data_DSC91 _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_letter ? _publ_requested_journal ? _publ_requested_category ? # TITLE AND AUTHOR LIST _publ_section_title ? _publ_section_title_footnote ? loop_ _publ-author_name _publ_author_footnote _publ_author_address # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1996. Schagen, J.D., Straver, L., van Meurs, F., Williams, G., CAD4 Version 5.0, Delft Instruments X-ray Diffraction, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_cell_refinement 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1996)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C31 H31 Mn N7 2+, 2(Cl O4 1-)' _chemical_formula_sum 'C31 H31 Cl2 Mn N7 O8' _chemical_formula_iupac ? _chemical_formula_weight 755.5 _chemical_absolute_configuration ? # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.480(6) _cell_length_b 12.232(7) _cell_length_c 14.203(8) _cell_angle_alpha 111.36(3) _cell_angle_beta 97.77(3) _cell_angle_gamma 111.22(3) _cell_volume 1648(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.10 _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778.0 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T-min ? _exptl_absorpt_correction_T-max ? # EXPERIMENTAL DATA _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4563 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_theta_max 23 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 4 # REFINEMENT DATA _refine_special_details ; All ligand atoms were included in a 15-parameter TLX group thermal parameter. Anions were refined as identical ideal tetrahedral groups with a single refineable Cl-O distance, and their thermal motion was described using two 15-parameter TLX group parameters. ; _reflns_number_total 4299 _reflns_number_gt 3347 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.077 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4299 _refine_ls_number_parameters 196 _refine_ls_goodness_of_fit_ref 1.79 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 0.64 _refine_diff_density_min -0.48 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Mn 0.20457(6) 0.36238(6) 0.22890(5) 0.0395(3) Uani Mn 1.0 N1 0.3304(3) 0.2724(3) 0.1465(3) 0.0475(4) Uani N 1.0 N2 -0.0096(3) 0.2456(3) 0.1122(3) 0.0450(4) Uani N 1.0 N3 0.2069(3) 0.3950(3) 0.0726(3) 0.0470(4) Uani N 1.0 N4 0.2347(3) 0.5678(3) 0.2607(3) 0.0449(4) Uani N 1.0 N5 0.4334(3) 0.5162(3) 0.3611(3) 0.0481(4) Uani N 1.0 N6 0.1388(4) 0.2085(3) 0.2924(3) 0.0480(4) Uani N 1.0 N7 0.1801(3) 0.4634(4) 0.3989(3) 0.0478(4) Uani N 1.0 C1 0.2362(5) 0.2958(5) -0.0022(3) 0.0527(4) Uani C 1.0 C2 0.3416(5) 0.2790(5) 0.0555(4) 0.0531(5) Uani C 1.0 C3 0.4438(5) 0.2691(5) 0.0170(4) 0.0658(8) Uani C 1.0 C4 0.5375(5) 0.2523(5) 0.0742(5) 0.072(1) Uani C 1.0 C5 0.5263(5) 0.2430(5) 0.1658(4) 0.0659(9) Uani C 1.0 C6 0.4216(4) 0.2537(5) 0.1992(4) 0.0539(5) Uani C 1.0 C7 0.0779(4) 0.3835(4) 0.0274(3) 0.0508(4) Uani C 1.0 C8 -0.0318(4) 0.2725(4) 0.0296(3) 0.0495(4) Uani C 1.0 C9 -0.1519(5) 0.2048(5) -0.0486(4) 0.0593(5) Uani C 1.0 C10 -0.2540(5) 0.1087(5) -0.0422(4) 0.0641(5) Uani C 1.0 C11 -0.2343(4) 0.0829(5) 0.0434(4) 0.0600(5) Uani C 1.0 C12 -0.1111(4) 0.1512(4) 0.1174(4) 0.0506(4) Uani C 1.0 C13 0.3092(5) 0.5297(5) 0.1075(4) 0.0522(4) Uani C 1.0 C14 0.2972(4) 0.6226(4) 0.2044(4) 0.0502(4) Uani C 1.0 C15 0.3477(5) 0.7552(5) 0.2352(4) 0.0597(6) Uani C 1.0 C16 0.3325(5) 0.8338(5) 0.3281(4) 0.0629(8) Uani C 1.0 C17 0.2652(5) 0.7772(5) 0.3839(4) 0.0581(7) Uani C 1.0 C18 0.2184(4) 0.6432(4) 0.3494(3) 0.0494(4) Uani C 1.0 C19 0.1448(4) 0.5704(5) 0.4042(3) 0.0512(4) Uani C 1.0 C20 0.3060(5) 0.5161(5) 0.4815(3) 0.0531(3) Uani C 1.0 C21 0.4220(4) 0.5881(4) 0.4533(3) 0.0518(3) Uani C 1.0 C22 0.5073(5) 0.7176(5) 0.5149(4) 0.0600(4) Uani C 1.0 C23 0.6113(5) 0.7769(5) 0.4816(4) 0.0651(5) Uani C 1.0 C24 0.6265(5) 0.7032(5) 0.3902(4) 0.0628(6) Uani C 1.0 C25 0.5371(4) 0.5738(5) 0.3319(4) 