# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Keith Murray,' _publ_contact_author_email k.s.murray@sci.monash.edu.au _publ_section_title ; Spin crossover in polynuclear and heterometallic FeII species containing polytopic mono-aza-crown/dipyridylamino ligands ; loop_ _publ_author_name K.Murray T.Ross B.Moubaraki S.Batten # Attachment '- DaltonCrown.CIF' #TrackingRef '- DaltonCrown.CIF' data_1a _database_code_depnum_ccdc_archive 'CCDC 823862' #TrackingRef '- DaltonCrown.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DCrCr5)2(Na)2](ClO4)2.4CH3CH2CH2OH ; _chemical_name_common trans-(Fe(ii)(NCS)2(DCrCr5)2(Na)2)(ClO4)2.4CH3CH2CH2OH _chemical_melting_point ? _chemical_formula_moiety '(Fe S2 Na2 C68 H96 O16 N18), 2(Cl O4), 4(C3 H8 O)' _chemical_formula_sum 'C80 H128 Cl2 Fe N18 Na2 O28 S2' _chemical_formula_weight 2026.85 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2574(7) _cell_length_b 13.2322(8) _cell_length_c 16.4992(10) _cell_angle_alpha 76.909(2) _cell_angle_beta 87.406(2) _cell_angle_gamma 65.031(2) _cell_volume 2359.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 15330 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9652 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15330 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8052 _reflns_number_gt 5387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8052 _refine_ls_number_parameters 608 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.0000 0.0000 0.5000 0.01194(18) Uani 1 2 d S . . S1 S -0.16832(9) 0.35544(8) 0.57996(6) 0.0257(2) Uani 1 1 d . . . O2 O 0.4986(2) 0.26460(19) 0.94098(14) 0.0192(6) Uani 1 1 d . . . O1 O 0.3579(2) 0.23048(19) 0.82673(14) 0.0197(6) Uani 1 1 d . . . O6 O -0.6664(2) 0.61850(19) 0.75881(14) 0.0193(6) Uani 1 1 d . . . O8 O -0.4156(2) 0.28530(19) 0.71626(14) 0.0184(6) Uani 1 1 d . . . O7 O -0.6430(2) 0.46298(19) 0.66461(14) 0.0178(6) Uani 1 1 d . . . O5 O -0.4191(2) 0.48618(19) 0.81348(14) 0.0198(6) Uani 1 1 d . . . O4 O 0.1362(2) 0.4780(2) 0.85121(14) 0.0215(6) Uani 1 1 d . . . N7 N -0.0360(2) 0.2586(2) 0.78640(17) 0.0163(7) Uani 1 1 d . . . N4 N -0.0036(2) -0.0920(2) 0.61244(16) 0.0110(6) Uani 1 1 d . . . O3 O 0.3344(2) 0.4850(2) 0.93767(14) 0.0221(6) Uani 1 1 d . . . N1 N -0.0755(2) 0.1421(2) 0.53751(16) 0.0144(7) Uani 1 1 d . . . N5 N 0.1181(2) 0.1449(2) 0.70789(17) 0.0163(7) Uani 1 1 d . . . N2 N 0.1632(2) -0.0227(2) 0.53676(17) 0.0134(6) Uani 1 1 d . . . N3 N 0.0980(2) -0.0066(2) 0.67174(16) 0.0129(6) Uani 1 1 d . . . N6 N -0.0455(2) 0.0963(2) 0.75137(16) 0.0138(6) Uani 1 1 d . . . C5 C 0.3041(3) -0.0349(3) 0.6399(2) 0.0170(8) Uani 1 1 d . . . H5 H 0.3195 -0.0324 0.6952 0.020 Uiso 1 1 calc R . . N8 N 0.1194(3) 0.3062(2) 0.73871(18) 0.0201(7) Uani 1 1 d . . . N9 N -0.1930(2) 0.2089(2) 0.82308(17) 0.0160(7) Uani 1 1 d . . . C12 C 0.0558(3) 0.0828(3) 0.7138(2) 0.0134(8) Uani 1 1 d . . . C34 C -0.2602(3) 0.1419(3) 0.8170(2) 0.0179(8) Uani 1 1 d . . . H34A H -0.3216 0.1541 0.8593 0.022 Uiso 1 1 calc R . . H34B H -0.2040 0.0596 0.8304 0.022 Uiso 1 1 calc R . . C1 C -0.1153(3) 0.2304(3) 0.5553(2) 0.0159(8) Uani 1 1 d . . . C14 C 0.0649(3) 0.2343(3) 0.7449(2) 0.0165(8) Uani 1 1 d . . . C2 C 0.2539(3) -0.0442(3) 0.4834(2) 0.0170(8) Uani 1 1 d . . . H2 H 0.2381 -0.0497 0.4291 0.020 Uiso 1 1 calc R . . C6 C 0.1910(3) -0.0194(3) 0.6143(2) 0.0148(8) Uani 1 1 d . . . C26 C -0.2953(3) 0.4242(3) 0.7979(2) 0.0194(8) Uani 1 1 d . . . H26A H -0.2483 0.4671 0.8049 0.023 Uiso 1 1 calc R . . H26B H -0.2883 0.4131 0.7402 0.023 Uiso 1 1 calc R . . C13 C -0.0882(3) 0.1883(3) 0.7859(2) 0.0150(8) Uani 1 1 d . . . C33 C -0.3221(3) 0.1713(3) 0.7324(2) 0.0177(8) Uani 1 1 d . . . H33A H -0.2627 0.1651 0.6890 0.021 Uiso 1 1 calc R . . H33B H -0.3570 0.1166 0.7305 0.021 Uiso 1 1 calc R . . C7 C 0.0404(3) -0.0816(3) 0.6815(2) 0.0128(8) Uani 1 1 d . . . C9 C -0.0145(3) -0.2201(3) 0.7687(2) 0.0193(8) Uani 1 1 d . . . H9 H -0.0211 -0.2616 0.8224 0.023 Uiso 1 1 calc R . . C11 C -0.0483(3) -0.1714(3) 0.6217(2) 0.0157(8) Uani 1 1 d . . . H11 H -0.0748 -0.1838 0.5732 0.019 Uiso 1 1 calc R . . C31 C -0.5435(3) 0.4466(3) 0.6131(2) 0.0206(9) Uani 1 1 d . . . H31A H -0.5002 0.4908 0.6245 0.025 Uiso 1 1 calc R . . H31B H -0.5721 0.4735 0.5537 0.025 Uiso 1 1 calc R . . C16 C 0.3402(3) 0.1873(3) 0.7584(2) 0.0208(9) Uani 1 1 d . . . H16A H 0.3236 0.1193 0.7800 0.025 Uiso 1 1 calc R . . H16B H 0.4144 0.1636 0.7271 0.025 Uiso 1 1 calc R . . C10 C -0.0570(3) -0.2350(3) 0.6981(2) 0.0198(8) Uani 1 1 d . . . H10 H -0.0915 -0.2881 0.7023 0.024 Uiso 1 1 calc R . . C30 C -0.7359(3) 0.5782(3) 0.6454(2) 0.0210(9) Uani 1 1 d . . . H30A H -0.8092 0.5798 0.6739 0.025 Uiso 1 1 calc R . . H30B H -0.7562 0.6029 0.5846 0.025 Uiso 1 1 calc R . . C8 C 0.0372(3) -0.1449(3) 0.7606(2) 0.0167(8) Uani 1 1 d . . . H8 H 0.0704 -0.1361 0.8081 0.020 Uiso 1 1 calc R . . C21 C 0.2097(3) 0.5622(3) 0.9357(2) 0.0209(9) Uani 1 1 d . . . H21A H 0.1917 0.6278 0.8873 0.025 Uiso 1 1 calc R . . H21B H 0.1947 0.5924 0.9868 0.025 Uiso 1 1 calc R . . C32 C -0.4610(3) 0.3216(3) 0.6318(2) 0.0212(9) Uani 1 1 d . . . H32A H -0.5053 0.2775 0.6221 0.025 Uiso 1 1 calc R . . H32B H -0.3932 0.3074 0.5944 0.025 Uiso 1 1 calc R . . C25 C -0.2474(3) 0.3083(3) 0.8603(2) 0.0202(9) Uani 1 1 d . . . H25A H -0.1865 0.3056 0.8992 0.024 Uiso 1 1 calc R . . H25B H -0.3147 0.3025 0.8935 0.024 Uiso 1 1 calc R . . C4 C 0.3936(3) -0.0540(3) 0.5846(2) 0.0207(9) Uani 1 1 d . . . H4 H 0.4716 -0.0641 0.6006 0.025 Uiso 1 1 calc R . . C29 C -0.6980(3) 0.6600(3) 0.6718(2) 0.0220(9) Uani 1 1 d . . . H29A H -0.6281 0.6637 0.6410 0.026 Uiso 1 1 calc R . . H29B H -0.7650 0.7377 0.6606 0.026 Uiso 1 1 calc R . . C3 C 0.3675(3) -0.0584(3) 0.5045(2) 0.0229(9) Uani 1 1 d . . . H3 H 0.4277 -0.0711 0.4648 0.028 Uiso 1 1 calc R . . C22 C 0.1268(3) 0.5083(3) 0.9299(2) 0.0222(9) Uani 1 1 d . . . H22A H 0.1479 0.4389 0.9755 0.027 Uiso 1 1 calc R . . H22B H 0.0429 0.5624 0.9357 0.027 Uiso 1 1 calc R . . C27 C -0.4627(3) 0.6038(3) 0.7712(2) 0.0211(9) Uani 1 1 d . . . H27A H -0.4545 0.6105 0.7105 0.025 Uiso 1 1 calc R . . H27B H -0.4154 0.6393 0.7910 0.025 Uiso 1 1 calc R . . C28 C -0.5933(3) 0.6635(3) 0.7890(2) 0.0218(9) Uani 1 1 d . . . H28A H -0.6002 0.6555 0.8499 0.026 Uiso 1 1 calc R . . H28B H -0.6235 0.7462 0.7626 0.026 Uiso 1 1 calc R . . C15 C 0.2364(3) 0.2782(3) 0.7013(2) 0.0230(9) Uani 1 1 d . . . H15A H 0.2501 0.3485 0.6850 0.028 Uiso 1 1 calc R . . H15B H 0.2341 0.2520 0.6500 0.028 Uiso 1 1 calc R . . C24 C 0.0477(3) 0.4214(3) 0.7522(2) 0.0249(9) Uani 1 1 d . . . H24A H -0.0372 0.4451 0.7340 0.030 Uiso 1 1 calc R . . H24B H 0.0762 0.4748 0.7157 0.030 Uiso 1 1 calc R . . C23 C 0.0503(4) 0.4354(3) 0.8406(2) 0.0272(9) Uani 1 1 d . . . H23A H -0.0306 0.4891 0.8528 0.033 Uiso 1 1 calc R . . H23B H 0.0715 0.3605 0.8802 0.033 Uiso 1 1 calc R . . Na1 Na 0.40703(14) 0.40478(12) 0.81224(8) 0.0261(4) Uani 1 1 d . . . Cl1 Cl 0.36387(8) 0.14247(8) 0.20833(6) 0.0244(2) Uani 1 1 d . . . O11 O 0.2829(2) 0.2620(2) 0.19475(18) 0.0366(7) Uani 1 1 d . . . O9 O 0.3234(2) 0.0916(2) 0.15368(16) 0.0328(7) Uani 1 1 d . . . O10 O 0.3639(3) 0.0852(2) 0.29336(16) 0.0418(8) Uani 1 1 d . . . O12 O 0.4843(2) 0.1300(2) 0.18940(17) 0.0376(7) Uani 1 1 d . . . C19 C 0.5003(3) 0.3189(3) 1.0065(2) 0.0218(9) Uani 1 1 d . . . H19A H 0.5576 0.3546 0.9940 0.026 Uiso 1 1 calc R . . H19B H 0.5294 0.2602 1.0594 0.026 Uiso 1 1 calc R . . C17 C 0.4398(3) 0.1404(3) 0.8893(2) 0.0219(9) Uani 1 1 d . . . H17A H 0.5212 0.1090 0.8676 0.026 Uiso 1 1 calc R . . H17B H 0.4133 0.0779 0.9055 0.026 Uiso 1 1 calc R . . C18 C 0.4436(3) 0.1867(3) 0.9634(2) 0.0239(9) Uani 1 1 d . . . H18A H 0.3609 0.2268 0.9807 0.029 Uiso 1 1 calc R . . H18B H 0.4908 0.1232 1.0106 0.029 Uiso 1 1 calc R . . C20 C 0.3774(3) 0.4096(3) 1.0173(2) 0.0237(9) Uani 1 1 d . . . H20A H 0.3218 0.3739 1.0378 0.028 Uiso 1 1 calc R . . H20B H 0.3835 0.4520 1.0579 0.028 Uiso 1 1 calc R . . O13 O 0.1147(3) 0.2304(2) 0.03802(18) 0.0451(8) Uani 1 1 d . . . H13 H 0.1699 0.1993 0.0760 0.054 Uiso 1 1 calc R . . C37 C 0.0901(4) 0.1450(4) 0.0145(3) 0.0381(11) Uani 1 1 d . . . H37A H 0.0151 0.1825 -0.0217 0.046 Uiso 1 1 calc R . . H37B H 0.0765 0.0959 0.0651 0.046 Uiso 1 1 calc R . . C36 C 0.1906(3) 0.0709(3) -0.0310(2) 0.0327(10) Uani 1 1 d . . . H36A H 0.2661 0.0354 0.0047 0.039 Uiso 1 1 calc R . . H36B H 0.2025 0.1199 -0.0823 0.039 Uiso 1 1 calc R . . C35 C 0.1674(4) -0.0233(4) -0.0545(3) 0.0517(13) Uani 1 1 d . . . H35A H 0.1601 -0.0750 -0.0038 0.078 Uiso 1 1 calc R . . H35B H 0.2346 -0.0666 -0.0853 0.078 Uiso 1 1 calc R . . H35C H 0.0925 0.0109 -0.0895 0.078 Uiso 1 1 calc R . . C39 C 0.2302(4) 0.3453(4) 0.4165(3) 0.0452(12) Uani 1 1 d . A . H39A H 0.2421 0.2827 0.3888 0.054 Uiso 1 1 calc R . . H39B H 0.2149 0.4154 0.3727 0.054 Uiso 1 1 calc R . . C38 C 0.3418(4) 0.3142(4) 0.4681(3) 0.0513(13) Uani 1 1 d . . . H38A H 0.3290 0.3748 0.4972 0.077 Uiso 1 1 calc R . . H38B H 0.4092 0.3056 0.4318 0.077 Uiso 1 1 calc R . . H38C H 0.3603 0.2419 0.5089 0.077 Uiso 1 1 calc R . . C40 C 0.1229(4) 0.3656(3) 0.4690(3) 0.0526(14) Uani 1 1 d D . . O14A O 0.1430(4) 0.2559(4) 0.5199(3) 0.0465(11) Uani 0.65 1 d PD A 1 O14B O 0.0051(5) 0.3997(7) 0.4332(5) 0.0465(11) Uani 0.35 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 0.0122(4) 0.0101(4) 0.0130(4) -0.0039(3) 0.0009(3) -0.0036(3) S1 0.0367(6) 0.0139(5) 0.0211(5) -0.0077(4) -0.0018(4) -0.0035(4) O2 0.0231(13) 0.0198(14) 0.0182(14) -0.0068(11) 0.0021(10) -0.0113(11) O1 0.0225(13) 0.0164(14) 0.0194(14) -0.0043(11) -0.0033(10) -0.0070(11) O6 0.0230(13) 0.0187(14) 