Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Larsen, Finn Krebs' 'Arion, Vladimir' 'Bousseksou, Azzedine' 'Gerbeleu, Nichole V.' 'Overgaard, Jacob' 'Rentschler, Eva' 'Timco, Grigore A.' 'Tuchagues, Jean-pierre' _publ_contact_author_name 'Prof Finn Krebs Larsen' _publ_contact_author_address ; Department of Chemistry University of Aarhus Langelandsgade 140 Aarhus DK-8000 DENMARK ; _publ_contact_author_email 'KRE@CHEM.AU.DK' _publ_contact_author_fax '+45 8619 6199' _publ_contact_author_phone '+45 8942 3897' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Multi-Temperature X-ray Diffraction, Mossbauer Spectroscopy and Magnetic Susceptibility Studies of a Solvated Mixed-Valence Trinuclear Iron Formate, [Fe3O(HCO2)6(NC5H4CH3)3]1.3(NC5H4CH3) ; data_p87_100 _database_code_CSD 173994 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.76 H27 Fe3 N4.29 O13' _chemical_formula_weight 844.40 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' #============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.291(3) _cell_length_b 27.373(4) _cell_length_c 12.4263(18) _cell_angle_alpha 90.00 _cell_angle_beta 96.796(4) _cell_angle_gamma 90.00 _cell_volume 8204(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2910 _cell_measurement_theta_min 2.689 _cell_measurement_theta_max 31.523 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3437 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS, Sheldrick 1996)' #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none' _diffrn_reflns_number 45240 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 32.11 _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 32.11 _diffrn_measured_fraction_theta_full 0.870 _reflns_number_total 12517 _reflns_number_gt 8306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'SAINT+ V5.01 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1229P)^2^+55.4831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12517 _refine_ls_number_parameters 454 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2373 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.080 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 2.198 _refine_diff_density_min -0.747 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.35999(2) 0.22693(2) 0.36304(4) 0.01884(14) Uani 1 1 d . . . Fe2 Fe 0.23410(2) 0.226560(18) 0.24025(4) 0.01637(13) Uani 1 1 d . . . Fe3 Fe 0.29513(2) 0.12063(2) 0.30857(4) 0.02125(14) Uani 1 1 d . . . O1 O 0.29613(10) 0.19446(9) 0.30539(19) 0.0178(5) Uani 1 1 d . . . O2 O 0.21313(13) 0.11508(11) 0.3519(3) 0.0314(6) Uani 1 1 d . . . O3 O 0.17487(11) 0.18740(10) 0.3033(2) 0.0236(5) Uani 1 1 d . . . O4 O 0.26604(15) 0.11589(11) 0.1395(2) 0.0337(7) Uani 1 1 d . . . O5 O 0.22348(12) 0.18744(10) 0.1018(2) 0.0240(5) Uani 1 1 d . . . O6 O 0.41691(12) 0.18608(12) 0.2959(2) 0.0285(6) Uani 1 1 d . . . O7 O 0.37725(13) 0.11276(12) 0.2673(3) 0.0365(7) Uani 1 1 d . . . O8 O 0.37370(11) 0.18899(11) 0.5029(2) 0.0242(6) Uani 1 1 d . . . O9 O 0.32466(13) 0.11912(11) 0.4774(2) 0.0308(6) Uani 1 1 d . . . O10 O 0.31907(11) 0.28115(10) 0.4346(2) 0.0248(6) Uani 1 1 d . . . O11 O 0.23017(11) 0.27672(10) 0.3607(2) 0.0227(5) Uani 1 1 d . . . O12 O 0.36555(12) 0.27285(11) 0.2333(2) 0.0266(6) Uani 1 1 d . . . O13 O 0.27674(11) 0.27699(10) 0.1592(2) 0.0226(5) Uani 1 1 d . . . C1 C 0.17447(16) 0.14446(14) 0.3399(3) 0.0246(7) Uani 1 1 d . . . H1A H 0.1409 0.1336 0.3603 0.037 Uiso 1 1 calc R . . C2 C 0.23942(18) 0.14539(14) 0.0792(3) 0.0257(8) Uani 1 1 d . . . H2A H 0.2299 0.1352 0.0081 0.039 Uiso 1 1 calc R . . C3 C 0.41555(17) 0.14197(17) 0.2678(3) 0.0295(8) Uani 1 1 d . . . H3A H 0.4479 0.1299 0.2443 0.044 Uiso 1 1 calc R . . C4 C 0.35560(17) 0.14851(15) 0.5313(3) 0.0262(8) Uani 1 1 d . . . H4A H 0.3669 0.1393 0.6024 0.039 Uiso 1 1 calc R . . C5 C 0.26879(16) 0.29236(14) 0.4269(3) 0.0222(7) Uani 1 1 d . . . H5A H 0.2590 0.3152 0.4766 0.033 Uiso 1 1 calc R . . C6 C 0.32699(16) 0.28740(14) 0.1654(3) 0.0230(7) Uani 1 1 d . . . H6A H 0.3371 0.3087 0.1129 0.035 Uiso 1 1 calc R . . N1 N 0.43247(14) 0.26910(13) 0.4355(3) 0.0244(7) Uani 1 1 d . . . C11 C 0.43505(16) 0.28912(15) 0.5348(3) 0.0244(7) Uani 1 1 d . . . H11A H 0.4048 0.2856 0.5736 0.037 Uiso 1 1 calc R . . C12 C 0.48034(17) 0.31455(17) 0.5816(3) 0.0298(9) Uani 1 1 d . . . H12A H 0.4802 0.3277 0.6505 0.045 Uiso 1 1 calc R . . C13 C 0.52632(16) 0.32064(16) 0.5263(4) 0.0282(8) Uani 1 1 d . . . C14 C 0.52374(17) 0.30018(18) 0.4234(4) 0.0326(9) Uani 1 1 d . . . H14A H 0.5534 0.3033 0.3830 0.049 Uiso 1 1 calc R . . C15 C 0.47657(19) 0.27507(19) 0.3818(4) 0.0351(10) Uani 1 1 d . . . H15A H 0.4755 0.2616 0.3129 0.053 Uiso 1 1 calc R . . C16 C 0.57719(19) 0.3469(2) 0.5743(5) 0.0440(12) Uani 1 1 d . . . H16A H 0.5717 0.3588 0.6450 0.066 Uiso 1 1 calc R . . H16B H 0.5844 0.3740 0.5288 0.066 Uiso 1 1 calc R . . H16C H 0.6082 0.3249 0.5801 0.066 Uiso 1 1 calc R . . N2 N 0.16190(13) 0.26694(11) 0.1632(2) 0.0192(6) Uani 1 1 d . . . C21 C 0.12025(16) 0.27974(14) 0.2199(3) 0.0239(7) Uani 1 1 d . . . H21A H 0.1231 0.2721 0.2933 0.036 Uiso 1 1 calc R . . C22 C 0.07357(17) 0.30368(17) 0.1735(4) 0.0317(9) Uani 1 1 d . . . H22A H 0.0456 0.3119 0.2152 0.048 Uiso 1 1 calc R . . C23 C 0.06844(19) 0.31558(18) 0.0634(4) 0.0358(10) Uani 1 1 d . . . C24 C 0.1118(2) 0.30254(18) 0.0056(4) 0.0355(10) Uani 1 1 d . . . H24A H 0.1100 0.3096 -0.0678 0.053 Uiso 1 1 calc R . . C25 C 0.15753(17) 0.27903(14) 0.0575(3) 0.0236(7) Uani 1 1 d . . . H25A H 0.1865 0.2712 0.0180 0.035 Uiso 1 1 calc R . . C26 C 0.0182(2) 0.3415(3) 0.0105(5) 0.0601(17) Uani 1 1 d . . . H26A H -0.0072 0.3472 0.0629 0.090 Uiso 1 1 calc R . . H26B H 0.0005 0.3218 -0.0474 0.090 Uiso 1 1 calc R . . H26C H 0.0289 0.3723 -0.0180 0.090 Uiso 1 1 calc R . . N3 N 0.29454(14) 0.04146(13) 0.3082(3) 0.0266(7) Uani 1 1 d . . . C31 C 0.3090(2) 0.01638(17) 0.2241(4) 0.0400(11) Uani 1 1 d . . . H31A H 0.3204 0.0338 0.1664 0.060 Uiso 1 1 calc R . . C32 C 0.3082(3) -0.03417(17) 0.2177(5) 0.0461(13) Uani 1 1 d . . . H32A H 0.3167 -0.0499 0.1553 0.069 Uiso 1 1 calc R . . C33 C 0.2947(2) -0.06094(17) 0.3052(4) 0.0379(11) Uani 1 1 d . . . C34 C 0.2811(2) -0.03517(17) 0.3944(4) 0.0425(12) Uani 1 1 d . . . H34A H 0.2721 -0.0517 0.4553 0.064 Uiso 1 1 calc R . . C35 C 0.2812(2) 0.01555(17) 0.3921(4) 0.0392(11) Uani 1 1 d . . . H35A H 0.2715 0.0323 0.4522 0.059 Uiso 1 1 calc R . . C36 C 0.2946(3) -0.11587(18) 0.3035(6) 0.062(2) Uani 1 1 d . . . H36A H 0.2839 -0.1280 0.3704 0.093 Uiso 1 1 calc R . . H36B H 0.3311 -0.1275 0.2946 0.093 Uiso 1 1 calc R . . H36C H 0.2689 -0.1272 0.2444 0.093 Uiso 1 1 calc R . . N5 N 0.0000 0.0782(4) 0.2500 0.082(3) Uiso 0.888(16) 2 d SPD . . C51 C 0.0136(5) 0.0497(4) 0.3412(7) 0.112(4) Uiso 0.888(16) 1 d PD . . C52 C 0.0155(6) -0.0031(5) 0.3454(7) 0.128(5) Uiso 0.888(16) 1 d PD . . C53 C 0.0000 -0.0280(6) 0.2500 0.110(6) Uiso 0.888(16) 2 d SPD . . C54 C 0.0000 -0.0845(8) 0.2500 0.180(11) Uiso 0.888(16) 2 d SPD . . C41 C 0.1424(5) -0.0616(4) 0.1239(10) 0.111(4) Uiso 0.849(13) 1 d PD . . C43 C 0.1565(4) -0.0147(3) 0.1606(8) 0.079(3) Uiso 0.849(13) 1 d PD A . N7 N 0.0803(8) 0.0195(6) 0.1570(16) 0.073(8) Uiso 0.235(9) 1 d PD A 1 C75 C 0.0832(8) -0.0675(10) 0.115(2) 0.086(11) Uiso 0.235(9) 1 d PD A 1 C76 C 0.1732(15) -0.1064(10) 0.111(2) 0.087(11) Uiso 0.235(9) 1 d PD A 1 C72 C 0.1332(9) 0.0301(7) 0.1711(17) 0.058(7) Uiso 0.235(9) 1 d PD A 1 C71 C 0.0578(13) -0.0233(9) 0.132(2) 0.102(14) Uiso 0.235(9) 1 d PD . 