# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- kn432.cif' # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Dr. Birgit Weber' _publ_contact_author_address ; Anorganische Chemie II Universit\"at Bayreuth Universit\"atsstra\&se 30, NW 1 D-95440 Bayreuth Germany ; _publ_contact_author_email weber@uni-bayreuth.de _publ_contact_author_fax +49-921-552157 _publ_contact_author_phone +49-921-552555 _publ_contact_letter ; Submission dated :2012-03-29 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as part of a journal submission to Chemical Communications Birgit Weber. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; A Ladder type Iron(II) Coordination Polymer with Cooperative Spin Transition ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' W.Bauer ; Anorganische Chemie II Universit\"at Bayreuth Universit\"atsstra\&se 30, NW 1 D-95440 Bayreuth Germany ; S.Schlamp ; Anorganische Chemie II Universit\"at Bayreuth Universit\"atsstra\&se 30, NW 1 D-95440 Bayreuth Germany ; B.Weber ; Anorganische Chemie II Universit\"at Bayreuth Universit\"atsstra\&se 30, NW 1 D-95440 Bayreuth Germany ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# #:---------------------------------------------------------------------------- #:------------------------------CRYSTAL SOURCE-------------------------------- #:---------------------------------------------------------------------------- data_kn432 _database_code_depnum_ccdc_archive 'CCDC 873866' _audit_update_record 15-Aug-2012 _chemical_name_common Fe7abpea _chemical_compound_source ; Crystals formed by slow diffusion from the reaction of Fe7a(MeOH)with bpea in methanol. ; _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Albrecht, S.' #?# X-ray operator _audit_creation_date 12-Sept-06 #?# style: 18-Aug-1998 _diffrn_ambient_temperature 200(2) #?# in K _diffrn_source_type 'FR 591 generator' _diffrn_source_power 3.025 #?# in kW _diffrn_source_voltage 55.00 #?# in kV _diffrn_source_current 55.00 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? # 'no? crystal decay in terms of mean intensity per image' #?# Source instability, crystal motion, degradation, formation of ice _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0009697 _diffrn_orient_matrix_UB_12 -0.0234243 _diffrn_orient_matrix_UB_13 -0.0343298 _diffrn_orient_matrix_UB_21 0.0723464 _diffrn_orient_matrix_UB_22 0.0055671 _diffrn_orient_matrix_UB_23 -0.0016036 _diffrn_orient_matrix_UB_31 0.0084472 _diffrn_orient_matrix_UB_32 -0.0449904 _diffrn_orient_matrix_UB_33 0.0176754 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _cell_length_a 13.7280(9) _cell_length_b 19.5970(13) _cell_length_c 25.8760(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6961.4(7) _cell_measurement_temperature 200(2) #?