0.0159(14) -0.0025(11) -0.0023(10) -0.0091(11) O8 0.0212(13) 0.0168(13) 0.0145(13) -0.0064(11) -0.0018(10) -0.0037(11) O7 0.0189(13) 0.0147(13) 0.0176(14) -0.0015(11) -0.0004(10) -0.0061(10) O5 0.0193(13) 0.0145(13) 0.0229(14) -0.0046(11) 0.0027(10) -0.0046(11) O4 0.0282(14) 0.0226(14) 0.0195(14) -0.0112(11) 0.0050(11) -0.0135(12) N7 0.0172(15) 0.0166(17) 0.0159(17) -0.0060(13) -0.0007(12) -0.0066(13) N4 0.0101(14) 0.0095(15) 0.0153(16) -0.0044(12) 0.0008(11) -0.0051(12) O3 0.0251(14) 0.0232(15) 0.0134(14) -0.0019(11) 0.0004(11) -0.0070(11) N1 0.0132(15) 0.0145(17) 0.0146(17) -0.0044(13) -0.0004(12) -0.0043(13) N5 0.0169(15) 0.0158(16) 0.0179(17) -0.0064(13) 0.0006(12) -0.0071(13) N2 0.0132(14) 0.0091(15) 0.0162(16) -0.0040(12) 0.0000(12) -0.0024(12) N3 0.0148(14) 0.0133(16) 0.0121(16) -0.0050(12) 0.0009(12) -0.0062(12) N6 0.0141(15) 0.0147(16) 0.0123(16) -0.0044(13) 0.0008(12) -0.0050(12) C5 0.0178(18) 0.017(2) 0.018(2) -0.0059(16) 0.0032(15) -0.0079(15) N8 0.0245(17) 0.0185(17) 0.0199(18) -0.0044(13) 0.0006(13) -0.0116(14) N9 0.0157(15) 0.0162(16) 0.0162(17) -0.0063(13) 0.0020(12) -0.0058(13) C12 0.0162(18) 0.0110(18) 0.0106(18) -0.0006(14) -0.0033(14) -0.0042(15) C34 0.0156(18) 0.018(2) 0.016(2) -0.0035(16) 0.0035(15) -0.0043(16) C1 0.0165(18) 0.018(2) 0.0081(19) 0.0003(16) -0.0007(14) -0.0040(16) C14 0.0205(19) 0.015(2) 0.0125(19) 0.0007(15) -0.0067(15) -0.0072(16) C2 0.0172(18) 0.0155(19) 0.019(2) -0.0065(16) 0.0050(15) -0.0066(15) C6 0.0149(17) 0.0076(18) 0.019(2) -0.0018(15) 0.0003(15) -0.0028(14) C26 0.0174(18) 0.0134(19) 0.023(2) -0.0054(16) 0.0015(15) -0.0018(15) C13 0.0152(18) 0.0121(19) 0.0127(19) 0.0002(15) -0.0027(14) -0.0021(15) C33 0.0159(18) 0.016(2) 0.020(2) -0.0062(16) 0.0015(15) -0.0052(15) C7 0.0112(17) 0.0083(18) 0.017(2) -0.0044(15) 0.0002(14) -0.0018(14) C9 0.0229(19) 0.018(2) 0.014(2) -0.0008(16) 0.0046(15) -0.0073(16) C11 0.0140(17) 0.0149(19) 0.019(2) -0.0070(16) 0.0031(14) -0.0055(15) C31 0.024(2) 0.022(2) 0.015(2) -0.0038(16) 0.0033(16) -0.0098(17) C16 0.0225(19) 0.024(2) 0.023(2) -0.0148(17) 0.0056(16) -0.0118(17) C10 0.0178(19) 0.015(2) 0.028(2) -0.0051(17) 0.0038(16) -0.0079(16) C30 0.0157(18) 0.021(2) 0.020(2) -0.0013(16) -0.0036(15) -0.0031(16) C8 0.0162(18) 0.017(2) 0.015(2) -0.0053(16) -0.0007(14) -0.0041(15) C21 0.0212(19) 0.018(2) 0.022(2) -0.0088(16) 0.0022(16) -0.0049(16) C32 0.0230(19) 0.026(2) 0.014(2) -0.0070(16) 0.0001(15) -0.0081(17) C25 0.0206(19) 0.016(2) 0.017(2) -0.0053(16) 0.0031(15) -0.0007(16) C4 0.0134(18) 0.017(2) 0.033(2) -0.0053(17) -0.0035(16) -0.0067(15) C29 0.0218(19) 0.015(2) 0.022(2) -0.0022(16) -0.0013(16) -0.0020(16) C3 0.0196(19) 0.023(2) 0.026(2) -0.0087(17) 0.0071(16) -0.0081(17) C22 0.024(2) 0.022(2) 0.019(2) -0.0101(17) 0.0044(16) -0.0071(17) C27 0.025(2) 0.015(2) 0.021(2) -0.0038(16) -0.0018(16) -0.0062(16) C28 0.024(2) 0.017(2) 0.024(2) -0.0099(16) -0.0024(16) -0.0051(16) C15 0.031(2) 0.027(2) 0.017(2) -0.0040(17) -0.0007(16) -0.0186(18) C24 0.034(2) 0.014(2) 0.026(2) -0.0028(17) -0.0018(17) -0.0103(17) C23 0.036(2) 0.027(2) 0.030(2) -0.0118(19) 0.0065(18) -0.0215(19) Na1 0.0419(9) 0.0198(8) 0.0150(8) -0.0026(6) -0.0036(6) -0.0116(7) Cl1 0.0270(5) 0.0245(5) 0.0251(5) -0.0072(4) 0.0022(4) -0.0135(4) O11 0.0354(17) 0.0209(16) 0.055(2) -0.0128(14) 0.0061(14) -0.0120(13) O9 0.0401(17) 0.0291(16) 0.0347(17) -0.0149(13) -0.0055(13) -0.0153(13) O10 0.055(2) 0.055(2) 0.0201(16) 0.0014(14) -0.0009(14) -0.0324(16) O12 0.0274(15) 0.0450(19) 0.0432(19) -0.0082(15) 0.0035(13) -0.0190(14) C19 0.025(2) 0.027(2) 0.016(2) -0.0068(17) -0.0007(16) -0.0126(17) C17 0.0187(19) 0.015(2) 0.032(2) -0.0039(17) 0.0015(16) -0.0076(16) C18 0.026(2) 0.025(2) 0.021(2) 0.0025(17) -0.0041(16) -0.0132(17) C20 0.031(2) 0.028(2) 0.010(2) -0.0041(17) 0.0013(16) -0.0114(18) O13 0.052(2) 0.0362(19) 0.0305(19) -0.0068(14) -0.0067(14) -0.0027(16) C37 0.025(2) 0.046(3) 0.028(3) 0.006(2) -0.0027(18) -0.007(2) C36 0.029(2) 0.037(3) 0.024(2) -0.0012(19) -0.0008(18) -0.009(2) C35 0.061(3) 0.043(3) 0.044(3) 0.001(2) -0.021(2) -0.019(3) C39 0.053(3) 0.044(3) 0.042(3) -0.008(2) -0.008(2) -0.023(2) C38 0.033(3) 0.053(3) 0.060(3) -0.010(3) -0.002(2) -0.011(2) C40 0.031(3) 0.055(3) 0.075(4) -0.022(3) 0.002(2) -0.018(2) O14A 0.061(3) 0.070(3) 0.029(2) -0.007(2) -0.003(2) -0.050(2) O14B 0.061(3) 0.070(3) 0.029(2) -0.007(2) -0.003(2) -0.050(2) _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 N1 1.945(3) 2_556 ? Fe1 N1 1.945(3) . ? Fe1 N4 1.985(3) . ? Fe1 N4 1.985(3) 2_556 ? Fe1 N2 1.995(3) 2_556 ? Fe1 N2 1.995(3) . ? S1 C1 1.642(4) . ? O2 C18 1.430(4) . ? O2 C19 1.433(4) . ? O2 Na1 2.426(3) . ? O1 C17 1.421(4) . ? O1 C16 1.437(4) . ? O1 Na1 2.578(3) . ? O6 C29 1.423(4) . ? O6 C28 1.425(4) . ? O6 Na1 2.526(3) 1_455 ? O8 C32 1.422(4) . ? O8 C33 1.430(4) . ? O8 Na1 2.767(3) 1_455 ? O7 C31 1.422(4) . ? O7 C30 1.438(4) . ? O7 Na1 2.406(3) 1_455 ? O5 C27 1.426(4) . ? O5 C26 1.433(4) . ? O5 Na1 2.766(3) 1_455 ? O4 C23 1.421(4) . ? O4 C22 1.429(4) . ? N7 C13 1.335(4) . ? N7 C14 1.338(4) . ? N4 C7 1.340(4) . ? N4 C11 1.355(4) . ? O3 C20 1.422(4) . ? O3 C21 1.433(4) . ? O3 Na1 2.496(3) . ? N1 C1 1.162(4) . ? N5 C12 1.324(4) . ? N5 C14 1.356(4) . ? N2 C6 1.353(4) . ? N2 C2 1.360(4) . ? N3 C12 1.404(4) . ? N3 C7 1.421(4) . ? N3 C6 1.428(4) . ? N6 C12 1.323(4) . ? N6 C13 1.352(4) . ? C5 C4 1.370(5) . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? N8 C14 1.359(4) . ? N8 C24 1.467(4) . ? N8 C15 1.466(4) . ? N9 C13 1.346(4) . ? N9 C34 1.462(4) . ? N9 C25 1.463(4) . ? C34 C33 1.509(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C2 C3 1.374(5) . ? C2 H2 0.9500 . ? C26 C25 1.528(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C7 C8 1.391(4) . ? C9 C8 1.369(5) . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C11 C10 1.375(5) . ? C11 H11 0.9500 . ? C31 C32 1.496(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C16 C15 1.502(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C10 H10 0.9500 . ? C30 C29 1.495(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C8 H8 0.9500 . ? C21 C22 1.484(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C4 C3 1.393(5) . ? C4 H4 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C3 H3 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C27 C28 1.505(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C24 C23 1.515(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? Na1 O7 2.406(3) 1_655 ? Na1 O6 2.526(3) 1_655 ? Na1 O5 2.766(3) 1_655 ? Na1 O8 2.767(3) 1_655 ? Cl1 O10 1.436(3) . ? Cl1 O11 1.439(3) . ? Cl1 O12 1.443(3) . ? Cl1 O9 1.453(3) . ? C19 C20 1.512(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C17 C18 1.496(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O13 C37 1.420(5) . ? O13 H13 0.8400 . ? C37 C36 1.507(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C36 C35 1.521(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C39 C38 1.495(6) . ? C39 C40 1.502(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C40 O14A 1.4281(10) . ? C40 O14B 1.4288(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 N1 Fe1 N1 180.00(14) 2_556 . ? N1 Fe1 N4 88.24(11) 2_556 . ? N1 Fe1 N4 91.76(11) . . ? N1 Fe1 N4 91.76(11) 2_556 2_556 ? N1 Fe1 N4 88.24(11) . 2_556 ? N4 Fe1 N4 180.0 . 2_556 ? N1 Fe1 N2 91.30(11) 2_556 2_556 ? N1 Fe1 N2 88.70(11) . 2_556 ? N4 Fe1 N2 93.68(11) . 2_556 ? N4 Fe1 N2 86.32(11) 2_556 2_556 ? N1 Fe1 N2 88.70(11) 2_556 . ? N1 Fe1 N2 91.30(11) . . ? N4 Fe1 N2 86.32(11) . . ? N4 Fe1 N2 93.68(11) 2_556 . ? N2 Fe1 N2 180.0 2_556 . ? C18 O2 C19 112.8(3) . . ? C18 O2 Na1 111.7(2) . . ? C19 O2 Na1 111.2(2) . . ? C17 O1 C16 110.8(3) . . ? C17 O1 Na1 107.4(2) . . ? C16 O1 Na1 125.0(2) . . ? C29 O6 C28 114.0(3) . . ? C29 O6 Na1 115.4(2) . 1_455 ? C28 O6 Na1 113.36(19) . 1_455 ? C32 O8 C33 110.7(2) . . ? C32 O8 Na1 108.99(18) . 1_455 ? C33 O8 Na1 132.93(19) . 1_455 ? C31 O7 C30 113.4(2) . . ? C31 O7 Na1 115.4(2) . 1_455 ? C30 O7 Na1 108.82(19) . 1_455 ? C27 O5 C26 110.9(2) . . ? C27 O5 Na1 111.55(19) . 1_455 ? C26 O5 Na1 123.9(2) . 1_455 ? C23 O4 C22 110.9(3) . . ? C13 N7 C14 113.8(3) . . ? C7 N4 C11 117.1(3) . . ? C7 N4 Fe1 122.5(2) . . ? C11 N4 Fe1 120.3(2) . . ? C20 O3 C21 112.4(3) . . ? C20 O3 Na1 117.6(2) . . ? C21 O3 Na1 117.2(2) . . ? C1 N1 Fe1 174.5(3) . . ? C12 N5 C14 112.3(3) . . ? C6 N2 C2 116.5(3) . . ? C6 N2 Fe1 123.3(2) . . ? C2 N2 Fe1 120.2(2) . . ? C12 N3 C7 119.1(3) . . ? C12 N3 C6 122.1(3) . . ? C7 N3 C6 118.6(3) . . ? C12 N6 C13 112.8(3) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C14 N8 C24 118.2(3) . . ? C14 N8 C15 119.8(3) . . ? C24 N8 C15 120.6(3) . . ? C13 N9 C34 120.3(3) . . ? C13 N9 C25 119.5(3) . . ? C34 N9 C25 119.7(3) . . ? N6 C12 N5 128.7(3) . . ? N6 C12 N3 114.4(3) . . ? N5 C12 N3 116.8(3) . . ? N9 C34 C33 114.0(3) . . ? N9 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? N9 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? N1 C1 S1 178.6(3) . . ? N7 C14 N5 126.2(3) . . ? N7 C14 N8 117.1(3) . . ? N5 C14 N8 116.6(3) . . ? N2 C2 C3 122.9(3) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? N2 C6 C5 123.4(3) . . ? N2 C6 N3 115.8(3) . . ? C5 C6 N3 120.6(3) . . ? O5 C26 C25 107.5(3) . . ? O5 C26 H26A 110.2 . . ? C25 C26 H26A 110.2 . . ? O5 C26 H26B 110.2 . . ? C25 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? N7 C13 N9 118.1(3) . . ? N7 C13 N6 126.1(3) . . ? N9 C13 N6 115.8(3) . . ? O8 C33 C34 110.0(3) . . ? O8 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? O8 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N4 C7 C8 122.9(3) . . ? N4 C7 N3 117.7(3) . . ? C8 C7 N3 