1 N8 N 0.1419(5) -0.0983(6) 0.3009(13) 0.118(5) Uiso 0.614(11) 1 d PD A 2 C82 C 0.1536(6) -0.0097(7) 0.2726(12) 0.132(7) Uiso 0.614(11) 1 d PD A 2 C85 C 0.1426(7) -0.1046(6) 0.1903(14) 0.129(7) Uiso 0.614(11) 1 d PD A 2 C81 C 0.1481(6) -0.0523(7) 0.3359(18) 0.175(11) Uiso 0.614(11) 1 d PD A 2 C86 C 0.1585(7) 0.0300(6) 0.1021(14) 0.101(5) Uiso 0.614(11) 1 d PD A 2 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 0.0180(3) 0.0240(3) 0.0150(2) -0.00082(18) 0.00404(18) -0.00376(19) Fe2 0.0178(2) 0.0170(2) 0.0149(2) -0.00049(17) 0.00418(17) -0.00115(18) Fe3 0.0241(3) 0.0183(3) 0.0212(3) -0.00012(19) 0.00169(19) -0.0001(2) O1 0.0183(12) 0.0185(12) 0.0171(11) 0.0003(9) 0.0040(9) -0.0023(9) O2 0.0294(15) 0.0224(14) 0.0436(17) 0.0034(12) 0.0098(13) -0.0016(11) O3 0.0215(13) 0.0258(14) 0.0242(13) 0.0027(10) 0.0048(10) -0.0030(10) O4 0.0505(19) 0.0244(14) 0.0241(14) -0.0020(11) -0.0038(13) 0.0102(13) O5 0.0296(14) 0.0219(13) 0.0197(12) -0.0027(10) -0.0002(10) 0.0045(11) O6 0.0209(13) 0.0374(16) 0.0282(14) -0.0045(12) 0.0069(11) -0.0024(12) O7 0.0291(16) 0.0293(16) 0.053(2) -0.0033(14) 0.0123(14) 0.0020(13) O8 0.0217(13) 0.0317(15) 0.0189(12) 0.0011(10) 0.0013(10) -0.0055(11) O9 0.0392(17) 0.0268(15) 0.0251(14) 0.0043(11) -0.0023(12) -0.0062(12) O10 0.0214(13) 0.0297(14) 0.0236(13) -0.0062(11) 0.0040(10) -0.0048(11) O11 0.0209(13) 0.0265(14) 0.0209(12) -0.0058(10) 0.0032(10) -0.0012(10) O12 0.0251(14) 0.0338(15) 0.0211(12) 0.0033(11) 0.0034(10) -0.0087(11) O13 0.0210(13) 0.0244(13) 0.0233(12) 0.0040(10) 0.0058(10) -0.0016(10) C1 0.0251(18) 0.0253(19) 0.0250(17) 0.0010(14) 0.0092(14) -0.0067(15) C2 0.036(2) 0.0232(18) 0.0180(16) -0.0050(14) 0.0032(14) 0.0031(16) C3 0.0235(19) 0.038(2) 0.0281(19) -0.0039(17) 0.0070(15) 0.0074(17) C4 0.0277(19) 0.032(2) 0.0185(16) 0.0050(14) 0.0029(14) -0.0022(16) C5 0.0246(18) 0.0240(18) 0.0189(16) -0.0051(13) 0.0069(13) -0.0015(14) C6 0.0248(18) 0.0254(18) 0.0210(16) 0.0013(14) 0.0118(14) -0.0049(14) N1 0.0216(15) 0.0335(18) 0.0186(14) -0.0011(12) 0.0036(12) -0.0067(13) C11 0.0221(18) 0.032(2) 0.0198(16) -0.0014(14) 0.0071(13) -0.0048(15) C12 0.026(2) 0.039(2) 0.0242(18) -0.0072(16) -0.0009(15) -0.0032(17) C13 0.0193(18) 0.029(2) 0.036(2) -0.0038(16) -0.0005(15) -0.0029(15) C14 0.0212(19) 0.042(2) 0.036(2) -0.0030(18) 0.0078(16) -0.0112(17) C15 0.030(2) 0.052(3) 0.0249(19) -0.0089(18) 0.0087(16) -0.0150(19) C16 0.025(2) 0.045(3) 0.060(3) -0.015(2) -0.004(2) -0.009(2) N2 0.0215(15) 0.0173(14) 0.0194(14) -0.0013(11) 0.0046(11) -0.0007(11) C21 0.0223(18) 0.0255(19) 0.0249(17) -0.0015(14) 0.0072(14) -0.0018(14) C22 0.0197(19) 0.037(2) 0.039(2) 0.0004(18) 0.0062(16) 0.0040(16) C23 0.027(2) 0.041(3) 0.037(2) 0.0001(19) -0.0040(17) 0.0093(18) C24 0.038(2) 0.042(3) 0.0243(19) 0.0005(17) -0.0054(17) 0.010(2) C25 0.0268(19) 0.0262(19) 0.0183(16) -0.0033(14) 0.0044(13) 0.0029(15) C26 0.036(3) 0.078(4) 0.062(4) 0.005(3) -0.010(3) 0.021(3) N3 0.0290(17) 0.0219(16) 0.0279(16) 0.0027(13) -0.0004(13) 0.0015(13) C31 0.055(3) 0.024(2) 0.044(3) 0.0072(19) 0.023(2) 0.005(2) C32 0.070(4) 0.023(2) 0.051(3) 0.002(2) 0.030(3) 0.009(2) C33 0.037(2) 0.025(2) 0.054(3) 0.0065(19) 0.017(2) 0.0067(18) C34 0.066(3) 0.023(2) 0.041(3) 0.0058(18) 0.016(2) -0.004(2) C35 0.060(3) 0.027(2) 0.032(2) -0.0007(17) 0.012(2) -0.003(2) C36 0.094(5) 0.018(2) 0.082(5) 0.004(2) 0.045(4) 0.007(3) #============================================================================== # MOLECULAR GEOMETRY 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 1.859(2) . ? Fe1 O8 2.019(3) . ? Fe1 O6 2.031(3) . ? Fe1 O10 2.046(3) . ? Fe1 O12 2.062(3) . ? Fe1 N1 2.209(3) . ? Fe2 O1 1.849(3) . ? Fe2 O5 2.018(3) . ? Fe2 O3 2.024(3) . ? Fe2 O11 2.042(3) . ? Fe2 O13 2.058(3) . ? Fe2 N2 2.198(3) . ? Fe3 O1 2.021(3) . ? Fe3 O7 2.128(3) . ? Fe3 O2 2.129(3) . ? Fe3 O9 2.139(3) . ? Fe3 O4 2.143(3) . ? Fe3 N3 2.166(4) . ? O2 C1 1.232(5) . ? O3 C1 1.260(5) . ? O4 C2 1.232(5) . ? O5 C2 1.256(5) . ? O6 C3 1.256(5) . ? O7 C3 1.226(5) . ? O8 C4 1.257(5) . ? O9 C4 1.242(5) . ? O10 C5 1.253(5) . ? O11 C5 1.250(5) . ? O12 C6 1.251(5) . ? O13 C6 1.248(5) . ? N1 C15 1.337(5) . ? N1 C11 1.345(5) . ? C11 C12 1.373(6) . ? C12 C13 1.388(6) . ? C13 C14 1.391(6) . ? C13 C16 1.494(6) . ? C14 C15 1.385(6) . ? N2 C21 1.346(5) . ? N2 C25 1.346(5) . ? C21 C22 1.377(6) . ? C22 C23 1.398(6) . ? C23 C24 1.389(7) . ? C23 C26 1.499(7) . ? C24 C25 1.378(6) . ? N3 C31 1.331(6) . ? N3 C35 1.332(6) . ? C31 C32 1.385(6) . ? C32 C33 1.383(7) . ? C33 C34 1.386(7) . ? C33 C36 1.503(7) . ? C34 C35 1.388(6) . ? N5 C51 1.385(10) 2 ? N5 C51 1.385(10) . ? C51 C52 1.445(13) . ? C52 C53 1.382(11) . ? C52 C71 1.92(3) 2 ? C53 C52 1.382(11) 2 ? C53 C54 1.544(17) . ? C41 C43 1.393(12) . ? C41 C85 1.436(15) . ? C41 C75 1.440(16) . ? C41 C76 1.453(18) . ? C43 C72 1.362(17) . ? C43 C82 1.410(14) . ? C43 C86 1.426(14) . ? N7 C72 1.311(16) . ? N7 C71 1.313(16) . ? C75 C71 1.385(19) . ? C71 C52 1.92(3) 2 ? N8 C81 1.333(16) . ? N8 C85 1.389(15) . ? C82 C81 1.420(17) . ? 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 O8 97.68(11) . . ? O1 Fe1 O6 99.01(11) . . ? O8 Fe1 O6 91.06(12) . . ? O1 Fe1 O10 95.06(11) . . ? O8 Fe1 O10 92.20(12) . . ? O6 Fe1 O10 165.00(12) . . ? O1 Fe1 O12 96.72(11) . . ? O8 Fe1 O12 165.44(11) . . ? O6 Fe1 O12 84.51(12) . . ? O10 Fe1 O12 88.72(12) . . ? O1 Fe1 N1 176.34(12) . . ? O8 Fe1 N1 82.70(12) . . ? O6 Fe1 N1 84.61(12) . . ? O10 Fe1 N1 81.29(12) . . ? O12 Fe1 N1 83.07(12) . . ? O1 Fe2 O5 97.99(11) . . ? O1 Fe2 O3 99.16(11) . . ? O5 Fe2 O3 91.33(12) . . ? O1 Fe2 O11 95.91(11) . . ? O5 Fe2 O11 165.93(11) . . ? O3 Fe2 O11 88.62(11) . . ? O1 Fe2 O13 95.84(11) . . ? O5 Fe2 O13 87.71(11) . . ? O3 Fe2 O13 164.96(11) . . ? O11 Fe2 O13 88.70(11) . . ? O1 Fe2 N2 178.15(11) . . ? O5 Fe2 N2 82.98(11) . . ? O3 Fe2 N2 82.38(11) . . ? O11 Fe2 N2 83.06(11) . . ? O13 Fe2 N2 82.61(11) . . ? O1 Fe3 O7 94.74(11) . . ? O1 Fe3 O2 95.16(11) . . ? O7 Fe3 O2 170.09(13) . . ? O1 Fe3 O9 92.01(11) . . ? O7 Fe3 O9 90.97(13) . . ? O2 Fe3 O9 88.17(13) . . ? O1 Fe3 O4 92.56(11) . . ? O7 Fe3 O4 88.26(14) . . ? O2 Fe3 O4 91.80(13) . . ? O9 Fe3 O4 175.42(12) . . ? O1 Fe3 N3 178.68(11) . . ? O7 Fe3 N3 84.52(13) . . ? O2 Fe3 N3 85.59(12) . . ? O9 Fe3 N3 89.10(12) . . ? O4 Fe3 N3 86.33(12) . . ? Fe2 O1 Fe1 122.96(14) . . ? Fe2 O1 Fe3 118.20(12) . . ? Fe1 O1 Fe3 118.80(13) . . ? C1 O2 Fe3 130.2(3) . . ? C1 O3 Fe2 132.0(3) . . ? C2 O4 Fe3 130.3(3) . . ? C2 O5 Fe2 131.6(3) . . ? C3 O6 Fe1 130.2(3) . . ? C3 O7 Fe3 131.7(3) . . ? C4 O8 Fe1 131.8(3) . . ? C4 O9 Fe3 129.0(3) . . ? C5 O10 Fe1 131.5(2) . . ? C5 O11 Fe2 128.1(2) . . ? C6 O12 Fe1 127.6(2) . . ? C6 O13 Fe2 131.9(3) . . ? O2 C1 O3 127.9(4) . . ? O4 C2 O5 128.1(4) . . ? O7 C3 O6 128.6(4) . . ? O9 C4 O8 128.9(4) . . ? O11 C5 O10 128.2(3) . . ? O13 C6 O12 128.3(3) . . ? C15 N1 C11 117.0(3) . . ? C15 N1 Fe1 120.5(3) . . ? C11 N1 Fe1 122.5(3) . . ? N1 C11 C12 123.0(4) . . ? C11 C12 C13 120.2(4) . . ? C12 C13 C14 117.0(4) . . ? C12 C13 C16 122.4(4) . . ? C14 C13 C16 120.6(4) . . ? C15 C14 C13 119.4(4) . . ? N1 C15 C14 123.4(4) . . ? C21 N2 C25 117.9(3) . . ? C21 N2 Fe2 120.9(3) . . ? C25 N2 Fe2 121.2(3) . . ? N2 C21 C22 122.5(4) . . ? C21 C22 C23 119.8(4) . . ? C24 C23 C22 117.4(4) . . ? C24 C23 C26 121.6(5) . . ? C22 C23 C26 121.1(5) . . ? C25 C24 C23 119.8(4) . . ? N2 C25 C24 122.7(4) . . ? C31 N3 C35 116.8(4) . . ? C31 N3 Fe3 121.0(3) . . ? C35 N3 Fe3 122.2(3) . . ? N3 C31 C32 123.8(4) . . ? C33 C32 C31 119.1(5) . . ? C32 C33 C34 117.4(4) . . ? C32 C33 C36 121.2(5) . . ? C34 C33 C36 121.4(4) . . ? C33 C34 C35 119.4(4) . . ? N3 C35 C34 123.3(4) . . ? C51 N5 C51 111.3(12) 2 . ? N5 C51 C52 126.7(9) . . ? C53 C52 C51 117.2(10) . . ? C53 C52 C71 79.4(10) . 