# in K _cell_measurement_reflns_used 21174 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? #?# supposed (pseudo-)symmetries,subcells,deviation from standard setting loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.060000 -1 0 0 0.080000 0 1 0 0.040000 0 -1 0 0.025000 0 0 1 0.030000 0 0 -1 0.020000 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 37138 #xl _diffrn_reflns_av_R_equivalents 0.1965 #xl _diffrn_reflns_av_sigmaI/netI 0.2303 #xl _diffrn_reflns_limit_h_min -17 #xl _diffrn_reflns_limit_h_max 17 #xl _diffrn_reflns_limit_k_min -23 #xl _diffrn_reflns_limit_k_max 25 #xl _diffrn_reflns_limit_l_min -33 #xl _diffrn_reflns_limit_l_max 32 #xl _diffrn_reflns_theta_min 3.15 #xl _diffrn_reflns_theta_max 27.52 #xl _diffrn_measured_fraction_theta_max 0.994 #xl _diffrn_reflns_theta_full 27.52 #xl _diffrn_measured_fraction_theta_full 0.994 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I 2 2 2' _symmetry_Int_Tables_number ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 7968 #xl _reflns_number_gt 2946 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #xl _refine_ls_abs_structure_Flack 0.43(6) #xl _refine_ls_number_reflns 7968 #xl _refine_ls_number_parameters 348 #xl _refine_ls_number_restraints 1 #xl _refine_ls_R_factor_all 0.2688 #xl _refine_ls_R_factor_gt 0.0857 #xl _refine_ls_wR_factor_ref 0.2841 #xl _refine_ls_wR_factor_gt 0.2040 #xl _refine_ls_goodness_of_fit_ref 0.980 #xl _refine_ls_restrained_S_all 0.980 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.619 #xl _refine_diff_density_min -0.554 #xl _refine_diff_density_rms 0.087 #xl _refine_special_details ; twin axis: [-1-1-1], volume fraction of the twin component from refinement: 0.43408 The remaining residue densities cannot be assigned to any solvent molecule - probably because they are strongly disordered details of H atom refinement: C-bonded H: constr O-bonded H: not considered Solvent-bonded H: not considered disorder: Disorder was observed for one of the pyridin rings and the ethylene group of the bispyridylethan axial ligand. This (approx. 