119.3(3) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N4 C11 C10 123.1(3) . . ? N4 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? O7 C31 C32 108.3(3) . . ? O7 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O7 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? O1 C16 C15 110.0(3) . . ? O1 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? O1 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C11 C10 C9 118.6(3) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? O7 C30 C29 112.0(3) . . ? O7 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? O7 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C9 C8 C7 118.8(3) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? O3 C21 C22 113.3(3) . . ? O3 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? O3 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? O8 C32 C31 109.4(3) . . ? O8 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O8 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? N9 C25 C26 114.8(3) . . ? N9 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? N9 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.5 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? O6 C29 C30 106.8(3) . . ? O6 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O6 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? O4 C22 C21 109.5(3) . . ? O4 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? O4 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? O5 C27 C28 108.3(3) . . ? O5 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O5 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O6 C28 C27 112.3(3) . . ? O6 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? O6 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? N8 C15 C16 113.5(3) . . ? N8 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? N8 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N8 C24 C23 116.3(3) . . ? N8 C24 H24A 108.2 . . ? C23 C24 H24A 108.2 . . ? N8 C24 H24B 108.2 . . ? C23 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? O4 C23 C24 110.3(3) . . ? O4 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? O4 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? O7 Na1 O2 153.74(10) 1_655 . ? O7 Na1 O3 137.47(9) 1_655 . ? O2 Na1 O3 67.79(8) . . ? O7 Na1 O6 68.14(8) 1_655 1_655 ? O2 Na1 O6 137.04(10) . 1_655 ? O3 Na1 O6 75.52(8) . 1_655 ? O7 Na1 O1 91.98(9) 1_655 . ? O2 Na1 O1 69.08(8) . . ? O3 Na1 O1 107.27(9) . . ? O6 Na1 O1 146.13(10) 1_655 . ? O7 Na1 O5 98.10(9) 1_655 1_655 ? O2 Na1 O5 90.05(9) . 1_655 ? O3 Na1 O5 85.45(9) . 1_655 ? O6 Na1 O5 64.95(8) 1_655 1_655 ? O1 Na1 O5 147.86(9) . 1_655 ? O7 Na1 O8 64.90(8) 1_655 1_655 ? O2 Na1 O8 93.50(8) . 1_655 ? O3 Na1 O8 153.41(10) . 1_655 ? O6 Na1 O8 111.46(9) 1_655 1_655 ? O1 Na1 O8 81.51(8) . 1_655 ? O5 Na1 O8 75.48(8) 1_655 1_655 ? O10 Cl1 O11 110.35(17) . . ? O10 Cl1 O12 109.46(17) . . ? O11 Cl1 O12 109.87(16) . . ? O10 Cl1 O9 109.21(17) . . ? O11 Cl1 O9 108.50(17) . . ? O12 Cl1 O9 109.42(17) . . ? O2 C19 C20 112.4(3) . . ? O2 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? O2 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? O1 C17 C18 108.8(3) . . ? O1 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O1 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O2 C18 C17 108.4(3) . . ? O2 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O2 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? O3 C20 C19 106.9(3) . . ? O3 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? O3 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? C37 O13 H13 109.5 . . ? O13 C37 C36 112.9(4) . . ? O13 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? O13 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C36 C35 113.6(4) . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C39 C40 111.3(4) . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O14A C40 O14B 100.1(5) . . ? O14A C40 C39 105.5(4) . . ? O14B C40 C39 121.6(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O9 0.84 2.08 2.906(4) 166.0 . _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.508 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.073 #=END data_1b _database_code_depnum_ccdc_archive 'CCDC 823863' #TrackingRef '- DaltonCrown.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DCrCr5)2(Na)2](ClO4)2.4CH3CH2CH2OH ; _chemical_name_common trans-(Fe(ii)(NCS)2(DCrCr5)2(Na)2)(ClO4)2.4CH3CH2CH2OH _chemical_melting_point ? _chemical_formula_moiety '(Fe S2 Na2 C68 H96 O16 N18), 2(Cl O4), 4(C3 H8 O)' _chemical_formula_sum 'C80 H128 Cl2 Fe N18 Na2 O28 S2' _chemical_formula_weight 2026.85 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.304(2) _cell_length_b 13.400(2) _cell_length_c 16.754(3) _cell_angle_alpha 78.495(7) _cell_angle_beta 88.175(7) _cell_angle_gamma 65.049(7) _cell_volume 2449.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used 20028 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 270(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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20028 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8449 _reflns_number_gt 4797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8449 _refine_ls_number_parameters 569 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2541 _refine_ls_wR_factor_gt 0.1938 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.0000 0.0000 0.5000 0.0304(3) Uani 1 2 d S . . S1 S -0.18149(17) 0.35996(13) 0.58089(10) 0.0654(5) Uani 1 1 d . . . O2 O 0.4967(3) 0.2661(3) 0.9378(2) 0.0423(9) Uani 1 1 d . . . O1 O 0.3546(3) 0.2313(3) 0.8265(2) 0.0423(9) Uani 1 1 d . . . O6 O -0.6666(3) 0.6115(3) 0.7601(2) 0.0448(9) Uani 1 1 d . . . O8 O -0.4197(3) 0.2830(3) 0.7159(2) 0.0420(9) Uani 1 1 d . . . O7 O -0.6469(3) 0.4581(3) 0.6659(2) 0.0416(9) Uani 1 1 d . . . O5 O -0.4219(3) 0.4855(3) 0.8151(2) 0.0453(9) Uani 1 1 d . . . O4 O 0.1329(3) 0.4785(3) 0.8511(2) 0.0491(10) Uani 1 1 d U . . N7 N -0.0417(4) 0.2627(3) 0.7849(3) 0.0362(10) Uani 1 1 d . . . N4 N -0.0014(4) -0.0935(3) 0.6196(3) 0.0383(10) Uani 1 1 d . . . O3 O 0.3320(3) 0.4828(3) 0.9356(2) 0.0498(10) Uani 1 1 d . . . N1 N -0.0859(4) 0.1510(4) 0.5378(3) 0.0418(11) Uani 1 1 d . . . N5 N 0.1132(4) 0.1481(4) 0.7101(3) 0.0367(10) Uani 1 1 d . . . N2 N 0.1730(4) -0.0220(4) 0.5462(3) 0.0402(11) Uani 1 1 d . . . N3 N 0.0991(3) -0.0054(3) 0.6763(2) 0.0318(10) Uani 1 1 d . . . N6 N -0.0486(3) 0.1016(3) 0.7507(2) 0.0335(10) Uani 1 1 d . . . C5 C 0.3073(5) -0.0389(5) 0.6541(4) 0.0440(14) Uani 1 1 d . . . H5 H 0.3195 -0.0370 0.7081 0.053 Uiso 1 1 calc R . . N8 N 0.1146(4) 0.3069(4) 0.7416(3) 0.0443(11) Uani 1 1 d . . . N9 N -0.1972(4) 0.2137(4) 0.8193(3) 0.0395(11) Uani 1 1 d . . . C12 C 0.0532(4) 0.0860(4) 0.7146(3) 0.0325(12) Uani 1 1 d . . . C34 C -0.2627(5) 0.1471(5) 0.8130(3) 0.0443(14) Uani 1 1 d . . . H34A H -0.3220 0.1592 0.8539 0.053 Uiso 1 1 calc R . . H34B H -0.2070 0.0682 0.8255 0.053 Uiso 1 1 calc R . . C1 C -0.1269(5) 0.2382(5) 0.5561(3) 0.0362(12) Uani 1 1 d . . . C14 C 0.0596(5) 0.2378(4) 0.7461(3) 0.0365(12) Uani 1 1 d . . . C2 C 0.2659(5) -0.0435(5) 0.4964(4) 0.0488(15) Uani 1 1 d . . . H2 H 0.2528 -0.0466 0.4428 0.059 Uiso 1 1 calc R . . C6 C 0.1961(4) -0.0218(4) 0.6243(3) 0.0343(12) Uani 1 1 d . . . C26 C -0.2998(5) 0.4236(5) 0.7995(4) 0.0512(15) Uani 1 1 d . . . H26A H -0.2531 0.4642 0.8074 0.061 Uiso 1 1 calc R . . H26B H -0.2939 0.4133 0.7436 0.061 Uiso 1 1 calc R . . C13 C -0.0925(4) 0.1925(4) 0.7835(3) 0.0331(12) Uani 1 1 d . . . C33 C -0.3251(5) 0.1722(5) 0.7314(3) 0.0432(14) Uani 1 1 d . . . H33A H -0.2679 0.1658 0.6892 0.052 Uiso 1 1 calc R . . H33B H -0.3576 0.1180 0.7300 0.052 Uiso 1 1 calc R . . C7 C 0.0437(4) -0.0817(4) 0.6868(3) 0.0332(12) Uani 1 1 d . . . C31 C -0.5467(5) 0.4383(5) 0.6163(3) 0.0501(15) Uani 1 1 d . . . H31A H -0.5032 0.4800 0.6279 0.060 Uiso 1 1 calc R . . H31B H -0.5739 0.4631 0.5591 0.060 Uiso 1 1 calc R . . C16 C 0.3331(5) 0.1897(5) 0.7603(4) 0.0521(16) Uani 1 1 d . . . H16A H 0.3151 0.1256 0.7808 0.062 Uiso 1 1 calc R . . H16B H 0.4045 0.1648 0.7295 0.062 Uiso 1 1 calc R . . C30 C -0.7373(5) 0.5720(5) 0.6473(4) 0.0498(15) Uani 1 1 d . . . H30A H -0.8097 0.5758 0.6739 0.060 Uiso 1 1 calc R . . H30B H -0.7565 0.5947 0.5889 0.060 Uiso 1 1 calc R . . C21 C 0.2076(5) 0.5614(5) 0.9347(4) 0.0487(15) Uani 1 1 d . . . H21A H 0.1901 0.6237 0.8886 0.058 Uiso 1 1 calc R . . H21B H 0.1946 0.5913 0.9841 0.058 Uiso 1 1 calc R . . C32 C -0.4657(5) 0.3141(5) 0.6345(3) 0.0492(15) Uani 1 1 d . . . H32A H -0.5107 0.2720 0.6265 0.059 Uiso 1 1 calc R . . H32B H -0.4005 0.2978 0.5979 0.059 Uiso 1 1 calc R . . C25 C -0.2518(5) 0.3110(5) 0.8574(3) 0.0465(14) Uani 1 1 d . . . H25A H -0.1924 0.3086 0.8954 0.056 Uiso 1 1 calc R . . H25B H -0.3171 0.3048 0.8888 0.056 Uiso 1 1 calc R . . C4 C 0.3995(5) -0.0587(5) 0.6021(4) 0.0608(18) Uani 1 1 d . . . H4 H 0.4753 -0.0705 0.6206 0.073 Uiso 1 1 calc R . . C29 C -0.6982(5) 0.6512(5) 0.6741(3) 0.0492(15) Uani 1 1 d . . . H29A H -0.6295 0.6530 0.6449 0.059 Uiso 1 1 calc R . . H29B H -0.7626 0.7265 0.6636 0.059 Uiso 1 1 calc R . . C3 C 0.3781(5) -0.0608(6) 0.5219(4) 0.0624(18) Uani 1 1 d . . . H3 H 0.4393 -0.0739 0.4859 0.075 Uiso 1 1 calc R . . C22 C 0.1246(5) 0.5092(5) 0.9291(3) 0.0505(15) Uani 1 1 d . . . H22A H 0.1456 0.4430 0.9724 0.061 Uiso 1 1 calc R . . H22B H 0.0430 0.5619 0.9353 0.061 Uiso 1 1 calc R . . C27 C -0.4669(5) 0.5997(4) 0.7741(4) 0.0472(14) Uani 1 1 d . . . H27A H -0.4587 0.6043 0.7158 0.057 Uiso 1 1 calc R . . H27B H -0.4220 0.6357 0.7932 0.057 Uiso 1 1 calc R . . C28 C -0.5965(5) 0.6573(5) 0.7911(4) 