# 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 #TrackingRef 'MegaCIF.CIF' _publ_contact_author_name 'Prof. Keith S. Murray' _publ_contact_author_address ; School of Chemistry Monash University 3800 Australia ; _publ_contact_author_phone '+61 3 9905 4512' _publ_contact_author_fax '+61 3 9905 4597' _publ_contact_author_email keith.murray@monash.edu _publ_section_title ; Polymorphism and spin crossover in mononuclear FeII species containing new triazine/dipyridylamino ligands ; loop_ _publ_author_name _publ_author_footnote _publ_author_address T.M.Ross . ; School of Chemistry Monash University 3800 Australia ; B.Moubaraki . ; School of Chemistry Monash University 3800 Australia ; S.R.Batten . ; School of Chemistry Monash University 3800 Australia ; K.S.Murray . ; School of Chemistry Monash University 3800 Australia ; data_1a _database_code_depnum_ccdc_archive 'CCDC 836942' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DBB)2] ; _chemical_name_common trans-[Fe(II)(NCS)2(DBB)2] _chemical_melting_point ? _chemical_formula_moiety '(C84 H72 Fe N18 S2)' _chemical_formula_sum 'C84 H72 Fe N18 S2' _chemical_formula_weight 1453.57 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' 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 11.535(6) _cell_length_b 23.340(10) _cell_length_c 13.616(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.69(2) _cell_angle_gamma 90.00 _cell_volume 3633(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40776 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 26.45 _exptl_crystal_description 'needle ' _exptl_crystal_colour yellow _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 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9839 _exptl_absorpt_correction_T_max 0.9967 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77506 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _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 40776 _diffrn_reflns_av_R_equivalents 0.1112 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.45 _reflns_number_total 5704 _reflns_number_gt 4598 _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^)+(0.0705P)^2^+1.3084P] 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 SHELXL _refine_ls_extinction_coef 0.0238(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5704 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.5000 0.0000 0.00976(17) Uani 1 2 d S . . S1 S 0.17828(6) 0.58789(3) 0.29648(5) 0.0204(2) Uani 1 1 d . . . N6 N 0.37921(17) 0.51029(8) 0.13291(16) 0.0132(5) Uani 1 1 d . . . N3 N 0.25934(17) 0.52538(8) -0.01425(15) 0.0119(5) Uani 1 1 d . . . N8 N 0.42749(18) 0.68121(9) 0.15936(16) 0.0169(5) Uani 1 1 d . . . N2 N 0.12998(17) 0.44673(8) -0.01960(15) 0.0116(5) Uani 1 1 d . . . N7 N 0.46565(17) 0.59093(9) 0.22461(16) 0.0143(5) Uani 1 1 d . . . N4 N 0.07168(17) 0.55447(8) -0.08754(15) 0.0122(5) Uani 1 1 d . . . C12 C 0.3341(2) 0.54809(10) 0.06568(18) 0.0118(5) Uani 1 1 d . . . N5 N 0.34856(17) 0.60469(8) 0.06661(16) 0.0138(5) Uani 1 1 d . . . N9 N 0.49306(18) 0.49838(8) 0.28397(16) 0.0144(5) Uani 1 1 d . . . C14 C 0.4129(2) 0.62336(10) 0.15045(19) 0.0131(6) Uani 1 1 d . . . C36 C 0.4825(2) 0.43613(10) 0.2741(2) 0.0159(6) Uani 1 1 d . . . H36A H 0.5617 0.4190 0.2832 0.019 Uiso 1 1 calc R . . H36B H 0.4451 0.4267 0.2064 0.019 Uiso 1 1 calc R . . N1 N 0.08726(17) 0.53377(9) 0.11875(16) 0.0136(5) Uani 1 1 d . . . C1 C 0.1257(2) 0.55635(10) 0.19270(19) 0.0125(5) Uani 1 1 d . . . C13 C 0.4444(2) 0.53422(10) 0.21213(18) 0.0123(5) Uani 1 1 d . . . C30 C 0.6941(2) 0.50794(10) 0.36884(19) 0.0148(6) Uani 1 1 d . . . C37 C 0.4116(2) 0.41005(10) 0.34844(19) 0.0152(6) Uani 1 1 d . . . C11 C 0.0038(2) 0.58499(10) -0.15829(19) 0.0149(6) Uani 1 1 d . . . H11 H -0.0785 0.5792 -0.1661 0.018 Uiso 1 1 calc R . . C29 C 0.5662(2) 0.51835(11) 0.37376(19) 0.0169(6) Uani 1 1 d . . . H29A H 0.5431 0.4982 0.4320 0.020 Uiso 1 1 calc R . . H29B H 0.5531 0.5599 0.3824 0.020 Uiso 1 1 calc R . . C6 C 0.2401(2) 0.46518(10) -0.02062(18) 0.0112(5) Uani 1 1 d . . . C2 C 0.1101(2) 0.38955(10) -0.03467(19) 0.0142(5) Uani 1 1 d . . . H2 H 0.0322 0.3758 -0.0381 0.017 Uiso 1 1 calc R . . C8 C 0.2390(2) 0.59973(11) -0.14177(19) 0.0169(6) Uani 1 1 d . . . H8 H 0.3217 0.6037 -0.1353 0.020 Uiso 1 1 calc R . . C7 C 0.1884(2) 0.56137(10) -0.08193(18) 0.0122(5) Uani 1 1 d . . . C35 C 0.7605(2) 0.47340(11) 0.4381(2) 0.0198(6) Uani 1 1 d . . . H35 H 0.7245 0.4550 0.4885 0.024 Uiso 1 1 calc R . . C9 C 0.1685(2) 0.63184(11) -0.2104(2) 0.0208(6) Uani 1 1 d . . . H9 H 0.2013 0.6589 -0.2510 0.025 Uiso 1 1 calc R . . C17 C 0.1862(2) 0.71844(11) 0.1337(2) 0.0217(6) Uani 1 1 d . . . H17 H 0.2126 0.6896 0.1807 0.026 Uiso 1 1 calc R . . C16 C 0.2621(2) 0.74065(10) 0.0728(2) 0.0183(6) Uani 1 1 d . . . C5 C 0.3331(2) 0.42866(11) -0.03156(19) 0.0168(6) Uani 1 1 d . . . H5 H 0.4099 0.4434 -0.0314 0.020 Uiso 1 1 calc R . . C38 C 0.4580(2) 0.36711(11) 0.4126(2) 0.0191(6) Uani 1 1 d . . . H38 H 0.5367 0.3553 0.4121 0.023 Uiso 1 1 calc R . . C3 C 0.1975(2) 0.35103(11) -0.04511(19) 0.0176(6) Uani 1 1 d . . . H3 H 0.1803 0.3114 -0.0540 0.021 Uiso 1 1 calc R . . C10 C 0.0484(2) 0.62385(11) -0.2190(2) 0.0184(6) Uani 1 1 d . . . H10 H -0.0024 0.6450 -0.2664 0.022 Uiso 1 1 calc R . . C22 C 0.4643(2) 0.70773(11) 0.2560(2) 0.0200(6) Uani 1 1 d . . . H22A H 0.4527 0.6798 0.3085 0.024 Uiso 1 1 calc R . . H22B H 0.4130 0.7410 0.2636 0.024 Uiso 1 1 calc R . . C31 C 0.7481(2) 0.53361(11) 0.2944(2) 0.0179(6) Uani 1 1 d . . . H31 H 0.7029 0.5560 0.2450 0.021 Uiso 1 1 calc R . . C23 C 0.5905(2) 0.72782(11) 0.27221(19) 0.0191(6) Uani 1 1 d . . . C15 C 0.3871(2) 0.71904(11) 0.0763(2) 0.0185(6) Uani 1 1 d . . . H15A H 0.3938 0.6983 0.0139 0.022 Uiso 1 1 calc R . . H15B H 0.4401 0.7526 0.0792 0.022 Uiso 1 1 calc R . . C39 C 0.3911(3) 0.34139(12) 0.4773(2) 0.0245(7) Uani 1 1 d . . . H39 H 0.4236 0.3117 0.5201 0.029 Uiso 1 1 calc R . . C28 C 0.6811(2) 0.68874(13) 0.2691(2) 0.0257(7) Uani 1 1 d . . . H28 H 0.6631 0.6497 0.2541 0.031 Uiso 1 1 calc R . . C42 C 0.2970(2) 0.42827(11) 0.3522(2) 0.0232(6) Uani 1 1 d . . . H42 H 0.2646 0.4583 0.3101 0.028 Uiso 1 1 calc R . . C41 C 0.2307(2) 0.40249(12) 0.4172(2) 0.0278(7) Uani 1 1 d . . . H41 H 0.1525 0.4148 0.4191 0.033 Uiso 1 1 calc R . . C34 C 0.8791(2) 0.46564(12) 0.4342(2) 0.0240(7) Uani 1 1 d . . . H34 H 0.9237 0.4414 0.4810 0.029 Uiso 1 1 calc R . . C40 C 0.2769(3) 0.35887(12) 0.4797(2) 0.0278(7) Uani 1 1 d . . . H40 H 0.2306 0.3412 0.5238 0.033 Uiso 1 1 calc R . . C32 C 0.8665(2) 0.52696(12) 0.2915(2) 0.0216(6) Uani 1 1 d . . . H32 H 0.9026 0.5454 0.2413 0.026 Uiso 1 1 calc R . . C24 C 0.6184(3) 0.78483(12) 0.2928(2) 0.0281(7) Uani 1 1 d . . . H24 H 0.5580 0.8122 0.2953 0.034 Uiso 1 1 calc R . . C21 C 0.2222(3) 0.78308(12) 0.0045(2) 0.0297(7) Uani 1 1 d . . . H21 H 0.2739 0.7990 -0.0370 0.036 Uiso 1 1 calc R . . C4 C 0.3114(2) 0.37083(11) -0.0425(2) 0.0191(6) Uani 1 1 d . . . H4 H 0.3735 0.3448 -0.0483 0.023 Uiso 1 1 calc R . . C33 C 0.9327(2) 0.49331(11) 0.3619(2) 0.0232(6) Uani 1 1 d . . . H33 H 1.0145 0.4892 0.3607 0.028 Uiso 1 1 calc R . . C19 C 0.0323(3) 0.77982(13) 0.0570(3) 0.0347(8) Uani 1 1 d . . . H19 H -0.0463 0.7929 0.0513 0.042 Uiso 1 1 calc R . . C25 C 0.7356(3) 0.80173(14) 0.3099(2) 0.0386(9) Uani 1 1 d . . . H25 H 0.7543 0.8408 0.3231 0.046 Uiso 1 1 calc R . . C18 C 0.0715(2) 0.73802(12) 0.1263(2) 0.0272(7) Uani 1 1 d . . . H18 H 0.0199 0.7228 0.1686 0.033 Uiso 1 1 calc R . . C20 C 0.1076(3) 0.80225(13) -0.0033(3) 0.0364(8) Uani 1 1 d . . . H20 H 0.0810 0.8310 -0.0504 0.044 Uiso 1 1 calc R . . C26 C 0.8240(3) 0.76252(14) 0.3077(2) 0.0345(8) Uani 1 1 d . . . H26 H 0.9034 0.7744 0.3199 0.041 Uiso 1 1 calc R . . C27 C 0.7968(3) 0.70575(13) 0.2876(2) 0.0303(7) Uani 1 1 d . . . H27 H 0.8576 0.6784 0.2864 0.036 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 0.0085(3) 0.0080(3) 0.0123(3) -0.0007(2) 0.0000(2) -0.00013(19) S1 0.0233(4) 0.0218(4) 0.0153(4) -0.0047(3) -0.0003(3) -0.0067(3) N6 0.0094(10) 0.0112(10) 0.0179(12) 0.0010(9) -0.0019(9) -0.0001(8) N3 0.0102(10) 0.0091(10) 0.0155(11) 0.0000(9) -0.0013(9) 0.0010(8) N8 0.0182(11) 0.0102(11) 0.0205(12) -0.0009(9) -0.0037(10) -0.0017(9) N2 0.0127(11) 0.0107(10) 0.0108(10) -0.0006(8) -0.0013(9) -0.0016(8) N7 0.0099(10) 0.0117(11) 0.0213(12) -0.0012(9) 0.0027(9) -0.0011(8) N4 0.0126(11) 0.0088(10) 0.0142(11) -0.0019(9) -0.0020(9) 0.0008(8) C12 0.0061(12) 0.0128(13) 0.0173(13) -0.0005(11) 0.0045(11) -0.0005(10) N5 0.0107(10) 0.0103(11) 0.0200(12) -0.0003(9) 0.0011(9) -0.0024(8) N9 0.0149(11) 0.0101(10) 