50:50) disorder was refined by setting a free variable. The disordered atoms were not set anisotrop. solvent molecules: The solvent atoms were left isotrop, free variables were set to deterime the occupancies, H-atoms were not considered. terminal carbon C18 of ethyl ester group: During the structure refinement difficulties were encountered for the terminal carbon C18 of the ethyl ester group of the schiff base ligand (large U compared to neighbours) thus a free variable was set to allow for partial occupancies. A chemical explanation might be, that a partial replacement of the ethyl ester group by a methyl group did occur during the complex synthesis with methanol as solvent. Such a behaviour was already frequently observed for iron complexes of this ligand type. ; #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). #-- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.06310(6) 0.24989(12) 0.34532(3) 0.0448(3) Uani 1 1 d . . . O1 O 0.0734(7) 0.3363(4) 0.3027(3) 0.048(2) Uani 1 1 d . . . O2 O 0.0747(7) 0.1643(5) 0.3013(3) 0.058(3) Uani 1 1 d . . . O3 O 0.1786(9) 0.5291(4) 0.3424(4) 0.090(4) Uani 1 1 d . . . O4 O 0.1600(11) 0.5017(6) 0.4253(4) 0.116(5) Uani 1 1 d . . . O5 O 0.1830(10) -0.0272(4) 0.3436(3) 0.095(4) Uani 1 1 d . . . O6 O 0.1520(8) -0.0030(5) 0.4265(3) 0.068(3) Uani 1 1 d . . . N1 N 0.0567(9) 0.3173(5) 0.4083(3) 0.042(3) Uani 1 1 d . . . N2 N 0.0535(9) 0.1822(5) 0.4083(3) 0.043(3) Uani 1 1 d . . . N3 N -0.0946(3) 0.2504(7) 0.33348(18) 0.0453(13) Uani 1 1 d . . . C1 C 0.1000(9) 0.3960(7) 0.3129(5) 0.050(4) Uani 1 1 d . . . C2 C 0.1060(9) 0.4184(6) 0.3652(6) 0.053(4) Uani 1 1 d . . . C3 C 0.0810(11) 0.3788(7) 0.4081(4) 0.057(4) Uani 1 1 d . . . H3 H 0.0827 0.4006 0.4400 0.068 Uiso 1 1 calc R . . C4 C 0.0237(10) 0.2855(6) 0.4542(5) 0.047(4) Uani 1 1 d . . . C5 C 0.0280(8) 0.2133(7) 0.4566(4) 0.040(3) Uani 1 1 d . . . C6 C 0.0867(9) 0.1179(6) 0.4081(5) 0.044(4) Uani 1 1 d . . . H6 H 0.0903 0.0963 0.4401 0.053 Uiso 1 1 calc R . . C7 C 0.1179(10) 0.0782(6) 0.3638(5) 0.047(3) Uani 1 1 d . . . C8 C 0.1017(10) 0.1029(6) 0.3129(5) 0.050(4) Uani 1 1 d . . . C9 C 0.0000 0.3165(9) 0.5000 0.054(6) Uani 1 2 d S . . H9 H 0.0000 0.3639 0.5000 0.065 Uiso 1 2 calc SR . . C10 C 0.0000 0.1775(8) 0.5000 0.032(4) Uani 1 2 d S . . H10 H 0.0000 0.1301 0.5000 0.039 Uiso 1 2 calc SR . . C11 C 0.1235(11) 0.4401(6) 0.2686(5) 0.067(5) Uani 1 1 d . . . H11A H 0.1913 0.4353 0.2601 0.101 Uiso 1 1 calc R . . H11B H 0.1101 0.4868 0.2773 0.101 Uiso 1 1 calc R . . H11C H 0.0846 0.4270 0.2394 0.101 Uiso 1 1 calc R . . C12 C 0.1525(12) 0.4915(7) 0.3738(6) 0.065(4) Uani 1 1 d . . . C13 C 0.1881(13) 0.5693(7) 0.4396(5) 0.087(5) Uani 1 1 d . . . H13A H 0.1747 0.6021 0.4124 0.104 Uiso 1 1 calc R . . H13B H 0.1569 0.5839 0.4714 0.104 Uiso 1 1 calc R . . C14 C 0.288(2) 0.5584(12) 0.4461(14) 0.42(3) Uani 1 1 d . . . H14A H 0.3050 0.5147 0.4321 0.625 Uiso 1 1 calc R . . H14B H 0.3034 