2 ? C51 C52 C71 105.5(12) . 2 ? C52 C53 C52 120.9(16) . 2 ? C52 C53 C54 119.6(8) . . ? C52 C53 C54 119.6(8) 2 . ? C43 C41 C85 125.6(12) . . ? C43 C41 C75 109.5(12) . . ? C85 C41 C75 83.6(14) . . ? C43 C41 C76 134.6(19) . . ? C85 C41 C76 53.7(14) . . ? C75 C41 C76 115(2) . . ? C72 C43 C41 140.5(12) . . ? C72 C43 C82 75.5(12) . . ? C41 C43 C82 111.9(10) . . ? C72 C43 C86 47.0(10) . . ? C41 C43 C86 130.1(11) . . ? C82 C43 C86 115.5(13) . . ? C72 N7 C71 127.1(16) . . ? C71 C75 C41 110.5(19) . . ? N7 C72 C43 101.6(13) . . ? N7 C71 C75 129(2) . . ? N7 C71 C52 94.4(18) . 2 ? C75 C71 C52 135.5(17) . 2 ? C81 N8 C85 115.3(15) . . ? C43 C82 C81 119.2(15) . . ? N8 C85 C41 117.9(14) . . ? N8 C81 C82 127.3(18) . . ? _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #============================================================================== data_p87_180 _database_code_CSD 173995 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.40 H27 Fe3 N4.24 O13' _chemical_formula_weight 839.25 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' #============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.382(3) _cell_length_b 27.485(4) _cell_length_c 12.5125(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.562(4) _cell_angle_gamma 90.00 _cell_volume 8330(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4204 _cell_measurement_theta_min 2.241 _cell_measurement_theta_max 33.506 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3417 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS, Sheldrick 1996)' #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_number 62634 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 34.13 _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 34.13 _diffrn_measured_fraction_theta_full 0.895 _reflns_number_total 15372 _reflns_number_gt 8429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'SAINT+ V5.01 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1517P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15372 _refine_ls_number_parameters 450 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1675 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.2839 _refine_ls_wR_factor_gt 0.2510 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.795 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.166 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36025(2) 0.22765(2) 0.36253(4) 0.02129(15) Uani 1 1 d . . . Fe2 Fe 0.23465(2) 0.226635(19) 0.24002(4) 0.01768(14) Uani 1 1 d . . . Fe3 Fe 0.29637(2) 0.12120(2) 0.30802(4) 0.02427(15) Uani 1 1 d . . . O1 O 0.29657(9) 0.19453(10) 0.30489(18) 0.0192(5) Uani 1 1 d . . . O2 O 0.21492(12) 0.11545(12) 0.3521(3) 0.0371(7) Uani 1 1 d . . . O3 O 0.17576(11) 0.18704(11) 0.3028(2) 0.0267(6) Uani 1 1 d . . . O4 O 0.26699(15) 0.11622(12) 0.1402(3) 0.0413(8) Uani 1 1 d . . . O5 O 0.22402(12) 0.18739(11) 0.1028(2) 0.0278(6) Uani 1 1 d . . . O6 O 0.41739(11) 0.18674(13) 0.2963(2) 0.0350(7) Uani 1 1 d . . . O7 O 0.37789(13) 0.11369(13) 0.2657(3) 0.0441(8) Uani 1 1 d . . . O8 O 0.37349(11) 0.18975(11) 0.5019(2) 0.0279(6) Uani 1 1 d . . . O9 O 0.32606(14) 0.11956(12) 0.4754(2) 0.0378(7) Uani 1 1 d . . . O10 O 0.31874(11) 0.28161(10) 0.4336(2) 0.0275(6) Uani 1 1 d . . . O11 O 0.23065(11) 0.27679(11) 0.3597(2) 0.0261(6) Uani 1 1 d . . . O12 O 0.36536(12) 0.27334(12) 0.2329(2) 0.0320(7) Uani 1 1 d . . . O13 O 0.27683(11) 0.27689(10) 0.1588(2) 0.0261(6) Uani 1 1 d . . . C1 C 0.17601(16) 0.14454(16) 0.3404(3) 0.0288(8) Uani 1 1 d . . . H1A H 0.1429 0.1337 0.3621 0.043 Uiso 1 1 calc R . . C2 C 0.24068(18) 0.14565(17) 0.0807(3) 0.0327(9) Uani 1 1 d . . . H2A H 0.2319 0.1357 0.0097 0.049 Uiso 1 1 calc R . . C3 C 0.41578(17) 0.14299(19) 0.2668(4) 0.0348(10) Uani 1 1 d . . . H3A H 0.4479 0.1312 0.2425 0.052 Uiso 1 1 calc R . . C4 C 0.35602(16) 0.14926(17) 0.5297(3) 0.0302(9) Uani 1 1 d . . . H4A H 0.3670 0.1402 0.6006 0.045 Uiso 1 1 calc R . . C5 C 0.26875(15) 0.29229(15) 0.4255(3) 0.0238(7) Uani 1 1 d . . . H5A H 0.2586 0.3148 0.4751 0.036 Uiso 1 1 calc R . . C6 C 0.32702(16) 0.28772(15) 0.1651(3) 0.0261(8) Uani 1 1 d . . . H6A H 0.3370 0.3091 0.1131 0.039 Uiso 1 1 calc R . . N1 N 0.43263(13) 0.26958(14) 0.4346(3) 0.0288(8) Uani 1 1 d . . . C11 C 0.43498(16) 0.28943(17) 0.5343(3) 0.0295(9) Uani 1 1 d . . . H11A H 0.4046 0.2861 0.5724 0.044 Uiso 1 1 calc R . . C12 C 0.47965(17) 0.31384(18) 0.5808(4) 0.0352(10) Uani 1 1 d . . . H12A H 0.4794 0.3266 0.6496 0.053 Uiso 1 1 calc R . . C13 C 0.52628(17) 0.32022(18) 0.5267(4) 0.0348(10) Uani 1 1 d . . . C14 C 0.52365(18) 0.3005(2) 0.4246(4) 0.0435(12) Uani 1 1 d . . . H14A H 0.5534 0.3036 0.3848 0.065 Uiso 1 1 calc R . . C15 C 0.47611(19) 0.2759(2) 0.3818(4) 0.0448(13) Uani 1 1 d . . . H15A H 0.4749 0.2633 0.3126 0.067 Uiso 1 1 calc R . . C16 C 0.5764(2) 0.3466(2) 0.5777(5) 0.0567(15) Uani 1 1 d . . . H16A H 0.5699 0.3579 0.6476 0.085 Uiso 1 1 calc R . . H16B H 0.5840 0.3738 0.5336 0.085 Uiso 1 1 calc R . . H16C H 0.6075 0.3248 0.5844 0.085 Uiso 1 1 calc R . . N2 N 0.16217(13) 0.26686(12) 0.1637(3) 0.0220(6) Uani 1 1 d . . . C21 C 0.12045(16) 0.27959(16) 0.2200(3) 0.0283(8) Uani 1 1 d . . . H21A H 0.1234 0.2720 0.2928 0.043 Uiso 1 1 calc R . . C22 C 0.07414(17) 0.30303(19) 0.1752(4) 0.0385(11) Uani 1 1 d . . . H22A H 0.0463 0.3110 0.2170 0.058 Uiso 1 1 calc R . . C23 C 0.06898(19) 0.3150(2) 0.0657(4) 0.0441(12) Uani 1 1 d . . . C24 C 0.1122(2) 0.30223(19) 0.0075(4) 0.0406(11) Uani 1 1 d . . . H24A H 0.1104 0.3095 -0.0654 0.061 Uiso 1 1 calc R . . C25 C 0.15748(17) 0.27892(15) 0.0585(3) 0.0271(8) Uani 1 1 d . . . H25A H 0.1863 0.2710 0.0189 0.041 Uiso 1 1 calc R . . C26 C 0.0186(3) 0.3414(3) 0.0127(6) 0.074(2) Uani 1 1 d . . . H26A H -0.0067 0.3471 0.0648 0.111 Uiso 1 1 calc R . . H26B H 0.0010 0.3219 -0.0450 0.111 Uiso 1 1 calc R . . H26C H 0.0296 0.3719 -0.0154 0.111 Uiso 1 1 calc R . . N3 N 0.29626(14) 0.04180(14) 0.3084(3) 0.0312(8) Uani 1 1 d . . . C31 C 0.3107(2) 0.01691(18) 0.2251(4) 0.0439(12) Uani 1 1 d . . . H31A H 0.3215 0.0343 0.1673 0.066 Uiso 1 1 calc R . . C32 C 0.3106(3) -0.03324(19) 0.2191(5) 0.0515(14) Uani 1 1 d . . . H32A H 0.3203 -0.0488 0.1579 0.077 Uiso 1 1 calc R . . C33 C 0.2961(2) -0.06021(18) 0.3052(4) 0.0437(12) Uani 1 1 d . . . C34 C 0.2829(3) -0.0340(2) 0.3944(4) 0.0499(13) Uani 1 1 d . . . H34A H 0.2742 -0.0503 0.4555 0.075 Uiso 1 1 calc R . . C35 C 0.2827(2) 0.01629(18) 0.3915(4) 0.0421(11) Uani 1 1 d . . . H35A H 0.2727 0.0331 0.4508 0.063 Uiso 1 1 calc R . . C36 C 0.2953(3) -0.1148(2) 0.3033(6) 0.072(2) Uani 1 1 d . . . H36A H 0.2846 -0.1268 0.3699 0.108 Uiso 1 1 calc R . . H36B H 0.3315 -0.1267 0.2939 0.108 Uiso 1 1 calc R . . H36C H 0.2694 -0.1258 0.2448 0.108 Uiso 1 1 calc R . . N5 N 0.0000 0.0756(4) 0.2500 0.126(6) Uiso 0.881(18) 2 d SPD . . C51 C 0.0166(7) 0.0504(4) 0.3405(4) 0.175(7) Uiso 0.881(18) 1 d PD . . C52 C 0.0183(7) 0.0003(4) 0.3436(4) 0.186(8) Uiso 0.881(18) 1 d PD . . C53 C 0.0000 -0.0252(5) 0.2500 0.174(10) Uiso 0.881(18) 2 d SPD . . C54 C 0.0000 -0.0803(5) 0.2500 0.30(2) Uiso 0.881(18) 2 d SPD . . C41 C 0.1472(5) -0.0647(5) 