0.0173(12) 0.0001(9) -0.0017(9) -0.0005(9) C14 0.0088(12) 0.0108(13) 0.0200(14) 0.0008(11) 0.0030(11) -0.0007(10) C36 0.0162(13) 0.0098(12) 0.0214(14) 0.0005(11) 0.0008(11) 0.0027(10) N1 0.0096(10) 0.0127(11) 0.0183(12) 0.0023(9) 0.0015(9) 0.0012(9) C1 0.0090(12) 0.0124(13) 0.0163(14) 0.0028(11) 0.0026(11) -0.0006(10) C13 0.0085(12) 0.0126(13) 0.0163(13) -0.0018(11) 0.0039(11) -0.0011(10) C30 0.0173(13) 0.0136(13) 0.0129(13) -0.0043(10) -0.0003(11) -0.0015(10) C37 0.0159(13) 0.0114(12) 0.0171(14) -0.0036(11) -0.0024(11) -0.0026(10) C11 0.0126(13) 0.0144(13) 0.0166(13) -0.0027(11) -0.0025(11) 0.0017(10) C29 0.0164(13) 0.0185(13) 0.0157(13) -0.0033(11) 0.0018(11) -0.0021(11) C6 0.0110(12) 0.0107(12) 0.0114(12) 0.0015(10) -0.0001(10) -0.0002(10) C2 0.0160(13) 0.0088(12) 0.0172(13) 0.0004(10) -0.0007(11) -0.0013(10) C8 0.0145(13) 0.0157(13) 0.0208(14) 0.0002(11) 0.0030(11) -0.0053(11) C7 0.0124(13) 0.0110(12) 0.0127(13) -0.0028(10) -0.0006(11) 0.0016(10) C35 0.0234(15) 0.0165(14) 0.0181(14) 0.0025(11) -0.0026(12) -0.0038(11) C9 0.0235(15) 0.0167(14) 0.0222(15) 0.0038(12) 0.0033(12) -0.0018(11) C17 0.0242(15) 0.0115(13) 0.0277(16) -0.0022(12) -0.0029(13) 0.0003(11) C16 0.0217(14) 0.0091(12) 0.0226(15) -0.0042(11) -0.0022(12) -0.0019(11) C5 0.0125(13) 0.0198(14) 0.0179(14) -0.0026(11) 0.0009(11) -0.0004(11) C38 0.0205(14) 0.0138(13) 0.0219(15) -0.0003(11) -0.0018(12) -0.0002(11) C3 0.0206(14) 0.0086(12) 0.0230(15) -0.0020(11) 0.0005(12) 0.0011(11) C10 0.0229(14) 0.0136(13) 0.0179(14) 0.0019(11) 0.0001(12) 0.0037(11) C22 0.0235(15) 0.0154(13) 0.0204(15) -0.0041(11) 0.0005(12) -0.0005(11) C31 0.0171(14) 0.0187(14) 0.0166(14) 0.0014(11) -0.0020(11) 0.0027(11) C23 0.0269(15) 0.0151(13) 0.0137(13) -0.0003(11) -0.0032(12) -0.0063(11) C15 0.0228(14) 0.0089(12) 0.0230(15) 0.0014(11) -0.0004(12) -0.0031(11) C39 0.0326(17) 0.0167(14) 0.0225(15) 0.0011(12) -0.0029(13) -0.0041(12) C28 0.0266(16) 0.0225(15) 0.0279(16) -0.0047(13) 0.0036(13) -0.0069(13) C42 0.0216(15) 0.0181(14) 0.0291(16) 0.0001(12) 0.0000(13) 0.0001(12) C41 0.0184(15) 0.0267(16) 0.0386(18) -0.0043(14) 0.0052(14) -0.0044(12) C34 0.0193(14) 0.0207(14) 0.0293(16) 0.0025(13) -0.0071(13) 0.0019(12) C40 0.0311(17) 0.0265(16) 0.0265(16) -0.0042(13) 0.0065(14) -0.0128(13) C32 0.0207(15) 0.0245(15) 0.0200(15) -0.0016(12) 0.0040(12) -0.0027(12) C24 0.0421(18) 0.0171(14) 0.0213(16) 0.0038(12) -0.0090(14) -0.0089(13) C21 0.0356(18) 0.0197(15) 0.0316(17) 0.0050(13) -0.0033(15) -0.0011(13) C4 0.0188(14) 0.0155(14) 0.0230(15) -0.0020(11) 0.0025(12) 0.0053(11) C33 0.0148(14) 0.0235(15) 0.0298(16) -0.0060(13) -0.0030(13) 0.0014(12) C19 0.0237(16) 0.0262(16) 0.050(2) -0.0085(15) -0.0103(16) 0.0107(13) C25 0.055(2) 0.0258(17) 0.0305(18) -0.0001(14) -0.0119(17) -0.0265(16) C18 0.0222(15) 0.0243(15) 0.0352(18) -0.0097(13) 0.0037(14) -0.0016(13) C20 0.0345(19) 0.0233(16) 0.046(2) 0.0050(15) -0.0145(16) 0.0101(14) C26 0.0343(18) 0.045(2) 0.0221(16) 0.0048(15) -0.0033(14) -0.0231(16) C27 0.0250(16) 0.0361(18) 0.0295(17) -0.0009(14) 0.0028(14) -0.0076(14) _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 1.953(2) 3_565 ? Fe1 N1 1.953(2) . ? Fe1 N2 1.993(2) 3_565 ? Fe1 N2 1.993(2) . ? Fe1 N4 1.996(2) . ? Fe1 N4 1.996(2) 3_565 ? S1 C1 1.636(3) . ? N6 C12 1.327(3) . ? N6 C13 1.351(3) . ? N3 C12 1.399(3) . ? N3 C7 1.422(3) . ? N3 C6 1.423(3) . ? N8 C14 1.364(3) . ? N8 C15 1.461(3) . ? N8 C22 1.465(3) . ? N2 C6 1.343(3) . ? N2 C2 1.365(3) . ? N7 C14 1.341(3) . ? N7 C13 1.353(3) . ? N4 C7 1.348(3) . ? N4 C11 1.359(3) . ? C12 N5 1.331(3) . ? N5 C14 1.348(3) . ? N9 C13 1.351(3) . ? N9 C36 1.463(3) . ? N9 C29 1.466(3) . ? C36 C37 1.511(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N1 C1 1.170(3) . ? C30 C35 1.391(4) . ? C30 C31 1.394(4) . ? C30 C29 1.505(4) . ? C37 C38 1.389(4) . ? C37 C42 1.396(4) . ? C11 C10 1.373(4) . ? C11 H11 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C6 C5 1.394(4) . ? C2 C3 1.372(4) . ? C2 H2 0.9500 . ? C8 C9 1.377(4) . ? C8 C7 1.391(4) . ? C8 H8 0.9500 . ? C35 C34 1.388(4) . ? C35 H35 0.9500 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C17 C16 1.384(4) . ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C16 C21 1.394(4) . ? C16 C15 1.522(4) . ? C5 C4 1.377(4) . ? C5 H5 0.9500 . ? C38 C39 1.383(4) . ? C38 H38 0.9500 . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C10 H10 0.9500 . ? C22 C23 1.517(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C31 C32 1.380(4) . ? C31 H31 0.9500 . ? C23 C24 1.388(4) . ? C23 C28 1.392(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C39 C40 1.383(4) . ? C39 H39 0.9500 . ? C28 C27 1.384(4) . ? C28 H28 0.9500 . ? C42 C41 1.383(4) . ? C42 H42 0.9500 . ? C41 C40 1.387(4) . ? C41 H41 0.9500 . ? C34 C33 1.390(4) . ? C34 H34 0.9500 . ? C40 H40 0.9500 . ? C32 C33 1.387(4) . ? C32 H32 0.9500 . ? C24 C25 1.397(4) . ? C24 H24 0.9500 . ? C21 C20 1.386(4) . ? C21 H21 0.9500 . ? C4 H4 0.9500 . ? C33 H33 0.9500 . ? C19 C20 1.376(5) . ? C19 C18 1.390(4) . ? C19 H19 0.9500 . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C18 H18 0.9500 . ? C20 H20 0.9500 . ? C26 C27 1.381(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? 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) 3_565 . ? N1 Fe1 N2 92.81(9) 3_565 3_565 ? N1 Fe1 N2 87.19(8) . 3_565 ? N1 Fe1 N2 87.19(8) 3_565 . ? N1 Fe1 N2 92.81(9) . . ? N2 Fe1 N2 180.00(9) 3_565 . ? N1 Fe1 N4 88.36(9) 3_565 . ? N1 Fe1 N4 91.64(9) . . ? N2 Fe1 N4 93.54(9) 3_565 . ? N2 Fe1 N4 86.46(9) . . ? N1 Fe1 N4 91.64(9) 3_565 3_565 ? N1 Fe1 N4 88.36(9) . 3_565 ? N2 Fe1 N4 86.46(9) 3_565 3_565 ? N2 Fe1 N4 93.54(9) . 3_565 ? N4 Fe1 N4 180.0 . 3_565 ? C12 N6 C13 113.7(2) . . ? C12 N3 C7 121.43(19) . . ? C12 N3 C6 119.76(19) . . ? C7 N3 C6 118.16(19) . . ? C14 N8 C15 120.5(2) . . ? C14 N8 C22 121.0(2) . . ? C15 N8 C22 117.6(2) . . ? C6 N2 C2 116.9(2) . . ? C6 N2 Fe1 122.06(16) . . ? C2 N2 Fe1 121.05(16) . . ? C14 N7 C13 113.7(2) . . ? C7 N4 C11 117.0(2) . . ? C7 N4 Fe1 122.18(16) . . ? C11 N4 Fe1 120.76(17) . . ? N6 C12 N5 128.0(2) . . ? N6 C12 N3 115.4(2) . . ? N5 C12 N3 116.5(2) . . ? C12 N5 C14 112.5(2) . . ? C13 N9 C36 121.8(2) . . ? C13 N9 C29 123.0(2) . . ? C36 N9 C29 115.1(2) . . ? N7 C14 N5 126.7(2) . . ? N7 C14 N8 117.0(2) . . ? N5 C14 N8 116.3(2) . . ? N9 C36 C37 112.6(2) . . ? N9 C36 H36A 109.1 . . ? C37 C36 H36A 109.1 . . ? N9 C36 H36B 109.1 . . ? C37 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? C1 N1 Fe1 171.3(2) . . ? N1 C1 S1 179.5(2) . . ? N6 C13 N9 117.1(2) . . ? N6 C13 N7 125.2(2) . . ? N9 C13 N7 117.7(2) . . ? C35 C30 C31 118.9(2) . . ? C35 C30 C29 121.2(2) . . ? C31 C30 C29 119.9(2) . . ? C38 C37 C42 118.9(3) . . ? C38 C37 C36 121.0(2) . . ? C42 C37 C36 120.1(2) . . ? N4 C11 C10 123.1(2) . . ? N4 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? N9 C29 C30 111.7(2) . . ? N9 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N9 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? N2 C6 C5 123.2(2) . . ? N2 C6 N3 117.1(2) . . ? C5 C6 N3 119.6(2) . . ? N2 C2 C3 123.0(2) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C9 C8 C7 119.5(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? N4 C7 C8 122.6(2) . . ? N4 C7 N3 116.7(2) . . ? C8 C7 N3 120.6(2) . . ? C34 C35 C30 120.4(3) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C8 C9 C10 118.5(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C16 C21 119.1(3) . . ? C17 C16 C15 122.0(2) . . ? C21 C16 C15 118.9(3) . . ? C4 C5 C6 118.7(2) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C2 C3 C4 119.0(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N8 C22 C23 114.7(2) . . ? N8 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? N8 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C32 C31 C30 120.8(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C24 C23 C28 118.7(3) . . ? C24 C23 C22 121.1(3) . . ? C28 C23 C22 120.2(2) . . ? N8 C15 C16 115.3(2) . . ? N8 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N8 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C40 C39 C38 120.1(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C27 C28 C23 121.1(3) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? C41 C42 C37 119.9(3) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C42 C41 C40 120.8(3) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C39 C40 C41 119.4(3) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C31 C32 C33 120.0(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C20 C21 C16 120.5(3) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C32 C33 C34 119.8(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C26 C25 C24 120.9(3) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C25 C26 C27 119.6(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 120.0(3) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.449 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.106 #=END data_1b _database_code_depnum_ccdc_archive 'CCDC 836943' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DBB)2] ; _chemical_name_common trans-[Fe(II)(NCS)2(DBB)2] _chemical_melting_point ? _chemical_formula_moiety '(C84 H72 Fe N18 S2)' _chemical_formula_sum 'C84 H72 Fe N18 S2' _chemical_formula_weight 1453.57 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' 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 11.6430(10) _cell_length_b 23.3950(9) _cell_length_c 13.8820(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.520(3) _cell_angle_gamma 90.00 _cell_volume 3739.