0.5595 0.4823 0.625 Uiso 1 1 calc R . . H14C H 0.3235 0.5935 0.4285 0.625 Uiso 1 1 calc R . . C15 C 0.1217(12) 0.0591(8) 0.2646(5) 0.081(5) Uani 1 1 d . . . H15A H 0.1158 0.0868 0.2342 0.121 Uiso 1 1 calc R . . H15B H 0.0753 0.0224 0.2630 0.121 Uiso 1 1 calc R . . H15C H 0.1864 0.0406 0.2665 0.121 Uiso 1 1 calc R . . C16 C 0.1503(12) 0.0163(7) 0.3751(5) 0.061(4) Uani 1 1 d . . . C17 C 0.2062(15) -0.0663(8) 0.4402(7) 0.111(7) Uani 1 1 d D . . H17A H 0.1855 -0.1024 0.4171 0.133 Uiso 1 1 calc R . . H17B H 0.1875 -0.0796 0.4750 0.133 Uiso 1 1 calc R . . C18 C 0.316(2) -0.062(2) 0.4381(13) 0.071(13) Uiso 0.30(3) 1 d PD . . H18A H 0.3433 -0.1049 0.4474 0.106 Uiso 0.30(3) 1 calc PR . . H18B H 0.3376 -0.0273 0.4619 0.106 Uiso 0.30(3) 1 calc PR . . H18C H 0.3355 -0.0497 0.4037 0.106 Uiso 0.30(3) 1 calc PR . . C20 C -0.1479(10) 0.1919(7) 0.3302(5) 0.056(4) Uani 1 1 d . . . H20 H -0.1161 0.1500 0.3295 0.067 Uiso 1 1 calc R . . C21 C -0.2457(12) 0.1937(8) 0.3279(6) 0.069(5) Uani 1 1 d . . . H21 H -0.2781 0.1521 0.3263 0.082 Uiso 1 1 calc R . . C22 C -0.2984(5) 0.2478(11) 0.3278(3) 0.0546(18) Uani 1 1 d . . . C23 C -0.2459(8) 0.3123(7) 0.3301(5) 0.052(4) Uani 1 1 d . . . H23 H -0.2778 0.3541 0.3293 0.062 Uiso 1 1 calc R . . C24 C -0.1439(10) 0.3074(6) 0.3336(5) 0.050(4) Uani 1 1 d . . . H24 H -0.1088 0.3479 0.3361 0.060 Uiso 1 1 calc R . . N4A N -0.7728(5) 0.2410(7) 0.3513(4) 0.021(4) Uiso 0.481(9) 1 d PG . 1 C27A C -0.7213(6) 0.2387(7) 0.3050(3) 0.044(4) Uiso 0.481(9) 1 d PG . 1 H27A H -0.7542 0.2421 0.2737 0.052 Uiso 0.481(9) 1 calc PR . 1 C28A C -0.6206(6) 0.2312(6) 0.3056(4) 0.055(5) Uiso 0.481(9) 1 d PG . 1 H28A H -0.5861 0.2297 0.2747 0.066 Uiso 0.481(9) 1 calc PR . 1 C29A C -0.5714(6) 0.2261(7) 0.3524(5) 0.046(6) Uiso 0.481(9) 1 d PG . 1 C30A C -0.6229(9) 0.2284(9) 0.3986(4) 0.087(10) Uiso 0.481(9) 1 d PG . 1 H30A H -0.5900 0.2249 0.4299 0.105 Uiso 0.481(9) 1 calc PR . 1 C31A C -0.7236(9) 0.2358(9) 0.3981(3) 0.113(12) Uiso 0.481(9) 1 d PG . 1 H31A H -0.7581 0.2374 0.4290 0.136 Uiso 0.481(9) 1 calc PR . 1 C26A C -0.4619(12) 0.1971(9) 0.3471(7) 0.045(5) Uiso 0.481(9) 1 d P . 1 H26A H -0.4407 0.1806 0.3806 0.054 Uiso 0.481(9) 1 calc PR . 1 H26B H -0.4625 0.1585 0.3236 0.054 Uiso 0.481(9) 1 calc PR . 1 C25A C -0.4084(19) 0.2347(14) 0.3330(9) 0.071(9) Uiso 0.481(9) 1 d P . 1 H25A H -0.4295 0.2756 0.3508 0.086 Uiso 0.481(9) 1 calc PR . 1 H25B H -0.4300 0.2412 0.2976 0.086 Uiso 0.481(9) 1 calc PR . 1 N4B N -0.7728(6) 0.2673(7) 0.3446(4) 0.059(6) Uiso 0.519(9) 1 d PG . 2 C27B C -0.7225(9) 0.2870(7) 0.3005(4) 0.062(5) Uiso 0.519(9) 1 d PG . 