0.0540(4) Uani C 1.0 C26 0.0766(5) 0.3626(5) 0.4137(4) 0.0545(4) Uani C 1.0 C27 0.0862(5) 0.2349(5) 0.3725(4) 0.0547(4) Uani C 1.0 C28 0.0324(5) 0.1446(5) 0.4107(4) 0.0682(6) Uani C 1.0 C29 0.0278(6) 0.0221(5) 0.3615(4) 0.0733(8) Uani C 1.0 C30 0.0798(5) -0.0073(5) 0.2787(4) 0.0654(7) Uani C 1.0 C31 0.1345(5) 0.0886(4) 0.2472(4) 0.0534(4) Uani C 1.0 Cl1A -0.1492(3) 0.5769(3) 0.2336(2) 0.058(2) Uani Cl 0.80 O1A -0.2642(5) 0.5693(7) 0.1767(5) 0.097(3) Uani O 0.80 O2A -0.1740(4) 0.5392(6) 0.3140(4) 0.120(3) Uani O 0.80 O3A -0.0497(5) 0.7062(3) 0.2794(5) 0.187(2) Uani O 0.80 O4A -0.1089(6) 0.4927(6) 0.1643(3) 0.141(4) Uani O 0.80 Cl1A' -0.1271(13) 0.5870(13) 0.2442(11) 0.064(2) Uani Cl 0.20 O1A' -0.2401(19) 0.5758(25) 0.1812(19) 0.087(3) Uani O 0.20 O2A' -0.0227(20) 0.6242(28) 0.2030(23) 0.173(4) Uani O 0.20 O3A' -0.1516(18) 0.4657(15) 0.2439(21) 0.105(3) Uani O 0.20 O4A' -0.0938(28) 0.6822(23) 0.3488(15) 0.201(4) Uani O 0.20 Cl1B 0.3278(5) 0.9577(6) -0.2906(4) 0.068(3) Uani Cl 0.51 O1B 0.2466(8) 0.8223(6) -0.3348(11) 0.108(4) Uani O 0.51 O2B 0.3437(13) 0.9948(15) -0.3724(7) 0.125(4) Uani O 0.51 O3B 0.4510(6) 0.9874(9) -0.2281(8) 0.113(2) Uani O 0.51 O4B 0.2699(10) 1.0262(8) -0.2270(8) 0.132(4) Uani O 0.51 Cl1B' 0.3471(6) 0.9478(6) -0.2968(4) 0.069(3) Uani Cl 0.49 O1B' 0.2430(8) 0.8271(7) -0.3206(11) 0.104(4) Uani O 0.49 O2B' 0.3704(11) 1.0390(8) -0.1928(5) 0.118(3) Uani O 0.49 O3B' 0.3143(14) 0.9940(15) -0.3686(8) 0.126(4) Uani O 0.49 O4B' 0.4607(8) 0.9312(9) -0.3051(10) 0.130(3) Uani O 0.49 H1C1 0.2659 0.3247 -0.0558 0.061 Uani H 1.0 H2C1 0.1551 0.2103 -0.0392 0.053 Uani H 1.0 HC3 0.4496 0.2742 -0.0511 0.075 Uani H 1.0 HC4 0.6132 0.2468 0.0487 0.085 Uani H 1.0 HC5 0.5921 0.2290 0.2076 0.075 Uani H 1.0 HC6 0.4135 0.2470 0.2664 0.054 Uani H 1.0 H1C7 0.0669 0.3686 -0.0480 0.058 Uani H 1.0 H2C7 0.0738 0.4671 0.0693 0.052 Uani H 1.0 HC9 -0.1641 0.2259 -0.1099 0.067 Uani H 1.0 HC10 -0.3412 0.0584 -0.0987 0.075 Uani H 1.0 HC11 -0.3078 0.0159 0.0520 0.068 Uani H 1.0 HC12 -0.0967 0.1294 0.1780 0.052 Uani H 1.0 H1C13 0.2981 0.5562 0.0493 0.060 Uani H 1.0 H2C13 0.3979 0.5323 0.1241 0.054 Uani H 1.0 HC15 0.3941 0.7944 0.1924 0.068 Uani H 1.0 HC16 0.3706 0.9309 0.3538 0.073 Uani H 1.0 HC17 0.2501 0.8318 0.4485 0.065 Uani H 1.0 H1C19 0.0483 0.5319 0.3688 0.053 Uani H 1.0 H2C19 0.1672 0.6327 0.4803 0.058 Uani H 1.0 H1C20 0.3154 0.4415 0.4896 0.056 Uani H 1.0 H2C20 0.3047 0.5778 0.5502 0.060 Uani H 1.0 HC22 0.4955 0.7691 0.5828 0.066 Uani H 1.0 HC23 0.6736 0.8721 0.5243 0.074 Uani H 1.0 HC24 0.7017 0.7427 0.3658 0.071 Uani H 1.0 HC25 0.5493 0.5200 0.2651 0.056 Uani H 1.0 H1C26 -0.0112 0.3477 0.3746 0.056 Uani H 1.0 H2C26 0.0859 0.3942 0.4912 0.063 Uani H 1.0 HC28 -0.0021 0.1678 0.4724 0.078 Uani H 1.0 HC29 -0.0134 -0.0456 0.3860 0.087 Uani H 1.0 HC30 0.0778 -0.0954 0.2428 0.073 Uani H 1.0 HC31 0.1730 0.0683 0.1876 0.053 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Mn 0.0424(4) 0.0451(4) 0.0363(4) 0.0207(3) 0.0155(3) 0.0210(3) Mn N1 0.0433(6) 0.0532(5) 0.0495(6) 0.0248(5) 0.0174(4) 0.0223(4) N N2 0.0397(6) 0.0495(5) 0.0454(6) 0.0199(4) 0.0115(4) 0.0215(4) N N3 0.0490(5) 0.0544(5) 0.0429(6) 0.0231(4) 0.0170(4) 0.0260(4) N N4 0.0438(6) 0.0469(6) 0.0466(5) 0.0211(4) 0.0138(4) 0.0227(4) N N5 0.0410(6) 0.0519(6) 0.0482(5) 0.0201(4) 0.0095(4) 0.0213(4) N N6 0.0495(6) 0.0520(5) 0.0482(5) 0.0223(4) 0.0162(4) 0.0283(5) N N7 0.0494(6) 0.0551(5) 0.0415(5) 0.0243(4) 0.0173(4) 0.0222(4) N C1 0.0563(6) 0.0618(6) 0.0440(6) 0.0269(5) 0.0218(5) 0.0251(5) C C2 0.0507(6) 0.0613(6) 0.0516(6) 0.0276(5) 0.0242(5) 0.0239(5) C C3 0.0596(8) 0.076(1) 0.0666(9) 0.0344(9) 0.0351(8) 0.0272(7) C C4 0.0562(8) 0.080(1) 0.083(1) 0.038(1) 0.0344(9) 0.0273(9) C C5 0.0499(7) 0.071(1) 0.079(1) 0.0358(8) 0.0222(7) 0.0259(8) C C6 0.0454(6) 0.0583(7) 0.0609(8) 0.0289(6) 0.0160(5) 0.0240(6) C C7 0.0539(6) 0.0576(6) 0.0445(6) 0.0256(4) 0.0118(5) 0.0271(5) C C8 0.0463(5) 0.0549(6) 