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 40520 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 26.16 _exptl_crystal_description needle _exptl_crystal_colour yellow _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 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9843 _exptl_absorpt_correction_T_max 0.9968 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.77487 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _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 40520 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.16 _reflns_number_total 5654 _reflns_number_gt 4659 _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^)+(0.0643P)^2^+1.8558P] 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 5654 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.5000 0.0000 0.01668(14) Uani 1 2 d S . . S1 S 0.17448(7) 0.58989(3) 0.30232(5) 0.0424(2) Uani 1 1 d . . . N6 N 0.38148(15) 0.50988(8) 0.13616(14) 0.0198(4) Uani 1 1 d . . . N3 N 0.26841(15) 0.52500(8) -0.01236(14) 0.0198(4) Uani 1 1 d . . . N8 N 0.42291(17) 0.68086(8) 0.16599(15) 0.0275(5) Uani 1 1 d . . . N2 N 0.14633(15) 0.44411(8) -0.02140(14) 0.0207(4) Uani 1 1 d . . . N7 N 0.46198(16) 0.59045(8) 0.22984(14) 0.0211(4) Uani 1 1 d . . . N4 N 0.08713(16) 0.55957(8) -0.08917(13) 0.0212(4) Uani 1 1 d . . . C12 C 0.33730(17) 0.54764(9) 0.06920(16) 0.0174(5) Uani 1 1 d . . . N5 N 0.34902(15) 0.60433(8) 0.07203(14) 0.0210(4) Uani 1 1 d . . . N9 N 0.49159(17) 0.49807(8) 0.28747(14) 0.0236(4) Uani 1 1 d . . . C14 C 0.41027(19) 0.62303(9) 0.15626(17) 0.0212(5) Uani 1 1 d . . . C36 C 0.4814(2) 0.43602(10) 0.27758(18) 0.0254(5) Uani 1 1 d . . . H36A H 0.5593 0.4192 0.2874 0.030 Uiso 1 1 calc R . . H36B H 0.4449 0.4268 0.2112 0.030 Uiso 1 1 calc R . . N1 N 0.08955(16) 0.53437(9) 0.12819(15) 0.0277(5) Uani 1 1 d . . . C1 C 0.12498(19) 0.55773(10) 0.20056(18) 0.0239(5) Uani 1 1 d . . . C13 C 0.44334(18) 0.53393(9) 0.21590(16) 0.0194(5) Uani 1 1 d . . . C30 C 0.6926(2) 0.50803(10) 0.37056(17) 0.0232(5) Uani 1 1 d . . . C37 C 0.4108(2) 0.40961(10) 0.34932(18) 0.0267(5) Uani 1 1 d . . . C11 C 0.0246(2) 0.59250(11) -0.15783(18) 0.0321(6) Uani 1 1 d . . . H11 H -0.0568 0.5902 -0.1652 0.039 Uiso 1 1 calc R . . C29 C 0.5657(2) 0.51823(11) 0.37546(17) 0.0246(5) Uani 1 1 d . . . H29A H 0.5442 0.4983 0.4323 0.030 Uiso 1 1 calc R . . H29B H 0.5526 0.5592 0.3837 0.030 Uiso 1 1 calc R . . C6 C 0.25301(18) 0.46457(9) -0.02200(16) 0.0193(5) Uani 1 1 d . . . C2 C 0.1298(2) 0.38722(10) -0.03636(18) 0.0280(6) Uani 1 1 d . . . H2 H 0.0544 0.3724 -0.0387 0.034 Uiso 1 1 calc R . . C8 C 0.2593(2) 0.59752(11) -0.14061(19) 0.0344(6) Uani 1 1 d . . . H8 H 0.3408 0.5981 -0.1338 0.041 Uiso 1 1 calc R . . C7 C 0.20255(19) 0.56225(9) -0.08244(16) 0.0199(5) Uani 1 1 d . . . C35 C 0.7598(2) 0.47344(12) 0.43818(19) 0.0344(6) Uani 1 1 d . . . H35 H 0.7258 0.4552 0.4873 0.041 Uiso 1 1 calc R . . C9 C 0.1936(3) 0.63166(12) -0.2085(2) 0.0429(7) Uani 1 1 d . . . H9 H 0.2297 0.6564 -0.2483 0.051 Uiso 1 1 calc R . . C17 C 0.1824(2) 0.71688(11) 0.1354(2) 0.0376(7) Uani 1 1 d . . . H17 H 0.2085 0.6889 0.1822 0.045 Uiso 1 1 calc R . . C16 C 0.2585(2) 0.73927(10) 0.07701(19) 0.0299(6) Uani 1 1 d . . . C5 C 0.3472(2) 0.43010(11) -0.03316(19) 0.0282(6) Uani 1 1 d . . . H5 H 0.4215 0.4460 -0.0323 0.034 Uiso 1 1 calc R . . C38 C 0.4571(2) 0.36746(11) 0.41306(19) 0.0340(6) Uani 1 1 d . . . H38 H 0.5348 0.3563 0.4142 0.041 Uiso 1 1 calc R . . C3 C 0.2185(2) 0.35030(11) -0.0483(2) 0.0348(6) Uani 1 1 d . . . H3 H 0.2041 0.3110 -0.0582 0.042 Uiso 1 1 calc R . . C10 C 0.0736(3) 0.62899(12) -0.2172(2) 0.0408(7) Uani 1 1 d . . . H10 H 0.0268 0.6518 -0.2630 0.049 Uiso 1 1 calc R . . C22 C 0.4603(2) 0.70712(11) 0.26104(19) 0.0334(6) Uani 1 1 d . . . H22A H 0.4510 0.6792 0.3119 0.040 Uiso 1 1 calc R . . H22B H 0.4091 0.7395 0.2688 0.040 Uiso 1 1 calc R . . C31 C 0.7450(2) 0.53340(11) 0.29788(18) 0.0301(6) Uani 1 1 d . . . H31 H 0.7001 0.5561 0.2506 0.036 Uiso 1 1 calc R . . C23 C 0.5847(2) 0.72797(11) 0.27634(18) 0.0317(6) Uani 1 1 d . . . C15 C 0.3828(2) 0.71859(10) 0.08396(19) 0.0306(6) Uani 1 1 d . . . H15A H 0.3912 0.6984 0.0235 0.037 Uiso 1 1 calc R . . H15B H 0.4340 0.7521 0.0882 0.037 Uiso 1 1 calc R . . C39 C 0.3905(3) 0.34126(13) 0.4755(2) 0.0468(8) Uani 1 1 d . . . H39 H 0.4225 0.3120 0.5175 0.056 Uiso 1 1 calc R . . C28 C 0.6754(3) 0.69014(14) 0.2734(2) 0.0494(8) Uani 1 1 d . . . H28 H 0.6589 0.6514 0.2598 0.059 Uiso 1 1 calc R . . C42 C 0.2965(2) 0.42704(12) 0.3513(2) 0.0421(7) Uani 1 1 d . . . H42 H 0.2640 0.4565 0.3100 0.051 Uiso 1 1 calc R . . C41 C 0.2310(3) 0.40080(15) 0.4143(3) 0.0547(9) Uani 1 1 d . . . H41 H 0.1538 0.4123 0.4150 0.066 Uiso 1 1 calc R . . C34 C 0.8771(2) 0.46577(13) 0.4335(2) 0.0460(8) Uani 1 1 d . . . H34 H 0.9221 0.4423 0.4794 0.055 Uiso 1 1 calc R . . C40 C 0.2778(3) 0.35828(14) 0.4756(2) 0.0517(8) Uani 1 1 d . . . H40 H 0.2325 0.3407 0.5179 0.062 Uiso 1 1 calc R . . C32 C 0.8621(2) 0.52601(13) 0.2935(2) 0.0376(7) Uani 1 1 d . . . H32 H 0.8965 0.5438 0.2442 0.045 Uiso 1 1 calc R . . C24 C 0.6113(3) 0.78499(13) 0.2960(2) 0.0546(9) Uani 1 1 d . . . H24 H 0.5512 0.8116 0.2985 0.066 Uiso 1 1 calc R . . C21 C 0.2181(3) 0.78080(13) 0.0088(2) 0.0539(8) Uani 1 1 d . . . H21 H 0.2690 0.7967 -0.0305 0.065 Uiso 1 1 calc R . . C4 C 0.3297(2) 0.37215(11) -0.0455(2) 0.0356(6) Uani 1 1 d . . . H4 H 0.3922 0.3478 -0.0520 0.043 Uiso 1 1 calc R . . C33 C 0.9280(2) 0.49227(13) 0.3622(2) 0.0444(7) Uani 1 1 d . . . H33 H 1.0078 0.4874 0.3602 0.053 Uiso 1 1 calc R . . C19 C 0.0289(3) 0.77669(15) 0.0558(3) 0.0660(11) Uani 1 1 d . . . H19 H -0.0486 0.7893 0.0483 0.079 Uiso 1 1 calc R . . C25 C 0.7262(4) 0.80301(17) 0.3120(3) 0.0757(13) Uani 1 1 d . . . H25 H 0.7433 0.8418 0.3249 0.091 Uiso 1 1 calc R . . C18 C 0.0674(3) 0.73570(13) 0.1249(3) 0.0499(8) Uani 1 1 d . . . H18 H 0.0163 0.7205 0.1647 0.060 Uiso 1 1 calc R . . C20 C 0.1044(3) 0.79896(16) -0.0018(3) 0.0712(11) Uani 1 1 d . . . H20 H 0.0782 0.8268 -0.0488 0.085 Uiso 1 1 calc R . . C26 C 0.8150(4) 0.76481(19) 0.3090(2) 0.0684(12) Uani 1 1 d . . . H26 H 0.8925 0.7774 0.3198 0.082 Uiso 1 1 calc R . . C27 C 0.7906(3) 0.70814(17) 0.2903(2) 0.0602(9) Uani 1 1 d . . . H27 H 0.8511 0.6817 0.2888 0.072 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 0.0089(2) 0.0202(3) 0.0209(3) -0.00193(19) 0.00220(18) 0.00043(17) S1 0.0507(5) 0.0487(5) 0.0270(4) -0.0085(3) 0.0027(3) -0.0184(4) N6 0.0145(9) 0.0169(10) 0.0276(11) -0.0003(8) 0.0016(8) -0.0020(8) N3 0.0123(9) 0.0171(10) 0.0291(10) -0.0001(8) 0.0005(8) -0.0012(7) N8 0.0293(11) 0.0147(10) 0.0365(12) -0.0009(9) -0.0013(9) -0.0010(8) N2 0.0160(10) 0.0186(10) 0.0273(10) -0.0022(8) 0.0027(8) -0.0024(8) N7 0.0148(9) 0.0168(10) 0.0313(11) -0.0012(8) 0.0016(8) -0.0009(8) N4 0.0179(10) 0.0226(10) 0.0227(10) 0.0015(8) 0.0020(8) 0.0048(8) C12 0.0067(10) 0.0182(12) 0.0283(12) -0.0012(10) 0.0060(9) -0.0024(9) N5 0.0165(10) 0.0158(10) 0.0301(11) -0.0004(8) 0.0020(8) -0.0017(8) N9 0.0239(10) 0.0176(10) 0.0281(11) 0.0000(8) 0.0002(9) -0.0002(8) C14 0.0136(11) 0.0166(12) 0.0340(13) -0.0005(10) 0.0058(10) -0.0015(9) C36 0.0265(13) 0.0178(12) 0.0316(13) 0.0008(10) 0.0035(11) 0.0054(10) N1 0.0164(10) 0.0390(13) 0.0277(11) -0.0055(10) 0.0032(9) -0.0001(9) C1 0.0141(11) 0.0301(14) 0.0282(14) 0.0026(11) 0.0050(10) -0.0007(10) C13 0.0096(10) 0.0200(12) 0.0296(13) -0.0001(10) 0.0063(10) -0.0001(9) C30 0.0234(12) 0.0231(13) 0.0215(12) -0.0040(10) -0.0020(10) -0.0013(10) C37 0.0290(13) 0.0178(12) 0.0324(14) -0.0032(10) 0.0016(11) -0.0017(10) C11 0.0297(14) 0.0355(15) 0.0298(14) 0.0053(12) -0.0001(11) 0.0114(12) C29 0.0249(13) 0.0274(13) 