2 H27B H -0.7558 0.2929 0.2695 0.074 Uiso 0.519(9) 1 calc PR . 2 C28B C -0.6226(9) 0.2980(7) 0.3026(4) 0.068(6) Uiso 0.519(9) 1 d PG . 2 H28B H -0.5889 0.3112 0.2731 0.081 Uiso 0.519(9) 1 calc PR . 2 C29B C -0.5729(6) 0.2892(7) 0.3490(5) 0.072(7) Uiso 0.519(9) 1 d PG . 2 C30B C -0.6231(7) 0.2695(6) 0.3931(4) 0.048(6) Uiso 0.519(9) 1 d PG . 2 H30B H -0.5899 0.2636 0.4241 0.058 Uiso 0.519(9) 1 calc PR . 2 C31B C -0.7231(7) 0.2585(7) 0.3910(3) 0.038(4) Uiso 0.519(9) 1 d PG . 2 H31B H -0.7567 0.2453 0.4205 0.045 Uiso 0.519(9) 1 calc PR . 2 C26B C -0.4645(19) 0.2807(13) 0.3568(10) 0.102(10) Uiso 0.519(9) 1 d P . 2 H26C H -0.4382 0.3252 0.3653 0.122 Uiso 0.519(9) 1 calc PR . 2 H26D H -0.4555 0.2520 0.3870 0.122 Uiso 0.519(9) 1 calc PR . 2 C25B C -0.4076(12) 0.2542(16) 0.3181(7) 0.052(5) Uiso 0.519(9) 1 d P . 2 H25C H -0.4166 0.2823 0.2876 0.062 Uiso 0.519(9) 1 calc PR . 2 H25D H -0.4323 0.2091 0.3099 0.062 Uiso 0.519(9) 1 calc PR . 2 O10 O -0.6399(11) 0.2553(10) 0.5236(5) 0.235(5) Uiso 1 1 d . . . C40 C -0.7484(16) 0.2373(15) 0.5266(7) 0.206(8) Uiso 1 1 d . . . O11 O -0.597(2) 0.4366(13) 0.3440(10) 0.293(16) Uiso 0.76(3) 1 d P . . C41 C -0.533(2) 0.4380(15) 0.3920(12) 0.216(16) Uiso 0.76(3) 1 d P . . O12 O -0.5000 0.3562(15) 0.5000 0.312(14) Uiso 1 2 d S . . 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 0.0407(5) 0.0466(6) 0.0472(5) -0.0005(13) 0.0009(4) -0.0002(14) O1 0.055(7) 0.048(5) 0.041(5) 0.007(4) 0.011(5) -0.004(6) O2 0.050(7) 0.068(6) 0.056(6) -0.008(5) -0.010(6) 0.011(6) O3 0.133(11) 0.041(6) 0.097(8) 0.004(6) 0.033(9) -0.033(6) O4 0.201(14) 0.082(7) 0.065(7) -0.023(6) 0.030(8) -0.083(9) O5 0.160(13) 0.072(8) 0.054(6) -0.002(5) 0.018(9) 0.036(7) O6 0.084(6) 0.050(5) 0.069(6) -0.002(5) 0.007(6) 0.011(5) N1 0.042(7) 0.041(6) 0.042(7) 0.000(5) -0.005(6) -0.001(6) N2 0.034(7) 0.050(7) 0.047(7) -0.003(5) 0.006(6) 0.002(6) N3 0.040(3) 0.044(3) 0.052(3) 0.007(8) 0.001(2) 0.011(8) C1 0.036(9) 0.071(9) 0.041(8) 0.009(7) 0.010(7) 0.021(7) C2 0.037(7) 0.049(8) 0.073(10) -0.008(7) 0.006(7) 0.002(6) C3 0.074(11) 0.065(9) 0.031(7) 0.019(6) 0.001(7) -0.013(8) C4 0.067(10) 0.029(7) 0.045(8) -0.011(6) 0.004(7) 0.001(7) C5 0.016(6) 0.067(9) 0.038(7) -0.013(6) -0.003(5) 0.002(6) C6 0.034(8) 0.041(7) 0.058(9) 0.022(6) 0.006(7) -0.002(6) C7 0.059(8) 0.034(7) 0.047(7) -0.001(6) 0.015(6) 0.013(6) C8 0.039(9) 0.040(7) 0.071(10) -0.010(7) 0.001(8) 0.020(6) C9 0.059(14) 0.043(11) 0.059(13) 0.000 -0.017(11) 0.000 C10 0.033(10) 0.031(9) 0.033(9) 0.000 0.015(8) 0.000 C11 0.091(13) 0.051(9) 0.060(8) 0.011(7) 0.018(9) -0.011(9) C12 0.074(11) 0.034(7) 0.088(11) -0.023(7) 