0.0456(6) 0.0230(4) 0.0081(5) 0.0224(5) C C9 0.0519(6) 0.0632(8) 0.0533(7) 0.0249(5) 0.0015(6) 0.0222(6) C C10 0.0460(6) 0.0638(9) 0.0651(9) 0.0207(5) 0.0003(6) 0.0207(7) C C11 0.0406(6) 0.0583(7) 0.0679(9) 0.0167(5) 0.0088(5) 0.0230(6) C C12 0.0398(6) 0.0522(5) 0.0557(6) 0.0177(5) 0.0131(4) 0.0234(5) C C13 0.0539(6) 0.0573(6) 0.0522(6) 0.0224(4) 0.0213(5) 0.0320(5) C C14 0.0503(6) 0.0500(5) 0.0542(6) 0.0208(4) 0.0165(4) 0.0286(4) C C15 0.0608(9) 0.0512(5) 0.069(1) 0.0212(5) 0.0177(6) 0.0332(5) C C16 0.064(1) 0.0477(6) 0.073(1) 0.0233(5) 0.0143(8) 0.0266(5) C C17 0.059(1) 0.0486(6) 0.0623(9) 0.0260(5) 0.0138(7) 0.0193(5) C C18 0.0488(6) 0.0486(5) 0.0502(6) 0.0240(5) 0.0143(5) 0.0197(4) C C19 0.0515(6) 0.0556(6) 0.0473(5) 0.0271(5) 0.0188(5) 0.0194(5) C C20 0.0571(7) 0.0599(6) 0.0403(6) 0.0259(5) 0.0125(4) 0.0215(4) C C21 0.0485(6) 0.0544(6) 0.0451(5) 0.0215(4) 0.0072(5) 0.0187(5) C C22 0.0535(7) 0.0562(6) 0.0523(6) 0.0201(5) 0.0032(6) 0.0150(5) C C23 0.0483(7) 0.0559(6) 0.0678(9) 0.0148(6) 0.0030(6) 0.0176(6) C C24 0.0416(6) 0.0582(7) 0.073(1) 0.0146(5) 0.0098(5) 0.0237(6) C C25 0.0392(6) 0.0558(6) 0.0607(7) 0.0183(4) 0.0121(4) 0.0237(5) C C26 0.0575(7) 0.0643(7) 0.0480(5) 0.0265(5) 0.0251(5) 0.0290(5) C C27 0.0591(7) 0.0615(6) 0.0515(6) 0.0245(5) 0.0228(5) 0.0337(6) C C28 0.078(1) 0.0737(9) 0.0652(9) 0.0275(7) 0.0309(8) 0.046(1) C C29 0.084(1) 0.0705(8) 0.077(1) 0.0270(8) 0.0285(9) 0.051(1) C C30 0.072(1) 0.0582(6) 0.073(1) 0.0258(6) 0.0197(8) 0.0412(8) C C31 0.0559(7) 0.0516(5) 0.0578(7) 0.0238(5) 0.0156(5) 0.0307(5) C Cl1A 0.057(2) 0.069(3) 0.054(3) 0.031(2) 0.019(2) 0.032(3) Cl O1A 0.076(3) 0.151(5) 0.102(4) 0.061(3) 0.028(3) 0.086(5) O O2A 0.131(4) 0.226(7) 0.102(5) 0.119(4) 0.072(3) 0.122(5) O O3A 0.096(3) 0.093(2) 0.306(9) 0.003(2) -0.002(4) 0.083(3) O O4A 0.192(5) 0.202(6) 0.118(4) 0.153(5) 0.100(5) 0.079(4) O Cl1A' 0.057(2) 0.073(3) 0.065(3) 0.029(2) 0.017(2) 0.036(3) Cl O1A' 0.076(3) 0.135(5) 0.087(4) 0.058(3) 0.030(3) 0.075(4) O O2A' 0.109(3) 0.278(8) 0.317(9) 0.125(5) 0.136(5) 0.256(9) O O3A' 0.097(4) 0.111(4) 0.169(7) 0.067(3) 0.062(5) 0.097(5) O O4A' 0.211(7) 0.163(5) 0.098(5) 0.079(4) -0.038(3) -0.042(3) O Cl1B 0.064(4) 0.057(2) 0.058(6) 0.009(1) 0.014(2) 0.019(3) Cl O1B 0.089(4) 0.060(3) 0.118(7) -0.001(2) 0.018(3) 0.019(3) O O2B 0.142(6) 0.133(4) 0.091(6) 0.034(4) 0.031(4) 0.069(4) O O3B 0.074(2) 0.104(4) 0.123(7) 0.009(1) -0.005(2) 0.055(4) O O4B 0.140(5) 0.092(4) 0.179(8) 0.053(4) 0.103(5) 0.055(5) O Cl1B' 0.065(3) 0.057(2) 0.057(6) 0.009(1) 0.015(2) 0.018(3) Cl O1B' 0.082(4) 0.062(3) 0.124(7) 0.002(2) 0.023(3) 0.029(3) O O2B' 0.142(5) 0.085(3) 0.065(6) 0.016(2) 0.030(1) 0.006(3) O O3B' 0.127(6) 0.135(4) 0.103(6) 0.030(3) 0.015(4) 0.076(4) O O4B' 0.100(3) 0.104(5) 0.215(9) 0.048(3) 0.084(5) 0.084(6) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N1 2.310(3) 1_555 1_555 no Mn N2 2.337(3) 1_555 1_555 no Mn N3 2.396(3) 1_555 1_555 no Mn N4 2.267(3) 1_555 1_555 no Mn N5 2.546(3) 1_555 1_555 no Mn N6 2.306(3) 1_555 1_555 no Mn N7 2.387(3) 1_555 1_555 no N1 C2 1.344(5) 1_555 1_555 no N1 C6 1.341(5) 1_555 1_555 no N2 C8 1.345(5) 1_555 1_555 no N2 C12 1.345(5) 1_555 1_555 no N3 C1 1.472(6) 1_555 1_555 no N3 C7 1.468(5) 1_555 1_555 no N3 C13 1.480(5) 1_555 1_555 no N4 C14 1.342(5) 1_555 1_555 no N4 C18 1.348(5) 1_555 1_555 no N5 C21 1.340(5) 1_555 1_555 no N5 C25 1.351(5) 1_555 1_555 no N6 C27 1.350(5) 1_555 1_555 no N6 C31 1.349(5) 1_555 1_555 no N7 C19 1.484(6) 1_555 1_555 no N7 C20 1.483(5) 1_555 1_555 no N7 C26 1.475(5) 1_555 1_555 no C1 C2 1.488(6) 1_555 1_555 no C2 C3 1.386(6) 1_555 1_555 no C3 C4 1.381(7) 1_555 1_555 no C4 C5 1.366(7) 1_555 1_555 no C5 C6 1.382(6) 1_555 1_555 no C7 C8 1.496(6) 1_555 1_555 no C8 C9 1.382(6) 1_555 1_555 no C9 C10 1.368(7) 1_555 1_555 no C10 C11 1.374(7) 1_555 1_555 no C11 C12 1.380(6) 1_555 1_555 no C13 C14 1.493(6) 1_555 1_555 no C14 C15 1.376(6) 1_555 1_555 no C15 C16 