0.1204(10) 0.128(5) Uiso 0.794(13) 1 d PD . . C43 C 0.1547(4) -0.0184(4) 0.1669(9) 0.105(4) Uiso 0.794(13) 1 d PD A . N7 N 0.0711(14) 0.0038(12) 0.163(3) 0.19(2) Uiso 0.151(11) 1 d PD A 1 C75 C 0.0934(7) -0.0807(8) 0.089(2) 0.19(2) Uiso 0.151(11) 1 d PD A 1 C76 C 0.181(4) -0.108(2) 0.090(4) 0.19(2) Uiso 0.151(11) 1 d PD A 1 C72 C 0.1226(15) 0.0199(9) 0.193(2) 0.19(2) Uiso 0.151(11) 1 d PD A 1 C71 C 0.0646(15) -0.0408(12) 0.118(3) 0.19(2) Uiso 0.151(11) 1 d PD A 1 N8 N 0.1411(5) -0.0981(6) 0.2959(13) 0.172(8) Uiso 0.643(12) 1 d PD A 2 C82 C 0.1537(6) -0.0136(6) 0.2774(10) 0.162(9) Uiso 0.643(12) 1 d PD A 2 C85 C 0.1416(6) -0.1029(6) 0.1890(13) 0.206(12) Uiso 0.643(12) 1 d PD A 2 C81 C 0.1472(6) -0.0537(7) 0.3403(15) 0.201(12) Uiso 0.643(12) 1 d PD A 2 C86 C 0.1613(6) 0.0270(5) 0.1020(14) 0.142(7) Uiso 0.643(12) 1 d PD A 2 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 0.0195(2) 0.0279(3) 0.0160(3) -0.0010(2) 0.00000(18) -0.0028(2) Fe2 0.0197(2) 0.0177(3) 0.0150(2) -0.00019(19) -0.00063(17) -0.00044(18) Fe3 0.0284(3) 0.0201(3) 0.0232(3) 0.0000(2) -0.0022(2) 0.0015(2) O1 0.0170(10) 0.0225(14) 0.0170(11) 0.0002(10) -0.0033(8) -0.0027(9) O2 0.0315(15) 0.0272(17) 0.053(2) 0.0051(14) 0.0059(14) -0.0017(12) O3 0.0250(13) 0.0292(16) 0.0259(14) 0.0041(12) 0.0033(10) -0.0016(11) O4 0.062(2) 0.0257(18) 0.0327(16) -0.0033(13) -0.0108(15) 0.0134(15) O5 0.0369(15) 0.0237(15) 0.0211(13) -0.0044(11) -0.0043(11) 0.0086(12) O6 0.0214(13) 0.048(2) 0.0355(16) -0.0100(14) 0.0040(11) -0.0015(13) O7 0.0323(16) 0.039(2) 0.062(2) -0.0047(17) 0.0090(15) 0.0043(14) O8 0.0277(13) 0.0354(17) 0.0198(13) 0.0010(12) -0.0003(10) -0.0054(12) O9 0.0485(18) 0.0327(19) 0.0297(15) 0.0049(13) -0.0064(13) -0.0048(14) O10 0.0274(13) 0.0272(16) 0.0271(14) -0.0071(11) 0.0000(11) -0.0049(11) O11 0.0236(12) 0.0339(17) 0.0203(13) -0.0081(11) -0.0001(10) -0.0001(11) O12 0.0290(14) 0.0431(19) 0.0233(14) 0.0040(13) 0.0011(11) -0.0118(13) O13 0.0228(12) 0.0278(16) 0.0272(14) 0.0069(11) 0.0013(10) -0.0013(11) C1 0.0272(18) 0.032(2) 0.028(2) 0.0028(17) 0.0036(15) -0.0065(16) C2 0.043(2) 0.033(3) 0.0212(18) -0.0053(17) -0.0023(16) 0.0057(19) C3 0.0263(19) 0.045(3) 0.033(2) -0.004(2) 0.0040(16) 0.0092(18) C4 0.0303(19) 0.039(3) 0.0203(18) 0.0033(17) -0.0009(14) -0.0004(17) C5 0.0260(17) 0.027(2) 0.0183(16) -0.0033(15) 0.0021(13) 0.0007(15) C6 0.0326(19) 0.027(2) 0.0188(17) 0.0032(15) 0.0048(14) -0.0060(16) N1 0.0227(14) 0.042(2) 0.0211(15) -0.0015(14) -0.0007(12) -0.0053(14) C11 0.0272(18) 0.040(3) 0.0216(18) -0.0021(17) 0.0029(14) -0.0034(17) C12 0.032(2) 0.045(3) 0.027(2) -0.0077(19) -0.0066(16) -0.0028(18) C13 0.0259(19) 0.035(3) 0.042(2) -0.003(2) -0.0017(17) -0.0060(17) C14 0.0247(19) 0.063(4) 0.044(3) -0.009(2) 0.0057(18) -0.013(2) C15 0.035(2) 0.073(4) 0.029(2) -0.016(2) 0.0094(18) -0.021(2) C16 0.032(2) 0.067(4) 0.068(4) -0.013(3) -0.006(2) -0.014(2) N2 0.0251(14) 0.0193(17) 0.0213(15) -0.0010(12) 0.0008(11) -0.0013(12) C21 0.0269(18) 0.032(2) 0.0265(19) -0.0005(16) 0.0041(15) -0.0025(16) C22 0.0251(19) 0.044(3) 0.047(3) 0.002(2) 0.0037(18) 0.0065(18) C23 0.031(2) 0.056(3) 0.042(3) 0.001(2) -0.0114(19) 0.015(2) C24 0.046(3) 0.045(3) 0.027(2) 0.005(2) -0.0115(18) 0.011(2) C25 0.0300(18) 0.028(2) 0.0219(18) -0.0037(15) -0.0014(14) 0.0028(16) C26 0.049(3) 0.093(6) 0.073(4) 0.012(4) -0.019(3) 0.033(3) N3 0.0350(17) 0.029(2) 0.0283(18) 0.0027(14) -0.0032(14) 0.0039(15) C31 0.062(3) 0.029(3) 0.043(3) 0.005(2) 0.018(2) 0.006(2) C32 0.077(4) 0.025(3) 0.058(3) 0.001(2) 0.030(3) 0.008(2) C33 0.053(3) 0.021(2) 0.059(3) 0.010(2) 0.019(2) 0.015(2) C34 0.079(4) 0.029(3) 0.043(3) 0.006(2) 0.010(3) -0.002(2) C35 0.066(3) 0.028(3) 0.033(2) -0.0021(19) 0.007(2) -0.004(2) C36 0.115(6) 0.020(3) 0.088(5) 0.005(3) 0.045(5) 0.005(3) #============================================================================== # MOLECULAR GEOMETRY 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 1.872(2) . ? Fe1 O8 2.025(3) . ? Fe1 O6 2.039(3) . ? Fe1 O10 2.054(3) . ? Fe1 O12 2.066(3) . ? Fe1 N1 2.212(3) . ? Fe2 O1 1.854(2) . ? Fe2 O5 2.020(3) . ? Fe2 O3 2.030(3) . ? Fe2 O11 2.046(3) . ? Fe2 O13 2.058(3) . ? Fe2 N2 2.207(3) . ? Fe3 O1 2.016(3) . ? Fe3 O7 2.125(3) . ? Fe3 O2 2.127(3) . ? Fe3 O9 2.137(3) . ? Fe3 O4 2.144(3) . ? Fe3 N3 2.182(4) . ? O2 C1 1.237(5) . ? O3 C1 1.259(5) . ? O4 C2 1.229(5) . ? O5 C2 1.258(5) . ? O6 C3 1.257(6) . ? O7 C3 1.224(6) . ? O8 C4 1.255(5) . ? O9 C4 1.245(5) . ? O10 C5 1.247(4) . ? O11 C5 1.244(4) . ? O12 C6 1.252(5) . ? O13 C6 1.253(5) . ? N1 C15 1.323(5) . ? N1 C11 1.357(5) . ? C11 C12 1.353(6) . ? C12 C13 1.399(6) . ? C13 C14 1.382(7) . ? C13 C16 1.500(6) . ? C14 C15 1.395(6) . ? N2 C21 1.348(5) . ? N2 C25 1.349(5) . ? C21 C22 1.363(6) . ? C22 C23 1.401(7) . ? C23 C24 1.393(7) . ? C23 C26 1.512(7) . ? C24 C25 1.369(6) . ? N3 C31 1.327(6) . ? N3 C35 1.327(6) . ? C31 C32 1.381(7) . ? C32 C33 1.387(7) . ? C33 C34 1.397(7) . ? C33 C36 1.501(7) . ? C34 C35 1.383(7) . ? N5 C51 1.350(4) 2 ? N5 C51 1.350(4) . ? C51 C52 1.379(4) . ? C52 C53 1.394(4) . ? C53 C52 1.394(4) 2 ? C53 C54 1.512(4) . ? C41 C85 1.373(4) . ? C41 C75 1.396(4) . ? C41 C43 1.403(4) . ? C41 C76 1.509(4) . ? C43 C72 1.373(4) . ? C43 C82 1.392(4) . ? C43 C86 1.507(4) . ? N7 C72 1.346(4) . ? N7 C71 1.347(4) . ? C75 C71 1.373(4) . ? N8 C81 1.342(4) . ? N8 C85 1.346(4) . ? C82 C81 1.375(4) . ? 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 O8 97.20(11) . . ? O1 Fe1 O6 98.66(12) . . ? O8 Fe1 O6 90.97(13) . . ? O1 Fe1 O10 95.16(11) . . ? O8 Fe1 O10 92.10(12) . . ? O6 Fe1 O10 165.35(12) . . ? O1 Fe1 O12 96.60(11) . . ? O8 Fe1 O12 166.04(11) . . ? O6 Fe1 O12 84.90(13) . . ? O10 Fe1 O12 88.72(12) . . ? O1 Fe1 N1 176.94(13) . . ? O8 Fe1 N1 82.86(12) . . ? O6 Fe1 N1 84.40(13) . . ? O10 Fe1 N1 81.78(12) . . ? O12 Fe1 N1 83.47(12) . . ? O1 Fe2 O5 97.87(11) . . ? O1 Fe2 O3 98.74(11) . . ? O5 Fe2 O3 90.87(12) . . ? O1 Fe2 O11 96.02(11) . . ? O5 Fe2 O11 165.96(11) . . ? O3 Fe2 O11 89.01(12) . . ? O1 Fe2 O13 96.18(11) . . ? O5 Fe2 O13 87.79(12) . . ? O3 Fe2 O13 165.06(11) . . ? O11 Fe2 O13 88.72(12) . . ? O1 Fe2 N2 178.36(12) . . ? O5 Fe2 N2 83.16(11) . . ? O3 Fe2 N2 82.49(11) . . ? O11 Fe2 N2 82.91(11) . . ? O13 Fe2 N2 82.57(11) . . ? O1 Fe3 O7 95.04(12) . . ? O1 Fe3 O2 94.81(11) . . ? O7 Fe3 O2 170.14(14) . . ? O1 Fe3 O9 92.23(11) . . ? O7 Fe3 O9 91.18(14) . . ? O2 Fe3 O9 88.05(13) . . ? O1 Fe3 O4 92.64(11) . . ? O7 Fe3 O4 88.11(15) . . ? O2 Fe3 O4 91.82(14) . . ? O9 Fe3 O4 175.12(13) . . ? O1 Fe3 N3 179.00(11) . . ? O7 Fe3 N3 84.54(14) . . ? O2 Fe3 N3 85.62(13) . . ? O9 Fe3 N3 88.70(12) . . ? O4 Fe3 N3 86.43(12) . . ? Fe2 O1 Fe1 122.37(15) . . ? Fe2 O1 Fe3 118.74(12) . . ? Fe1 O1 Fe3 118.85(12) . . ? C1 O2 Fe3 130.4(3) . . ? C1 O3 Fe2 132.0(3) . . ? C2 O4 Fe3 130.1(3) . . ? C2 O5 Fe2 131.3(3) . . ? C3 O6 Fe1 130.3(3) . . ? C3 O7 Fe3 131.2(3) . . ? C4 O8 Fe1 132.0(3) . . ? C4 O9 Fe3 129.3(3) . . ? C5 O10 Fe1 131.3(3) . . ? C5 O11 Fe2 128.3(3) . . ? C6 O12 Fe1 128.0(3) . . ? C6 O13 Fe2 131.9(3) . . ? O2 C1 O3 127.9(4) . . ? O4 C2 O5 128.8(4) . . ? O7 C3 O6 129.1(4) . . ? O9 C4 O8 128.8(4) . . ? O11 C5 O10 128.5(4) . . ? O12 C6 O13 128.0(4) . . ? C15 N1 C11 117.0(4) . . ? C15 N1 Fe1 120.8(3) . . ? C11 N1 Fe1 122.1(3) . . ? C12 C11 N1 122.8(4) . . ? C11 C12 C13 120.9(4) . . ? C14 C13 C12 116.3(4) . . ? C14 C13 C16 122.1(4) . . ? C12 C13 C16 121.5(4) . . ? C13 C14 C15 119.6(4) . . ? N1 C15 C14 123.3(4) . . ? C21 N2 C25 117.4(3) . . ? C21 N2 Fe2 121.2(3) . . ? C25 N2 Fe2 121.3(3) . . ? N2 C21 C22 123.2(4) . . ? C21 C22 C23 119.4(4) . . ? C24 C23 C22 117.6(4) . . ? C24 C23 C26 121.1(5) . . ? C22 C23 C26 121.3(5) . . ? C25 C24 C23 119.5(4) . . ? N2 C25 C24 122.9(4) . . ? C31 N3 C35 117.1(4) . . ? C31 N3 Fe3 120.9(3) . . ? C35 N3 Fe3 122.0(3) . . ? N3 C31 C32 124.0(5) . . ? C31 C32 C33 119.3(5) . . ? C32 C33 C34 116.6(5) . . ? C32 C33 C36 121.7(5) . . ? C34 C33 C36 121.6(5) . . ? C35 C34 C33 119.6(5) . . ? N3 C35 C34 123.3(5) . . ? C51 N5 C51 118.2(6) 2 . ? N5 C51 C52 122.8(4) . . ? C51 C52 C53 118.3(4) . . ? C52 C53 C52 119.6(6) . 