0.0498(15) Uani 1 1 d . . . H28A H -0.6037 0.6502 0.8496 0.060 Uiso 1 1 calc R . . H28B H -0.6269 0.7367 0.7666 0.060 Uiso 1 1 calc R . . C15 C 0.2305(6) 0.2791(6) 0.7061(4) 0.0550(17) Uani 1 1 d . . . H15A H 0.2443 0.3465 0.6927 0.066 Uiso 1 1 calc R . . H15B H 0.2282 0.2547 0.6557 0.066 Uiso 1 1 calc R . . C24 C 0.0433(6) 0.4210(5) 0.7538(4) 0.0562(16) Uani 1 1 d U . . H24A H -0.0394 0.4432 0.7361 0.067 Uiso 1 1 calc R . . H24B H 0.0713 0.4711 0.7186 0.067 Uiso 1 1 calc R . . C23 C 0.0457(6) 0.4386(6) 0.8393(4) 0.0660(18) Uani 1 1 d U . . H23A H -0.0329 0.4925 0.8501 0.079 Uiso 1 1 calc R . . H23B H 0.0640 0.3681 0.8776 0.079 Uiso 1 1 calc R . . Na1 Na 0.4048(2) 0.40257(18) 0.81117(12) 0.0543(6) Uani 1 1 d . . . C19 C 0.4968(5) 0.3217(5) 1.0024(3) 0.0536(16) Uani 1 1 d . . . H19A H 0.5523 0.3564 0.9911 0.064 Uiso 1 1 calc R . . H19B H 0.5254 0.2663 1.0530 0.064 Uiso 1 1 calc R . . C17 C 0.4372(5) 0.1442(5) 0.8850(4) 0.0511(15) Uani 1 1 d . . . H17A H 0.5155 0.1143 0.8625 0.061 Uiso 1 1 calc R . . H17B H 0.4118 0.0840 0.8999 0.061 Uiso 1 1 calc R . . C18 C 0.4453(6) 0.1880(5) 0.9586(4) 0.0547(16) Uani 1 1 d . . . H18A H 0.3659 0.2246 0.9781 0.066 Uiso 1 1 calc R . . H18B H 0.4947 0.1264 1.0018 0.066 Uiso 1 1 calc R . . C20 C 0.3768(6) 0.4088(5) 1.0129(3) 0.0577(17) Uani 1 1 d . . . H20A H 0.3231 0.3742 1.0321 0.069 Uiso 1 1 calc R . . H20B H 0.3824 0.4503 1.0526 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.36103(15) 0.14860(14) 0.19953(10) 0.0598(5) Uani 1 1 d . . . O9 O 0.3233(5) 0.0957(5) 0.1477(4) 0.0996(18) Uani 1 1 d . . . O12 O 0.4795(4) 0.1354(5) 0.1821(3) 0.0938(17) Uani 1 1 d . . . O10 O 0.3584(6) 0.0966(6) 0.2807(3) 0.123(2) Uani 1 1 d . . . O11 O 0.2819(5) 0.2624(4) 0.1859(4) 0.110(2) Uani 1 1 d . . . C8 C 0.0415(5) -0.1410(5) 0.7643(3) 0.0440(14) Uani 1 1 d . . . H8 H 0.0745 -0.1311 0.8096 0.053 Uiso 1 1 calc R . . C9 C -0.0104(5) -0.2142(5) 0.7722(4) 0.0521(16) Uani 1 1 d . . . H9 H -0.0157 -0.2535 0.8235 0.062 Uiso 1 1 calc R . . C10 C -0.0547(5) -0.2293(5) 0.7036(4) 0.0525(16) Uani 1 1 d . . . H10 H -0.0900 -0.2792 0.7079 0.063 Uiso 1 1 calc R . . C11 C -0.0467(5) -0.1707(5) 0.6293(4) 0.0487(15) Uani 1 1 d . . . H11 H -0.0737 -0.1843 0.5832 0.058 Uiso 1 1 calc R . . O13 O 0.1077(6) 0.2276(6) 0.0344(4) 0.126(2) Uiso 1 1 d . . . H13 H 0.1673 0.1995 0.0660 0.151 Uiso 1 1 calc R . . C37 C 0.0875(9) 0.1416(9) 0.0103(7) 0.124(3) Uiso 1 1 d D . . H37A H 0.0157 0.1749 -0.0259 0.149 Uiso 1 1 calc R . . H37B H 0.0741 0.0947 0.0581 0.149 Uiso 1 1 calc R . . C35 C 0.1746(9) -0.0242(9) -0.0581(7) 0.128(4) Uiso 1 1 d . . . H35A H 0.0948 0.0021 -0.0817 0.192 Uiso 1 1 calc R . . H35B H 0.1884 -0.0842 -0.0118 0.192 Uiso 1 1 calc R . . H35C H 0.2318 -0.0512 -0.0979 0.192 Uiso 1 1 calc R . . C36 C 0.1886(8) 0.0722(8) -0.0311(6) 0.116(3) Uiso 1 1 d D . . H36A H 0.2602 0.0409 0.0052 0.139 Uiso 1 1 calc R . . H36B H 0.2010 0.1199 -0.0787 0.139 Uiso 1 1 calc R . . C40 C 0.1234(9) 0.3685(9) 0.4747(7) 0.154(3) Uiso 1 1 d D . . O14A O 0.1359(14) 0.2616(11) 0.5203(9) 0.154(3) Uiso 0.50 1 d PD A 1 O14B O 0.0132(10) 0.3933(13) 0.4320(9) 0.154(3) Uiso 0.50 1 d PD A 2 C39A C 0.2227(15) 0.3570(17) 0.4137(9) 0.154(3) Uiso 0.50 1 d PD A 1 C38A C 0.3402(12) 0.310(2) 0.4656(15) 0.154(3) Uiso 0.50 1 d PD A 1 C39B C 0.2389(11) 0.2877(14) 0.4502(14) 0.154(3) Uiso 0.50 1 d PD A 2 C38B C 0.3270(15) 0.335(2) 0.4232(16) 0.154(3) Uiso 0.50 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 0.0311(6) 0.0310(6) 0.0323(6) -0.0113(5) 0.0019(4) -0.0142(5) S1 0.0943(14) 0.0389(9) 0.0507(10) -0.0160(8) -0.0011(9) -0.0132(9) O2 0.049(2) 0.048(2) 0.037(2) -0.0097(18) 0.0061(17) -0.0272(19) O1 0.042(2) 0.038(2) 0.050(2) -0.0170(18) -0.0006(17) -0.0167(18) O6 0.048(2) 0.048(2) 0.038(2) -0.0079(18) -0.0022(17) -0.0203(19) O8 0.039(2) 0.043(2) 0.039(2) -0.0145(17) 0.0004(16) -0.0099(18) O7 0.044(2) 0.043(2) 0.037(2) -0.0084(17) -0.0003(17) -0.0170(18) O5 0.045(2) 0.036(2) 0.052(2) -0.0105(18) 0.0057(18) -0.0144(18) O4 0.0508(13) 0.0493(13) 0.0506(13) -0.0128(9) 0.0032(9) -0.0234(9) N7 0.033(2) 0.037(3) 0.040(3) -0.015(2) -0.0039(19) -0.013(2) N4 0.038(2) 0.035(3) 0.047(3) -0.014(2) 0.004(2) -0.019(2) O3 0.054(3) 0.054(2) 0.038(2) -0.0085(19) 0.0035(18) -0.020(2) N1 0.045(3) 0.044(3) 0.034(3) -0.011(2) -0.002(2) -0.015(2) N5 0.032(2) 0.045(3) 0.043(3) -0.014(2) 0.0016(19) -0.024(2) N2 0.040(3) 0.041(3) 0.041(3) -0.013(2) 0.012(2) -0.018(2) N3 0.029(2) 0.034(2) 0.039(2) -0.015(2) 0.0050(18) -0.0171(19) N6 0.030(2) 0.034(2) 0.038(2) -0.012(2) 0.0044(19) -0.0126(19) C5 0.030(3) 0.049(3) 0.054(4) -0.018(3) 0.004(2) -0.015(3) N8 0.046(3) 0.040(3) 0.056(3) -0.015(2) -0.003(2) -0.024(2) N9 0.032(2) 0.044(3) 0.041(3) -0.015(2) 0.0046(19) -0.013(2) C12 0.033(3) 0.038(3) 0.028(3) -0.007(2) -0.002(2) -0.016(2) C34 0.035(3) 0.047(3) 0.050(3) -0.014(3) 0.013(2) -0.015(3) C1 0.044(3) 0.039(3) 0.027(3) -0.010(3) 0.000(2) -0.018(3) C14 0.044(3) 0.039(3) 0.033(3) -0.012(2) -0.006(2) -0.022(3) C2 0.037(3) 0.058(4) 0.053(4) -0.017(3) 0.018(3) -0.020(3) C6 0.035(3) 0.027(3) 0.043(3) -0.009(2) 0.005(2) -0.014(2) C26 0.044(3) 0.054(4) 0.057(4) -0.023(3) 0.021(3) -0.018(3) C13 0.032(3) 0.034(3) 0.031(3) -0.009(2) -0.001(2) -0.011(2) C33 0.039(3) 0.051(4) 0.048(3) -0.021(3) 0.006(3) -0.022(3) C7 0.033(3) 0.028(3) 0.042(3) -0.013(2) 0.008(2) -0.013(2) C31 0.055(4) 0.058(4) 0.037(3) -0.007(3) 0.000(3) -0.024(3) C16 0.050(4) 0.059(4) 0.064(4) -0.028(3) 0.008(3) -0.032(3) C30 0.042(3) 0.047(4) 0.049(4) -0.007(3) -0.008(3) -0.008(3) C21 0.052(4) 0.049(4) 0.048(4) -0.022(3) 0.007(3) -0.019(3) C32 0.049(3) 0.062(4) 0.039(3) -0.021(3) 0.002(3) -0.022(3) C25 0.043(3) 0.045(4) 0.046(3) -0.022(3) 0.011(3) -0.009(3) C4 0.037(3) 0.069(5) 0.084(5) -0.025(4) 0.010(3) -0.025(3) C29 0.053(4) 0.034(3) 0.047(4) 0.001(3) -0.002(3) -0.009(3) C3 0.041(4) 0.071(5) 0.082(5) -0.028(4) 0.024(3) -0.025(3) C22 0.054(4) 0.053(4) 0.046(4) -0.025(3) 0.013(3) -0.018(3) C27 0.052(4) 0.035(3) 0.060(4) -0.011(3) -0.001(3) -0.023(3) C28 0.049(4) 0.040(3) 0.060(4) -0.019(3) -0.001(3) -0.014(3) C15 0.066(4) 0.078(5) 0.045(4) -0.017(3) 0.006(3) -0.053(4) C24 0.0575(18) 0.0556(18) 0.0569(19) -0.0121(10) 0.0022(10) -0.0252(11) C23 0.067(2) 0.066(2) 0.067(2) -0.0143(10) 0.0040(10) -0.0300(12) Na1 0.0852(18) 0.0455(14) 0.0330(12) -0.0061(10) -0.0062(11) -0.0286(13) C19 0.059(4) 0.065(4) 0.037(3) -0.014(3) -0.002(3) -0.025(3) C17 0.047(4) 0.039(3) 0.069(4) -0.010(3) 0.003(3) -0.021(3) C18 0.060(4) 0.053(4) 0.053(4) 0.000(3) 0.003(3) -0.031(3) C20 0.067(4) 0.069(4) 0.030(3) -0.016(3) 0.004(3) -0.020(4) Cl1 0.0632(11) 0.0611(11) 0.0646(11) -0.0160(8) 0.0041(8) -0.0339(9) O9 0.100(4) 0.105(4) 0.111(4) -0.047(4) -0.014(3) -0.048(4) O12 0.066(3) 0.127(5) 0.098(4) -0.023(4) 0.014(3) -0.050(3) O10 0.122(5) 0.185(7) 0.073(4) 0.012(4) -0.008(3) -0.093(5) O11 0.096(4) 0.061(4) 0.177(6) -0.026(4) 0.028(4) -0.038(3) C8 0.046(3) 0.041(3) 0.042(3) -0.007(3) 0.003(3) -0.017(3) C9 0.059(4) 0.040(3) 0.056(4) 0.002(3) 0.010(3) -0.025(3) C10 0.050(4) 0.043(4) 0.071(4) -0.005(3) 0.010(3) -0.029(3) C11 0.051(4) 0.039(3) 0.066(4) -0.013(3) 0.002(3) -0.028(3) _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 N1 2.068(5) . ? Fe1 N1 2.068(5) 2_556 ? Fe1 N4 2.145(4) . ? Fe1 N4 2.145(4) 2_556 ? Fe1 N2 2.168(4) 2_556 ? Fe1 N2 2.168(4) . ? S1 C1 1.617(6) . ? O2 C18 1.418(6) . ? O2 C19 1.433(6) . ? O2 Na1 2.446(4) . ? O1 C17 1.401(6) . ? O1 C16 1.414(6) . ? O1 Na1 2.581(4) . ? O6 C28 1.412(6) . ? O6 C29 1.437(6) . ? O6 Na1 2.522(4) 1_455 ? O8 C32 1.406(6) . ? O8 C33 1.426(6) . ? O8 Na1 2.768(4) 1_455 ? O7 C31 1.424(6) . ? O7 C30 1.437(6) . ? O7 Na1 2.420(4) 1_455 ? O5 C27 1.417(6) . ? O5 C26 1.423(6) . ? O5 Na1 2.798(4) 1_455 ? O4 C23 1.420(7) . ? O4 C22 1.435(6) . ? N7 C14 1.332(6) . ? N7 C13 1.335(6) . ? N4 C7 1.336(6) . ? N4 C11 1.349(6) . ? O3 C20 1.427(7) . ? O3 C21 1.444(6) . ? O3 Na1 2.503(4) . ? N1 C1 1.161(6) . ? N5 C12 1.316(6) . ? N5 C14 1.355(6) . ? N2 C6 1.348(7) . ? N2 C2 1.358(6) . ? N3 C12 1.392(6) . ? N3 C6 1.421(6) . ? N3 C7 1.432(6) . ? N6 C12 1.327(6) . ? N6 C13 1.330(6) . ? C5 C4 1.375(8) . ? C5 C6 1.381(7) . ? C5 H5 0.9300 . ? N8 C14 1.348(6) . ? N8 C15 1.453(7) . ? N8 C24 1.460(7) . ? N9 C13 1.346(6) . ? N9 C34 1.452(7) . ? N9 C25 1.458(6) . ? C34 C33 1.496(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C2 C3 1.367(8) . ? C2 H2 0.9300 . ? C26 C25 1.505(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C7 C8 1.386(7) . ? C31 C32 1.507(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C16 C15 1.489(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C30 C29 1.481(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C21 C22 1.475(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C4 C3 1.385(9) . ? C4 H4 0.9300 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C3 H3 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C27 C28 1.496(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C24 C23 1.502(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? Na1 O7 2.420(4) 1_655 ? Na1 O6 2.522(4) 1_655 ? Na1 O8 2.768(4) 1_655 ? Na1 O5 2.798(4) 1_655 ? C19 C20 1.479(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C17 C18 1.490(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? Cl1 O11 1.396(5) . ? Cl1 O10 1.406(6) . ? Cl1 O12 1.420(5) . ? Cl1 O9 1.421(5) . ? C8 C9 1.364(8) . ? C8 H8 0.9300 . ? C9 C10 1.374(9) . ? C9 H9 0.9300 . ? C10 C11 1.356(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? O13 C37 1.409(10) . ? O13 H13 0.8200 . ? C37 C36 1.456(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C35 C36 1.526(12) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C40 O14B 1.4294(11) . ? C40 O14A 1.4299(11) . ? C40 C39B 1.483(9) . ? C40 C39A 1.545(9) . ? C39A C38A 1.529(10) . ? C39B C38B 1.487(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 N1 Fe1 N1 180.0(2) . 