1.398(7) 1_555 1_555 no C16 C17 1.371(7) 1_555 1_555 no C17 C18 1.385(6) 1_555 1_555 no C18 C19 1.501(6) 1_555 1_555 no C20 C21 1.504(6) 1_555 1_555 no C21 C22 1.368(6) 1_555 1_555 no C22 C23 1.396(7) 1_555 1_555 no C23 C24 1.361(7) 1_555 1_555 no C24 C25 1.372(6) 1_555 1_555 no C26 C27 1.507(7) 1_555 1_555 no C27 C28 1.389(6) 1_555 1_555 no C28 C29 1.381(7) 1_555 1_555 no C29 C30 1.381(7) 1_555 1_555 no C30 C31 1.378(6) 1_555 1_555 no Cl1A O1A 1.405(2) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn N2 107.3(1) 1_555 1_555 1_555 no N1 Mn N3 71.9(1) 1_555 1_555 1_555 no N1 Mn N4 121.7(1) 1_555 1_555 1_555 no N1 Mn N5 78.3(1) 1_555 1_555 1_555 no N1 Mn N6 91.4(1) 1_555 1_555 1_555 no N1 Mn N7 142.5(1) 1_555 1_555 1_555 no N2 Mn N3 71.6(1) 1_555 1_555 1_555 no N2 Mn N4 98.6(1) 1_555 1_555 1_555 no N2 Mn N5 172.5(1) 1_555 1_555 1_555 no N2 Mn N6 85.2(1) 1_555 1_555 1_555 no N2 Mn N7 104.3(1) 1_555 1_555 1_555 no N3 Mn N4 68.3(1) 1_555 1_555 1_555 no N3 Mn N5 106.3(1) 1_555 1_555 1_555 no N3 Mn N6 145.0(1) 1_555 1_555 1_555 no N3 Mn N7 138.6(1) 1_555 1_555 1_555 no N4 Mn N5 74.1(1) 1_555 1_555 1_555 no N4 Mn N6 143.0(1) 1_555 1_555 1_555 no N4 Mn N7 71.8(1) 1_555 1_555 1_555 no N5 Mn N6 99.7(1) 1_555 1_555 1_555 no N5 Mn N7 72.3(1) 1_555 1_555 1_555 no N6 Mn N7 71.6(1) 1_555 1_555 1_555 no Mn N1 C2 117.0(3) 1_555 1_555 1_555 no Mn N1 C6 122.1(3) 1_555 1_555 1_555 no C2 N1 C6 117.5(4) 1_555 1_555 1_555 no Mn N2 C8 116.6(3) 1_555 1_555 1_555 no Mn N2 C12 126.4(3) 1_555 1_555 1_555 no C8 N2 C12 117.0(4) 1_555 1_555 1_555 no Mn N3 C1 108.6(3) 1_555 1_555 1_555 no Mn N3 C7 108.0(2) 1_555 1_555 1_555 no Mn N3 C13 106.7(2) 1_555 1_555 1_555 no C1 N3 C7 111.8(3) 1_555 1_555 1_555 no C1 N3 C13 111.9(3) 1_555 1_555 1_555 no C7 N3 C13 109.7(3) 1_555 1_555 1_555 no Mn N4 C14 118.5(3) 1_555 1_555 1_555 no Mn N4 C18 119.9(3) 1_555 1_555 1_555 no C14 N4 C18 119.8(4) 1_555 1_555 1_555 no Mn N5 C21 108.7(3) 1_555 1_555 1_555 no Mn N5 C25 122.4(3) 1_555 1_555 1_555 no C21 N5 C25 117.9(4) 1_555 1_555 1_555 no Mn N6 C27 117.1(3) 1_555 1_555 1_555 no Mn N6 C31 124.6(3) 1_555 1_555 1_555 no C27 N6 C31 117.8(4) 1_555 1_555 1_555 no Mn N7 C19 109.4(2) 1_555 1_555 1_555 no Mn N7 C20 108.4(2) 1_555 1_555 1_555 no Mn N7 C26 108.4(3) 1_555 1_555 1_555 no C19 N7 C20 110.6(3) 1_555 1_555 1_555 no C19 N7 C26 110.8(3) 1_555 1_555 1_555 no C20 N7 C26 109.2(3) 1_555 1_555 1_555 no N3 C1 C2 110.3(4) 1_555 1_555 1_555 no N1 C2 C1 115.8(4) 1_555 1_555 1_555 no N1 C2 C3 122.3(4) 1_555 1_555 1_555 no C1 C2 C3 121.9(4) 1_555 1_555 1_555 no C2 C3 C4 118.8(5) 1_555 1_555 1_555 no C3 C4 C5 119.7(4) 1_555 1_555 1_555 no C4 C5 C6 118.2(5) 1_555 1_555 1_555 no N1 C6 C5 123.5(5) 1_555 1_555 1_555 no N3 C7 C8 112.0(4) 1_555 1_555 1_555 no N2 C8 C7 117.2(4) 1_555 1_555 1_555 no N2 C8 C9 122.3(4) 1_555 1_555 1_555 no C7 C8 C9 120.4(4) 1_555 1_555 1_555 no C8 C9 C10 119.9(4) 1_555 1_555 1_555 no C9 C10 C11 118.6(4) 1_555 1_555 1_555 no C10 C11 C12 118.8(4) 1_555 1_555 1_555 no N2 C12 C11 123.4(4) 1_555 1_555 1_555 no N3 C13 C14 109.8(4) 1_555 1_555 1_555 no N4 C14 C13 115.2(4) 1_555 1_555 1_555 no N4 C14 C15 121.9(4) 1_555 1_555 1_555 no C13 C14 C15 122.8(4) 1_555 1_555 1_555 no C14 C15 C16 118.3(4) 1_555 1_555 1_555 no C15 C16 C17 119.7(4) 1_555 1_555 1_555 no C16 C17 C18 119.1(4) 1_555 1_555 1_555 no N4 C18 C17 121.1(4) 1_555 1_555 1_555 no N4 C18 C19 114.8(4) 1_555 1_555 1_555 no C17 C18 C19 124.1(4) 1_555 1_555 1_555 no N7 C19 C18 110.8(3) 1_555 1_555 1_555 no N7 C20 C21 112.0(4) 1_555 1_555 1_555 no N5 C21 C20 114.7(4) 1_555 1_555 1_555 no N5 C21 C22 122.3(4) 1_555 1_555 1_555 no C20 C21 C22 123.0(4) 1_555 1_555 1_555 no C21 C22 C23 119.0(5) 1_555 1_555 1_555 no C22 C23 C24 119.0(5) 1_555 1_555 1_555 no C23 C24 C25 119.1(5) 1_555 1_555 1_555 no N5 C25 C24 122.7(4) 1_555 1_555 1_555 no N7 C26 C27 111.3(4) 1_555 1_555 1_555 no N6 C27 C26 117.5(4) 1_555 1_555 1_555 no