2 ? C52 C53 C54 120.2(3) . . ? C52 C53 C54 120.2(3) 2 . ? C85 C41 C75 77.0(13) . . ? C85 C41 C43 116.9(12) . . ? C75 C41 C43 118.4(4) . . ? C85 C41 C76 69.9(18) . . ? C75 C41 C76 102(4) . . ? C43 C41 C76 140(4) . . ? C72 C43 C82 67.3(10) . . ? C72 C43 C41 138.1(18) . . ? C82 C43 C41 118.8(5) . . ? C72 C43 C86 66.0(13) . . ? C82 C43 C86 118.2(13) . . ? C41 C43 C86 123.0(12) . . ? C72 N7 C71 118.7(5) . . ? C71 C75 C41 99.7(17) . . ? N7 C72 C43 102.6(17) . . ? N7 C71 C75 143(2) . . ? C81 N8 C85 119.2(5) . . ? C81 C82 C43 120.6(12) . . ? N8 C85 C41 124.0(12) . . ? N8 C81 C82 120.4(13) . . ? _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #============================================================================== data_p87_240 _database_code_CSD 173996 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H27 Fe3 N4.06 O13' _chemical_formula_weight 825.99 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' #============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.466(2) _cell_length_b 27.516(3) _cell_length_c 12.6020(12) _cell_angle_alpha 90.000(3) _cell_angle_beta 96.440(3) _cell_angle_gamma 90.000(2) _cell_volume 8430.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 4005 _cell_measurement_theta_min 2.199 _cell_measurement_theta_max 33.725 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3364 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS, Sheldrick 1996)' #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_reflns_number 55826 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 34.03 _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 34.03 _diffrn_measured_fraction_theta_full 0.889 _reflns_number_total 15326 _reflns_number_gt 8197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'SAINT+ V5.01 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1297P)^2^+158.1073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15326 _refine_ls_number_parameters 441 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2372 _refine_ls_R_factor_gt 0.1575 _refine_ls_wR_factor_ref 0.3726 _refine_ls_wR_factor_gt 0.3229 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.176 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 1.699 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.173 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36056(4) 0.22872(4) 0.36176(7) 0.0268(2) Uani 1 1 d . . . Fe2 Fe 0.23540(3) 0.22692(3) 0.23982(7) 0.0218(2) Uani 1 1 d . . . Fe3 Fe 0.29781(4) 0.12217(4) 0.30716(8) 0.0301(2) Uani 1 1 d . . . O1 O 0.29735(16) 0.19512(16) 0.3041(3) 0.0239(8) Uani 1 1 d . . . O2 O 0.2170(2) 0.1159(2) 0.3520(5) 0.0454(13) Uani 1 1 d . . . O3 O 0.17707(19) 0.18702(18) 0.3028(4) 0.0323(11) Uani 1 1 d . . . O4 O 0.2682(3) 0.1167(2) 0.1416(5) 0.0491(15) Uani 1 1 d . . . O5 O 0.2250(2) 0.18734(18) 0.1041(4) 0.0360(11) Uani 1 1 d . . . O6 O 0.4179(2) 0.1876(2) 0.2959(4) 0.0428(13) Uani 1 1 d . . . O7 O 0.3784(2) 0.1151(2) 0.2642(6) 0.0543(16) Uani 1 1 d . . . O8 O 0.3736(2) 0.1904(2) 0.5007(4) 0.0350(11) Uani 1 1 d . . . O9 O 0.3271(3) 0.1201(2) 0.4723(4) 0.0467(14) Uani 1 1 d . . . O10 O 0.31846(19) 0.28226(18) 0.4327(4) 0.0324(11) Uani 1 1 d . . . O11 O 0.23095(19) 0.27705(18) 0.3588(4) 0.0315(10) Uani 1 1 d . . . O12 O 0.3651(2) 0.2744(2) 0.2326(4) 0.0411(13) Uani 1 1 d . . . O13 O 0.27744(19) 0.27704(18) 0.1587(4) 0.0331(11) Uani 1 1 d . . . C1 C 0.1784(3) 0.1447(3) 0.3409(6) 0.0361(16) Uani 1 1 d . . . H1A H 0.1457 0.1338 0.3637 0.054 Uiso 1 1 calc R . . C2 C 0.2421(3) 0.1460(3) 0.0828(6) 0.0399(17) Uani 1 1 d . . . H2A H 0.2338 0.1361 0.0122 0.060 Uiso 1 1 calc R . . C3 C 0.4161(3) 0.1444(4) 0.2654(7) 0.045(2) Uani 1 1 d . . . H3A H 0.4480 0.1328 0.2401 0.068 Uiso 1 1 calc R . . C4 C 0.3563(3) 0.1500(3) 0.5269(6) 0.0390(17) Uani 1 1 d . . . H4A H 0.3667 0.1409 0.5973 0.058 Uiso 1 1 calc R . . C5 C 0.2683(3) 0.2925(3) 0.4244(5) 0.0299(14) Uani 1 1 d . . . H5A H 0.2577 0.3145 0.4741 0.045 Uiso 1 1 calc R . . C6 C 0.3266(3) 0.2878(3) 0.1647(5) 0.0315(14) Uani 1 1 d . . . H6A H 0.3365 0.3087 0.1120 0.047 Uiso 1 1 calc R . . N1 N 0.4325(2) 0.2708(3) 0.4343(5) 0.0363(14) Uani 1 1 d . . . C11 C 0.4347(3) 0.2895(3) 0.5331(6) 0.0361(16) Uani 1 1 d . . . H11A H 0.4044 0.2858 0.5707 0.054 Uiso 1 1 calc R . . C12 C 0.4794(3) 0.3135(3) 0.5805(7) 0.046(2) Uani 1 1 d . . . H12A H 0.4791 0.3256 0.6494 0.069 Uiso 1 1 calc R . . C13 C 0.5259(3) 0.3205(3) 0.5273(7) 0.0463(19) Uani 1 1 d . . . C14 C 0.5231(4) 0.3011(4) 0.4263(8) 0.057(2) Uani 1 1 d . . . H14A H 0.5530 0.3039 0.3872 0.086 Uiso 1 1 calc R . . C15 C 0.4761(3) 0.2775(4) 0.3826(7) 0.056(3) Uani 1 1 d . . . H15A H 0.4750 0.2656 0.3133 0.084 Uiso 1 1 calc R . . C16 C 0.5760(4) 0.3464(5) 0.5803(10) 0.074(3) Uani 1 1 d . . . H16A H 0.5690 0.3575 0.6497 0.110 Uiso 1 1 calc R . . H16B H 0.5843 0.3738 0.5375 0.110 Uiso 1 1 calc R . . H16C H 0.6067 0.3245 0.5874 0.110 Uiso 1 1 calc R . . N2 N 0.1627(2) 0.2671(2) 0.1643(4) 0.0276(11) Uani 1 1 d . . . C21 C 0.1212(3) 0.2795(3) 0.2199(6) 0.0330(15) Uani 1 1 d . . . H21A H 0.1243 0.2722 0.2924 0.049 Uiso 1 1 calc R . . C22 C 0.0749(3) 0.3021(3) 0.1759(7) 0.047(2) Uani 1 1 d . . . H22A H 0.0470 0.3095 0.2177 0.070 Uiso 1 1 calc R . . C23 C 0.0692(3) 0.3140(4) 0.0680(8) 0.053(2) Uani 1 1 d . . . C24 C 0.1124(4) 0.3016(3) 0.0090(7) 0.049(2) Uani 1 1 d . . . H24A H 0.1104 0.3089 -0.0634 0.073 Uiso 1 1 calc R . . C25 C 0.1579(3) 0.2784(3) 0.0597(6) 0.0331(15) Uani 1 1 d . . . H25A H 0.1864 0.2703 0.0202 0.050 Uiso 1 1 calc R . . C26 C 0.0185(5) 0.3396(5) 0.0158(11) 0.087(4) Uani 1 1 d . . . H26A H -0.0066 0.3452 0.0679 0.131 Uiso 1 1 calc R . . H26B H 0.0010 0.3198 -0.0408 0.131 Uiso 1 1 calc R . . H26C H 0.0289 0.3702 -0.0129 0.131 Uiso 1 1 calc R . . N3 N 0.2980(3) 0.0429(2) 0.3079(5) 0.0387(14) Uani 1 1 d . . . C31 C 0.3120(4) 0.0178(3) 0.2247(8) 0.053(2) Uani 1 1 d . . . H31A H 0.3228 0.0351 0.1672 0.080 Uiso 1 1 calc R . . C32 C 0.3113(5) -0.0324(3) 0.2190(8) 0.060(3) Uani 1 1 d . . . H32A H 0.3203 -0.0481 0.1579 0.090 Uiso 1 1 calc R . . C33 C 0.2972(4) -0.0591(3) 0.3048(8) 0.057(2) Uani 1 1 d . . . C34 C 0.2841(5) -0.0330(4) 0.3927(8) 0.061(3) Uani 1 1 d . . . H34A H 0.2752 -0.0493 0.4531 0.092 Uiso 1 1 calc R . . C35 C 0.2843(4) 0.0173(3) 0.3904(7) 0.050(2) Uani 1 1 d . . . H35A H 0.2744 0.0340 0.4495 0.075 Uiso 1 1 calc R . . C36 C 0.2965(6) -0.1135(4) 0.3029(11) 0.094(5) Uani 1 1 d . . . H36A H 0.2859 -0.1255 0.3691 0.141 Uiso 1 1 calc R . . H36B H 0.3325 -0.1254 0.2934 0.141 Uiso 1 1 calc R . . H36C H 0.2706 -0.1245 0.2450 0.141 Uiso 1 1 calc R . . N5 N 0.0000 0.0755(10) 0.2500 0.206(12) Uiso 0.75(3) 2 d SPD . . C51 C 0.0169(16) 0.0511(10) 0.3397(8) 0.206(12) Uiso 0.75(3) 1 d PD . . C52 C 0.0148(17) 0.0013(10) 0.3445(7) 0.206(12) Uiso 0.75(3) 1 d PD . . C53 C 0.0000 -0.0239(10) 0.2500 0.206(12) Uiso 0.75(3) 2 d SPD . . C54 C 0.0000 -0.0788(10) 0.2500 0.247(15) Uiso 0.75(3) 2 d SPD . . C41 C 0.1484(9) -0.0659(8) 0.116(2) 0.154(11) Uiso 0.75 1 d PD . . C43 C 0.1544(8) -0.0209(7) 0.1661(17) 0.153(10) Uiso 0.75 1 d PD . . N7 N 0.060(2) -0.012(2) 0.161(5) 0.5(3) Uiso 0.09(4) 1 d PD . 