2_556 ? N1 Fe1 N4 91.58(16) . . ? N1 Fe1 N4 88.42(16) 2_556 . ? N1 Fe1 N4 88.42(16) . 2_556 ? N1 Fe1 N4 91.58(16) 2_556 2_556 ? N4 Fe1 N4 180.0 . 2_556 ? N1 Fe1 N2 88.52(16) . 2_556 ? N1 Fe1 N2 91.48(16) 2_556 2_556 ? N4 Fe1 N2 97.24(16) . 2_556 ? N4 Fe1 N2 82.76(16) 2_556 2_556 ? N1 Fe1 N2 91.48(16) . . ? N1 Fe1 N2 88.52(16) 2_556 . ? N4 Fe1 N2 82.76(16) . . ? N4 Fe1 N2 97.24(16) 2_556 . ? N2 Fe1 N2 180.0 2_556 . ? C18 O2 C19 113.1(4) . . ? C18 O2 Na1 112.5(3) . . ? C19 O2 Na1 110.9(3) . . ? C17 O1 C16 111.0(4) . . ? C17 O1 Na1 107.7(3) . . ? C16 O1 Na1 124.3(3) . . ? C28 O6 C29 114.2(4) . . ? C28 O6 Na1 114.1(3) . 1_455 ? C29 O6 Na1 115.6(3) . 1_455 ? C32 O8 C33 110.5(4) . . ? C32 O8 Na1 109.3(3) . 1_455 ? C33 O8 Na1 132.9(3) . 1_455 ? C31 O7 C30 113.6(4) . . ? C31 O7 Na1 114.4(3) . 1_455 ? C30 O7 Na1 109.3(3) . 1_455 ? C27 O5 C26 111.9(4) . . ? C27 O5 Na1 110.8(3) . 1_455 ? C26 O5 Na1 122.5(3) . 1_455 ? C23 O4 C22 111.1(4) . . ? C14 N7 C13 113.9(4) . . ? C7 N4 C11 116.8(5) . . ? C7 N4 Fe1 123.2(3) . . ? C11 N4 Fe1 120.0(4) . . ? C20 O3 C21 113.1(4) . . ? C20 O3 Na1 117.1(3) . . ? C21 O3 Na1 118.3(3) . . ? C1 N1 Fe1 174.4(4) . . ? C12 N5 C14 113.5(4) . . ? C6 N2 C2 117.2(5) . . ? C6 N2 Fe1 123.2(3) . . ? C2 N2 Fe1 119.5(4) . . ? C12 N3 C6 121.5(4) . . ? C12 N3 C7 119.1(4) . . ? C6 N3 C7 119.4(4) . . ? C12 N6 C13 113.7(4) . . ? C4 C5 C6 118.6(6) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C14 N8 C15 120.5(5) . . ? C14 N8 C24 118.0(5) . . ? C15 N8 C24 119.8(5) . . ? C13 N9 C34 120.3(4) . . ? C13 N9 C25 120.1(4) . . ? C34 N9 C25 119.4(4) . . ? N5 C12 N6 127.2(5) . . ? N5 C12 N3 117.4(4) . . ? N6 C12 N3 115.4(4) . . ? N9 C34 C33 114.8(5) . . ? N9 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? N9 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.5 . . ? N1 C1 S1 178.8(5) . . ? N7 C14 N8 118.0(5) . . ? N7 C14 N5 125.5(4) . . ? N8 C14 N5 116.5(5) . . ? N2 C2 C3 122.6(6) . . ? N2 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? N2 C6 C5 123.1(5) . . ? N2 C6 N3 116.1(4) . . ? C5 C6 N3 120.8(5) . . ? O5 C26 C25 108.6(4) . . ? O5 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O5 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? N6 C13 N7 126.2(5) . . ? N6 C13 N9 116.2(4) . . ? N7 C13 N9 117.6(5) . . ? O8 C33 C34 110.2(4) . . ? O8 C33 H33A 109.6 . . ? C34 C33 H33A 109.6 . . ? O8 C33 H33B 109.6 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? N4 C7 C8 123.3(5) . . ? N4 C7 N3 117.1(4) . . ? C8 C7 N3 119.5(5) . . ? O7 C31 C32 108.6(5) . . ? O7 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O7 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.3 . . ? O1 C16 C15 110.1(5) . . ? O1 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? O1 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? O7 C30 C29 112.3(4) . . ? O7 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? O7 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? O3 C21 C22 112.4(5) . . ? O3 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? O3 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? O8 C32 C31 108.5(4) . . ? O8 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? O8 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? N9 C25 C26 115.4(5) . . ? N9 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? N9 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? O6 C29 C30 106.9(4) . . ? O6 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? O6 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? O4 C22 C21 109.0(4) . . ? O4 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O4 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? O5 C27 C28 108.4(5) . . ? O5 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O5 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O6 C28 C27 111.9(5) . . ? O6 C28 H28A 109.2 . . ? C27 C28 H28A 109.2 . . ? O6 C28 H28B 109.2 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? N8 C15 C16 114.0(5) . . ? N8 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N8 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.6 . . ? N8 C24 C23 116.2(5) . . ? N8 C24 H24A 108.2 . . ? C23 C24 H24A 108.2 . . ? N8 C24 H24B 108.2 . . ? C23 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? O4 C23 C24 111.0(5) . . ? O4 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? O4 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O7 Na1 O2 154.07(16) 1_655 . ? O7 Na1 O3 137.37(16) 1_655 . ? O2 Na1 O3 67.39(13) . . ? O7 Na1 O6 67.90(13) 1_655 1_655 ? O2 Na1 O6 136.98(15) . 1_655 ? O3 Na1 O6 76.21(14) . 1_655 ? O7 Na1 O1 92.96(14) 1_655 . ? O2 Na1 O1 68.35(13) . . ? O3 Na1 O1 105.63(14) . . ? O6 Na1 O1 146.63(15) 1_655 . ? O7 Na1 O8 64.98(12) 1_655 1_655 ? O2 Na1 O8 93.82(13) . 1_655 ? O3 Na1 O8 153.86(15) . 1_655 ? O6 Na1 O8 111.03(14) 1_655 1_655 ? O1 Na1 O8 82.28(13) . 1_655 ? O7 Na1 O5 98.63(14) 1_655 1_655 ? O2 Na1 O5 90.04(13) . 1_655 ? O3 Na1 O5 85.18(13) . 1_655 ? O6 Na1 O5 64.14(12) 1_655 1_655 ? O1 Na1 O5 148.57(15) . 1_655 ? O8 Na1 O5 76.49(12) 1_655 1_655 ? O2 C19 C20 112.8(5) . . ? O2 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? O2 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? O1 C17 C18 109.6(5) . . ? O1 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O1 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? O2 C18 C17 108.9(5) . . ? O2 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? O2 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O3 C20 C19 107.9(5) . . ? O3 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O3 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O11 Cl1 O10 110.0(4) . . ? O11 Cl1 O12 110.5(3) . . ? O10 Cl1 O12 110.3(4) . . ? O11 Cl1 O9 108.8(4) . . ? O10 Cl1 O9 108.0(4) . . ? O12 Cl1 O9 109.2(4) . . ? C9 C8 C7 118.2(5) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N4 C11 C10 122.8(6) . . ? N4 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? C37 O13 H13 109.5 . . ? O13 C37 C36 111.7(9) . . ? O13 C37 H37A 109.3 . . ? C36 C37 H37A 109.3 . . ? O13 C37 H37B 109.3 . . ? C36 C37 H37B 109.3 . . ? H37A C37 H37B 107.9 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C35 115.0(9) . . ? C37 C36 H36A 108.5 . . ? C35 C36 H36A 108.5 . . ? C37 C36 H36B 108.5 . . ? C35 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? O14B C40 O14A 94.9(12) . . ? O14B C40 C39B 120.1(9) . . ? O14A C40 C39B 76.0(10) . . ? O14B C40 C39A 109.8(12) . . ? O14A C40 C39A 112.0(8) . . ? C39B C40 C39A 36.5(10) . . ? C38A C39A C40 105.9(8) . . ? C40 C39B C38B 115.2(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O9 0.82 2.16 2.965(9) 169.0 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.882 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.162 #=END data_2 _database_code_depnum_ccdc_archive 'CCDC 823864' #TrackingRef '- DaltonCrown.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DDCr5)].CH3OH ; _chemical_name_common trans-(Fe(ii)(NCS)2(DDCr5)).CH3OH _chemical_melting_point ? _chemical_formula_moiety '(C35H36FeN12O4S2), (CH4O)' _chemical_formula_sum 'C36 H40 Fe N12 O5 S2' _chemical_formula_weight 840.77 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.495(2) _cell_length_b 12.702(2) _cell_length_c 18.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.548(3) _cell_angle_gamma 90.00 _cell_volume 3974.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 56749 _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 27.07 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9734 _exptl_absorpt_correction_T_max 0.9946 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71079 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron MX1' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56749 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.07 _reflns_number_total 8543 _reflns_number_gt 7441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0963P)^2^+14.2572P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8543 _refine_ls_number_parameters 535 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.29266(3) 0.23196(4) 0.23512(3) 0.02064(16) Uani 1 1 d . . . N3 N 0.2161(2) 0.2828(3) 0.06835(18) 0.0259(7) Uani 1 1 d . . . C6 C 0.2222(2) 0.1711(3) 0.0734(2) 0.0289(8) Uani 1 1 d . . . N2 N 0.2486(2) 0.1310(3) 0.1419(2) 0.0308(7) Uani 1 1 d . . . N1 N 0.3694(2) 0.2965(3) 0.17821(17) 0.0279(7) Uani 1 1 d . . . N10 N 0.3919(2) 0.3624(3) -0.21035(18) 0.0271(7) Uani 1 1 d . . . C13 C 0.3337(2) 0.3483(3) -0.05082(19) 0.0250(8) Uani 1 1 d . . . N9 N 0.3745(2) 0.2984(3) -0.09596(17) 0.0257(7) Uani 1 1 d . . . N6 N 0.3370(2) 0.4528(3) -0.05028(18) 0.0279(7) Uani 1 1 d . . . N11 N 0.2965(2) 0.6033(3) -0.0013(2) 0.0360(8) Uani 1 1 d . . . N5 N 0.29441(19) 0.2866(2) -0.01471(16) 0.0233(6) Uani 1 1 d . . . N7 N 0.2566(2) 0.4447(3) 0.03676(18) 0.0284(7) Uani 1 1 d . . . N4 N 0.1936(2) 0.3280(3) 0.18469(19) 0.0321(8) Uani 1 1 d . . . N8 N 0.33637(19) 0.1566(3) -0.17851(18) 0.0256(7) Uani 1 1 d . . . N12 N 0.2211(2) 0.1602(3) 0.29157(19) 0.0311(7) Uani 1 1 d . C . C14 C 0.2960(2) 0.4967(3) -0.0055(2) 0.0292(8) Uani 1 1 d . . . C12 C 0.2570(2) 0.3402(3) 0.02808(19) 0.0234(7) Uani 1 1 d . . . C7 C 0.1702(2) 0.3363(3) 0.1107(2) 0.0278(8) Uani 1 1 d . . . C8 C 0.1032(3) 0.3905(4) 0.0744(3) 0.0424(11) Uani 1 1 d . . . H8 H 0.0886 0.3951 0.0214 0.051 Uiso 