N6 C27 C28 122.2(4) 1_555 1_555 1_555 no C26 C27 C28 120.1(4) 1_555 1_555 1_555 no C27 C28 C29 118.4(5) 1_555 1_555 1_555 no C28 C29 C30 120.2(5) 1_555 1_555 1_555 no C29 C30 C31 117.8(5) 1_555 1_555 1_555 no N6 C31 C30 123.4(4) 1_555 1_555 1_555 no O1A Cl1A O2A 109.47 1_555 1_555 1_555 no #===END data_DSC111 _audit_creation_method 'RAELSPUB and manual entry' # SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_letter ? _publ_requested_journal ? _publ_requested_category ? # TITLE AND AUTHOR LIST _publ_section_title ? _publ_section_title_footnote ? loop_ _publ_author_name _publ_author_footnote _publ_author_address ? ? ? # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1996. Schagen, J.D., Straver, L., van Meurs, F., Williams, G., CAD4 Version 5.0, Delft Instruments X-ray Diffraction, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_cell_refinement 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1996)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C31 H31 Fe N7 2+,2(Cl O4 1-)' _chemical_formula_sum 'C31 H31 Cl2 Fe N7 O8' _chemical_formula_iupac ? _chemical_formula_weight 756.4 _chemical_absolute_configuration ? # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.409(6) _cell_length_b 12.660(6) _cell_length_c 13.691(8) _cell_angle_alpha 71.41(3) _cell_angle_beta 67.61(3) _cell_angle_gamma 70.58(3) _cell_volume 1682(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780.0 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.97 # EXPERIMENTAL DATA _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6246 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 25 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; All ligand atoms were included in a 15-parameter TLX group thermal parameter. Anions were refined as identical ideal tetrahedral groups with a single refineable Cl-O distance, and their thermal motion was described using two 15-parameter TLX group parameters. ; _reflns_number_total 5917 _reflns_number_gt 4001 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_ref 0.075 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5917 _refine_ls_number_parameters 189 _refine_ls_goodness_of_fit_ref 1.43 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.91 _refine_diff_density_min -1.16 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.35712(5) 0.70414(5) 0.22631(4) 0.0364(2) Uani Fe 1.0 N1 0.2392(3) 0.7458(3) 0.1163(3) 0.0501(4) Uani N 1.0 N2 0.4136(3) 0.5058(3) 0.2896(3) 0.0412(4) Uani N 1.0 N3 0.1628(3) 0.6450(3) 0.3289(3) 0.0422(4) Uani N 1.0 N4 0.2795(3) 0.7590(3) 0.3782(3) 0.0403(3) Uani N 1.0 N5 0.3037(4) 0.9221(3) 0.1766(3) 0.0512(4) Uani N 1.0 N6 0.5355(3) 0.6660(3) 0.0835(3) 0.0446(4) Uani N 1.0 N7 0.5227(3) 0.7642(3) 0.2372(3) 0.0438(3) Uani N 1.0 C1 0.1070(4) 0.6242(4) 0.2584(4) 0.0513(4) Uani C 1.0 C2 0.1320(4) 0.7059(4) 0.1508(4) 0.0564(5) Uani C 1.0 C3 0.0492(5) 0.7362(5) 0.0896(4) 0.0755(7) Uani C 1.0 C4 0.0795(6) 0.8088(6) -0.0109(5) 0.0888(8) Uani C 1.0 C5 0.1879(6) 0.8517(5) -0.0472(4) 0.0817(7) Uani C 1.0 C6 0.2662(5) 0.8174(4) 0.0186(4) 0.0617(5) Uani C 1.0 C7 0.1922(4) 0.5397(4) 0.4109(3) 0.0446(4) Uani C 1.0 C8 0.3168(4) 0.4588(3) 0.3645(3) 0.0458(4) Uani C 1.0 C9 0.3320(5) 0.3416(4) 0.4014(4) 0.0586(6) Uani C 1.0 C10 0.4503(5) 0.2686(4) 0.3635(4) 0.0674(8) Uani C 1.0 C11 0.5510(5) 0.3154(4) 0.2892(4) 0.0616(6) Uani C 1.0 C12 0.5288(4) 0.4327(3) 0.2546(4) 0.0484(4) Uani C 1.0 C13 0.0757(4) 0.7388(4) 0.3827(3) 0.0466(4) Uani C 1.0 C14 0.1501(4) 0.7834(4) 0.4245(3) 0.0448(4) Uani C 1.0 C15 0.0895(4) 0.8468(4) 0.5041(4) 0.0550(4) Uani C 1.0 C16 0.1678(5) 0.8878(4) 0.5329(4) 0.0612(4) Uani C 1.0 C17 0.3008(5) 0.8629(4) 0.4854(4) 0.0575(3) Uani C 1.0 C18 0.3543(4) 0.7968(4) 0.4084(3) 0.0463(3) Uani C 1.0 C19 0.4983(4) 0.7604(4) 0.3530(4) 0.0481(3) Uani C 1.0 C20 0.5262(4) 0.8820(4) 0.1704(4) 0.0526(5) Uani C 1.0 C21 0.3933(5) 0.9609(4) 0.1872(4) 0.0557(5) Uani C 1.0 C22 