0.019(10) -0.020(7) C13 0.119(13) 0.074(10) 0.067(9) -0.022(8) 0.023(9) -0.052(9) C14 0.29(4) 0.17(2) 0.79(8) -0.07(3) -0.35(5) -0.03(3) C15 0.095(14) 0.065(11) 0.081(11) -0.013(9) -0.017(10) 0.005(11) C16 0.074(11) 0.068(10) 0.040(7) -0.023(7) 0.006(8) -0.011(8) C17 0.157(19) 0.064(10) 0.111(13) 0.005(10) -0.035(13) 0.024(12) C20 0.032(8) 0.046(8) 0.090(11) 0.004(8) -0.012(8) -0.007(7) C21 0.088(13) 0.042(9) 0.076(12) -0.002(7) -0.017(9) -0.018(9) C22 0.043(4) 0.057(5) 0.064(4) -0.008(11) 0.000(3) 0.005(11) C23 0.021(7) 0.061(9) 0.074(10) 0.002(7) 0.007(6) 0.006(6) C24 0.051(9) 0.044(8) 0.055(8) 0.009(6) 0.016(7) -0.012(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 2.026(7) . ? Fe1 O2 2.034(8) . ? Fe1 N1 2.100(9) . ? Fe1 N2 2.105(9) . ? Fe1 N3 2.186(5) . ? Fe1 N4A 2.265(8) 1_655 ? Fe1 N4B 2.279(8) 1_655 ? O1 C1 1.254(14) . ? O2 C8 1.295(13) . ? O3 C12 1.153(16) . ? O4 C12 1.352(13) . ? O4 C13 1.428(16) . ? O5 C16 1.261(14) . ? O6 C16 1.382(12) . ? O6 C17 1.490(17) . ? N1 C3 1.251(13) . ? N1 C4 1.415(14) . ? N2 C6 1.340(13) . ? N2 C5 1.433(13) . ? N3 C24 1.308(15) . ? N3 C20 1.362(15) . ? C1 C2 1.424(16) . ? C1 C11 1.474(14) . ? C2 C3 1.396(16) . ? C2 C12 1.585(17) . ? C4 C9 1.372(13) . ? C4 C5 1.417(9) . ? C5 C10 1.380(14) . ? C6 C7 1.450(15) . ? C7 C16 1.325(17) . ? C7 C8 1.422(16) . ? C8 C15 1.539(15) . ? C9 C4 1.372(13) 4_556 ? C10 C5 1.380(14) 4_556 ? C13 C14 1.40(3) . ? C17 C18 1.505(18) . ? C20 C21 1.344(19) . ? C21 C22 1.283(18) . ? C22 C23 1.456(18) . ? C22 C25B 1.525(18) . ? C22 C25A 1.54(3) . ? C23 C24 1.406(16) . ? N4A C27A 1.3900 . ? N4A C31A 1.3900 . ? N4A Fe1 2.265(8) 1_455 ? C27A C28A 1.3900 . ? C28A C29A 1.3900 . ? C29A C30A 1.3900 . ? C29A C26A 1.613(19) . ? C30A C31A 1.3900 . ? C26A C25A 1.10(3) . ? N4B C27B 1.3900 . ? N4B C31B 1.3900 . ? N4B Fe1 2.279(8) 1_455 ? C27B C28B 1.3900 . ? C28B C29B 1.3900 . ? C29B C30B 1.3900 . ? C29B C26B 1.51(3) . ? C30B C31B 1.3900 . ? C26B C25B 1.37(3) . ? O10 C40 1.53(2) . ? O11 C41 1.52(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 112.23(18) . . ? O1 Fe1 N1 84.3(3) . . ? O2 Fe1 N1 163.1(4) . . ? O1 Fe1 N2 162.3(3) . . ? O2 Fe1 N2 85.4(4) . . ? N1 Fe1 N2 78.04(19) . . ? O1 Fe1 N3 89.4(4) . . ? O2 Fe1 N3 90.1(4) . . ? N1 Fe1 N3 93.7(4) . . ? N2 Fe1 N3 92.8(4) . . ? O1 Fe1 N4A 91.8(5) . 1_655 ? O2 Fe1 N4A 84.1(4) . 1_655 ? N1 Fe1 N4A 92.1(4) . 1_655 ? N2 Fe1 N4A 87.8(5) . 1_655 ? N3 Fe1 N4A 174.1(4) . 1_655 ? O1 Fe1 N4B 78.5(5) . 1_655 ? O2 Fe1 N4B 92.4(5) . 1_655 ? N1 Fe1 N4B 87.3(5) . 1_655 ? N2 Fe1 N4B 99.3(5) . 1_655 ? N3 Fe1 N4B 167.7(4) . 