(10) -0.0043(8) 0.0126(8) 0.0036(8) C29 0.0338(11) 0.0364(12) 0.0417(12) 0.0013(9) 0.0248(9) 0.0036(9) C30 0.0310(11) 0.0249(10) 0.0336(10) -0.0085(9) -0.0041(9) 0.0050(8) C31 0.0350(11) 0.0223(10) 0.0378(11) -0.0088(9) -0.0056(9) 0.0076(9) C32 0.0249(9) 0.0197(9) 0.0234(9) -0.0002(7) 0.0046(7) 0.0029(7) C33 0.0339(11) 0.0264(11) 0.0304(10) 0.0032(8) -0.0025(8) 0.0083(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6863(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O1 . 1.9202(13) yes Fe1 . O2 . 1.8612(13) yes Fe1 . O3 . 1.8686(13) yes Fe1 . N1 . 2.2005(15) yes Fe1 . N2 . 2.0957(16) yes O1 . C1 . 1.333(2) yes O2 . C8 . 1.342(2) yes O3 . C19 . 1.339(2) yes N1 . C6 . 1.456(2) yes N1 . C14 . 1.509(2) yes N1 . C25 . 1.484(2) yes N2 . C30 . 1.370(3) yes N2 . C32 . 1.314(2) yes N3 . C31 . 1.366(3) yes N3 . C32 . 1.338(3) yes N3 . C33 . 1.465(2) yes C1 . C2 . 1.402(3) yes C1 . C6 . 1.404(3) yes C2 . C3 . 1.389(3) yes C2 . H21 . 0.999 no C3 . C4 . 1.396(3) yes C3 . H31 . 1.000 no C4 . C5 . 1.402(3) yes C4 . C7 . 1.510(3) yes C5 . C6 . 1.387(3) yes C5 . H51 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.001 no C7 . H73 . 0.999 no C8 . C9 . 1.421(3) yes C8 . C13 . 1.409(3) yes C9 . C10 . 1.399(3) yes C9 . C15 . 1.527(3) yes C10 . C11 . 1.390(4) yes C10 . H101 . 0.999 no C11 . C12 . 1.378(4) yes C11 . H111 . 0.999 no C12 . C13 . 1.392(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.499(3) yes C14 . H141 . 0.999 no C14 . H142 . 1.001 no C15 . C16 . 1.538(3) yes C15 . C17 . 1.538(3) yes C15 . C18 . 1.541(3) yes C16 . H161 . 1.000 no C16 . H162 . 1.001 no C16 . H163 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 0.999 no C18 . H183 . 1.001 no C19 . C20 . 1.424(2) yes C19 . C24 . 1.411(3) yes C20 . C21 . 1.396(3) yes C20 . C26 . 1.536(3) yes C21 . C22 . 1.383(3) yes C21 . H211 . 0.999 no C22 . C23 . 1.386(3) yes C22 . H221 . 1.000 no C23 . C24 . 1.388(3) yes C23 . H231 . 1.000 no C24 . C25 . 1.505(2) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.538(3) yes C26 . C28 . 1.536(3) yes C26 . C29 . 1.537(3) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C29 . H291 . 1.001 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . C31 . 1.355(3) yes C30 . H301 . 1.001 no C31 . H311 . 1.000 no C32 . H321 . 1.002 no C33 . H331 . 1.000 no C33 . H332 . 1.000 no C33 . H333 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Fe1 . O2 . 130.67(6) yes O1 . Fe1 . O3 . 117.15(6) yes O2 . Fe1 . O3 . 111.37(6) yes O1 . Fe1 . N1 . 80.68(6) yes O2 . Fe1 . N1 . 90.77(6) yes O3 . Fe1 . N1 . 90.47(6) yes O1 . Fe1 . N2 . 87.90(6) yes O2 . Fe1 . N2 . 92.53(6) yes O3 . Fe1 . N2 . 99.69(6) yes N1 . Fe1 . N2 . 167.32(6) yes Fe1 . O1 . C1 . 117.36(12) yes Fe1 . O2 . C8 . 133.67(13) yes Fe1 . O3 . C19 . 128.59(11) yes Fe1 . N1 . C6 . 105.80(11) yes Fe1 . N1 . C14 . 107.05(11) yes C6 . N1 . C14 . 107.78(14) yes Fe1 . N1 . C25 . 109.84(11) yes C6 . N1 . C25 . 114.53(15) yes C14 . N1 . C25 . 111.44(14) yes Fe1 . N2 . C30 . 128.16(13) yes Fe1 . N2 . C32 . 124.54(13) yes C30 . N2 . C32 . 106.04(16) yes C31 . N3 . C32 . 107.03(16) yes C31 . N3 . C33 . 126.96(17) yes C32 . N3 . C33 . 125.99(17) yes O1 . C1 . C2 . 122.60(18) yes O1 . C1 . C6 . 119.53(17) yes C2 . C1 . C6 . 117.87(18) yes C1 . C2 . C3 . 120.2(2) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 119.9 no C2 . C3 . C4 . 122.04(19) yes C2 . C3 . H31 . 119.0 no C4 . C3 . H31 . 119.0 no C3 . C4 . C5 . 117.75(19) yes C3 . C4 . C7 . 121.5(2) yes C5 . C4 . C7 . 