0.3635(5) 1.0658(4) 0.2137(4) 0.0702(8) Uani C 1.0 C23 0.2366(6) 1.1332(4) 0.2272(5) 0.0802(9) Uani C 1.0 C24 0.1469(5) 1.0955(4) 0.2127(5) 0.0760(9) Uani C 1.0 C25 0.1830(5) 0.9899(4) 0.1883(4) 0.0614(6) Uani C 1.0 C26 0.6479(4) 0.6854(4) 0.1943(4) 0.0485(4) Uani C 1.0 C27 0.6518(4) 0.6589(4) 0.0927(4) 0.0487(4) Uani C 1.0 C28 0.7686(4) 0.6203(4) 0.0188(4) 0.0602(7) Uani C 1.0 C29 0.7680(5) 0.5845(5) -0.0657(4) 0.0671(8) Uani C 1.0 C30 0.6501(5) 0.5907(4) -0.0765(4) 0.0641(6) Uani C 1.0 C31 0.5376(4) 0.6306(4) -0.0002(3) 0.0528(4) Uani C 1.0 Cl1 0.7642(3) 0.9226(2) 0.3309(2) 0.053(2) Uani Cl 0.80 O1A 0.6472(3) 1.0024(4) 0.3169(5) 0.092(3) Uani O 0.80 O2A 0.7560(6) 0.8919(4) 0.4420(2) 0.084(2) Uani O 0.80 O3A 0.8716(4) 0.9731(4) 0.2692(3) 0.069(2) Uani O 0.80 O4A 0.7819(5) 0.8229(3) 0.2955(5) 0.108(3) Uani O 0.80 Cl1A' 0.7441(12) 0.9397(11) 0.3187(10) 0.057(2) Uani Cl 0.20 O1A' 0.6497(19) 1.0048(19) 0.2647(19) 0.120(4) Uani O 0.20 O2A' 0.6823(20) 0.9208(17) 0.4324(11) 0.084(2) Uani O 0.20 O3A' 0.8409(17) 1.0007(16) 0.2900(12) 0.063(2) Uani O 0.20 O4A' 0.8035(21) 0.8326(15) 0.2879(19) 0.101(3) Uani O 0.20 Cl1B 0.10354(9) 0.58691(9) 0.71909(8) 0.057(1) Uani Cl 1.0 O1B 0.0852(2) 0.4841(2) 0.7978(2) 0.089(1) Uani O 1.0 O2B 0.2267(2) 0.5644(2) 0.6392(2) 0.095(2) Uani O 1.0 O3B 0.0992(3) 0.6706(2) 0.7698(2) 0.123(2) Uani O 1.0 O4B 0.0031(2) 0.6285(2) 0.6696(2) 0.086(2) Uani O 1.0 H1C1 0.0106 0.6343 0.2936 0.059 Uani H 1.0 H2C1 0.1476 0.5439 0.2478 0.053 Uani H 1.0 HC3 -0.0310 0.7063 0.1175 0.085 Uani H 1.0 HC4 0.0221 0.8303 -0.0575 0.109 Uani H 1.0 HC5 0.2096 0.9061 -0.1191 0.096 Uani H 1.0 HC6 0.3464 0.8472 -0.0075 0.061 Uani H 1.0 H1C7 0.1191 0.5004 0.4389 0.052 Uani H 1.0 H2C7 0.2000 0.5615 0.4719 0.045 Uani H 1.0 HC9 0.2570 0.3098 0.4556 0.067 Uani H 1.0 HC10 0.4628 0.1834 0.3893 0.082 Uani H 1.0 HC11 0.6390 0.2650 0.2608 0.072 Uani H 1.0 HC12 0.6029 0.4658 0.2002 0.049 Uani H 1.0 H1C13 0.0038 0.7098 0.4447 0.052 Uani H 1.0 H2C13 0.0376 0.8025 0.3297 0.052 Uani H 1.0 HC15 -0.0073 0.8625 0.5395 0.062 Uani H 1.0 HC16 0.1271 0.9357 0.5885 0.073 Uani H 1.0 HC17 0.3577 0.8918 0.5060 0.067 Uani H 1.0 H1C19 0.5332 0.6803 0.3899 0.050 Uani H 1.0 H2C19 0.5434 0.8134 0.3574 0.057 Uani H 1.0 H1C20 0.5650 0.8783 0.0923 0.055 Uani H 1.0 H2C20 0.5819 0.9130 0.1904 0.061 Uani H 1.0 HC22 0.4314 1.0922 0.2228 0.079 Uani H 1.0 HC23 0.2115 1.2089 0.2473 0.095 Uani H 1.0 HC24 0.0560 1.1441 0.2198 0.089 Uani H 1.0 HC25 0.1162 0.9624 0.1789 0.064 Uani H 1.0 H1C26 0.6585 0.6124 0.2502 0.050 Uani H 1.0 H2C26 0.7209 0.7221 0.1769 0.057 Uani H 1.0 HC28 0.8530 0.6183 0.0266 0.068 Uani H 1.0 HC29 0.8521 0.5543 -0.1190 0.079 Uani H 1.0 HC30 0.6471 0.5667 -0.1382 0.075 Uani H 1.0 HC31 0.4523 0.6337 -0.0070 0.056 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0298(3) 0.0421(3) 0.0389(3) -0.0076(2) -0.0107(2) -0.0121(2) Fe N1 0.0449(6) 0.0592(6) 0.0486(6) -0.0040(4) -0.0261(5) -0.0097(4) N N2 0.0364(5) 0.0381(5) 0.0474(5) -0.0028(4) -0.0153(4) -0.0108(4) N N3 0.0319(5) 0.0474(5) 0.0492(5) -0.0055(4) -0.0152(4) -0.0140(4) N N4 0.0351(5) 0.0420(5) 0.0445(5) -0.0043(3) -0.0141(4) -0.0135(4) N N5 0.0498(6) 0.0389(5) 0.0562(5) -0.0028(4) -0.0180(4) -0.0055(4) N N6 0.0395(5) 0.0494(5) 0.0433(6) -0.0081(4) -0.0108(4) -0.0131(4) N N7 0.0358(5) 0.0476(6) 0.0508(5) -0.0094(4) -0.0136(4) -0.0148(4) N C1 0.0368(5) 0.0649(7) 0.0608(7) -0.0099(4) -0.0203(4) -0.0209(5) C C2 0.0441(6) 0.0737(8) 0.0601(8) -0.0061(5) -0.0299(6) -0.0174(6) C C3 0.0575(8) 0.106(1) 0.077(1) -0.0081(9) -0.044(1) -0.023(1) C C4 0.078(1) 0.122(2) 0.078(1) -0.007(1) -0.057(1) -0.015(1) C C5 0.082(2) 0.101(1) 0.0620(9) -0.006(1) -0.049(1) -0.0033(7) C C6 0.0622(9) 0.0710(8) 0.0501(6) -0.0055(6) -0.0323(7) -0.0038(5) C C7 0.0389(6) 0.0453(5) 0.0486(5) -0.0101(4) -0.0114(4) -0.0115(4) C C8 0.0433(5) 0.0397(5) 0.0513(5) -0.0075(4) -0.0137(4) -0.0098(4) C C9 0.0603(9) 0.0404(6) 