0.0216(12) -0.0008(10) 0.0039(10) 0.0008(10) C6 0.0169(11) 0.0177(12) 0.0227(12) -0.0017(9) 0.0016(9) -0.0011(9) C2 0.0255(13) 0.0197(13) 0.0387(14) -0.0040(11) 0.0049(11) -0.0061(10) C8 0.0324(15) 0.0331(15) 0.0385(15) 0.0060(12) 0.0082(12) -0.0092(12) C7 0.0188(12) 0.0180(11) 0.0226(12) -0.0030(9) 0.0018(10) -0.0004(9) C35 0.0334(15) 0.0348(15) 0.0323(14) 0.0075(12) -0.0039(12) -0.0032(12) C9 0.0562(19) 0.0368(16) 0.0365(15) 0.0127(13) 0.0097(14) -0.0060(14) C17 0.0360(16) 0.0262(14) 0.0499(17) -0.0021(12) 0.0043(13) 0.0034(12) C16 0.0352(14) 0.0155(12) 0.0370(14) -0.0026(11) -0.0009(12) -0.0024(11) C5 0.0167(12) 0.0275(14) 0.0417(15) -0.0058(11) 0.0081(11) 0.0019(10) C38 0.0376(15) 0.0262(14) 0.0372(15) 0.0013(12) 0.0023(12) -0.0005(12) C3 0.0366(15) 0.0174(13) 0.0513(17) -0.0067(12) 0.0092(13) 0.0004(11) C10 0.0540(19) 0.0343(16) 0.0331(15) 0.0123(12) 0.0030(13) 0.0134(14) C22 0.0400(15) 0.0202(13) 0.0400(15) -0.0056(11) 0.0055(13) -0.0006(11) C31 0.0301(14) 0.0358(15) 0.0241(13) 0.0041(11) 0.0025(11) 0.0015(11) C23 0.0460(16) 0.0242(14) 0.0225(13) 0.0009(10) -0.0028(12) -0.0126(12) C15 0.0351(15) 0.0157(12) 0.0412(15) 0.0022(11) 0.0061(12) -0.0046(10) C39 0.062(2) 0.0367(16) 0.0404(16) 0.0075(13) 0.0043(15) -0.0126(15) C28 0.0432(18) 0.0416(18) 0.064(2) -0.0121(15) 0.0105(15) -0.0171(15) C42 0.0316(15) 0.0350(16) 0.0601(19) 0.0041(14) 0.0081(14) 0.0040(12) C41 0.0339(17) 0.057(2) 0.078(2) -0.0074(19) 0.0222(17) -0.0087(15) C34 0.0341(16) 0.0448(18) 0.0528(18) 0.0090(15) -0.0139(14) 0.0082(14) C40 0.058(2) 0.052(2) 0.0476(18) -0.0048(15) 0.0171(16) -0.0289(17) C32 0.0282(14) 0.0496(17) 0.0362(15) -0.0035(13) 0.0086(12) -0.0062(13) C24 0.077(2) 0.0269(16) 0.0504(18) 0.0054(14) -0.0230(17) -0.0157(16) C21 0.057(2) 0.0393(18) 0.061(2) 0.0164(15) -0.0068(17) 0.0021(15) C4 0.0276(14) 0.0269(14) 0.0531(17) -0.0061(12) 0.0085(13) 0.0114(11) C33 0.0228(14) 0.0545(19) 0.0539(19) -0.0054(15) -0.0010(13) 0.0034(13) C19 0.043(2) 0.050(2) 0.096(3) -0.014(2) -0.018(2) 0.0221(17) C25 0.099(3) 0.047(2) 0.067(2) 0.0110(18) -0.033(2) -0.052(2) C18 0.0349(17) 0.0438(18) 0.071(2) -0.0186(16) 0.0084(15) 0.0016(14) C20 0.062(2) 0.053(2) 0.090(3) 0.019(2) -0.021(2) 0.0146(19) C26 0.067(3) 0.090(3) 0.0428(19) 0.0159(19) -0.0118(18) -0.055(2) C27 0.0431(19) 0.079(3) 0.059(2) -0.0092(19) 0.0081(16) -0.0215(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.086(2) . ? Fe1 N1 2.086(2) 3_565 ? Fe1 N2 2.2025(18) 3_565 ? Fe1 N2 2.2025(18) . ? Fe1 N4 2.2081(19) . ? Fe1 N4 2.2081(19) 3_565 ? S1 C1 1.629(3) . ? N6 C12 1.329(3) . ? N6 C13 1.351(3) . ? N3 C12 1.392(3) . ? N3 C6 1.429(3) . ? N3 C7 1.440(3) . ? N8 C14 1.365(3) . ? N8 C15 1.462(3) . ? N8 C22 1.462(3) . ? N2 C6 1.332(3) . ? N2 C2 1.356(3) . ? N7 C14 1.343(3) . ? N7 C13 1.349(3) . ? N4 C7 1.335(3) . ? N4 C11 1.351(3) . ? C12 N5 1.333(3) . ? N5 C14 1.349(3) . ? N9 C13 1.357(3) . ? N9 C36 1.461(3) . ? N9 C29 1.465(3) . ? C36 C37 1.514(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C1 1.164(3) . ? C30 C31 1.387(3) . ? C30 C35 1.390(4) . ? C30 C29 1.509(3) . ? C37 C38 1.380(4) . ? C37 C42 1.396(4) . ? C11 C10 1.368(4) . ? C11 H11 0.9400 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C6 C5 1.389(3) . ? C2 C3 1.375(4) . ? C2 H2 0.9400 . ? C8 C9 1.377(4) . ? C8 C7 1.388(3) . ? C8 H8 0.9400 . ? C35 C34 1.389(4) . ? C35 H35 0.9400 . ? C9 C10 1.386(4) . ? C9 H9 0.9400 . ? C17 C16 1.389(4) . ? C17 C18 1.396(4) . ? C17 H17 0.9400 . ? C16 C21 1.389(4) . ? C16 C15 1.516(4) . ? C5 C4 1.378(4) . ? C5 H5 0.9400 . ? C38 C39 1.388(4) . ? C38 H38 0.9400 . ? C3 C4 1.387(4) . ? C3 H3 0.9400 . ? C10 H10 0.9400 . ? C22 C23 1.513(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C31 C32 1.385(4) . ? C31 H31 0.9400 . ? C23 C28 1.383(4) . ? C23 C24 1.387(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C39 C40 1.372(5) . ? C39 H39 0.9400 . ? C28 C27 1.392(4) . ? C28 H28 0.9400 . ? C42 C41 1.386(4) . ? C42 H42 0.9400 . ? C41 C40 1.369(5) . ? C41 H41 0.9400 . ? C34 C33 1.374(4) . ? C34 H34 0.9400 . ? C40 H40 0.9400 . ? C32 C33 1.380(4) . ? C32 H32 0.9400 . ? C24 C25 1.389(5) . ? C24 H24 0.9400 . ? C21 C20 1.378(5) . ? C21 H21 0.9400 . ? C4 H4 0.9400 . ? C33 H33 0.9400 . ? C19 C20 1.376(6) . ? C19 C18 1.383(5) . ? C19 H19 0.9400 . ? C25 C26 1.372(6) . ? C25 H25 0.9400 . ? C18 H18 0.9400 . ? C20 H20 0.9400 . ? C26 C27 1.373(5) . ? C26 H26 0.9400 . ? C27 H27 0.9400 . ? 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(11) . 3_565 ? N1 Fe1 N2 87.42(7) . 3_565 ? N1 Fe1 N2 92.58(7) 3_565 3_565 ? N1 Fe1 N2 92.58(7) . . ? N1 Fe1 N2 87.42(7) 3_565 . ? N2 Fe1 N2 180.00(10) 3_565 . ? N1 Fe1 N4 91.25(7) . . ? N1 Fe1 N4 88.75(7) 3_565 . ? N2 Fe1 N4 97.45(7) 3_565 . ? N2 Fe1 N4 82.55(7) . . ? N1 Fe1 N4 88.75(7) . 3_565 ? N1 Fe1 N4 91.25(7) 3_565 3_565 ? N2 Fe1 N4 82.55(7) 3_565 3_565 ? N2 Fe1 N4 97.45(7) . 3_565 ? N4 Fe1 N4 180.0 . 3_565 ? C12 N6 C13 113.60(18) . . ? C12 N3 C6 120.13(18) . . ? C12 N3 C7 120.29(18) . . ? C6 N3 C7 119.26(18) . . ? C14 N8 C15 120.3(2) . . ? C14 N8 C22 121.3(2) . . ? C15 N8 C22 117.86(19) . . ? C6 N2 C2 117.6(2) . . ? C6 N2 Fe1 121.87(15) . . ? C2 N2 Fe1 120.55(15) . . ? C14 N7 C13 113.74(19) . . ? C7 N4 C11 117.0(2) . . ? C7 N4 Fe1 122.13(15) . . ? C11 N4 Fe1 120.73(16) . . ? N6 C12 N5 127.8(2) . . ? N6 C12 N3 115.63(19) . . ? N5 C12 N3 116.53(19) . . ? C12 N5 C14 112.76(19) . . ? C13 N9 C36 121.75(19) . . ? C13 N9 C29 122.70(19) . . ? C36 N9 C29 115.32(19) . . ? N7 C14 N5 126.5(2) . . ? N7 C14 N8 117.2(2) . . ? N5 C14 N8 116.3(2) . . ? N9 C36 C37 112.83(19) . . ? N9 C36 H36A 109.0 . . ? C37 C36 H36A 109.0 . . ? N9 C36 H36B 109.0 . . ? C37 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? C1 N1 Fe1 170.28(19) . . ? N1 C1 S1 179.5(2) . . ? N7 C13 N6 125.5(2) . . ? N7 C13 N9 117.4(2) . . ? N6 C13 N9 117.08(19) . . ? C31 C30 C35 118.5(2) . . ? C31 C30 C29 120.3(2) . . ? C35 C30 C29 121.3(2) . . ? C38 C37 C42 118.6(2) . . ? C38 C37 C36 121.0(2) . . ? C42 C37 C36 120.4(2) . . ? N4 C11 C10 123.5(2) . . ? N4 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N9 C29 C30 111.79(19) . . ? N9 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? N9 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? N2 C6 C5 123.0(2) . . ? N2 C6 N3 117.33(19) . . ? C5 C6 N3 119.66(19) . . ? N2 C2 C3 122.9(2) . . ? N2 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C9 C8 C7 118.6(2) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? N4 C7 C8 123.2(2) . . ? N4 C7 N3 116.66(19) . . ? C8 C7 N3 120.1(2) . . ? C34 C35 C30 120.2(3) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C8 C9 C10 118.9(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C16 C21 118.8(3) . . ? C17 C16 C15 121.9(2) . . ? C21 C16 C15 119.3(3) . . ? C4 C5 C6 118.7(2) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.6 . . ? C37 C38 C39 121.0(3) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C11 C10 C9 118.7(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? N8 C22 C23 114.4(2) . . ? N8 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N8 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C32 C31 C30 121.3(2) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C28 C23 C24 118.2(3) . . ? C28 C23 C22 120.6(2) . . ? C24 C23 C22 121.2(3) . . ? N8 C15 C16 115.7(2) . . ? N8 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N8 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.4 . . ? C40 C39 C38 119.7(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C23 C28 C27 121.5(3) . . ? C23 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C41 C42 C37 119.9(3) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? C40 C41 C42 120.6(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C23 C24 C25 120.3(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C21 C16 120.8(3) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 119.4(4) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.384 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.062 #=END data_2 _database_code_depnum_ccdc_archive 'CCDC 836944' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DDB)2] ; _chemical_name_common trans-[Fe(II)(NCS)2(DDB)2] _chemical_melting_point ? _chemical_formula_moiety '(C84 H72 Fe N18 S2)' _chemical_formula_sum 'C84 H72 Fe N18 S2' _chemical_formula_weight 1453.57 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.252(4) _cell_length_b 10.404(2) _cell_length_c 20.070(3) _cell_angle_alpha 98.439(2) _cell_angle_beta 92.244(3) _cell_angle_gamma 119.120(10) _cell_volume 1834.