1 1 calc R . . C5 C 0.1992(3) 0.1085(4) 0.0093(3) 0.0411(11) Uani 1 1 d . . . H5 H 0.1814 0.1393 -0.0389 0.049 Uiso 1 1 calc R . . C24 C 0.4361(3) 0.4153(3) -0.2481(2) 0.0331(9) Uani 1 1 d . . . H24 H 0.4189 0.4178 -0.3011 0.040 Uiso 1 1 calc R . . C11 C 0.1475(3) 0.3739(4) 0.2250(3) 0.0431(11) Uani 1 1 d . . . H11 H 0.1627 0.3675 0.2779 0.052 Uiso 1 1 calc R . . C20 C 0.4187(2) 0.3586(3) -0.1357(2) 0.0272(8) Uani 1 1 d . . . C19 C 0.3680(2) 0.1875(3) -0.1081(2) 0.0268(8) Uani 1 1 d . . . C18 C 0.3964(3) 0.1175(4) -0.0496(2) 0.0385(10) Uani 1 1 d . . . H18 H 0.4182 0.1421 -0.0002 0.046 Uiso 1 1 calc R . . C3 C 0.2276(3) -0.0414(4) 0.0896(4) 0.0538(15) Uani 1 1 d . . . H3 H 0.2290 -0.1155 0.0968 0.065 Uiso 1 1 calc R . . C17 C 0.3919(3) 0.0107(4) -0.0658(3) 0.0467(12) Uani 1 1 d . . . H17 H 0.4102 -0.0396 -0.0273 0.056 Uiso 1 1 calc R . . C23 C 0.5053(3) 0.4659(4) -0.2137(3) 0.0424(11) Uani 1 1 d . . . H23 H 0.5347 0.5026 -0.2424 0.051 Uiso 1 1 calc R . . C35 C 0.1726(2) 0.1327(4) 0.3198(2) 0.0400(11) Uani 1 1 d D . . C21 C 0.4875(3) 0.4081(4) -0.0969(3) 0.0381(10) Uani 1 1 d . . . H21 H 0.5040 0.4043 -0.0439 0.046 Uiso 1 1 calc R . . C15 C 0.3342(3) 0.0527(3) -0.1934(2) 0.0343(9) Uani 1 1 d . . . H15 H 0.3136 0.0300 -0.2435 0.041 Uiso 1 1 calc R . . C9 C 0.0578(3) 0.4379(4) 0.1163(3) 0.0508(13) Uani 1 1 d . . . H9 H 0.0117 0.4763 0.0926 0.061 Uiso 1 1 calc R . . C10 C 0.0802(3) 0.4288(5) 0.1928(3) 0.0541(14) Uani 1 1 d . . . H10 H 0.0495 0.4601 0.2228 0.065 Uiso 1 1 calc R . . C4 C 0.2032(3) -0.0002(4) 0.0184(4) 0.0512(14) Uani 1 1 d . . . H4 H 0.1894 -0.0455 -0.0238 0.061 Uiso 1 1 calc R . . C22 C 0.5313(3) 0.4627(4) -0.1365(3) 0.0437(11) Uani 1 1 d . . . H22 H 0.5785 0.4975 -0.1114 0.052 Uiso 1 1 calc R . . C2 C 0.2501(3) 0.0254(3) 0.1503(3) 0.0426(11) Uani 1 1 d . . . H2 H 0.2669 -0.0037 0.1991 0.051 Uiso 1 1 calc R . . C16 C 0.3605(3) -0.0218(4) -0.1390(3) 0.0457(12) Uani 1 1 d . . . H16 H 0.3572 -0.0945 -0.1513 0.055 Uiso 1 1 calc R . . C1 C 0.4245(2) 0.2858(3) 0.1537(2) 0.0291(8) Uani 1 1 d . . . S1 S 0.50203(7) 0.27024(11) 0.11994(7) 0.0415(3) Uani 1 1 d . . . O4 O 0.2205(3) 0.7467(3) -0.1293(2) 0.0606(11) Uani 1 1 d D B . C25 C 0.2609(2) 0.6564(4) 0.0530(3) 0.0399(10) Uani 1 1 d D . . H25A H 0.2858 0.7264 0.0649 0.048 Uiso 1 1 calc R . . H25B H 0.2721 0.6148 0.0998 0.048 Uiso 1 1 calc R . . C34 C 0.3318(3) 0.6637(4) -0.0526(2) 0.0402(10) Uani 1 1 d D . . H34A H 0.3819 0.6295 -0.0551 0.048 Uiso 1 1 calc R . . H34B H 0.3447 0.7353 -0.0318 0.048 Uiso 1 1 calc R . . C33 C 0.2805(3) 0.6731(4) -0.1293(2) 0.0456(11) Uani 1 1 d D . . H33A H 0.3121 0.6964 -0.1639 0.055 Uiso 1 1 calc R . . H33B H 0.2569 0.6038 -0.1465 0.055 Uiso 1 1 calc R . . C26 C 0.1744(2) 0.6702(4) 0.0255(3) 0.0417(10) Uani 1 1 d D . . H26A H 0.1618 0.7199 -0.0171 0.050 Uiso 1 1 calc R . . H26B H 0.1485 0.6020 0.0091 0.050 Uiso 1 1 calc R . . O1 O 0.1486(2) 0.7116(3) 0.0882(2) 0.0485(9) Uani 1 1 d D . . C27 C 0.0657(3) 0.7196(4) 0.0751(4) 0.0529(14) Uani 1 1 d D A . H27A H 0.0511 0.7038 0.1224 0.063 Uiso 1 1 calc R . . H27B H 0.0412 0.6648 0.0385 0.063 Uiso 1 1 calc R . . C32 C 0.1606(4) 0.7515(6) -0.1991(3) 0.074(2) Uani 1 1 d D . . C28 C 0.0313(4) 0.8227(5) 0.0471(4) 0.0680(17) Uani 1 1 d DU . . O3 O 0.0866(4) 0.8846(5) -0.1549(3) 0.099(2) Uani 1 1 d D . . O2B O 0.0327(4) 0.8027(6) -0.0337(4) 0.0522(18) Uani 0.50 1 d PDU A 1 C29 C -0.0071(5) 0.8833(8) -0.0748(4) 0.093(2) Uani 1 1 d DU . . O2A O 0.0500(5) 0.8835(8) -0.0079(5) 0.071(2) Uani 0.50 1 d PDU A 2 C31B C 0.0816(5) 0.7809(10) -0.1902(7) 0.084(4) Uani 0.60 1 d PDU B 2 C31A C 0.1320(9) 0.8615(7) -0.2076(7) 0.064(4) Uani 0.40 1 d PDU B 1 C30 C 0.0086(5) 0.8964(9) -0.1493(5) 0.109(3) Uani 1 1 d DU A . H30A H -0.0245 0.8449 -0.1836 0.131 Uiso 1 1 calc R . . H30B H -0.0097 0.9675 -0.1679 0.131 Uiso 1 1 calc R . . S2A S 0.1088(2) 0.0795(3) 0.3599(2) 0.0701(11) Uani 0.70 1 d PD C 1 S2B S 0.0960(4) 0.1368(8) 0.3573(4) 0.071(3) Uani 0.30 1 d PD C 2 O5 O 0.3807(3) 0.8313(5) 0.2075(3) 0.0892(16) Uani 1 1 d DU . . H5A H 0.4066 0.8103 0.2497 0.107 Uiso 1 1 calc R . . C36 C 0.4305(4) 0.8332(6) 0.1575(4) 0.0746(19) Uani 1 1 d DU . . H36A H 0.4129 0.8887 0.1202 0.112 Uiso 1 1 calc R . . H36B H 0.4280 0.7649 0.1323 0.112 Uiso 1 1 calc R . . H36C H 0.4850 0.8472 0.1856 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0265(3) 0.0215(3) 0.0190(3) -0.00033(19) 0.0152(2) -0.00343(19) N3 0.0342(17) 0.0242(16) 0.0246(15) -0.0027(12) 0.0172(13) 0.0018(13) C6 0.0307(19) 0.0250(19) 0.038(2) -0.0072(16) 0.0218(17) -0.0027(15) N2 0.0321(17) 0.0227(16) 0.0433(19) 0.0002(14) 0.0203(15) -0.0023(13) N1 0.0315(17) 0.0342(18) 0.0221(15) -0.0006(13) 0.0145(13) -0.0090(14) N10 0.0334(17) 0.0260(16) 0.0272(16) -0.0004(13) 0.0176(13) 0.0016(13) C13 0.0299(18) 0.0301(19) 0.0181(16) -0.0045(14) 0.0117(14) 0.0034(15) N9 0.0372(17) 0.0241(16) 0.0218(14) -0.0036(12) 0.0187(13) 0.0019(13) N6 0.0375(18) 0.0255(16) 0.0265(16) -0.0062(13) 0.0188(14) -0.0008(13) N11 0.0385(19) 0.0275(18) 0.049(2) -0.0079(16) 0.0236(17) -0.0022(14) N5 0.0326(17) 0.0230(15) 0.0185(14) -0.0032(12) 0.0143(12) 0.0006(12) N7 0.0358(18) 0.0263(16) 0.0285(16) -0.0055(13) 0.0180(14) -0.0009(13) N4 0.0428(19) 0.0304(18) 0.0325(17) -0.0058(14) 0.0269(15) -0.0030(15) N8 0.0328(17) 0.0236(16) 0.0262(15) -0.0041(13) 0.0181(13) 0.0031(13) N12 0.0344(18) 0.0349(19) 0.0281(16) 0.0002(14) 0.0153(14) -0.0028(14) C14 0.036(2) 0.0258(19) 0.0299(19) -0.0069(16) 0.0160(16) -0.0009(15) C12 0.0287(18) 0.0261(18) 0.0183(16) -0.0044(14) 0.0112(14) 0.0011(14) C7 0.036(2) 0.0237(18) 0.0315(19) -0.0038(15) 0.0223(16) 0.0004(15) C8 0.044(3) 0.044(3) 0.045(3) 0.001(2) 0.025(2) 0.010(2) C5 0.040(2) 0.041(3) 0.050(3) -0.020(2) 0.025(2) -0.0079(19) C24 0.041(2) 0.030(2) 0.036(2) -0.0011(17) 0.0246(18) -0.0032(17) C11 0.059(3) 0.045(3) 0.038(2) -0.004(2) 0.036(2) 0.006(2) C20 0.035(2) 0.0245(18) 0.0274(18) -0.0041(15) 0.0176(16) 0.0021(15) C19 0.037(2) 0.0261(19) 0.0236(17) 0.0003(15) 0.0202(16) 0.0039(15) C18 0.055(3) 0.036(2) 0.030(2) 0.0046(18) 0.0190(19) 0.010(2) C3 0.046(3) 0.024(2) 0.099(5) -0.011(3) 0.032(3) -0.0041(19) C17 0.071(3) 0.029(2) 0.045(3) 0.010(2) 0.024(2) 0.014(2) C23 0.043(2) 0.039(2) 0.055(3) -0.005(2) 0.029(2) -0.009(2) C35 0.037(2) 0.057(3) 0.0260(19) 0.0060(19) 0.0067(17) -0.016(2) C21 0.040(2) 0.040(2) 0.037(2) -0.0122(19) 0.0156(19) -0.0042(19) C15 0.045(2) 0.026(2) 0.036(2) -0.0073(17) 0.0177(18) 0.0062(17) C9 0.055(3) 0.048(3) 0.061(3) 0.008(2) 0.035(3) 0.019(2) C10 0.066(3) 0.055(3) 0.058(3) 0.002(3) 0.047(3) 0.017(3) C4 0.044(3) 0.039(3) 0.080(4) -0.032(3) 0.032(3) -0.012(2) C22 0.043(3) 0.042(3) 0.051(3) -0.011(2) 0.022(2) -0.013(2) C2 0.038(2) 0.023(2) 0.069(3) 0.000(2) 0.020(2) -0.0021(17) C16 0.063(3) 0.024(2) 0.056(3) -0.002(2) 0.025(2) 0.009(2) C1 0.034(2) 0.032(2) 0.0231(17) 0.0009(15) 0.0097(16) -0.0060(16) S1 0.0372(6) 0.0536(7) 0.0416(6) -0.0001(5) 0.0244(5) -0.0065(5) O4 0.086(3) 0.046(2) 0.046(2) 0.0061(17) 0.011(2) 0.025(2) C25 0.041(2) 0.028(2) 0.055(3) -0.015(2) 0.021(2) -0.0042(18) C34 0.040(2) 0.031(2) 0.056(3) -0.003(2) 0.022(2) -0.0049(18) C33 0.051(3) 0.041(3) 0.051(3) 0.000(2) 0.024(2) 0.001(2) C26 0.046(3) 0.035(2) 0.049(3) -0.003(2) 0.021(2) -0.0011(19) O1 0.048(2) 0.043(2) 0.063(2) -0.0087(17) 0.0297(17) 0.0058(15) C27 0.041(3) 0.045(3) 0.081(4) -0.006(3) 0.031(3) 0.001(2) C32 0.084(5) 0.081(5) 0.048(3) 0.007(3) 0.001(3) 0.027(4) C28 0.055(3) 0.067(4) 0.089(4) 0.027(3) 0.032(3) 0.012(3) O3 0.127(5) 0.103(4) 0.076(3) 0.020(3) 0.042(3) 0.055(4) O2B 0.047(4) 0.037(4) 0.068(4) 0.021(3) 0.006(3) -0.008(3) C29 0.063(4) 0.115(6) 0.096(5) 0.024(5) 0.013(4) 0.016(4) O2A 0.071(5) 0.070(5) 0.078(5) 0.012(5) 0.027(4) -0.002(4) C31B 0.081(7) 0.091(7) 0.072(6) -0.007(6) 0.004(5) 0.025(6) C31A 0.074(8) 0.049(7) 0.054(7) 0.009(6) -0.008(6) 0.017(6) C30 0.089(5) 0.134(7) 0.104(6) 0.037(5) 0.023(5) -0.001(5) S2A 0.0481(14) 0.119(3) 0.0415(13) 0.0301(19) 0.0093(10) -0.0428(17) S2B 0.048(3) 0.140(8) 0.030(2) 0.020(4) 0.016(2) -0.050(4) O5 0.068(3) 0.111(4) 0.083(3) 0.006(3) 0.008(3) 0.011(3) C36 0.072(4) 0.076(4) 0.071(4) -0.021(3) 0.010(3) 0.012(3) _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 N12 2.034(3) . ? Fe1 N1 2.071(3) . ? Fe1 N8 2.126(3) 4_566 ? Fe1 N2 2.130(4) . ? Fe1 N4 2.133(4) . ? Fe1 N10 2.141(3) 4_566 ? N3 C12 1.366(5) . ? N3 C6 1.424(5) . ? N3 C7 1.426(5) . ? C6 N2 1.335(6) . ? C6 C5 1.399(6) . ? N2 C2 1.350(6) . ? N1 C1 1.170(5) . ? N10 C20 1.341(5) . ? N10 C24 1.345(5) . ? N10 Fe1 2.141(3) 4_565 ? C13 N5 1.327(5) . ? C13 N6 1.329(5) . ? C13 N9 1.381(4) . ? N9 C20 1.417(5) . ? N9 C19 1.427(5) . ? N6 C14 1.346(5) . ? N11 C14 1.356(5) . ? N11 C34 1.471(6) . ? N11 C25 1.471(5) . ? N5 C12 1.333(4) . ? N7 C12 1.337(5) . ? N7 C14 1.339(5) . ? N4 C7 1.330(5) . ? N4 C11 1.358(5) . ? N8 C19 1.339(5) . ? N8 C15 1.348(5) . ? N8 Fe1 2.126(3) 4_565 ? N12 C35 1.156(5) . ? C7 C8 1.378(6) . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C5 C4 1.391(7) . ? C5 H5 0.9500 . ? C24 C23 1.377(7) . ? C24 H24 0.9500 . ? C11 C10 1.370(8) . ? C11 H11 0.9500 . ? C20 C21 1.387(6) . ? C19 C18 1.390(6) . ? C18 C17 1.388(7) . ? C18 H18 0.9500 . ? C3 C4 1.380(9) . ? C3 C2 1.383(8) . ? C3 H3 0.9500 . ? C17 C16 1.389(7) . ? C17 H17 0.9500 . ? C23 C22 1.384(7) . ? C23 H23 0.9500 . ? C35 S2A 1.634(4) . ? C35 S2B 1.657(5) . ? C21 C22 1.373(7) . ? C21 H21 0.9500 . ? C15 C16 1.372(7) . ? C15 H15 0.9500 . ? C9 C10 1.373(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C4 H4 0.9500 . ? C22 H22 0.9500 . ? C2 H2 0.9500 . ? C16 H16 0.9500 . ? C1 S1 1.642(4) . ? O4 C33 1.406(6) . ? O4 C32 1.445(7) . ? C25 C26 1.480(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C34 C33 1.480(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C26 O1 1.445(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O1 C27 1.414(6) . ? C27 C28 1.479(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C32 C31A 1.480(4) . ? C32 C31B 1.480(4) . ? C28 O2A 1.381(9) . ? C28 O2B 1.521(9) . ? O3 C30 1.403(9) . ? O3 C31A 1.433(12) . ? O3 C31B 1.464(11) . ? O2B C29 1.359(9) . ? C29 O2A 1.380(10) . ? C29 C30 1.479(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O5 C36 1.419(7) . ? O5 H5A 0.8400 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N12 Fe1 N1 176.47(15) . . ? N12 Fe1 N8 93.71(13) . 4_566 ? N1 Fe1 N8 87.76(12) . 4_566 ? N12 Fe1 N2 90.02(13) . . ? N1 Fe1 N2 88.69(13) . . ? N8 Fe1 N2 175.10(13) 4_566 . ? N12 Fe1 N4 86.75(14) . . ? N1 Fe1 N4 96.39(13) . . ? N8 Fe1 N4 92.67(13) 4_566 . ? N2 Fe1 N4 84.37(13) . . ? N12 Fe1 N10 92.19(13) . 4_566 ? N1 Fe1 N10 84.72(13) . 4_566 ? N8 Fe1 N10 85.59(13) 4_566 4_566 ? N2 Fe1 N10 97.45(13) . 4_566 ? N4 Fe1 N10 177.90(12) . 4_566 ? C12 N3 C6 121.8(3) . . ? C12 N3 C7 119.3(3) . . ? C6 N3 C7 118.8(3) . . ? N2 C6 C5 122.9(4) . . ? N2 C6 N3 116.4(3) . . ? C5 C6 N3 120.6(4) . . ? C6 N2 C2 118.8(4) . . ? C6 N2 Fe1 120.4(3) . . ? C2 N2 Fe1 120.8(3) . . ? C1 N1 Fe1 148.4(3) . . ? C20 N10 C24 116.9(4) . . ? C20 N10 Fe1 119.8(3) . 4_565 ? C24 N10 Fe1 122.7(3) . 4_565 ? N5 C13 N6 127.9(3) . . ? N5 C13 N9 116.4(3) . . ? N6 C13 N9 115.7(3) . . ? C13 N9 C20 119.9(3) . . ? C13 N9 C19 121.0(3) . . ? C20 N9 C19 118.9(3) . . ? C13 N6 C14 112.9(3) . . ? C14 N11 C34 118.8(3) . . ? C14 N11 C25 120.0(4) . . ? C34 N11 C25 121.2(4) . . ? C13 N5 C12 112.9(3) . . ? C12 N7 C14 113.7(3) . . ? C7 N4 C11 117.3(4) . . ? C7 N4 Fe1 120.1(3) . . ? C11 N4 Fe1 122.3(3) . . ? C19 N8 C15 118.0(4) . . ? C19 N8 Fe1 121.2(3) . 4_565 ? C15 N8 Fe1 120.8(3) . 4_565 ? C35 N12 Fe1 169.2(4) . . ? N7 C14 N6 125.9(4) . . ? N7 C14 N11 117.2(3) . . ? N6 C14 N11 116.9(4) . . ? N5 C12 N7 126.6(3) . . ? N5 C12 N3 117.0(3) . . ? N7 C12 N3 116.4(3) . . ? N4 C7 C8 123.0(4) . . ? N4 C7 N3 117.1(4) . . ? C8 C7 N3 119.9(4) . . ? C7 C8 C9 118.9(5) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C4 C5 C6 117.8(5) . . ? C4 C5 H5 121.1 . . ? C6 C5 H5 121.1 . . ? N10 C24 C23 123.2(4) . . ? N10 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? N4 C11 C10 122.9(4) . . ? N4 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? N10 C20 C21 123.4(4) . . ? N10 C20 N9 117.1(3) . . ? C21 C20 N9 119.4(4) . . ? N8 C19 C18 123.2(4) . . ? N8 C19 N9 116.0(3) . . ? C18 C19 N9 120.7(4) . . ? C17 C18 C19 117.9(4) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C4 C3 C2 119.9(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C18 C17 C16 119.1(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C24 C23 C22 119.0(4) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? N12 C35 S2A 173.0(5) . . ? N12 C35 S2B 160.3(6) . . ? S2A C35 S2B 26.7(3) . . ? C22 C21 C20 118.7(4) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? N8 C15 C16 122.6(4) . . ? N8 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 118.8(4) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C21 C22 C23 118.8(4) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N2 C2 C3 121.5(5) . . ? N2 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N1 C1 S1 179.6(4) . . ? C33 O4 C32 113.7(4) . . ? N11 C25 C26 113.0(4) . . ? N11 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? N11 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N11 C34 C33 114.1(4) . . ? N11 C34 H34A 108.7 . . ? C33 C34 H34A 108.7 . . ? N11 C34 H34B 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? O4 C33 C34 109.1(4) . . ? O4 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? O4 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O1 C26 C25 105.4(4) . . ? O1 C26 H26A 110.7 . . ? C25 C26 H26A 110.7 . . ? O1 C26 H26B 110.7 . . ? C25 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C27 O1 C26 113.8(4) . . ? O1 C27 C28 115.7(4) . . ? O1 C27 H27A 108.4 . . ? C28 C27 H27A 108.4 . . ? O1 C27 H27B 108.4 . . ? C28 C27 H27B 108.4 . . ? H27A C27 H27B 107.4 . . ? O4 C32 C31A 106.6(7) . . ? O4 C32 C31B 113.5(7) . . ? C31A C32 C31B 58.2(8) . . ? O2A C28 C27 127.0(6) . . ? O2A C28 O2B 46.0(5) . . ? C27 C28 O2B 95.2(5) . . ? C30 O3 C31A 141.9(9) . . ? C30 O3 C31B 100.3(8) . . ? C31A O3 C31B 59.5(7) . . ? C29 O2B C28 106.9(6) . . ? O2B C29 O2A 49.2(5) . . ? O2B C29 C30 114.6(8) . . ? O2A C29 C30 124.9(8) . . ? C29 O2A C28 114.0(8) . . ? O3 C31B C32 108.9(8) . . ? O3 C31A C32 110.6(8) . . ? O3 C30 C29 117.9(7) . . ? O3 C30 H30A 107.8 . . ? C29 C30 H30A 107.8 . . ? O3 C30 H30B 107.8 . . ? C29 C30 H30B 107.8 . . ? H30A C30 H30B 107.2 . . ? C36 O5 H5A 109.5 . . ? O5 C36 H36A 109.5 . . ? O5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A S1 0.84 2.59 3.419(5) 171.8 2_655 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.463 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.108 #=END data_3 _database_code_depnum_ccdc_archive 'CCDC 823865' #TrackingRef '- DaltonCrown.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-[(Fe(II))2(NCS)4(DCrCr5)2] ; _chemical_name_common cis-((Fe(ii))2(NCS)4(DCrCr5)2) _chemical_melting_point ? _chemical_formula_moiety '(C70 H72 Fe2 N24 O8 S4)' _chemical_formula_sum 'C70 H72 Fe2 N24 O8 S4' _chemical_formula_weight 1617.46 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.830(10) _cell_length_b 14.780(10) _cell_length_c 16.483(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.52(4) _cell_angle_gamma 90.00 _cell_volume 3602(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54682 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.75 _exptl_crystal_description 'plate ' _exptl_crystal_colour orange _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9941 _exptl_absorpt_correction_T_max 0.9970 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron MX2' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 315r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54682 _diffrn_reflns_av_R_equivalents 0.1964 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.75 _reflns_number_total 8046 _reflns_number_gt 4243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.1848P)^2^+6.4801P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8046 _refine_ls_number_parameters 479 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1862 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.3425 _refine_ls_wR_factor_gt 0.2933 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.38544(7) 0.37543(7) 0.25608(5) 0.0442(3) Uani 1 1 d . . . S1 S 0.10820(16) 0.32673(15) 0.09993(15) 0.0712(7) Uani 1 1 d . . . N2 N 0.5122(4) 0.3937(4) 0.3040(3) 0.0456(14) Uani 1 1 d . . . C5 C 0.6338(5) 0.3563(6) 0.4025(4) 0.056(2) Uani 1 1 d . . . H5 H 0.6549 0.3252 0.4508 0.067 Uiso 1 1 calc R . . N1 N 0.2623(4) 0.3542(4) 0.2030(4) 0.0530(15) Uani 1 1 d . . . N8 N 0.6745(4) 0.5689(4) 0.6492(3) 0.0455(14) Uani 1 1 d . . . N3 N 0.4779(4) 0.3114(4) 0.4194(3) 0.0371(12) Uani 1 1 d . . . N7 N 0.4044(4) 0.2843(4) 0.5358(3) 0.0427(13) Uani 1 1 d . . . C15 C 0.7408(5) 0.6143(6) 0.6158(4) 0.0505(18) Uani 1 1 d . . . H15 H 0.7493 0.6763 0.6293 0.061 Uiso 1 1 calc R . . N4 N 0.3891(4) 0.2520(4) 0.3077(3) 0.0421(13) Uani 1 1 d . . . C6 C 0.5432(5) 0.3560(5) 0.3753(4) 0.0415(15) Uani 1 1 d . . . C10 C 0.3521(5) 0.0943(5) 0.2981(5) 0.0486(17) Uani 1 1 d . . . H10 H 0.3224 0.0462 0.2685 0.058 Uiso 1 1 calc R . . C11 C 0.3513(5) 0.1801(5) 0.2664(4) 0.0488(17) Uani 1 1 d . . . H11 H 0.3231 0.1897 0.2133 0.059 Uiso 1 1 calc R . . C9 C 0.3966(5) 0.0787(5) 0.3736(5) 0.0501(17) Uani 1 1 d . . . H9 H 0.3982 0.0197 0.3966 0.060 Uiso 1 1 calc R . . C8 C 0.4386(5) 0.1499(5) 0.4151(4) 0.0429(15) Uani 1 1 d . . . H8 H 0.4716 0.1403 0.4662 0.051 Uiso 1 1 calc R . . C1 C 0.1982(6) 0.3442(5) 0.1596(4) 0.0494(17) Uani 1 1 d . . . C12 C 0.4716(4) 0.3292(4) 0.5025(4) 0.0368(14) Uani 1 1 d . . . C19 C 0.6627(4) 0.4818(5) 0.6293(4) 0.0443(16) Uani 1 1 d . . . C17 C 0.7876(5) 0.4826(7) 0.5477(5) 0.063(2) Uani 1 1 d . . . H17 H 0.8268 0.4530 0.5133 0.076 Uiso 1 1 calc R . . C18 C 0.7206(5) 0.4340(6) 0.5827(4) 0.0539(19) Uani 1 1 d . . . H18 H 0.7146 0.3705 0.5752 0.065 Uiso 1 1 calc R . . C16 C 0.7972(5) 0.5755(7) 0.5631(5) 0.061(2) Uani 1 1 d . . . H16 H 0.8411 0.6104 0.5381 0.073 Uiso 1 1 calc R . . C7 C 0.4321(4) 0.2364(4) 0.3812(4) 0.0377(14) Uani 1 1 d . . . N5 N 0.5315(4) 0.3846(4) 0.5394(3) 0.0389(12) Uani 1 1 d . . . C14 C 0.4039(4) 0.3006(5) 0.6169(4) 0.0412(15) Uani 1 1 d . . . N6 N 0.4616(4) 0.3523(4) 0.6613(3) 0.0436(13) Uani 1 1 d . . . N12 N 0.4333(5) 0.3208(5) 0.1595(4) 0.0620(18) Uani 1 1 d . . . C20 C 0.6033(5) 0.4251(5) 0.7525(4) 0.0474(17) Uani 1 1 d . . . N9 N 0.5934(4) 0.4352(4) 0.6663(3) 0.0415(13) Uani 1 1 d . . . C2 C 0.5739(6) 0.4346(5) 0.2595(4) 0.0527(19) Uani 1 1 d . . . H2 H 0.5539 0.4594 0.2080 0.063 Uiso 1 1 calc R . . C21 C 0.6047(5) 0.3404(5) 0.7883(4) 0.0513(18) Uani 1 1 d . . . H21 H 0.5986 0.2875 0.7555 0.062 Uiso 1 1 calc R . . C24 C 0.6333(6) 0.4924(6) 0.8776(4) 0.061(2) Uani 1 1 d . . . H24 H 0.6481 0.5450 0.9090 0.074 Uiso 1 1 calc R . . C4 C 0.6923(6) 0.4032(7) 0.3573(5) 0.068(3) Uani 1 1 d . . . H4 H 0.7540 0.4089 0.3767 0.081 Uiso 1 1 calc R . . C13 C 0.5251(4) 0.3886(4) 0.6202(4) 0.0363(14) Uani 1 1 d . . . C3 C 0.6626(6) 0.4416(6) 0.2850(5) 0.062(2) Uani 1 1 d . . . H3 H 0.7033 0.4727 0.2531 0.074 Uiso 1 1 calc R . . N10 N 0.6173(4) 0.5021(5) 0.7954(3) 0.0530(16) Uani 