1 C75 C 0.0961(12) -0.0847(13) 0.086(4) 0.5(3) Uiso 0.09(4) 1 d PD . 1 C76 C 0.1986(14) -0.0943(14) 0.093(4) 0.6(4) Uiso 0.09(4) 1 d PD . 1 C72 C 0.111(2) 0.007(2) 0.189(3) 0.5(3) Uiso 0.09(4) 1 d PD . 1 C71 C 0.055(2) -0.055(2) 0.112(5) 0.5(3) Uiso 0.09(4) 1 d PD . 1 N8 N 0.1369(10) -0.1006(10) 0.288(2) 0.197(12) Uiso 0.60(3) 1 d PD . 2 C82 C 0.1512(11) -0.0173(12) 0.2752(17) 0.197(12) Uiso 0.60(3) 1 d PD . 2 C85 C 0.1399(10) -0.1039(11) 0.182(2) 0.197(12) Uiso 0.60(3) 1 d PD . 2 C81 C 0.1425(11) -0.0572(12) 0.336(3) 0.197(12) Uiso 0.60(3) 1 d PD . 2 C86 C 0.1639(14) 0.0239(9) 0.102(3) 0.236(15) Uiso 0.60(3) 1 d PD . 2 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 0.0241(4) 0.0329(6) 0.0221(4) -0.0006(4) -0.0023(3) -0.0017(4) Fe2 0.0244(4) 0.0188(4) 0.0209(4) 0.0008(3) -0.0037(3) 0.0007(3) Fe3 0.0350(5) 0.0218(5) 0.0314(5) 0.0008(4) -0.0050(4) 0.0042(4) O1 0.0200(17) 0.026(2) 0.024(2) 0.0022(18) -0.0064(14) -0.0003(17) O2 0.039(3) 0.030(3) 0.067(4) 0.009(3) 0.004(3) 0.002(2) O3 0.028(2) 0.033(3) 0.036(3) 0.009(2) -0.0012(19) -0.0002(19) O4 0.072(4) 0.027(3) 0.043(3) -0.005(2) -0.014(3) 0.017(3) O5 0.047(3) 0.028(3) 0.031(2) -0.003(2) -0.008(2) 0.013(2) O6 0.025(2) 0.056(4) 0.047(3) -0.011(3) 0.003(2) -0.001(2) O7 0.039(3) 0.044(4) 0.080(5) -0.007(3) 0.008(3) 0.007(3) O8 0.035(3) 0.040(3) 0.028(2) 0.001(2) -0.0036(19) -0.007(2) O9 0.059(4) 0.039(3) 0.039(3) 0.006(2) -0.011(3) -0.006(3) O10 0.032(2) 0.027(3) 0.037(3) -0.009(2) -0.0054(19) -0.0041(19) O11 0.028(2) 0.036(3) 0.029(2) -0.009(2) -0.0041(18) 0.002(2) O12 0.036(3) 0.053(4) 0.033(3) 0.008(2) -0.001(2) -0.014(2) O13 0.028(2) 0.034(3) 0.036(3) 0.008(2) -0.0013(19) -0.003(2) C1 0.032(3) 0.037(4) 0.039(4) 0.001(3) 0.004(3) -0.010(3) C2 0.049(4) 0.041(5) 0.027(3) -0.007(3) -0.005(3) 0.007(3) C3 0.034(4) 0.060(6) 0.042(4) -0.003(4) 0.006(3) 0.015(4) C4 0.042(4) 0.045(5) 0.028(3) 0.003(3) -0.002(3) -0.001(3) C5 0.032(3) 0.033(4) 0.024(3) -0.005(3) 0.000(2) -0.001(3) C6 0.043(4) 0.027(4) 0.024(3) 0.003(3) 0.003(3) -0.006(3) N1 0.029(3) 0.051(4) 0.028(3) -0.001(3) 0.000(2) -0.007(3) C11 0.032(3) 0.045(5) 0.030(3) -0.001(3) 0.002(3) -0.003(3) C12 0.046(4) 0.055(6) 0.035(4) -0.010(4) -0.007(3) -0.006(4) C13 0.036(4) 0.041(5) 0.059(5) -0.002(4) -0.006(4) -0.005(3) C14 0.036(4) 0.081(7) 0.055(5) -0.007(5) 0.008(4) -0.016(4) C15 0.042(4) 0.090(8) 0.037(4) -0.013(4) 0.007(3) -0.024(5) C16 0.035(5) 0.093(9) 0.088(8) -0.008(7) -0.013(5) -0.017(5) N2 0.030(3) 0.023(3) 0.028(3) -0.001(2) -0.003(2) -0.003(2) C21 0.033(3) 0.029(4) 0.036(4) 0.001(3) 0.002(3) 0.001(3) C22 0.030(4) 0.049(5) 0.061(5) 0.003(4) 0.002(3) 0.011(3) C23 0.032(4) 0.063(6) 0.059(5) -0.004(4) -0.020(4) 0.015(4) C24 0.053(5) 0.053(6) 0.037(4) 0.005(4) -0.014(3) 0.015(4) C25 0.041(4) 0.025(4) 0.032(3) -0.003(3) -0.005(3) 0.004(3) C26 0.060(7) 0.103(10) 0.092(9) 0.012(7) -0.027(6) 0.038(7) N3 0.046(3) 0.031(3) 0.037(3) 0.005(3) -0.004(3) 0.008(3) C31 0.079(6) 0.031(5) 0.052(5) 0.003(4) 0.019(5) 0.008(4) C32 0.090(7) 0.029(5) 0.066(6) 0.001(4) 0.026(5) 0.012(5) C33 0.074(6) 0.026(4) 0.075(6) 0.008(4) 0.021(5) 0.014(4) C34 0.093(8) 0.038(5) 0.054(5) 0.006(4) 0.012(5) -0.001(5) C35 0.081(6) 0.024(4) 0.044(5) -0.001(3) 0.006(4) 0.001(4) C36 0.152(14) 0.024(5) 0.113(11) 0.005(6) 0.055(10) 0.005(6) #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.877(4) . ? Fe1 O8 2.038(5) . ? Fe1 O6 2.049(5) . ? Fe1 O10 2.058(5) . ? Fe1 O12 2.069(5) . ? Fe1 N1 2.217(6) . ? Fe2 O1 1.856(4) . ? Fe2 O5 2.020(5) . ? Fe2 O3 2.031(5) . ? Fe2 O11 2.049(5) . ? Fe2 O13 2.060(5) . ? Fe2 N2 2.215(6) . ? Fe3 O1 2.008(5) . ? Fe3 O7 2.111(6) . ? Fe3 O2 2.123(6) . ? Fe3 O9 2.124(5) . ? Fe3 O4 2.136(6) . ? Fe3 N3 2.182(7) . ? O2 C1 1.230(9) . ? O3 C1 1.258(9) . ? O4 C2 1.225(9) . ? O5 C2 1.252(9) . ? O6 C3 1.250(11) . ? O7 C3 1.225(11) . ? O8 C4 1.247(9) . ? O9 C4 1.245(9) . ? O10 C5 1.252(8) . ? O11 C5 1.236(8) . ? O12 C6 1.254(9) . ? O13 C6 1.233(8) . ? N1 C15 1.322(10) . ? N1 C11 1.343(9) . ? C11 C12 1.358(11) . ? C12 C13 1.396(12) . ? C13 C14 1.375(13) . ? C13 C16 1.508(12) . ? C14 C15 1.381(12) . ? N2 C21 1.342(9) . ? N2 C25 1.347(9) . ? C21 C22 1.354(10) . ? C22 C23 1.391(13) . ? C23 C24 1.401(13) . ? C23 C26 1.513(12) . ? C24 C25 1.376(10) . ? N3 C35 1.330(11) . ? N3 C31 1.331(11) . ? C31 C32 1.385(13) . ? C32 C33 1.383(13) . ? C33 C34 1.388(14) . ? C33 C36 1.497(14) . ? C34 C35 1.384(13) . ? N5 C51 1.341(4) 2 ? N5 C51 1.341(4) . ? C51 C52 1.371(4) . ? C52 C53 1.391(4) . ? C52 N7 1.86(6) 2 ? C53 C52 1.391(4) 2 ? C53 C54 1.511(4) . ? C41 C85 1.370(4) . ? C41 C75 1.391(4) . ? C41 C43 1.392(3) . ? C41 C76 1.509(4) . ? C43 C72 1.371(4) . ? C43 C82 1.389(4) . ? C43 C86 1.509(4) . ? N7 C71 1.342(4) . ? N7 C72 1.341(4) . ? N7 C52 1.86(6) 2 ? C75 C71 1.371(4) . ? N8 C81 1.340(4) . ? N8 C85 1.341(4) . ? C82 C81 1.372(4) . ? 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 O8 96.93(19) . . ? O1 Fe1 O6 98.3(2) . . ? O8 Fe1 O6 90.9(2) . . ? O1 Fe1 O10 95.16(19) . . ? O8 Fe1 O10 92.0(2) . . ? O6 Fe1 O10 165.9(2) . . ? O1 Fe1 O12 96.25(19) . . ? O8 Fe1 O12 166.6(2) . . ? O6 Fe1 O12 85.2(2) . . ? O10 Fe1 O12 88.9(2) . . ? O1 Fe1 N1 177.1(2) . . ? O8 Fe1 N1 82.8(2) . . ? O6 Fe1 N1 84.6(2) . . ? O10 Fe1 N1 82.0(2) . . ? O12 Fe1 N1 84.1(2) . . ? O1 Fe2 O5 97.74(19) . . ? O1 Fe2 O3 98.63(19) . . ? O5 Fe2 O3 90.7(2) . . ? O1 Fe2 O11 96.08(19) . . ? O5 Fe2 O11 166.07(19) . . ? O3 Fe2 O11 88.9(2) . . ? O1 Fe2 O13 95.94(19) . . ? O5 Fe2 O13 87.9(2) . . ? O3 Fe2 O13 165.42(19) . . ? O11 Fe2 O13 89.0(2) . . ? O1 Fe2 N2 178.2(2) . . ? O5 Fe2 N2 83.5(2) . . ? O3 Fe2 N2 82.7(2) . . ? O11 Fe2 N2 82.68(19) . . ? O13 Fe2 N2 82.8(2) . . ? O1 Fe3 O7 95.2(2) . . ? O1 Fe3 O2 94.8(2) . . ? O7 Fe3 O2 170.0(2) . . ? O1 Fe3 O9 92.7(2) . . ? O7 Fe3 O9 91.5(3) . . ? O2 Fe3 O9 87.7(2) . . ? O1 Fe3 O4 92.93(19) . . ? O7 Fe3 O4 88.1(3) . . ? O2 Fe3 O4 91.7(3) . . ? O9 Fe3 O4 174.4(2) . . ? O1 Fe3 N3 179.1(2) . . ? O7 Fe3 N3 84.7(3) . . ? O2 Fe3 N3 85.3(2) . . ? O9 Fe3 N3 88.2(2) . . ? O4 Fe3 N3 86.2(2) . . ? Fe2 O1 Fe1 122.3(2) . . ? Fe2 O1 Fe3 118.8(2) . . ? Fe1 O1 Fe3 118.8(2) . . ? C1 O2 Fe3 130.1(5) . . ? C1 O3 Fe2 131.3(5) . . ? C2 O4 Fe3 129.9(5) . . ? C2 O5 Fe2 131.2(5) . . ? C3 O6 Fe1 130.4(5) . . ? C3 O7 Fe3 131.4(6) . . ? C4 O8 Fe1 131.6(5) . . ? C4 O9 Fe3 129.3(5) . . ? C5 O10 Fe1 131.1(4) . . ? C5 O11 Fe2 128.6(4) . . ? C6 O12 Fe1 127.8(5) . . ? C6 O13 Fe2 131.9(5) . . ? O2 C1 O3 128.8(7) . . ? O4 C2 O5 129.2(7) . . ? O7 C3 O6 129.1(7) . . ? O9 C4 O8 129.3(7) . . ? O11 C5 O10 128.5(6) . . ? O13 C6 O12 128.6(6) . . ? C15 N1 C11 116.9(6) . . ? C15 N1 Fe1 121.0(5) . . ? C11 N1 Fe1 122.0(5) . . ? N1 C11 C12 122.7(7) . . ? C11 C12 C13 121.0(8) . . ? C14 C13 C12 115.7(7) . . ? C14 C13 C16 123.2(9) . . ? C12 C13 C16 121.2(9) . . ? C13 C14 C15 120.3(8) . . ? N1 C15 C14 123.4(8) . . ? C21 N2 C25 117.6(6) . . ? C21 N2 Fe2 121.4(5) . . ? C25 N2 Fe2 121.0(5) . . ? N2 C21 C22 123.4(7) . . ? C21 C22 C23 119.7(8) . . ? C22 C23 C24 117.6(7) . . ? C22 C23 C26 121.5(9) . . ? C24 C23 C26 120.9(9) . . ? C25 C24 C23 119.0(8) . . ? N2 C25 C24 122.7(7) . . ? C35 N3 C31 116.8(7) . . ? C35 N3 Fe3 122.2(5) . . ? C31 N3 Fe3 121.0(6) . . ? N3 C31 C32 123.8(9) . . ? C33 C32 C31 119.4(9) . . ? C32 C33 C34 116.7(9) . . ? C32 C33 C36 121.4(9) . . ? C34 C33 C36 121.8(9) . . ? C35 C34 C33 120.0(9) . . ? N3 C35 C34 123.2(9) . . ? C51 N5 C51 119.7(7) 2 . ? N5 C51 C52 121.9(5) . . ? C51 C52 C53 117.9(5) . . ? C51 C52 N7 103(4) . 