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20008 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 26.54 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9841 _exptl_absorpt_correction_T_max 0.9997 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77371 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _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 20008 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 26.54 _reflns_number_total 5339 _reflns_number_gt 4415 _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^)+(0.0000P)^2^+46.1619P] 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 SHELXL _refine_ls_extinction_coef 0.037(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5339 _refine_ls_number_parameters 476 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.1186 _refine_ls_wR_factor_ref 0.3111 _refine_ls_wR_factor_gt 0.3049 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.200 _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 0.0000 0.0069(5) Uani 1 2 d SU . . S1 S -0.3827(3) -0.1350(3) 0.14552(12) 0.0167(7) Uani 1 1 d . . . N1 N -0.1549(9) -0.0446(9) 0.0602(4) 0.0127(18) Uani 1 1 d U . . N9 N -0.1240(10) -0.0286(9) 0.3232(4) 0.018(2) Uani 1 1 d . . . C1 C -0.2493(12) -0.0831(10) 0.0962(5) 0.014(2) Uani 1 1 d . . . C4 C 0.3500(13) 0.0310(11) 0.1769(5) 0.020(2) Uani 1 1 d . . . H4 H 0.4187 0.0357 0.2116 0.024 Uiso 1 1 calc R . . N6 N -0.0040(9) 0.0812(8) 0.2360(4) 0.0128(18) Uani 1 1 d . . . C5 C 0.2762(12) 0.1106(11) 0.1884(5) 0.018(2) Uani 1 1 d . . . H5 H 0.2918 0.1705 0.2317 0.022 Uiso 1 1 calc R . . C18 C -0.4455(12) 0.2402(11) 0.0551(5) 0.019(2) Uani 1 1 d . . . H18 H -0.4810 0.1495 0.0232 0.023 Uiso 1 1 calc R . . N8 N -0.1935(9) 0.3436(8) 0.2560(4) 0.0135(18) Uani 1 1 d . . . N3 N 0.1061(9) 0.1909(9) 0.1447(4) 0.0123(17) Uani 1 1 d U . . C36 C -0.0552(13) -0.1233(10) 0.3124(5) 0.020(2) Uani 1 1 d . . . H36A H -0.0665 -0.1603 0.2630 0.024 Uiso 1 1 calc R . . H36B H -0.1116 -0.2116 0.3338 0.024 Uiso 1 1 calc R . . N5 N -0.0469(10) 0.2671(8) 0.1989(4) 0.0150(19) Uani 1 1 d . . . C15 C -0.1578(12) 0.4602(10) 0.2141(5) 0.014(2) Uani 1 1 d . . . H15A H -0.0633 0.4822 0.1948 0.016 Uiso 1 1 calc R . . H15B H -0.1410 0.5534 0.2435 0.016 Uiso 1 1 calc R . . N4 N 0.0850(9) 0.2205(8) 0.0308(4) 0.0112(17) Uani 1 1 d . . . N7 N -0.1597(10) 0.1605(9) 0.2944(4) 0.0144(18) Uani 1 1 d . . . C13 C -0.0957(11) 0.0755(10) 0.2834(5) 0.013(2) Uani 1 1 d . . . C37 C 0.1118(12) -0.0473(12) 0.3404(5) 0.020(2) Uani 1 1 d . . . C16 C -0.2823(11) 0.4126(10) 0.1566(5) 0.012(2) Uani 1 1 d . . . N2 N 0.1433(9) 0.0146(9) 0.0733(4) 0.0131(18) Uani 1 1 d U . . C17 C -0.3359(12) 0.2790(10) 0.1089(5) 0.016(2) Uani 1 1 d . . . H17 H -0.2967 0.2143 0.1136 0.019 Uiso 1 1 calc R . . C2 C 0.2217(11) -0.0598(10) 0.0632(5) 0.012(2) Uani 1 1 d . . . H2 H 0.2068 -0.1168 0.0191 0.014 Uiso 1 1 calc R . . C3 C 0.3208(11) -0.0585(10) 0.1117(5) 0.012(2) Uani 1 1 d . . . H3 H 0.3686 -0.1164 0.1019 0.015 Uiso 1 1 calc R . . C38 C 0.1956(12) 0.1002(11) 0.3745(5) 0.020(2) Uani 1 1 d . . . H38 H 0.1489 0.1597 0.3815 0.024 Uiso 1 1 calc R . . C14 C -0.1322(12) 0.2548(10) 0.2497(5) 0.013(2) Uani 1 1 d . . . C39 C 0.3455(14) 0.1617(14) 0.3982(6) 0.032(3) Uani 1 1 d . . . H39 H 0.4011 0.2632 0.4211 0.038 Uiso 1 1 calc R . . C6 C 0.1768(10) 0.1023(9) 0.1352(5) 0.0089(19) Uani 1 1 d . . . C23 C -0.2037(12) 0.4661(11) 0.3710(5) 0.015(2) Uani 1 1 d . . . C22 C -0.2907(12) 0.3418(11) 0.3085(5) 0.016(2) Uani 1 1 d . . . H22A H -0.3368 0.2433 0.3227 0.020 Uiso 1 1 calc R . . H22B H -0.3731 0.3543 0.2889 0.020 Uiso 1 1 calc R . . C12 C 0.0139(11) 0.1808(10) 0.1966(5) 0.012(2) Uani 1 1 d . . . C42 C 0.1821(16) -0.1328(14) 0.3301(7) 0.037(3) Uani 1 1 d . . . H42 H 0.1274 -0.2340 0.3068 0.044 Uiso 1 1 calc R . . C7 C 0.1187(11) 0.2829(10) 0.0963(5) 0.011(2) Uani 1 1 d . . . C21 C -0.3414(12) 0.5064(11) 0.1483(5) 0.019(2) Uani 1 1 d . . . H21 H -0.3055 0.5984 0.1793 0.023 Uiso 1 1 calc R . . C29 C -0.2185(12) -0.0462(11) 0.3782(5) 0.016(2) Uani 1 1 d . . . H29A H -0.2391 0.0381 0.3852 0.020 Uiso 1 1 calc R . . H29B H -0.1618 -0.0402 0.4207 0.020 Uiso 1 1 calc R . . C30 C -0.3667(13) -0.1923(12) 0.3646(5) 0.018(2) Uani 1 1 d . . . C9 C 0.1899(12) 0.5256(11) 0.0705(5) 0.016(2) Uani 1 1 d U . . H9 H 0.2226 0.6291 0.0841 0.019 Uiso 1 1 calc R . . C24 C -0.2775(13) 0.5313(11) 0.4071(5) 0.020(2) Uani 1 1 d . . . H24 H -0.3791 0.5013 0.3924 0.024 Uiso 1 1 calc R . . C8 C 0.1740(11) 0.4357(11) 0.1187(5) 0.014(2) Uani 1 1 d U . . H8 H 0.2003 0.4781 0.1658 0.017 Uiso 1 1 calc R . . C10 C 0.1566(11) 0.4588(11) 0.0022(5) 0.014(2) Uani 1 1 d U . . H10 H 0.1685 0.5170 -0.0318 0.016 Uiso 1 1 calc R . . C34 C -0.5591(15) -0.4199(14) 0.2912(7) 0.034(3) Uani 1 1 d . . . H34 H -0.5952 -0.4830 0.2476 0.041 Uiso 1 1 calc R . . C20 C -0.4528(12) 0.4647(11) 0.0945(5) 0.020(2) Uani 1 1 d . . . H20 H -0.4946 0.5274 0.0900 0.024 Uiso 1 1 calc R . . C35 C -0.4245(12) -0.2862(12) 0.3004(5) 0.021(2) Uani 1 1 d . . . H35 H -0.3704 -0.2574 0.2628 0.025 Uiso 1 1 calc R . . C25 C -0.1995(15) 0.6408(13) 0.4649(6) 0.029(3) Uani 1 1 d . . . H25 H -0.2499 0.6843 0.4898 0.035 Uiso 1 1 calc R . . C19 C -0.5032(12) 0.3348(12) 0.0480(5) 0.024(3) Uani 1 1 d . . . H19 H -0.5774 0.3093 0.0110 0.029 Uiso 1 1 calc R . . C11 C 0.1067(11) 0.3095(10) -0.0156(5) 0.013(2) Uani 1 1 d U . . H11 H 0.0861 0.2657 -0.0625 0.015 Uiso 1 1 calc R . . C26 C -0.0530(15) 0.6876(15) 0.4869(7) 0.037(3) Uani 1 1 d U . . H26 H -0.0021 0.7621 0.5267 0.044 Uiso 1 1 calc R . . C40 C 0.4163(15) 0.0765(16) 0.3890(6) 0.039(3) Uani 1 1 d . . . H40 H 0.5191 0.1179 0.4062 0.047 Uiso 1 1 calc R . . C27 C 0.020(2) 0.6251(18) 0.4506(8) 0.056(4) Uani 1 1 d U . . H27 H 0.1227 0.6596 0.4647 0.068 Uiso 1 1 calc R . . C28 C -0.0551(16) 0.5114(15) 0.3932(7) 0.040(3) Uani 1 1 d U . . H28 H -0.0048 0.4660 0.3697 0.047 Uiso 1 1 calc R . . C41 C 0.3342(18) -0.0677(18) 0.3547(8) 0.049(4) Uani 1 1 d . . . H41 H 0.3822 -0.1260 0.3473 0.059 Uiso 1 1 calc R . . C31 C -0.4521(14) -0.2374(13) 0.4187(6) 0.027(3) Uani 1 1 d . . . H31 H -0.4159 -0.1763 0.4627 0.033 Uiso 1 1 calc R . . C32 C -0.5873(14) -0.3692(15) 0.4081(7) 0.037(3) Uani 1 1 d . . . H32 H -0.6450 -0.3973 0.4447 0.044 Uiso 1 1 calc R . . C33 C -0.6410(14) -0.4626(14) 0.3439(7) 0.037(3) Uani 1 1 d . . . H33 H -0.7334 -0.5547 0.3371 0.044 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 0.0084(9) 0.0023(8) 0.0095(8) 0.0014(6) 0.0017(6) 0.0023(6) S1 0.0136(14) 0.0169(13) 0.0174(13) 0.0067(10) 0.0053(10) 0.0048(10) N1 0.013(2) 0.0125(19) 0.013(2) 0.0021(10) 0.0010(10) 0.0061(12) N9 0.022(5) 0.016(4) 0.017(4) 0.011(4) 0.006(4) 0.008(4) C1 0.019(6) 0.006(5) 0.019(5) 0.004(4) 0.002(4) 0.009(4) C4 0.033(7) 0.014(5) 0.021(6) 0.007(4) 0.003(5) 0.017(5) N6 0.017(5) 0.006(4) 0.011(4) -0.001(3) 0.001(3) 0.003(3) C5 0.018(6) 0.013(5) 0.016(5) 0.000(4) -0.002(4) 0.003(4) C18 0.017(6) 0.006(5) 0.020(5) 0.000(4) 0.001(4) -0.005(4) N8 0.013(5) 0.007(4) 0.021(4) 0.003(3) 0.008(3) 0.004(3) N3 0.012(2) 0.0120(19) 0.012(2) 0.0025(10) 0.0015(10) 0.0060(12) C36 0.028(7) 0.003(5) 0.025(6) 0.007(4) -0.001(5) 0.004(4) N5 0.022(5) 0.002(4) 0.016(4) -0.001(3) 0.001(3) 0.002(3) C15 0.019(6) 0.002(4) 0.017(5) 0.000(4) -0.002(4) 0.004(4) N4 0.009(5) 0.003(4) 0.018(4) 0.003(3) 0.004(3) 0.000(3) N7 0.021(5) 0.011(4) 0.016(4) 0.003(3) 0.002(3) 0.011(4) C13 0.011(5) 0.007(5) 0.014(5) -0.001(4) -0.005(4) 0.001(4) C37 0.022(6) 0.024(6) 0.019(5) 0.011(4) 0.006(4) 0.013(5) C16 0.011(5) 0.004(4) 0.019(5) 0.002(4) 0.001(4) 0.001(4) N2 0.013(2) 0.013(2) 0.013(2) 0.0025(10) 0.0021(10) 0.0059(12) C17 0.025(6) 0.003(5) 0.017(5) 0.003(4) 0.004(4) 0.006(4) C2 0.005(5) 0.002(4) 0.023(5) 0.001(4) -0.001(4) -0.001(4) C3 0.008(5) 0.003(4) 0.028(6) 0.003(4) 0.001(4) 0.004(4) C38 0.023(7) 0.017(5) 0.019(5) 0.009(4) 0.005(4) 0.006(5) C14 0.017(6) 0.009(5) 0.011(5) 0.000(4) 0.000(4) 0.005(4) C39 0.023(7) 0.027(6) 0.026(6) 0.005(5) 0.002(5) -0.004(5) C6 0.004(5) 0.002(4) 0.017(5) 0.001(4) 0.000(4) -0.002(4) C23 0.017(6) 0.015(5) 0.013(5) 0.005(4) 0.001(4) 0.007(4) C22 0.016(6) 0.012(5) 0.019(5) -0.002(4) 0.004(4) 0.007(4) C12 0.012(5) 0.006(5) 0.011(5) -0.006(4) -0.005(4) 0.001(4) C42 0.043(9) 0.030(7) 0.055(8) 0.015(6) 0.003(6) 0.031(6) C7 0.011(5) 0.003(4) 0.014(5) 0.001(4) 0.003(4) 0.001(4) C21 0.026(7) 0.010(5) 0.022(6) 0.004(4) 0.006(5) 0.010(5) C29 0.021(6) 0.017(5) 0.015(5) 0.009(4) 0.005(4) 0.011(5) C30 0.028(7) 0.023(6) 0.015(5) 0.009(4) 0.007(4) 0.020(5) C9 0.016(2) 0.016(2) 0.017(2) 0.0032(11) 0.0021(10) 0.0078(14) C24 0.032(7) 0.016(5) 0.019(5) 0.006(4) 0.005(5) 0.017(5) C8 