1 1 d . . . S2 S 0.4467(3) 0.2305(2) 0.01098(15) 0.1080(11) Uani 1 1 d . . . N11 N 0.3380(4) 0.2598(4) 0.6555(3) 0.0514(15) Uani 1 1 d . B . C22 C 0.6150(6) 0.3336(6) 0.8712(4) 0.065(2) Uani 1 1 d . . . H22 H 0.6123 0.2763 0.8969 0.078 Uiso 1 1 calc R . . C23 C 0.6294(6) 0.4118(6) 0.9172(4) 0.059(2) Uani 1 1 d . . . H23 H 0.6363 0.4091 0.9749 0.070 Uiso 1 1 calc R . . C35 C 0.4422(7) 0.2815(6) 0.0987(6) 0.074(3) Uani 1 1 d . . . C25 C 0.2736(5) 0.1981(5) 0.6124(5) 0.061(2) Uani 1 1 d D . . H25A H 0.2527 0.2254 0.5594 0.073 Uiso 1 1 calc R A 1 H25B H 0.2202 0.1915 0.6445 0.073 Uiso 1 1 calc R A 1 C34 C 0.3364(5) 0.2675(6) 0.7431(5) 0.070(2) Uani 1 1 d D . . C26 C 0.3111(5) 0.1064(5) 0.5978(7) 0.084(3) Uani 1 1 d D B 1 H26A H 0.3371 0.1047 0.5443 0.101 Uiso 1 1 calc R B 1 H26B H 0.3596 0.0917 0.6405 0.101 Uiso 1 1 calc R B 1 O1 O 0.2391(4) 0.0427(3) 0.5994(3) 0.0660(15) Uani 1 1 d D . . C27 C 0.2595(7) -0.0467(5) 0.5737(5) 0.080(3) Uani 1 1 d D B . H27A H 0.2741 -0.0442 0.5162 0.096 Uiso 1 1 calc R . . H27B H 0.2047 -0.0845 0.5760 0.096 Uiso 1 1 calc R . . C28 C 0.3359(7) -0.0915(8) 0.6226(4) 0.084(3) Uani 1 1 d D . . H28A H 0.3417 -0.1550 0.6045 0.101 Uiso 1 1 calc R B . H28B H 0.3932 -0.0597 0.6143 0.101 Uiso 1 1 calc R . . O2 O 0.3195(5) -0.0895(5) 0.7067(3) 0.091(2) Uani 1 1 d D B . C29 C 0.3873(6) -0.1345(8) 0.7580(5) 0.087(3) Uani 1 1 d D . . H29A H 0.4481 -0.1155 0.7437 0.104 Uiso 1 1 calc R B . H29B H 0.3820 -0.2007 0.7503 0.104 Uiso 1 1 calc R . . O3 O 0.3916(4) -0.0171(5) 0.8611(5) 0.103(2) Uani 1 1 d D . . C30 C 0.3752(7) -0.1107(6) 0.8449(6) 0.093(3) Uani 1 1 d D B . H30A H 0.3127 -0.1258 0.8572 0.112 Uiso 1 1 calc R . . H30B H 0.4172 -0.1474 0.8810 0.112 Uiso 1 1 calc R . . C31 C 0.4819(5) 0.0113(6) 0.8506(8) 0.126(5) Uiso 1 1 d D B . O4A O 0.4026(7) 0.1396(6) 0.8030(7) 0.073(3) Uiso 0.50 1 d PD B 1 O4B O 0.4631(6) 0.1623(6) 0.7797(7) 0.065(3) Uiso 0.50 1 d PD B 2 C32B C 0.4914(9) 0.0700(6) 0.7803(9) 0.087(4) Uiso 0.50 1 d PD B 2 C33A C 0.4059(11) 0.2360(6) 0.8032(11) 0.096(7) Uiso 0.50 1 d PD B 1 C32A C 0.4879(7) 0.1066(7) 0.8366(12) 0.087(4) Uiso 0.50 1 d PD B 1 C33B C 0.3681(6) 0.1770(7) 0.7798(9) 0.050(3) Uiso 0.50 1 d PD B 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 0.0528(6) 0.0527(6) 0.0262(5) -0.0026(4) -0.0023(4) -0.0023(5) S1 0.0719(14) 0.0569(13) 0.0780(15) 0.0091(11) -0.0368(12) -0.0133(11) N2 0.060(4) 0.046(3) 0.033(3) 0.002(2) 0.016(3) -0.001(3) C5 0.049(4) 0.087(6) 0.031(3) -0.012(4) 0.004(3) -0.017(4) N1 0.057(4) 0.062(4) 0.039(3) -0.005(3) -0.006(3) -0.008(3) N8 0.045(3) 0.059(4) 0.031(3) 0.007(3) -0.002(2) 0.000(3) N3 0.042(3) 0.047(3) 0.022(2) -0.002(2) 0.000(2) -0.008(2) N7 0.043(3) 0.051(3) 0.034(3) 0.000(2) 0.006(2) -0.002(3) C15 0.043(4) 0.065(5) 0.043(4) 0.005(3) 0.000(3) -0.010(4) N4 0.045(3) 0.051(3) 0.030(3) -0.004(2) -0.001(2) -0.005(3) C6 0.047(4) 0.048(4) 0.030(3) -0.005(3) 0.006(3) -0.009(3) C10 0.045(4) 0.048(4) 0.053(4) -0.008(3) 0.005(3) -0.007(3) C11 0.047(4) 0.058(5) 0.040(4) -0.006(3) -0.005(3) -0.008(3) C9 0.052(4) 0.047(4) 0.052(4) 0.004(3) 0.006(4) -0.001(3) C8 0.048(4) 0.046(4) 0.035(3) 0.000(3) 0.003(3) -0.002(3) C1 0.064(5) 0.042(4) 0.041(4) -0.001(3) -0.004(4) -0.006(3) C12 0.042(3) 0.042(3) 0.027(3) 0.005(3) 0.007(3) 0.001(3) C19 0.038(3) 0.066(5) 0.026(3) -0.001(3) -0.009(3) -0.004(3) C17 0.044(4) 0.098(7) 0.048(4) -0.023(4) 0.000(4) -0.004(4) C18 0.040(4) 0.087(6) 0.034(4) -0.015(4) -0.005(3) -0.002(4) C16 0.047(4) 0.092(6) 0.045(4) -0.008(4) 0.001(3) -0.020(4) C7 0.040(3) 0.046(4) 0.026(3) 0.001(3) -0.002(3) -0.002(3) N5 0.046(3) 0.045(3) 0.025(2) -0.001(2) 0.000(2) -0.001(3) C14 0.043(4) 0.051(4) 0.030(3) 0.004(3) 0.008(3) -0.001(3) N6 0.045(3) 0.057(3) 0.029(3) 0.002(2) 0.003(2) 0.007(3) N12 0.092(5) 0.062(4) 0.033(3) -0.002(3) 0.006(3) -0.008(4) C20 0.053(4) 0.063(5) 0.024(3) 0.001(3) -0.004(3) 0.008(4) N9 0.047(3) 0.052(3) 0.024(2) 0.000(2) -0.001(2) -0.002(3) C2 0.070(5) 0.052(4) 0.038(4) 0.000(3) 0.021(4) -0.010(4) C21 0.065(5) 0.056(4) 0.033(3) -0.001(3) 0.000(3) 0.019(4) C24 0.083(6) 0.069(5) 0.031(4) -0.002(3) -0.009(4) 0.008(4) C4 0.048(4) 0.110(7) 0.046(4) -0.022(5) 0.006(4) -0.028(5) C13 0.039(3) 0.041(3) 0.029(3) 0.002(3) 0.001(3) 0.004(3) C3 0.065(5) 0.080(6) 0.043(4) -0.017(4) 0.024(4) -0.031(4) N10 0.063(4) 0.070(4) 0.024(3) -0.003(3) -0.008(3) 0.010(3) S2 0.170(3) 0.108(2) 0.0497(13) -0.0121(14) 0.0309(17) 0.007(2) N11 0.055(4) 0.066(4) 0.033(3) 0.003(3) 0.010(3) -0.014(3) C22 0.082(6) 0.073(5) 0.037(4) 0.002(4) -0.008(4) 0.016(5) C23 0.069(5) 0.073(5) 0.030(3) 0.004(3) -0.012(4) 0.017(4) C35 0.100(7) 0.067(6) 0.058(5) 0.020(4) 0.028(5) 0.011(5) C25 0.052(4) 0.082(6) 0.051(4) -0.002(4) 0.017(4) -0.002(4) C34 0.069(5) 0.104(7) 0.040(4) 0.001(4) 0.015(4) -0.007(5) C26 0.068(6) 0.087(7) 0.102(8) -0.015(6) 0.037(6) -0.014(5) O1 0.069(4) 0.074(4) 0.055(3) -0.007(3) 0.004(3) -0.004(3) C27 0.090(7) 0.088(7) 0.060(5) -0.018(5) -0.006(5) 0.016(6) C28 0.087(7) 0.103(8) 0.065(6) -0.011(5) 0.019(5) 0.010(6) O2 0.100(5) 0.115(6) 0.062(4) 0.016(4) 0.031(4) 0.014(4) C29 0.074(6) 0.104(8) 0.085(7) 0.025(6) 0.025(6) 0.019(6) O3 0.075(5) 0.139(7) 0.096(5) 0.031(5) 0.016(4) 0.005(5) C30 0.068(6) 0.116(10) 0.097(8) 0.029(7) 0.010(6) -0.001(6) _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 N12 1.967(7) . ? Fe1 N1 1.986(7) . ? Fe1 N2 1.999(7) . ? Fe1 N10 1.999(7) 3_666 ? Fe1 N4 2.011(6) . ? Fe1 N8 2.030(6) 3_666 ? S1 C1 1.615(8) . ? N2 C6 1.348(9) . ? N2 C2 1.360(9) . ? C5 C4 1.376(11) . ? C5 C6 1.382(10) . ? N1 C1 1.154(9) . ? N8 C19 1.337(9) . ? N8 C15 1.344(9) . ? N8 Fe1 2.030(6) 3_666 ? N3 C12 1.406(7) . ? N3 C6 1.419(8) . ? N3 C7 1.421(8) . ? N7 C12 1.349(8) . ? N7 C14 1.359(8) . ? C15 C16 1.378(11) . ? N4 C7 1.344(8) . ? N4 C11 1.359(9) . ? C10 C11 1.371(10) . ? C10 C9 1.382(10) . ? C9 C8 1.378(10) . ? C8 C7 1.396(9) . ? C12 N5 1.321(8) . ? C19 C18 1.389(10) . ? C19 N9 1.415(9) . ? C17 C18 1.388(11) . ? C17 C16 1.401(13) . ? N5 C13 1.344(7) . ? C14 N6 1.324(9) . ? C14 N11 1.349(8) . ? N6 C13 1.316(8) . ? N12 C35 1.175(10) . ? C20 N10 1.347(10) . ? C20 C21 1.383(11) . ? C20 N9 1.426(7) . ? N9 C13 1.397(8) . ? C2 C3 1.352(11) . ? C21 C22 1.366(9) . ? C24 C23 1.362(11) . ? C24 N10 1.364(8) . ? C4 C3 1.361(12) . ? N10 Fe1 1.999(7) 3_666 ? S2 C35 1.637(10) . ? N11 C34 1.451(9) . ? N11 C25 1.463(10) . ? C22 C23 1.390(12) . ? C25 C26 1.492(8) . ? C34 C33A 1.448(9) . ? C34 C33B 1.527(8) . ? C26 O1 1.426(4) . ? O1 C27 1.426(4) . ? C27 C28 1.494(8) . ? C28 O2 1.426(4) . ? O2 C29 1.426(4) . ? C29 C30 1.500(8) . ? O3 C31 1.426(4) . ? O3 C30 1.426(4) . ? C31 C32A 1.432(8) . ? C31 C32B 1.463(9) . ? O4A C33A 1.426(4) . ? O4A C32A 1.426(4) . ? O4B C32B 1.426(4) . ? O4B C33B 1.426(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 N12 Fe1 N1 87.5(3) . . ? N12 Fe1 N2 89.3(3) . . ? N1 Fe1 N2 176.8(2) . . ? N12 Fe1 N10 91.4(3) . 3_666 ? N1 Fe1 N10 88.2(3) . 3_666 ? N2 Fe1 N10 91.9(2) . 3_666 ? N12 Fe1 N4 88.3(2) . . ? N1 Fe1 N4 92.1(3) . . ? N2 Fe1 N4 87.8(2) . . ? N10 Fe1 N4 179.6(2) 3_666 . ? N12 Fe1 N8 175.2(3) . 3_666 ? N1 Fe1 N8 87.7(2) . 3_666 ? N2 Fe1 N8 95.5(2) . 3_666 ? N10 Fe1 N8 88.0(2) 3_666 3_666 ? N4 Fe1 N8 92.4(2) . 3_666 ? C6 N2 C2 117.1(6) . . ? C6 N2 Fe1 122.3(4) . . ? C2 N2 Fe1 119.9(5) . . ? C4 C5 C6 117.6(7) . . ? C1 N1 Fe1 167.8(6) . . ? C19 N8 C15 117.8(6) . . ? C19 N8 Fe1 121.5(4) . 3_666 ? C15 N8 Fe1 119.4(5) . 3_666 ? C12 N3 C6 120.9(5) . . ? C12 N3 C7 120.8(5) . . ? C6 N3 C7 117.2(5) . . ? C12 N7 C14 111.9(5) . . ? N8 C15 C16 123.5(8) . . ? C7 N4 C11 117.7(6) . . ? C7 N4 Fe1 122.1(4) . . ? C11 N4 Fe1 120.1(5) . . ? N2 C6 C5 122.6(6) . . ? N2 C6 N3 116.0(6) . . ? C5 C6 N3 121.4(6) . . ? C11 C10 C9 119.1(7) . . ? N4 C11 C10 122.9(7) . . ? C8 C9 C10 119.0(7) . . ? C9 C8 C7 119.1(6) . . ? N1 C1 S1 178.1(7) . . ? N5 C12 N7 127.6(5) . . ? N5 C12 N3 118.1(5) . . ? N7 C12 N3 114.3(5) . . ? N8 C19 C18 123.5(7) . . ? N8 C19 N9 116.6(6) . . ? C18 C19 N9 119.5(7) . . ? C18 C17 C16 119.9(7) . . ? C17 C18 C19 117.4(8) . . ? C15 C16 C17 117.6(7) . . ? N4 C7 C8 122.1(6) . . ? N4 C7 N3 116.2(6) . . ? C8 C7 N3 121.4(6) . . ? C12 N5 C13 112.7(5) . . ? N6 C14 N11 117.3(6) . . ? N6 C14 N7 126.3(6) . . ? N11 C14 N7 116.4(6) . . ? C13 N6 C14 114.2(5) . . ? C35 N12 Fe1 164.9(8) . . ? N10 C20 C21 123.0(6) . . ? N10 C20 N9 115.7(6) . . ? C21 C20 N9 121.1(6) . . ? C13 N9 C19 121.7(5) . . ? C13 N9 C20 120.2(5) . . ? C19 N9 C20 117.4(5) . . ? C3 C2 N2 123.1(7) . . ? C22 C21 C20 119.3(7) . . ? C23 C24 N10 123.8(8) . . ? C3 C4 C5 120.7(7) . . ? N6 C13 N5 126.9(6) . . ? N6 C13 N9 116.0(5) . . ? N5 C13 N9 117.1(5) . . ? C2 C3 C4 118.7(7) . . ? C20 N10 C24 116.1(7) . . ? C20 N10 Fe1 123.0(4) . 3_666 ? C24 N10 Fe1 120.8(5) . 3_666 ? C14 N11 C34 120.2(6) . . ? C14 N11 C25 121.3(6) . . ? C34 N11 C25 118.1(6) . . ? C21 C22 C23 119.0(8) . . ? C24 C23 C22 118.5(7) . . ? N12 C35 S2 175.3(10) . . ? N11 C25 C26 114.0(7) . . ? C33A C34 N11 126.1(10) . . ? C33A C34 C33B 42.9(6) . . ? N11 C34 C33B 107.2(8) . . ? O1 C26 C25 107.9(6) . . ? C27 O1 C26 115.4(7) . . ? O1 C27 C28 114.8(7) . . ? O2 C28 C27 109.6(7) . . ? C29 O2 C28 113.6(7) . . ? O2 C29 C30 108.9(7) . . ? C31 O3 C30 114.3(8) . . ? O3 C30 C29 112.0(9) . . ? O3 C31 C32A 112.4(6) . . ? O3 C31 C32B 114.9(8) . . ? C32A C31 C32B 43.7(10) . . ? C33A O4A C32A 108.1(7) . . ? C32B O4B C33B 115.9(7) . . ? O4B C32B C31 121.8(8) . . ? O4A C33A C34 107.3(7) . . ? O4A C32A C31 109.5(6) . . ? O4B C33B C34 114.0(7) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.099 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.127 #=END OF CIF