0.0660(7) -0.0111(5) -0.0127(5) -0.0089(5) C C10 0.068(1) 0.0380(6) 0.0804(9) -0.0045(5) -0.0157(7) -0.0105(5) C C11 0.0553(7) 0.0398(6) 0.0768(9) 0.0027(5) -0.0170(6) -0.0149(4) C C12 0.0407(5) 0.0403(5) 0.0586(6) 0.0007(5) -0.0156(4) -0.0141(4) C C13 0.0313(6) 0.0509(6) 0.0558(6) -0.0024(4) -0.0138(4) -0.0170(4) C C14 0.0358(5) 0.0462(5) 0.0505(5) -0.0033(4) -0.0114(4) -0.0172(4) C C15 0.0451(6) 0.0568(7) 0.0600(6) -0.0062(5) -0.0063(5) -0.0273(6) C C16 0.0575(9) 0.0661(9) 0.0633(6) -0.0134(7) -0.0065(6) -0.0348(7) C C17 0.0558(9) 0.0661(8) 0.0598(6) -0.0162(6) -0.0122(6) -0.0312(6) C C18 0.0425(5) 0.0520(6) 0.0501(5) -0.0097(4) -0.0148(4) -0.0196(4) C C19 0.0403(5) 0.0582(7) 0.0546(6) -0.0115(4) -0.0179(4) -0.0201(5) C C20 0.0484(6) 0.0490(6) 0.0597(7) -0.0166(5) -0.0094(5) -0.0147(5) C C21 0.0561(7) 0.0408(6) 0.0636(7) -0.0113(4) -0.0122(5) -0.0108(4) C C22 0.073(1) 0.0431(7) 0.085(1) -0.0162(5) -0.0095(8) -0.0177(5) C C23 0.083(1) 0.0389(7) 0.100(1) -0.0060(4) -0.014(1) -0.0163(4) C C24 0.072(1) 0.0399(6) 0.093(1) 0.0062(5) -0.0224(9) -0.0092(5) C C25 0.0567(8) 0.0418(6) 0.0708(8) 0.0047(4) -0.0240(6) -0.0050(4) C C26 0.0328(5) 0.0567(7) 0.0580(7) -0.0086(4) -0.0132(4) -0.0186(5) C C27 0.0361(5) 0.0547(6) 0.0527(6) -0.0091(4) -0.0077(5) -0.0177(5) C C28 0.0401(5) 0.070(1) 0.0647(9) -0.0125(6) -0.0007(6) -0.0267(8) C C29 0.0523(6) 0.079(1) 0.0623(9) -0.0167(8) 0.0047(7) -0.0318(8) C C30 0.0605(8) 0.078(1) 0.0509(6) -0.0185(8) -0.0016(6) -0.0278(6) C C31 0.0512(6) 0.0631(7) 0.0439(6) -0.0130(5) -0.0099(4) -0.0182(4) C Cl1 0.038(2) 0.046(3) 0.078(3) -0.007(1) -0.022(1) -0.016(3) Cl O1A 0.057(2) 0.088(4) 0.150(5) 0.011(2) -0.063(2) -0.042(3) O O2A 0.085(3) 0.088(4) 0.074(2) -0.042(2) -0.026(2) 0.012(2) O O3A 0.057(2) 0.082(2) 0.069(3) -0.030(2) -0.013(2) -0.011(2) O O4A 0.063(3) 0.097(4) 0.196(6) -0.010(2) -0.036(3) -0.090(5) O Cl1A' 0.040(2) 0.055(3) 0.080(3) -0.006(1) -0.026(1) -0.019(3) Cl O1A' 0.094(4) 0.132(5) 0.162(6) 0.005(3) -0.095(5) -0.035(5) O O2A' 0.061(2) 0.105(4) 0.087(3) -0.043(2) -0.003(2) -0.023(2) O O3A' 0.058(2) 0.056(2) 0.073(4) -0.022(1) -0.023(1) 0.002(2) O O4A' 0.058(3) 0.097(4) 0.179(5) -0.007(2) -0.033(2) -0.087(5) O Cl1B 0.045(1) 0.055(2) 0.057(1) 0.0010(7) -0.0161(7) -0.008(1) Cl O1B 0.067(2) 0.082(2) 0.090(1) -0.016(1) -0.030(1) 0.022(2) O O2B 0.051(2) 0.120(2) 0.072(3) 0.001(1) -0.005(1) -0.007(2) O O3B 0.136(4) 0.098(3) 0.159(3) -0.002(2) -0.063(3) -0.065(3) O O4B 0.059(2) 0.096(2) 0.086(3) -0.006(2) -0.036(2) 0.007(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.219(3) 1_555 1_555 no Fe N2 2.331(3) 1_555 1_555 no Fe N3 2.347(3) 1_555 1_555 no Fe N4 2.167(3) 1_555 1_555 no Fe N5 2.539(3) 1_555 1_555 no Fe N6 2.261(3) 1_555 1_555 no Fe N7 2.326(3) 1_555 1_555 no N1 C2 1.339(5) 1_555 1_555 no N1 C6 1.343(5) 1_555 1_555 no N2 C8 1.347(5) 1_555 1_555 no N2 C12 1.344(5) 1_555 1_555 no N3 C1 1.466(5) 1_555 1_555 no N3 C7 1.478(5) 1_555 1_555 no N3 C13 1.469(5) 1_555 1_555 no N4 C14 1.336(5) 1_555 1_555 no N4 C18 1.340(5) 1_555 1_555 no N5 C21 1.342(6) 1_555 1_555 no N5 C25 1.339(5) 1_555 1_555 no N6 C27 1.350(5) 1_555 1_555 no N6 C31 1.347(5) 1_555 1_555 no N7 C19 1.489(5) 1_555 1_555 no N7 C20 1.485(5) 1_555 1_555 no N7 C26 1.472(5) 1_555 1_555 no C1 C2 1.492(6) 1_555 1_555 no C2 C3 1.377(6) 1_555 1_555 no C3 C4 1.378(8) 1_555 1_555 no C4 C5 1.370(8) 1_555 1_555 no C5 C6 1.380(6) 1_555 1_555 no C7 C8 1.494(5) 1_555 1_555 no C8 C9 1.379(6) 1_555 1_555 no C9 C10 1.375(6) 1_555 1_555 no C10 C11 1.372(7) 1_555 1_555 no C11 C12 1.374(6) 1_555 1_555 no C13 C14 1.503(6) 1_555 1_555 no C14 C15 1.388(6) 1_555 1_555 no C15 C16 1.389(6) 1_555 1_555 no C16 C17 1.373(6) 1_555 1_555 no C17 C18 1.385(6) 1_555 1_555 no C18 C19 1.502(6) 1_555 1_555 no C20 C21 1.491(6) 1_555 1_555 no C21 C22 1.386(6) 1_555 1_555 no C22 C23 1.390(7) 1_555 1_555 no C23 C24 1.362(8) 1_555 1_555 no C24 C25 1.373(7) 1_555 1_555 no C26 C27 1.514(6) 