0.014(2) 0.014(2) 0.014(2) 0.0024(11) 0.0017(10) 0.0068(13) C10 0.014(2) 0.013(2) 0.014(2) 0.0029(11) 0.0016(10) 0.0067(13) C34 0.030(8) 0.030(7) 0.037(7) 0.011(6) -0.003(5) 0.010(6) C20 0.022(6) 0.016(5) 0.028(6) 0.004(4) 0.000(5) 0.014(5) C35 0.016(6) 0.023(6) 0.025(6) 0.012(5) 0.004(4) 0.008(5) C25 0.042(8) 0.025(6) 0.027(6) 0.001(5) 0.005(5) 0.023(6) C19 0.013(6) 0.030(6) 0.021(6) 0.010(5) 0.002(4) 0.003(5) C11 0.013(2) 0.012(2) 0.013(2) 0.0027(11) 0.0013(10) 0.0062(13) C26 0.037(3) 0.037(3) 0.037(3) 0.0063(12) 0.0047(11) 0.0185(18) C40 0.018(7) 0.056(9) 0.032(7) 0.020(6) -0.001(5) 0.007(6) C27 0.056(4) 0.057(4) 0.057(4) 0.0099(13) 0.0072(12) 0.028(2) C28 0.039(3) 0.040(3) 0.039(3) 0.0065(12) 0.0051(11) 0.0200(18) C41 0.054(11) 0.059(10) 0.056(9) 0.024(8) 0.010(7) 0.041(9) C31 0.034(8) 0.035(7) 0.030(6) 0.022(5) 0.016(5) 0.025(6) C32 0.025(7) 0.052(8) 0.050(8) 0.038(7) 0.024(6) 0.024(6) C33 0.021(7) 0.027(7) 0.058(9) 0.020(6) 0.005(6) 0.005(5) _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 1.949(8) . ? Fe1 N1 1.949(8) 2 ? Fe1 N2 1.973(8) 2 ? Fe1 N2 1.973(8) . ? Fe1 N4 2.000(7) 2 ? Fe1 N4 2.000(7) . ? S1 C1 1.638(10) . ? N1 C1 1.176(13) . ? N9 C13 1.364(13) . ? N9 C36 1.464(14) . ? N9 C29 1.470(13) . ? C4 C5 1.370(15) . ? C4 C3 1.417(14) . ? C4 H4 0.9500 . ? N6 C12 1.342(13) . ? N6 C13 1.350(13) . ? C5 C6 1.410(14) . ? C5 H5 0.9500 . ? C18 C17 1.388(15) . ? C18 C19 1.393(16) . ? C18 H18 0.9500 . ? N8 C14 1.342(13) . ? N8 C22 1.474(12) . ? N8 C15 1.485(12) . ? N3 C12 1.414(12) . ? N3 C6 1.422(12) . ? N3 C7 1.428(12) . ? C36 C37 1.531(16) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C12 1.316(13) . ? N5 C14 1.349(13) . ? C15 C16 1.520(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N4 C7 1.328(12) . ? N4 C11 1.358(12) . ? N7 C13 1.334(13) . ? N7 C14 1.362(13) . ? C37 C38 1.387(15) . ? C37 C42 1.392(16) . ? C16 C21 1.401(14) . ? C16 C17 1.406(13) . ? N2 C6 1.349(12) . ? N2 C2 1.364(12) . ? C17 H17 0.9500 . ? C2 C3 1.374(14) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C38 C39 1.376(17) . ? C38 H38 0.9500 . ? C39 C40 1.39(2) . ? C39 H39 0.9500 . ? C23 C28 1.388(18) . ? C23 C24 1.397(14) . ? C23 C22 1.536(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C42 C41 1.40(2) . ? C42 H42 0.9500 . ? C7 C8 1.394(13) . ? C21 C20 1.394(15) . ? C21 H21 0.9500 . ? C29 C30 1.514(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C35 1.406(15) . ? C30 C31 1.409(15) . ? C9 C10 1.390(14) . ? C9 C8 1.403(14) . ? C9 H9 0.9500 . ? C24 C25 1.391(16) . ? C24 H24 0.9500 . ? C8 H8 0.9500 . ? C10 C11 1.361(14) . ? C10 H10 0.9500 . ? C34 C33 1.366(18) . ? C34 C35 1.382(16) . ? C34 H34 0.9500 . ? C20 C19 1.370(15) . ? C20 H20 0.9500 . ? C35 H35 0.9500 . ? C25 C26 1.365(19) . ? C25 H25 0.9500 . ? C19 H19 0.9500 . ? C11 H11 0.9500 . ? C26 C27 1.37(2) . ? C26 H26 0.9500 . ? C40 C41 1.36(2) . ? C40 H40 0.9500 . ? C27 C28 1.40(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C41 H41 0.9500 . ? C31 C32 1.375(18) . ? C31 H31 0.9500 . ? C32 C33 1.402(19) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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(8) . 2 ? N1 Fe1 N2 88.8(3) . 2 ? N1 Fe1 N2 91.2(3) 2 2 ? N1 Fe1 N2 91.2(3) . . ? N1 Fe1 N2 88.8(3) 2 . ? N2 Fe1 N2 180.0(5) 2 . ? N1 Fe1 N4 88.6(3) . 2 ? N1 Fe1 N4 91.4(3) 2 2 ? N2 Fe1 N4 86.5(3) 2 2 ? N2 Fe1 N4 93.5(3) . 2 ? N1 Fe1 N4 91.4(3) . . ? N1 Fe1 N4 88.6(3) 2 . ? N2 Fe1 N4 93.5(3) 2 . ? N2 Fe1 N4 86.5(3) . . ? N4 Fe1 N4 180.0(2) 2 . ? C1 N1 Fe1 174.4(7) . . ? C13 N9 C36 119.3(8) . . ? C13 N9 C29 122.1(9) . . ? C36 N9 C29 118.6(8) . . ? N1 C1 S1 178.7(9) . . ? C5 C4 C3 118.1(10) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C12 N6 C13 112.6(8) . . ? C4 C5 C6 119.2(9) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C17 C18 C19 119.7(9) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C14 N8 C22 122.9(8) . . ? C14 N8 C15 122.1(8) . . ? C22 N8 C15 114.8(8) . . ? C12 N3 C6 122.3(8) . . ? C12 N3 C7 119.3(8) . . ? C6 N3 C7 118.1(8) . . ? N9 C36 C37 115.4(8) . . ? N9 C36 H36A 108.4 . . ? C37 C36 H36A 108.4 . . ? N9 C36 H36B 108.4 . . ? C37 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C12 N5 C14 113.7(8) . . ? N8 C15 C16 112.5(8) . . ? N8 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N8 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C7 N4 C11 118.5(8) . . ? C7 N4 Fe1 121.5(6) . . ? C11 N4 Fe1 120.0(6) . . ? C13 N7 C14 113.9(8) . . ? N7 C13 N6 126.4(9) . . ? N7 C13 N9 118.1(9) . . ? N6 C13 N9 115.5(9) . . ? C38 C37 C42 118.7(11) . . ? C38 C37 C36 124.1(10) . . ? C42 C37 C36 117.2(10) . . ? C21 C16 C17 118.4(9) . . ? C21 C16 C15 119.9(8) . . ? C17 C16 C15 121.6(9) . . ? C6 N2 C2 115.0(8) . . ? C6 N2 Fe1 123.7(6) . . ? C2 N2 Fe1 121.2(6) . . ? C18 C17 C16 120.9(9) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? N2 C2 C3 124.9(9) . . ? N2 C2 H2 117.5 . . ? C3 C2 H2 117.5 . . ? C2 C3 C4 118.5(9) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C39 C38 C37 121.1(11) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? N8 C14 N5 116.5(8) . . ? N8 C14 N7 118.4(9) . . ? N5 C14 N7 125.1(9) . . ? C38 C39 C40 120.6(11) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? N2 C6 C5 124.1(9) . . ? N2 C6 N3 115.8(8) . . ? C5 C6 N3 120.1(8) . . ? C28 C23 C24 119.8(10) . . ? C28 C23 C22 121.1(10) . . ? C24 C23 C22 119.1(9) . . ? N8 C22 C23 112.3(8) . . ? N8 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N8 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? N5 C12 N6 128.1(9) . . ? N5 C12 N3 116.0(8) . . ? N6 C12 N3 115.8(9) . . ? C37 C42 C41 119.0(13) . . ? C37 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? N4 C7 C8 122.2(8) . . ? N4 C7 N3 118.3(8) . . ? C8 C7 N3 119.4(8) . . ? C20 C21 C16 119.9(9) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? N9 C29 C30 113.6(8) . . ? N9 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? N9 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C35 C30 C31 117.9(11) . . ? C35 C30 C29 123.2(9) . . ? C31 C30 C29 118.9(10) . . ? C10 C9 C8 118.1(9) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C25 C24 C23 118.9(11) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C7 C8 C9 118.8(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C11 C10 C9 119.5(9) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C33 C34 C35 120.9(12) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C19 C20 C21 121.1(10) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C34 C35 C30 120.8(10) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? C26 C25 C24 122.0(11) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C20 C19 C18 119.9(10) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? N4 C11 C10 122.8(9) . . ? N4 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? C25 C26 C27 118.8(13) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C41 C40 C39 118.2(12) . . ? C41 C40 H40 120.9 . . ? C39 C40 H40 120.9 . . ? C26 C27 C28 121.3(16) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C23 C28 C27 119.1(13) . . ? C23 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C40 C41 C42 122.3(14) . . ? C40 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C32 C31 C30 120.5(12) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.6(11) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119.4(12) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.422 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.155 #=END data_3 _database_code_depnum_ccdc_archive 'CCDC 836945' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[(Fe(II)(DCA)2(DBB)2].2CH3CH2OH ; _chemical_name_common trans-[(Fe(II)(DCA)2(DBB)2].2CH3CH2OH _chemical_melting_point ? _chemical_formula_moiety '(C86 H72 Fe N22), 2(C2 H6 O)' _chemical_formula_sum 'C90 H84 Fe N22 O2' _chemical_formula_weight 1561.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.973(2) _cell_length_b 10.341(2) _cell_length_c 21.440(4) _cell_angle_alpha 84.52(3) _cell_angle_beta 89.06(3) _cell_angle_gamma 62.86(3) _cell_volume 1957.