1_655 ? N4A Fe1 N4B 13.7(4) 1_655 1_655 ? C1 O1 Fe1 133.2(8) . . ? C8 O2 Fe1 131.3(8) . . ? C12 O4 C13 114.4(11) . . ? C16 O6 C17 117.8(12) . . ? C3 N1 C4 120.9(10) . . ? C3 N1 Fe1 126.2(9) . . ? C4 N1 Fe1 112.8(7) . . ? C6 N2 C5 119.1(10) . . ? C6 N2 Fe1 124.6(8) . . ? C5 N2 Fe1 114.9(7) . . ? C24 N3 C20 116.2(6) . . ? C24 N3 Fe1 121.0(10) . . ? C20 N3 Fe1 122.5(9) . . ? O1 C1 C2 120.4(12) . . ? O1 C1 C11 116.5(11) . . ? C2 C1 C11 123.1(13) . . ? C3 C2 C1 124.7(12) . . ? C3 C2 C12 119.3(12) . . ? C1 C2 C12 115.8(13) . . ? N1 C3 C2 127.2(12) . . ? C9 C4 N1 127.3(12) . . ? C9 C4 C5 114.5(14) . . ? N1 C4 C5 117.6(12) . . ? C10 C5 C4 122.1(13) . . ? C10 C5 N2 124.2(11) . . ? C4 C5 N2 113.4(12) . . ? N2 C6 C7 127.4(11) . . ? C16 C7 C8 124.6(12) . . ? C16 C7 C6 114.6(11) . . ? C8 C7 C6 120.3(11) . . ? O2 C8 C7 125.1(12) . . ? O2 C8 C15 112.4(11) . . ? C7 C8 C15 122.3(10) . . ? C4 C9 C4 127.4(17) . 4_556 ? C5 C10 C5 118.9(15) 4_556 . ? O3 C12 O4 125.2(13) . . ? O3 C12 C2 127.1(13) . . ? O4 C12 C2 107.6(12) . . ? C14 C13 O4 98.9(17) . . ? O5 C16 C7 126.6(12) . . ? O5 C16 O6 115.5(13) . . ? C7 C16 O6 117.8(12) . . ? O6 C17 C18 116(2) . . ? C21 C20 N3 121.2(13) . . ? C22 C21 C20 125.8(14) . . ? C21 C22 C23 115.9(7) . . ? C21 C22 C25B 128(2) . . ? C23 C22 C25B 115.0(18) . . ? C21 C22 C25A 114.6(19) . . ? C23 C22 C25A 128.9(16) . . ? C24 C23 C22 115.9(11) . . ? N3 C24 C23 125.0(12) . . ? C27A N4A C31A 120.0 . . ? C27A N4A Fe1 116.8(5) . 1_455 ? C31A N4A Fe1 123.2(5) . 1_455 ? N4A C27A C28A 120.0 . . ? C27A C28A C29A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A C26A 124.0(10) . . ? C28A C29A C26A 113.8(10) . . ? C31A C30A C29A 120.0 . . ? C30A C31A N4A 120.0 . . ? C25A C26A C29A 114(2) . . ? C26A C25A C22 143(3) . . ? C27B N4B C31B 120.0 . . ? C27B N4B Fe1 122.6(6) . 1_455 ? C31B N4B Fe1 117.4(6) . 1_455 ? N4B C27B C28B 120.0 . . ? C29B C28B C27B 120.0 . . ? C28B C29B C30B 120.0 . . ? C28B C29B C26B 127.8(13) . . ? C30B C29B C26B 110.4(12) . . ? C31B C30B C29B 120.0 . . ? C30B C31B N4B 120.0 . . ? C25B C26B C29B 120(2) . . ? C26B C25B C22 118.1(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L7a_bpea_kn432_weber _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? #?# style: 'lithium meso-oxolanediolate monohydrate' _chemical_formula_moiety 'C28 H34 Fe N4 O6, 2(C H4 O), 0.25(H2 O)' _chemical_formula_sum 'C30 H42.5 Fe N4 O8.25' _chemical_formula_weight 647.02 _chemical_melting_point ? #?# in K! _cell_formula_units_Z 8 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.21838 #?# include sigma (s) from: s(rho)=s(V)/V*rho _exptl_crystal_F_000 2672