2 ? C53 C52 N7 73(2) . 2 ? C52 C53 C52 120.1(7) . 2 ? C52 C53 C54 119.9(3) . . ? C52 C53 C54 119.9(3) 2 . ? C85 C41 C75 71.4(19) . . ? C85 C41 C43 114(2) . . ? C75 C41 C43 120.0(4) . . ? C85 C41 C76 84.6(19) . . ? C75 C41 C76 120.0(6) . . ? C43 C41 C76 120.0(6) . . ? C72 C43 C82 67.6(19) . . ? C72 C43 C41 123(3) . . ? C82 C43 C41 120.1(4) . . ? C72 C43 C86 80(2) . . ? C82 C43 C86 120.1(6) . . ? C41 C43 C86 119.8(6) . . ? C71 N7 C72 119.6(4) . . ? C71 N7 C52 96(2) . 2 ? C72 N7 C52 144(2) . 2 ? C71 C75 C41 113(3) . . ? N7 C72 C43 117(3) . . ? N7 C71 C75 127(4) . . ? C81 N8 C85 119.8(5) . . ? C81 C82 C43 122(2) . . ? N8 C85 C41 126(2) . . ? N8 C81 C82 118(2) . . ? #============================================================================== data_p87_295 _database_code_CSD 173997 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.64 H27 Fe3 N3.94 O13' _chemical_formula_weight 813.88 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' #============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.495(5) _cell_length_b 27.532(6) _cell_length_c 12.685(3) _cell_angle_alpha 90.000(12) _cell_angle_beta 96.221(9) _cell_angle_gamma 90.000(10) _cell_volume 8505(3) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 23.098 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3315 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS, Sheldrick 1996)' #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_reflns_number 42046 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.97 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.974 _reflns_number_total 9983 _reflns_number_gt 5596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'SAINT+ V5.01 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+18.6138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9983 _refine_ls_number_parameters 422 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1481 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2984 _refine_ls_wR_factor_gt 0.2401 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.278 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.126 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36123(3) 0.22950(3) 0.36080(6) 0.0463(3) Uani 1 1 d . . . Fe2 Fe 0.23653(3) 0.22743(3) 0.23980(6) 0.0390(2) Uani 1 1 d . . . Fe3 Fe 0.29916(4) 0.12320(3) 0.30549(7) 0.0510(3) Uani 1 1 d . . . O1 O 0.29813(14) 0.19518(13) 0.3027(3) 0.0420(8) Uani 1 1 d . . . O2 O 0.2201(2) 0.11658(16) 0.3518(4) 0.0690(13) Uani 1 1 d . . . O3 O 0.17822(17) 0.18666(14) 0.3029(3) 0.0512(10) Uani 1 1 d . . . O4 O 0.2695(2) 0.11770(17) 0.1427(4) 0.0721(14) Uani 1 1 d . . . O5 O 0.22644(18) 0.18723(15) 0.1047(3) 0.0543(10) Uani 1 1 d . . . O6 O 0.41843(18) 0.1883(2) 0.2955(4) 0.0676(13) Uani 1 1 d . . . O7 O 0.3785(2) 0.11631(19) 0.2612(5) 0.0765(14) Uani 1 1 d . . . O8 O 0.37323(17) 0.19040(17) 0.4987(3) 0.0573(11) Uani 1 1 d . . . O9 O 0.3286(2) 0.12040(16) 0.4682(4) 0.0672(12) Uani 1 1 d . . . O10 O 0.31825(17) 0.28298(15) 0.4320(3) 0.0536(10) Uani 1 1 d . . . O11 O 0.23201(16) 0.27706(15) 0.3583(3) 0.0500(9) Uani 1 1 d . . . O12 O 0.36546(18) 0.27539(18) 0.2320(4) 0.0639(12) Uani 1 1 d . . . O13 O 0.27846(17) 0.27723(15) 0.1591(3) 0.0521(10) Uani 1 1 d . . . C1 C 0.1807(3) 0.1453(2) 0.3413(5) 0.0575(16) Uani 1 1 d . . . H1A H 0.1485 0.1342 0.3658 0.086 Uiso 1 1 calc R . . C2 C 0.2433(3) 0.1462(2) 0.0841(5) 0.0598(17) Uani 1 1 d . . . H2A H 0.2348 0.1358 0.0144 0.090 Uiso 1 1 calc R . . C3 C 0.4160(3) 0.1452(3) 0.2638(5) 0.0654(19) Uani 1 1 d . . . H3A H 0.4478 0.1336 0.2385 0.098 Uiso 1 1 calc R . . C4 C 0.3562(3) 0.1499(3) 0.5240(5) 0.0610(16) Uani 1 1 d . . . H4A H 0.3655 0.1407 0.5942 0.091 Uiso 1 1 calc R . . C5 C 0.2688(2) 0.2927(2) 0.4228(4) 0.0485(13) Uani 1 1 d . . . H5A H 0.2579 0.3149 0.4715 0.073 Uiso 1 1 calc R . . C6 C 0.3273(3) 0.2886(2) 0.1659(5) 0.0516(14) Uani 1 1 d . . . H6A H 0.3369 0.3100 0.1143 0.077 Uiso 1 1 calc R . . N1 N 0.4328(2) 0.2719(2) 0.4344(4) 0.0588(14) Uani 1 1 d . . . C11 C 0.4351(3) 0.2897(3) 0.5330(5) 0.0588(16) Uani 1 1 d . . . H11A H 0.4047 0.2855 0.5700 0.088 Uiso 1 1 calc R . . C12 C 0.4785(3) 0.3129(3) 0.5807(6) 0.075(2) Uani 1 1 d . . . H12A H 0.4774 0.3246 0.6492 0.112 Uiso 1 1 calc R . . C13 C 0.5258(3) 0.3201(3) 0.5300(7) 0.072(2) Uani 1 1 d . . . C14 C 0.5230(3) 0.3015(4) 0.4278(7) 0.087(2) Uani 1 1 d . . . H14A H 0.5529 0.3051 0.3890 0.131 Uiso 1 1 calc R . . C15 C 0.4773(3) 0.2779(3) 0.3831(6) 0.081(2) Uani 1 1 d . . . H15A H 0.4770 0.2656 0.3148 0.121 Uiso 1 1 calc R . . C16 C 0.5753(4) 0.3448(4) 0.5815(9) 0.111(3) Uani 1 1 d . . . H16A H 0.5684 0.3559 0.6505 0.167 Uiso 1 1 calc R . . H16B H 0.5840 0.3720 0.5391 0.167 Uiso 1 1 calc R . . H16C H 0.6055 0.3225 0.5882 0.167 Uiso 1 1 calc R . . N2 N 0.16366(19) 0.26714(16) 0.1655(4) 0.0442(10) Uani 1 1 d . . . C21 C 0.1225(3) 0.2789(2) 0.2211(5) 0.0539(15) Uani 1 1 d . . . H21A H 0.1258 0.2717 0.2931 0.081 Uiso 1 1 calc R . . C22 C 0.0760(3) 0.3011(3) 0.1767(6) 0.0678(18) Uani 1 1 d . . . H22A H 0.0481 0.3082 0.2185 0.102 Uiso 1 1 calc R . . C23 C 0.0695(3) 0.3134(3) 0.0691(6) 0.075(2) Uani 1 1 d . . . C24 C 0.1130(3) 0.3014(3) 0.0115(6) 0.073(2) Uani 1 1 d . . . H24A H 0.1110 0.3086 -0.0604 0.109 Uiso 1 1 calc R . . C25 C 0.1589(3) 0.2789(2) 0.0615(5) 0.0506(14) Uani 1 1 d . . . H25A H 0.1878 0.2715 0.0223 0.076 Uiso 1 1 calc R . . C26 C 0.0198(4) 0.3378(4) 0.0196(10) 0.121(4) Uani 1 1 d . . . H26A H -0.0050 0.3433 0.0720 0.182 Uiso 1 1 calc R . . H26B H 0.0023 0.3177 -0.0360 0.182 Uiso 1 1 calc R . . H26C H 0.0296 0.3684 -0.0095 0.182 Uiso 1 1 calc R . . N3 N 0.2990(2) 0.0437(2) 0.3054(4) 0.0642(15) Uani 1 1 d . . . C31 C 0.3136(4) 0.0188(3) 0.2241(7) 0.075(2) Uani 1 1 d . . . H31A H 0.3252 0.0358 0.1672 0.113 Uiso 1 1 calc R . . C32 C 0.3126(4) -0.0315(3) 0.2197(8) 0.094(3) Uani 1 1 d . . . H32A H 0.3224 -0.0474 0.1601 0.141 Uiso 1 1 calc R . . C33 C 0.2970(4) -0.0575(3) 0.3030(7) 0.084(3) Uani 1 1 d . . . C34 C 0.2851(5) -0.0319(3) 0.3884(8) 0.097(3) Uani 1 1 d . . . H34A H 0.2770 -0.0484 0.4488 0.145 Uiso 1 1 calc R . . C35 C 0.2849(4) 0.0178(3) 0.3879(7) 0.078(2) Uani 1 1 d . . . H35A H 0.2745 0.0342 0.4467 0.117 Uiso 1 1 calc R . . C36 C 0.2938(6) -0.1127(3) 0.2986(10) 0.142(6) Uani 1 1 d . . . H36A H 0.2832 -0.1249 0.3644 0.213 Uiso 1 1 calc R . . H36B H 0.3291 -0.1257 0.2872 0.213 Uiso 1 1 calc R . . H36C H 0.2671 -0.1224 0.2415 0.213 Uiso 1 1 calc R . . C41 C 0.1475(10) -0.0679(8) 0.117(2) 0.244(8) Uiso 0.659(15) 1 d PD . . C43 C 0.1540(8) -0.0216(8) 0.1623(18) 0.244(8) Uiso 0.659(15) 1 d PD . . N8 N 0.1327(7) -0.0995(9) 0.287(2) 0.244(8) Uiso 0.659(15) 1 d PD . . C82 C 0.1499(9) -0.0148(10) 0.2685(18) 0.244(8) Uiso 0.659(15) 1 d PD . . C85 C 0.1370(9) -0.1052(10) 0.183(2) 0.244(8) Uiso 0.659(15) 1 d PD . . C81 C 0.1391(9) -0.0548(10) 0.329(2) 0.244(8) Uiso 0.659(15) 1 d PD . . C86 C 0.1658(13) 0.0208(10) 0.092(2) 0.293(10) Uiso 0.659(15) 1 d PD . . N5 N 0.0000 0.0685(14) 0.2500 0.301(19) Uiso 0.56(3) 2 d SPD . . C51 C 0.020(2) 0.0442(13) 0.3376(14) 0.301(19) Uiso 0.56(3) 1 d PD . . C52 C 0.007(2) -0.0043(14) 0.3455(4) 0.301(19) Uiso 0.56(3) 1 d PD . . C53 C 0.0000 -0.0291(15) 0.2500 0.301(19) Uiso 0.56(3) 2 d SPD . . C54 C 0.0000 -0.0840(15) 0.2500 0.36(2) Uiso 0.56(3) 2 d SPD . . 