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 11106 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9745 _exptl_absorpt_correction_T_max 0.9948 _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 11106 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6699 _reflns_number_gt 4659 _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 6699 _refine_ls_number_parameters 517 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.0000 0.01595(18) Uani 1 2 d S . . N9 N 0.2862(3) 0.1796(3) 0.23633(12) 0.0213(6) Uani 1 1 d . . . N10 N 0.4057(3) -0.1667(3) 0.12164(15) 0.0382(8) Uani 1 1 d . . . N11 N 0.5371(4) -0.3778(3) 0.19802(16) 0.0429(9) Uani 1 1 d . . . C10 C -0.2929(3) -0.1351(3) 0.09751(15) 0.0221(7) Uani 1 1 d . . . H10 H -0.3479 -0.1852 0.0873 0.026 Uiso 1 1 calc R . . N1 N 0.1755(3) -0.0808(3) 0.05713(12) 0.0193(6) Uani 1 1 d . . . C16 C 0.0059(4) -0.2814(3) 0.31061(15) 0.0224(8) Uani 1 1 d . . . C8 C -0.2199(4) -0.0176(4) 0.16964(15) 0.0247(8) Uani 1 1 d . . . H8 H -0.2228 0.0150 0.2098 0.030 Uiso 1 1 calc R . . N5 N 0.0812(3) -0.0725(3) 0.21549(12) 0.0186(6) Uani 1 1 d . . . C11 C -0.2078(3) -0.1057(3) 0.05399(15) 0.0184(7) Uani 1 1 d . . . H11 H -0.2058 -0.1353 0.0132 0.022 Uiso 1 1 calc R . . N8 N 0.2318(3) -0.2337(3) 0.29634(12) 0.0208(6) Uani 1 1 d . . . C39 C 0.4880(4) 0.4068(4) 0.08568(17) 0.0318(9) Uani 1 1 d . . . H39 H 0.5285 0.4743 0.0808 0.038 Uiso 1 1 calc R . . C43 C 0.4695(4) -0.2823(4) 0.16197(16) 0.0224(8) Uani 1 1 d . . . C3 C -0.1547(4) 0.4532(4) 0.00578(16) 0.0257(8) Uani 1 1 d . . . H3 H -0.1752 0.5336 -0.0246 0.031 Uiso 1 1 calc R . . C38 C 0.3978(4) 0.4094(4) 0.13568(16) 0.0261(8) Uani 1 1 d . . . H38 H 0.3770 0.4790 0.1650 0.031 Uiso 1 1 calc R . . C2 C -0.1095(3) 0.3164(3) -0.01209(15) 0.0198(7) Uani 1 1 d . . . H2 H -0.1034 0.3043 -0.0556 0.024 Uiso 1 1 calc R . . N4 N -0.1253(3) -0.0362(3) 0.06576(12) 0.0176(6) Uani 1 1 d . . . C36 C 0.2381(4) 0.3193(3) 0.19799(15) 0.0227(8) Uani 1 1 d . . . H36A H 0.2360 0.3926 0.2250 0.027 Uiso 1 1 calc R . . H36B H 0.1340 0.3527 0.1817 0.027 Uiso 1 1 calc R . . N2 N -0.0730(3) 0.1966(3) 0.02965(12) 0.0178(6) Uani 1 1 d . . . C5 C -0.1410(4) 0.3540(3) 0.11155(16) 0.0258(8) Uani 1 1 d . . . H5 H -0.1554 0.3655 0.1550 0.031 Uiso 1 1 calc R . . C37 C 0.3372(3) 0.3129(3) 0.14378(14) 0.0202(7) Uani 1 1 d . . . C28 C 0.2558(4) -0.1023(4) 0.42026(17) 0.0364(10) Uani 1 1 d . . . H28 H 0.2530 -0.0302 0.3886 0.044 Uiso 1 1 calc R . . C42 C 0.3683(4) 0.2116(3) 0.10003(15) 0.0239(8) Uani 1 1 d . . . H42 H 0.3272 0.1446 0.1046 0.029 Uiso 1 1 calc R . . C33 C 0.2234(6) 0.3303(5) 0.45903(18) 0.0479(12) Uani 1 1 d . . . H33 H 0.1860 0.3698 0.4975 0.058 Uiso 1 1 calc R . . C19 C -0.2769(4) -0.2193(4) 0.35784(17) 0.0340(9) Uani 1 1 d . . . H19 H -0.3733 -0.1977 0.3741 0.041 Uiso 1 1 calc R . . C23 C 0.3125(4) -0.2448(4) 0.40706(16) 0.0275(8) Uani 1 1 d . . . C41 C 0.4588(4) 0.2089(4) 0.05020(16) 0.0286(9) Uani 1 1 d . . . H41 H 0.4799 0.1397 0.0207 0.034 Uiso 1 1 calc R . . N6 N 0.1136(3) 0.1385(3) 0.18309(12) 0.0204(6) Uani 1 1 d . . . C21 C -0.0479(4) -0.1976(4) 0.36031(16) 0.0318(9) Uani 1 1 d . . . H21 H 0.0117 -0.1599 0.3784 0.038 Uiso 1 1 calc R . . C18 C -0.2254(4) -0.3019(4) 0.30811(17) 0.0340(9) Uani 1 1 d . . . H18 H -0.2857 -0.3387 0.2900 0.041 Uiso 1 1 calc R . . N7 N 0.2625(3) -0.0275(3) 0.26930(12) 0.0217(6) Uani 1 1 d . . . C9 C -0.2990(4) -0.0915(4) 0.15712(16) 0.0276(8) Uani 1 1 d . . . H9 H -0.3566 -0.1123 0.1885 0.033 Uiso 1 1 calc R . . C4 C -0.1698(4) 0.4724(4) 0.06895(17) 0.0291(9) Uani 1 1 d . . . H4 H -0.1997 0.5661 0.0827 0.035 Uiso 1 1 calc R . . C1 C 0.2822(4) -0.1295(3) 0.08883(15) 0.0205(7) Uani 1 1 d . . . C15 C 0.1628(4) -0.3273(3) 0.28549(16) 0.0248(8) Uani 1 1 d . . . H15A H 0.2297 -0.4271 0.3046 0.030 Uiso 1 1 calc R . . H15B H 0.1577 -0.3321 0.2397 0.030 Uiso 1 1 calc R . . C40 C 0.5189(4) 0.3060(4) 0.04292(17) 0.0322(9) Uani 1 1 d . . . H40 H 0.5813 0.3033 0.0086 0.039 Uiso 1 1 calc R . . C29 C 0.3984(4) 0.1459(4) 0.28620(15) 0.0262(8) Uani 1 1 d . . . H29A H 0.4712 0.1814 0.2710 0.031 Uiso 1 1 calc R . . H29B H 0.4549 0.0385 0.2953 0.031 Uiso 1 1 calc R . . C34 C 0.3753(6) 0.2444(5) 0.45286(19) 0.0510(12) Uani 1 1 d . . . H34 H 0.4431 0.2253 0.4871 0.061 Uiso 1 1 calc R . . C17 C -0.0852(4) -0.3315(4) 0.28448(17) 0.0288(8) Uani 1 1 d . . . H17 H -0.0510 -0.3874 0.2496 0.035 Uiso 1 1 calc R . . C12 C 0.0501(3) 0.0517(3) 0.18037(14) 0.0172(7) Uani 1 1 d . . . C20 C -0.1872(4) -0.1682(4) 0.38398(17) 0.0381(10) Uani 1 1 d . . . H20 H -0.2218 -0.1121 0.4187 0.046 Uiso 1 1 calc R . . C27 C 0.2030(5) -0.0623(5) 0.47863(18) 0.0473(11) Uani 1 1 d . . . H27 H 0.1627 0.0370 0.4868 0.057 Uiso 1 1 calc R . . C6 C -0.0908(3) 0.2179(3) 0.09021(14) 0.0194(7) Uani 1 1 d . . . C7 C -0.1354(3) 0.0092(3) 0.12286(14) 0.0186(7) Uani 1 1 d . . . N3 N -0.0610(3) 0.0939(3) 0.13327(11) 0.0176(6) Uani 1 1 d . . . C31 C 0.1806(4) 0.2987(4) 0.35302(16) 0.0323(9) Uani 1 1 d . . . H31 H 0.1127 0.3175 0.3188 0.039 Uiso 1 1 calc R . . C26 C 0.2083(6) -0.1650(5) 0.5247(2) 0.0572(13) Uani 1 1 d . . . H26 H 0.1748 -0.1372 0.5653 0.069 Uiso 1 1 calc R . . C22 C 0.3604(4) -0.2875(4) 0.34159(16) 0.0278(8) Uani 1 1 d . . . H22A H 0.4301 -0.2479 0.3267 0.033 Uiso 1 1 calc R . . H22B H 0.4160 -0.3953 0.3432 0.033 Uiso 1 1 calc R . . C32 C 0.1252(5) 0.3588(4) 0.40873(18) 0.0430(10) Uani 1 1 d . . . H32 H 0.0202 0.4192 0.4124 0.052 Uiso 1 1 calc R . . C30 C 0.3340(4) 0.2116(3) 0.34654(15) 0.0247(8) Uani 1 1 d . . . C35 C 0.4296(5) 0.1862(4) 0.39753(17) 0.0395(10) Uani 1 1 d . . . H35 H 0.5349 0.1272 0.3940 0.047 Uiso 1 1 calc R . . C14 C 0.1914(3) -0.1075(3) 0.25942(14) 0.0185(7) Uani 1 1 d . . . C13 C 0.2196(3) 0.0939(3) 0.22993(14) 0.0185(7) Uani 1 1 d . . . C24 C 0.3173(5) -0.3493(5) 0.45403(18) 0.0451(11) Uani 1 1 d . . . H24 H 0.3586 -0.4487 0.4458 0.054 Uiso 1 1 calc R . . C25 C 0.2625(4) -0.3104(4) 0.51286(15) 0.0627(14) Uani 1 1 d . . . H25 H 0.2619 -0.3812 0.5444 0.075 Uiso 1 1 calc R . . O1A O 0.5668(4) 0.3856(4) 0.28299(15) 0.0575(12) Uiso 0.35 1 d PR A 2 C44A C 0.7048(15) 0.2664(14) 0.2781(6) 0.0310(18) Uiso 0.35 1 d P B 1 C45A C 0.8365(8) 0.2913(7) 0.3030(3) 0.0455(17) Uiso 0.35 1 d P B 1 C44B C 0.6835(12) 0.3346(12) 0.3195(5) 0.0310(18) Uiso 0.35 1 d P A 2 O1C O 0.6252(10) 0.3196(10) 0.2517(4) 0.044(2) Uiso 0.30 1 d PD C 3 C45C C 0.8656(15) 0.224(2) 0.3084(8) 0.059(4) Uiso 0.30 1 d PD C 3 C44C C 0.713(2) 0.265(2) 0.3003(9) 0.059(4) Uiso 0.30 1 d P C 3 O1B O 0.5668(4) 0.3856(4) 0.28299(15) 0.0575(12) Uiso 0.35 1 d P B 1 C45B C 0.8365(8) 0.2913(7) 0.3030(3) 0.0455(17) Uiso 0.35 1 d P 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 0.0167(3) 0.0182(4) 0.0148(4) -0.0019(3) 0.0000(3) -0.0095(3) N9 0.0281(16) 0.0268(15) 0.0174(14) -0.0008(11) -0.0015(12) -0.0201(13) N10 0.0273(17) 0.050(2) 0.044(2) 0.0172(16) -0.0148(15) -0.0270(16) N11 0.044(2) 0.0344(19) 0.048(2) 0.0026(16) -0.0192(18) -0.0174(16) C10 0.0186(17) 0.0176(17) 0.031(2) -0.0002(14) -0.0031(15) -0.0097(14) N1 0.0255(16) 0.0188(14) 0.0155(14) -0.0018(11) 0.0027(13) -0.0118(12) C16 0.0280(19) 0.0193(17) 0.0189(17) 0.0054(13) -0.0034(14) -0.0111(15) C8 0.0269(19) 0.036(2) 0.0169(17) -0.0044(15) 0.0018(15) -0.0191(16) N5 0.0224(15) 0.0207(14) 0.0167(14) -0.0017(11) 0.0007(12) -0.0132(12) C11 0.0175(17) 0.0183(17) 0.0206(17) -0.0052(13) 0.0004(14) -0.0088(14) N8 0.0235(15) 0.0200(14) 0.0208(15) 0.0001(11) -0.0011(12) -0.0120(12) C39 0.029(2) 0.039(2) 0.035(2) -0.0010(17) 0.0024(17) -0.0229(18) C43 0.0157(17) 0.028(2) 0.0232(19) -0.0042(16) -0.0019(15) -0.0093(15) C3 0.0270(19) 0.0213(18) 0.028(2) 0.0036(14) -0.0032(16) -0.0115(15) C38 0.0275(19) 0.032(2) 0.0260(19) -0.0054(15) 0.0009(15) -0.0189(16) C2 0.0187(17) 0.0224(18) 0.0172(17) 0.0024(14) -0.0002(13) -0.0092(14) N4 0.0164(14) 0.0184(14) 0.0183(14) -0.0021(11) -0.0022(11) -0.0080(11) C36 0.0277(19) 0.0190(17) 0.0236(18) -0.0043(14) -0.0011(15) -0.0121(15) N2 0.0168(14) 0.0211(14) 0.0185(14) -0.0008(11) -0.0007(11) -0.0115(12) C5 0.032(2) 0.0264(19) 0.0216(18) -0.0068(15) -0.0004(15) -0.0145(16) C37 0.0188(17) 0.0227(17) 0.0182(17) 0.0012(13) -0.0042(14) -0.0092(14) C28 0.049(2) 0.037(2) 0.027(2) -0.0006(17) -0.0091(18) -0.0220(19) C42 0.0261(19) 0.0194(17) 0.0248(19) -0.0006(14) -0.0013(15) -0.0096(15) C33 0.079(4) 0.052(3) 0.023(2) -0.0073(19) 0.006(2) -0.038(3) C19 0.029(2) 0.046(2) 0.031(2) 0.0023(18) -0.0005(17) -0.0215(18) C23 0.0265(19) 0.031(2) 0.028(2) 0.0035(16) -0.0081(16) -0.0165(16) C41 0.031(2) 0.0243(19) 0.0227(19) -0.0023(15) -0.0025(16) -0.0053(16) N6 0.0266(15) 0.0237(15) 0.0169(14) -0.0050(11) 0.0018(12) -0.0163(13) C21 0.035(2) 0.038(2) 0.029(2) -0.0080(16) -0.0018(17) -0.0207(18) C18 0.035(2) 0.033(2) 0.042(2) 0.0015(18) -0.0083(18) -0.0228(18) N7 0.0248(15) 0.0259(15) 0.0182(15) -0.0006(12) -0.0002(12) -0.0152(13) C9 0.0268(19) 0.038(2) 0.0228(19) 0.0037(15) 0.0012(15) -0.0206(17) C4 0.031(2) 0.0180(18) 0.038(2) -0.0060(15) -0.0055(17) -0.0102(16) C1 0.0240(19) 0.0236(18) 0.0184(17) -0.0017(14) 0.0043(15) -0.0148(15) C15 0.0271(19) 0.0198(18) 0.0288(19) -0.0024(14) 