1_555 1_555 no C27 C28 1.375(6) 1_555 1_555 no C28 C29 1.374(7) 1_555 1_555 no C29 C30 1.382(7) 1_555 1_555 no C30 C31 1.371(6) 1_555 1_555 no Cl1 O1A 1.419(1) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe N2 109.4(1) 1_555 1_555 1_555 no N1 Fe N3 72.5(1) 1_555 1_555 1_555 no N1 Fe N4 122.5(1) 1_555 1_555 1_555 no N1 Fe N5 77.5(1) 1_555 1_555 1_555 no N1 Fe N6 87.0(1) 1_555 1_555 1_555 no N1 Fe N7 138.7(1) 1_555 1_555 1_555 no N2 Fe N3 72.6(1) 1_555 1_555 1_555 no N2 Fe N4 100.0(1) 1_555 1_555 1_555 no N2 Fe N5 172.8(1) 1_555 1_555 1_555 no N2 Fe N6 82.9(1) 1_555 1_555 1_555 no N2 Fe N7 103.1(1) 1_555 1_555 1_555 no N3 Fe N4 71.0(1) 1_555 1_555 1_555 no N3 Fe N5 108.7(1) 1_555 1_555 1_555 no N3 Fe N6 139.9(1) 1_555 1_555 1_555 no N3 Fe N7 143.5(1) 1_555 1_555 1_555 no N4 Fe N5 74.0(1) 1_555 1_555 1_555 no N4 Fe N6 146.1(1) 1_555 1_555 1_555 no N4 Fe N7 74.3(1) 1_555 1_555 1_555 no N5 Fe N6 99.7(1) 1_555 1_555 1_555 no N5 Fe N7 71.6(1) 1_555 1_555 1_555 no N6 Fe N7 72.2(1) 1_555 1_555 1_555 no Fe N1 C2 119.5(3) 1_555 1_555 1_555 no Fe N1 C6 121.8(3) 1_555 1_555 1_555 no C2 N1 C6 118.5(4) 1_555 1_555 1_555 no Fe N2 C8 115.8(3) 1_555 1_555 1_555 no Fe N2 C12 127.4(3) 1_555 1_555 1_555 no C8 N2 C12 116.6(3) 1_555 1_555 1_555 no Fe N3 C1 110.3(3) 1_555 1_555 1_555 no Fe N3 C7 108.5(2) 1_555 1_555 1_555 no Fe N3 C13 105.6(2) 1_555 1_555 1_555 no C1 N3 C7 110.9(3) 1_555 1_555 1_555 no C1 N3 C13 111.7(3) 1_555 1_555 1_555 no C7 N3 C13 109.8(3) 1_555 1_555 1_555 no Fe N4 C14 118.2(3) 1_555 1_555 1_555 no Fe N4 C18 119.7(3) 1_555 1_555 1_555 no C14 N4 C18 119.7(3) 1_555 1_555 1_555 no Fe N5 C21 110.5(3) 1_555 1_555 1_555 no Fe N5 C25 124.7(3) 1_555 1_555 1_555 no C21 N5 C25 118.0(4) 1_555 1_555 1_555 no Fe N6 C27 116.7(3) 1_555 1_555 1_555 no Fe N6 C31 125.0(3) 1_555 1_555 1_555 no C27 N6 C31 117.2(4) 1_555 1_555 1_555 no Fe N7 C19 108.2(2) 1_555 1_555 1_555 no Fe N7 C20 110.6(3) 1_555 1_555 1_555 no Fe N7 C26 108.0(2) 1_555 1_555 1_555 no C19 N7 C20 110.7(3) 1_555 1_555 1_555 no C19 N7 C26 110.9(3) 1_555 1_555 1_555 no C20 N7 C26 108.4(3) 1_555 1_555 1_555 no N3 C1 C2 111.0(4) 1_555 1_555 1_555 no N1 C2 C1 116.9(4) 1_555 1_555 1_555 no N1 C2 C3 122.1(5) 1_555 1_555 1_555 no C1 C2 C3 120.9(4) 1_555 1_555 1_555 no C2 C3 C4 118.5(5) 1_555 1_555 1_555 no C3 C4 C5 120.3(5) 1_555 1_555 1_555 no C4 C5 C6 117.9(5) 1_555 1_555 1_555 no N1 C6 C5 122.7(5) 1_555 1_555 1_555 no N3 C7 C8 111.6(3) 1_555 1_555 1_555 no N2 C8 C7 116.9(3) 1_555 1_555 1_555 no N2 C8 C9 122.3(4) 1_555 1_555 1_555 no C7 C8 C9 120.7(4) 1_555 1_555 1_555 no C8 C9 C10 120.0(4) 1_555 1_555 1_555 no C9 C10 C11 118.3(4) 1_555 1_555 1_555 no C10 C11 C12 118.8(4) 1_555 1_555 1_555 no N2 C12 C11 123.9(4) 1_555 1_555 1_555 no N3 C13 C14 110.3(3) 1_555 1_555 1_555 no N4 C14 C13 115.1(3) 1_555 1_555 1_555 no N4 C14 C15 122.1(4) 1_555 1_555 1_555 no C13 C14 C15 122.8(4) 1_555 1_555 1_555 no C14 C15 C16 117.7(4) 1_555 1_555 1_555 no C15 C16 C17 120.3(4) 1_555 1_555 1_555 no C16 C17 C18 118.5(4) 1_555 1_555 1_555 no N4 C18 C17 121.6(4) 1_555 1_555 1_555 no N4 C18 C19 114.5(3) 1_555 1_555 1_555 no C17 C18 C19 123.9(4) 1_555 1_555 1_555 no N7 C19 C18 110.1(3) 1_555 1_555 1_555 no N7 C20 C21 112.0(4) 1_555 1_555 1_555 no N5 C21 C20 115.0(4) 1_555 1_555 1_555 no N5 C21 C22 122.3(4) 1_555 1_555 1_555 no C20 C21 C22 122.7(5) 1_555 1_555 1_555 no C21 C22 C23 118.2(5) 1_555 1_555 1_555 no C22 C23 C24 119.5(5) 1_555 1_555 1_555 no C23 C24 C25 119.0(5) 1_555 1_555 1_555 no N5 C25 C24 122.9(5) 1_555 1_555 1_555 no N7 C26 C27 110.5(3) 1_555 1_555 1_555 no N6 C27 C26 116.4(4) 1_555 1_555 1_555 no N6 C27 C28 122.3(4) 1_555 1_555 1_555 no C26 C27 C28 121.1(4) 1_555 1_555 1_555 no C27 C28 C29 119.3(4) 1_555 1_555 1_555 no C28 C29 C30 119.4(4) 1_555 1_555 1_555 no C29 C30 C31 118.1(4) 1_555 1_555 1_555 no N6 C31 C30 123.6(4) 1_555 1_555 1_555 no O1A Cl1 O2A 109.47(0) 1_555 1_555 1_555 no #===END