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 0.0420(5) 0.0617(6) 0.0351(4) 0.0002(3) 0.0040(3) -0.0012(4) Fe2 0.0420(4) 0.0426(4) 0.0322(4) 0.0006(3) 0.0034(3) 0.0032(3) Fe3 0.0567(5) 0.0468(5) 0.0485(5) 0.0000(4) 0.0010(4) 0.0072(4) O1 0.046(2) 0.042(2) 0.0373(19) 0.0014(15) 0.0033(15) 0.0026(16) O2 0.066(3) 0.050(3) 0.092(4) 0.009(2) 0.011(3) 0.001(2) O3 0.053(2) 0.048(2) 0.052(2) 0.0118(18) 0.0064(19) 0.0008(18) O4 0.100(4) 0.056(3) 0.056(3) -0.006(2) -0.013(3) 0.027(3) O5 0.069(3) 0.050(2) 0.042(2) -0.0040(18) -0.0038(19) 0.011(2) O6 0.048(3) 0.086(4) 0.070(3) -0.013(3) 0.010(2) -0.001(2) O7 0.060(3) 0.071(3) 0.100(4) -0.008(3) 0.014(3) 0.010(3) O8 0.055(3) 0.074(3) 0.041(2) 0.005(2) -0.0010(18) -0.006(2) O9 0.087(3) 0.054(3) 0.058(3) 0.008(2) -0.008(2) -0.005(2) O10 0.048(2) 0.062(3) 0.049(2) -0.0108(19) 0.0000(18) -0.0029(19) O11 0.044(2) 0.060(2) 0.046(2) -0.0097(18) 0.0018(18) 0.0056(18) O12 0.051(3) 0.087(3) 0.053(3) 0.012(2) 0.002(2) -0.015(2) O13 0.048(2) 0.060(2) 0.049(2) 0.0101(18) 0.0043(18) -0.0021(19) C1 0.057(4) 0.059(4) 0.056(4) 0.005(3) 0.008(3) -0.013(3) C2 0.079(5) 0.057(4) 0.042(3) -0.011(3) 0.000(3) 0.012(3) C3 0.052(4) 0.090(6) 0.056(4) -0.003(4) 0.014(3) 0.023(4) C4 0.063(4) 0.073(5) 0.046(4) 0.010(3) 0.002(3) 0.001(4) C5 0.049(3) 0.059(4) 0.037(3) -0.007(3) 0.004(3) 0.002(3) C6 0.057(4) 0.057(4) 0.042(3) 0.004(3) 0.011(3) -0.012(3) N1 0.046(3) 0.088(4) 0.042(3) 0.001(3) 0.003(2) -0.013(3) C11 0.051(4) 0.078(4) 0.049(4) -0.007(3) 0.014(3) -0.006(3) C12 0.061(4) 0.102(6) 0.059(4) -0.015(4) -0.003(3) -0.010(4) C13 0.059(4) 0.075(5) 0.080(5) -0.008(4) -0.003(4) -0.009(4) C14 0.059(5) 0.115(7) 0.089(6) -0.003(5) 0.014(4) -0.024(5) C15 0.058(4) 0.128(7) 0.058(4) -0.015(4) 0.015(3) -0.029(4) C16 0.070(6) 0.131(9) 0.128(9) -0.019(7) -0.013(5) -0.024(6) N2 0.049(3) 0.040(2) 0.043(3) -0.0013(19) 0.002(2) -0.001(2) C21 0.047(3) 0.063(4) 0.052(4) 0.001(3) 0.009(3) -0.001(3) C22 0.048(4) 0.075(5) 0.081(5) 0.007(4) 0.009(3) 0.013(3) C23 0.060(4) 0.086(5) 0.074(5) -0.001(4) -0.013(4) 0.019(4) C24 0.078(5) 0.086(5) 0.049(4) 0.006(4) -0.014(3) 0.019(4) C25 0.055(3) 0.056(3) 0.039(3) 0.000(2) -0.001(3) 0.008(3) C26 0.088(7) 0.152(10) 0.117(9) 0.010(7) -0.018(6) 0.049(7) N3 0.080(4) 0.052(3) 0.059(3) 0.005(3) 0.003(3) 0.011(3) C31 0.103(6) 0.054(4) 0.072(5) 0.006(3) 0.025(4) 0.014(4) C32 0.131(8) 0.062(5) 0.093(7) -0.004(4) 0.033(6) 0.021(5) C33 0.113(7) 0.054(4) 0.090(6) 0.013(4) 0.029(5) 0.022(4) C34 0.154(9) 0.053(4) 0.088(6) 0.011(4) 0.035(6) 0.007(5) C35 0.111(6) 0.056(4) 0.069(5) -0.006(3) 0.024(4) 0.001(4) C36 0.234(16) 0.048(5) 0.157(12) 0.004(5) 0.077(11) 0.021(6) #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.892(4) . ? Fe1 O6 2.047(5) . ? Fe1 O8 2.048(4) . ? Fe1 O10 2.073(4) . ? Fe1 O12 2.077(5) . ? Fe1 N1 2.227(5) . ? Fe2 O1 1.855(4) . ? Fe2 O5 2.033(4) . ? Fe2 O11 2.043(4) . ? Fe2 O3 2.046(4) . ? Fe2 O13 2.052(4) . ? Fe2 N2 2.215(5) . ? Fe3 O1 1.982(4) . ? Fe3 O7 2.089(5) . ? Fe3 O2 2.093(5) . ? Fe3 O9 2.113(5) . ? Fe3 O4 2.119(5) . ? Fe3 N3 2.190(6) . ? O2 C1 1.244(8) . ? O3 C1 1.237(8) . ? O4 C2 1.214(8) . ? O5 C2 1.242(7) . ? O6 C3 1.251(9) . ? O7 C3 1.214(9) . ? O8 C4 1.245(8) . ? O9 C4 1.229(8) . ? O10 C5 1.232(7) . ? O11 C5 1.228(7) . ? O12 C6 1.240(8) . ? O13 C6 1.230(7) . ? N1 C11 1.338(8) . ? N1 C15 1.338(8) . ? C11 C12 1.330(9) . ? C12 C13 1.399(11) . ? C13 C14 1.389(12) . ? C13 C16 1.477(11) . ? C14 C15 1.364(11) . ? N2 C21 1.331(7) . ? N2 C25 1.350(7) . ? C21 C22 1.361(9) . ? C22 C23 1.399(11) . ? C23 C24 1.395(11) . ? C23 C26 1.471(11) . ? C24 C25 1.377(9) . ? N3 C31 1.319(9) . ? N3 C35 1.341(9) . ? C31 C32 1.384(11) . ? C32 C33 1.366(11) . ? C33 C34 1.350(12) . ? C33 C36 1.523(12) . ? C34 C35 1.370(11) . ? C41 C85 1.368(10) . ? C41 C43 1.401(9) . ? C43 C82 1.375(9) . ? C43 C86 1.512(9) . ? N8 C81 1.346(10) . ? N8 C85 1.347(10) . ? C82 C81 1.387(10) . ? N5 C51 1.340(10) 2 ? N5 C51 1.340(10) . ? C51 C52 1.374(10) . ? C52 C53 1.386(10) . ? C53 C52 1.386(10) 2 ? C53 C54 1.511(10) . ? 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 O6 97.57(18) . . ? O1 Fe1 O8 96.08(16) . . ? O6 Fe1 O8 90.8(2) . . ? O1 Fe1 O10 95.31(16) . . ? O6 Fe1 O10 166.48(19) . . ? O8 Fe1 O10 91.93(18) . . ? O1 Fe1 O12 96.06(17) . . ? O6 Fe1 O12 85.6(2) . . ? O8 Fe1 O12 167.69(18) . . ? O10 Fe1 O12 88.95(19) . . ? O1 Fe1 N1 177.08(18) . . ? O6 Fe1 N1 85.3(2) . . ? O8 Fe1 N1 83.34(19) . . ? O10 Fe1 N1 81.86(19) . . ? O12 Fe1 N1 84.63(19) . . ? O1 Fe2 O5 96.94(16) . . ? O1 Fe2 O11 96.32(16) . . ? O5 Fe2 O11 166.69(17) . . ? O1 Fe2 O3 97.98(16) . . ? O5 Fe2 O3 90.27(18) . . ? O11 Fe2 O3 89.05(17) . . ? O1 Fe2 O13 96.11(16) . . ? O5 Fe2 O13 88.01(18) . . ? O11 Fe2 O13 89.42(17) . . ? O3 Fe2 O13 165.90(16) . . ? O1 Fe2 N2 179.02(17) . . ? O5 Fe2 N2 83.75(17) . . ? O11 Fe2 N2 82.98(16) . . ? O3 Fe2 N2 82.70(17) . . ? O13 Fe2 N2 83.21(17) . . ? O1 Fe3 O7 95.53(18) . . ? O1 Fe3 O2 94.69(16) . . ? O7 Fe3 O2 169.8(2) . . ? O1 Fe3 O9 93.23(16) . . ? O7 Fe3 O9 91.7(2) . . ? O2 Fe3 O9 87.2(2) . . ? O1 Fe3 O4 92.96(16) . . ? O7 Fe3 O4 87.8(2) . . ? O2 Fe3 O4 92.1(2) . . ? O9 Fe3 O4 173.81(19) . . ? O1 Fe3 N3 178.70(19) . . ? O7 Fe3 N3 84.9(2) . . ? O2 Fe3 N3 84.9(2) . . ? O9 Fe3 N3 87.97(19) . . ? O4 Fe3 N3 85.84(19) . . ? Fe2 O1 Fe1 121.4(2) . . ? Fe2 O1 Fe3 119.64(19) . . ? Fe1 O1 Fe3 118.95(18) . . ? C1 O2 Fe3 130.2(4) . . ? C1 O3 Fe2 130.8(4) . . ? C2 O4 Fe3 130.8(4) . . ? C2 O5 Fe2 131.4(4) . . ? C3 O6 Fe1 130.2(5) . . ? C3 O7 Fe3 131.1(5) . . ? C4 O8 Fe1 132.0(4) . . ? C4 O9 Fe3 130.3(4) . . ? C5 O10 Fe1 130.7(4) . . ? C5 O11 Fe2 129.0(4) . . ? C6 O12 Fe1 127.7(4) . . ? C6 O13 Fe2 132.1(4) . . ? O3 C1 O2 129.2(6) . . ? O4 C2 O5 128.6(6) . . ? O7 C3 O6 129.8(6) . . ? O9 C4 O8 128.5(6) . . ? O11 C5 O10 129.1(6) . . ? O13 C6 O12 129.0(6) . . ? C11 N1 C15 117.1(6) . . ? C11 N1 Fe1 122.3(4) . . ? C15 N1 Fe1 120.4(5) . . ? C12 C11 N1 123.4(6) . . ? C11 C12 C13 121.3(7) . . ? C14 C13 C12 114.7(7) . . ? C14 C13 C16 122.5(8) . . ? C12 C13 C16 122.8(8) . . ? C15 C14 C13 121.2(7) . . ? N1 C15 C14 122.2(7) . . ? C21 N2 C25 118.0(5) . . ? C21 N2 Fe2 121.1(4) . . ? C25 N2 Fe2 120.9(4) . . ? N2 C21 C22 122.6(6) . . ? C21 C22 C23 120.9(6) . . ? C24 C23 C22 116.2(6) . . ? C24 C23 C26 121.9(8) . . ? C22 C23 C26 121.8(8) . . ? C25 C24 C23 119.8(7) . . ? N2 C25 C24 122.5(6) . . ? C31 N3 C35 116.7(6) . . ? C31 N3 Fe3 121.2(5) . . ? C35 N3 Fe3 122.0(5) . . ? N3 C31 C32 123.0(7) . . ? C33 C32 C31 120.0(8) . . ? C34 C33 C32 116.7(8) . . ? C34 C33 C36 122.4(8) . . ? C32 C33 C36 120.9(8) . . ? C33 C34 C35 121.3(8) . . ? N3 C35 C34 122.2(7) . . ? C85 C41 C43 117(2) . . ? C82 C43 C41 120.6(9) . . ? C82 C43 C86 120.6(9) . . ? C41 C43 C86 118.8(8) . . ? C81 N8 C85 118.6(12) . . ? C43 C82 C81 119(2) . . ? N8 C85 C41 124(2) . . ? N8 C81 C82 122(2) . . ? C51 N5 C51 120.1(17) 2 . ? N5 C51 C52 118.9(17) . . ? C51 C52 C53 115.0(17) . . ? C52 C53 C52 120.8(17) . 2 ? C52 C53 C54 119.6(8) . . ? C52 C53 C54 119.6(8) 2 . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ #========================================================================= # END of CIF #=========================================================================