120.7(2) yes C4 . C5 . C6 . 120.6(2) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 119.8 no N1 . C6 . C1 . 114.62(16) yes N1 . C6 . C5 . 123.67(18) yes C1 . C6 . C5 . 121.57(19) yes C4 . C7 . H71 . 109.5 no C4 . C7 . H72 . 109.4 no H71 . C7 . H72 . 109.4 no C4 . C7 . H73 . 109.6 no H71 . C7 . H73 . 109.6 no H72 . C7 . H73 . 109.4 no O2 . C8 . C9 . 120.42(18) yes O2 . C8 . C13 . 119.07(18) yes C9 . C8 . C13 . 120.48(18) yes C8 . C9 . C10 . 117.1(2) yes C8 . C9 . C15 . 120.97(17) yes C10 . C9 . C15 . 121.9(2) yes C9 . C10 . C11 . 122.3(2) yes C9 . C10 . H101 . 118.9 no C11 . C10 . H101 . 118.8 no C10 . C11 . C12 . 119.7(2) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.5(2) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 119.7 no C8 . C13 . C12 . 119.8(2) yes C8 . C13 . C14 . 120.29(17) yes C12 . C13 . C14 . 119.71(19) yes N1 . C14 . C13 . 115.28(15) yes N1 . C14 . H141 . 108.1 no C13 . C14 . H141 . 108.0 no N1 . C14 . H142 . 108.0 no C13 . C14 . H142 . 107.9 no H141 . C14 . H142 . 109.5 no C9 . C15 . C16 . 110.70(16) yes C9 . C15 . C17 . 109.54(18) yes C16 . C15 . C17 . 110.57(18) yes C9 . C15 . C18 . 112.03(19) yes C16 . C15 . C18 . 106.41(19) yes C17 . C15 . C18 . 107.52(18) yes C15 . C16 . H161 . 109.6 no C15 . C16 . H162 . 109.4 no H161 . C16 . H162 . 109.4 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.4 no C15 . C17 . H171 . 109.6 no C15 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.4 no C15 . C18 . H181 . 109.5 no C15 . C18 . H182 . 109.4 no H181 . C18 . H182 . 109.6 no C15 . C18 . H183 . 109.3 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no O3 . C19 . C20 . 120.50(16) yes O3 . C19 . C24 . 119.17(16) yes C20 . C19 . C24 . 120.31(17) yes C19 . C20 . C21 . 117.23(17) yes C19 . C20 . C26 . 120.70(17) yes C21 . C20 . C26 . 122.03(16) yes C20 . C21 . C22 . 122.50(18) yes C20 . C21 . H211 . 118.7 no C22 . C21 . H211 . 118.8 no C21 . C22 . C23 . 119.60(19) yes C21 . C22 . H221 . 120.2 no C23 . C22 . H221 . 120.2 no C22 . C23 . C24 . 120.63(18) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.6 no C19 . C24 . C23 . 119.67(16) yes C19 . C24 . C25 . 119.51(16) yes C23 . C24 . C25 . 120.65(16) yes C24 . C25 . N1 . 112.93(14) yes C24 . C25 . H251 . 108.6 no N1 . C25 . H251 . 108.6 no C24 . C25 . H252 . 108.6 no N1 . C25 . H252 . 108.7 no H251 . C25 . H252 . 109.4 no C20 . C26 . C27 . 110.71(15) yes C20 . C26 . C28 . 110.31(16) yes C27 . C26 . C28 . 109.52(18) yes C20 . C26 . C29 . 111.50(17) yes C27 . C26 . C29 . 106.98(17) yes C28 . C26 . C29 . 107.72(16) yes C26 . C27 . H271 . 109.5 no C26 . C27 . H272 . 109.5 no H271 . C27 . H272 . 109.5 no C26 . C27 . H273 . 109.5 no H271 . C27 . H273 . 109.4 no H272 . C27 . H273 . 109.4 no C26 . C28 . H281 . 109.5 no C26 . C28 . H282 . 109.5 no H281 . C28 . H282 . 109.5 no C26 . C28 . H283 . 109.4 no H281 . C28 . H283 . 109.5 no H282 . C28 . H283 . 109.5 no C26 . C29 . H291 . 109.5 no C26 . C29 . H292 . 109.5 no H291 . C29 . H292 . 109.4 no C26 . C29 . H293 . 109.5 no H291 . C29 . H293 . 109.4 no H292 . C29 . H293 . 109.5 no N2 . C30 . C31 . 109.02(18) yes N2 . C30 . H301 . 125.5 no C31 . C30 . H301 . 125.5 no N3 . C31 . C30 . 106.55(18) yes N3 . C31 . H311 . 126.7 no C30 . C31 . H311 . 126.7 no N3 . C32 . N2 . 111.36(17) yes N3 . C32 . H321 . 124.3 no N2 . C32 . H321 . 124.3 no N3 . C33 . H331 . 109.5 no N3 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.5 no N3 . C33 . H333 . 109.4 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no