0.0002(15) -0.0119(15) C40 0.0205(19) 0.041(2) 0.030(2) -0.0011(17) 0.0048(16) -0.0099(17) C29 0.0287(19) 0.032(2) 0.0251(19) -0.0026(15) -0.0049(15) -0.0196(16) C34 0.070(3) 0.066(3) 0.026(2) -0.007(2) -0.010(2) -0.038(3) C17 0.031(2) 0.028(2) 0.032(2) -0.0045(16) 0.0018(16) -0.0163(16) C12 0.0197(17) 0.0204(17) 0.0123(16) -0.0069(13) 0.0039(13) -0.0089(14) C20 0.034(2) 0.058(3) 0.027(2) -0.0141(18) 0.0061(17) -0.023(2) C27 0.062(3) 0.051(3) 0.031(2) -0.012(2) -0.005(2) -0.026(2) C6 0.0181(17) 0.0240(18) 0.0194(17) -0.0021(14) -0.0013(14) -0.0124(14) C7 0.0178(17) 0.0179(17) 0.0190(17) -0.0013(13) -0.0048(14) -0.0072(14) N3 0.0225(15) 0.0209(14) 0.0147(14) -0.0022(11) -0.0006(11) -0.0142(12) C31 0.041(2) 0.038(2) 0.023(2) -0.0028(16) -0.0021(17) -0.0221(19) C26 0.077(3) 0.081(3) 0.026(2) -0.008(2) 0.006(2) -0.047(3) C22 0.0250(19) 0.0275(19) 0.031(2) 0.0033(15) -0.0066(16) -0.0128(16) C32 0.049(3) 0.047(2) 0.034(2) -0.0067(19) 0.006(2) -0.021(2) C30 0.036(2) 0.0256(18) 0.0205(18) -0.0001(14) -0.0020(15) -0.0209(16) C35 0.047(2) 0.047(2) 0.029(2) -0.0026(18) -0.0091(19) -0.026(2) C14 0.0189(17) 0.0196(17) 0.0178(17) -0.0042(13) 0.0047(14) -0.0091(14) C13 0.0189(17) 0.0230(18) 0.0153(17) -0.0044(13) 0.0008(14) -0.0105(14) C24 0.062(3) 0.042(2) 0.034(2) 0.0050(19) -0.001(2) -0.028(2) C25 0.100(4) 0.070(3) 0.031(3) 0.007(2) 0.005(3) -0.053(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 1.950(3) 2 ? Fe1 N1 1.950(3) . ? Fe1 N2 1.987(3) 2 ? Fe1 N2 1.987(3) . ? Fe1 N4 1.989(3) 2 ? Fe1 N4 1.989(3) . ? N9 C13 1.345(4) . ? N9 C29 1.459(4) . ? N9 C36 1.465(4) . ? N10 C1 1.306(4) . ? N10 C43 1.307(4) . ? N11 C43 1.136(4) . ? C10 C11 1.356(5) . ? C10 C9 1.387(5) . ? C10 H10 0.9500 . ? N1 C1 1.148(4) . ? C16 C21 1.381(5) . ? C16 C17 1.382(5) . ? C16 C15 1.518(5) . ? C8 C9 1.369(5) . ? C8 C7 1.387(5) . ? C8 H8 0.9500 . ? N5 C12 1.331(4) . ? N5 C14 1.354(4) . ? C11 N4 1.356(4) . ? C11 H11 0.9500 . ? N8 C14 1.351(4) . ? N8 C15 1.456(4) . ? N8 C22 1.478(4) . ? C39 C40 1.379(5) . ? C39 C38 1.382(5) . ? C39 H39 0.9500 . ? C3 C2 1.367(4) . ? C3 C4 1.383(5) . ? C3 H3 0.9500 . ? C38 C37 1.380(5) . ? C38 H38 0.9500 . ? C2 N2 1.362(4) . ? C2 H2 0.9500 . ? N4 C7 1.339(4) . ? C36 C37 1.500(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N2 C6 1.333(4) . ? C5 C4 1.374(5) . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C37 C42 1.399(4) . ? C28 C23 1.374(5) . ? C28 C27 1.376(5) . ? C28 H28 0.9500 . ? C42 C41 1.381(5) . ? C42 H42 0.9500 . ? C33 C34 1.375(6) . ? C33 C32 1.386(5) . ? C33 H33 0.9500 . ? C19 C18 1.373(5) . ? C19 C20 1.377(5) . ? C19 H19 0.9500 . ? C23 C24 1.390(5) . ? C23 C22 1.516(5) . ? C41 C40 1.381(5) . ? C41 H41 0.9500 . ? N6 C12 1.319(4) . ? N6 C13 1.357(4) . ? C21 C20 1.379(5) . ? C21 H21 0.9500 . ? C18 C17 1.387(5) . ? C18 H18 0.9500 . ? N7 C13 1.338(4) . ? N7 C14 1.344(4) . ? C9 H9 0.9500 . ? C4 H4 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C40 H40 0.9500 . ? C29 C30 1.514(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C34 C35 1.371(5) . ? C34 H34 0.9500 . ? C17 H17 0.9500 . ? C12 N3 1.396(4) . ? C20 H20 0.9500 . ? C27 C26 1.363(6) . ? C27 H27 0.9500 . ? C6 N3 1.422(4) . ? C7 N3 1.415(4) . ? C31 C32 1.387(5) . ? C31 C30 1.389(5) . ? C31 H31 0.9500 . ? C26 C25 1.395(6) . ? C26 H26 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C32 H32 0.9500 . ? C30 C35 1.387(5) . ? C35 H35 0.9500 . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? O1A C44B 1.278(10) . ? C44A C45A 1.560(15) . ? O1C C44C 1.28(2) . ? C45C C44C 1.39(2) . ? 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(12) 2 . ? N1 Fe1 N2 91.51(10) 2 2 ? N1 Fe1 N2 88.49(10) . 2 ? N1 Fe1 N2 88.49(10) 2 . ? N1 Fe1 N2 91.51(10) . . ? N2 Fe1 N2 180.0(2) 2 . ? N1 Fe1 N4 91.63(11) 2 2 ? N1 Fe1 N4 88.37(11) . 2 ? N2 Fe1 N4 86.67(11) 2 2 ? N2 Fe1 N4 93.33(11) . 2 ? N1 Fe1 N4 88.37(11) 2 . ? N1 Fe1 N4 91.63(11) . . ? N2 Fe1 N4 93.33(11) 2 . ? N2 Fe1 N4 86.67(11) . . ? N4 Fe1 N4 180.00(19) 2 . ? C13 N9 C29 121.6(3) . . ? C13 N9 C36 121.6(3) . . ? C29 N9 C36 116.5(3) . . ? C1 N10 C43 125.1(3) . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C1 N1 Fe1 177.4(3) . . ? C21 C16 C17 118.2(3) . . ? C21 C16 C15 123.3(3) . . ? C17 C16 C15 118.5(3) . . ? C9 C8 C7 119.1(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C12 N5 C14 112.8(3) . . ? N4 C11 C10 123.3(3) . . ? N4 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C14 N8 C15 119.8(3) . . ? C14 N8 C22 120.2(3) . . ? C15 N8 C22 119.4(3) . . ? C40 C39 C38 119.8(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? N11 C43 N10 172.2(4) . . ? C2 C3 C4 118.7(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C37 C38 C39 121.3(3) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? N2 C2 C3 123.0(3) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C7 N4 C11 116.8(3) . . ? C7 N4 Fe1 122.2(2) . . ? C11 N4 Fe1 121.0(2) . . ? N9 C36 C37 113.9(3) . . ? N9 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? N9 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C6 N2 C2 117.3(3) . . ? C6 N2 Fe1 122.2(2) . . ? C2 N2 Fe1 120.5(2) . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C38 C37 C42 118.7(3) . . ? C38 C37 C36 120.2(3) . . ? C42 C37 C36 121.1(3) . . ? C23 C28 C27 121.0(4) . . ? C23 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C41 C42 C37 120.0(3) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C34 C33 C32 119.6(4) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C28 C23 C24 118.8(4) . . ? C28 C23 C22 121.2(3) . . ? C24 C23 C22 119.9(3) . . ? C40 C41 C42 120.6(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C12 N6 C13 113.3(3) . . ? C20 C21 C16 120.6(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C13 N7 C14 114.6(3) . . ? C8 C9 C10 118.4(3) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C1 N10 171.0(4) . . ? N8 C15 C16 116.1(3) . . ? N8 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N8 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C39 C40 C41 119.7(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? N9 C29 C30 114.5(3) . . ? N9 C29 H29A 108.6 . . ? C30 C29 H29A 108.6 . . ? N9 C29 H29B 108.6 . . ? C30 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C16 C17 C18 121.3(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? N6 C12 N5 128.4(3) . . ? N6 C12 N3 115.5(3) . . ? N5 C12 N3 116.1(3) . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? N2 C6 C5 122.9(3) . . ? N2 C6 N3 117.0(3) . . ? C5 C6 N3 120.1(3) . . ? N4 C7 C8 122.9(3) . . ? N4 C7 N3 116.8(3) . . ? C8 C7 N3 120.2(3) . . ? C12 N3 C7 122.2(2) . . ? C12 N3 C6 119.4(3) . . ? C7 N3 C6 118.2(2) . . ? C32 C31 C30 120.9(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C27 C26 C25 120.6(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N8 C22 C23 112.9(3) . . ? N8 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N8 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C33 C32 C31 119.8(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C35 C30 C31 117.9(3) . . ? C35 C30 C29 119.8(3) . . ? C31 C30 C29 122.3(3) . . ? C34 C35 C30 121.4(4) . . ? C34 C35 H35 119.3 . . ? C30 C35 H35 119.3 . . ? N7 C14 N8 117.9(3) . . ? N7 C14 N5 125.6(3) . . ? N8 C14 N5 116.5(3) . . ? N7 C13 N9 118.3(3) . . ? N7 C13 N6 125.3(3) . . ? N9 C13 N6 116.4(3) . . ? C25 C24 C23 120.8(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 118.6(3) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? O1C C44C C45C 131.0(18) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.535 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.064 #=END data_4 _database_code_depnum_ccdc_archive 'CCDC 836946' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCSe)2(DDB)2].2CH3OH ; _chemical_name_common trans-[Fe(II)(NCSe)2(DDB)2].2CH3OH _chemical_melting_point ? _chemical_formula_moiety '(C60 H88 Fe N18 Se2), 2(C H4 O)' _chemical_formula_sum 'C62 H96 Fe N18 O2 Se2' _chemical_formula_weight 1339.34 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' _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 8.4438(2) _cell_length_b 10.2305(3) _cell_length_c 20.6112(7) _cell_angle_alpha 94.4410(10) _cell_angle_beta 93.2030(10) _cell_angle_gamma 109.6780(10) _cell_volume 1665.09(8) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 14922 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'block ' _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.375 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.9344 _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 14922 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7481 _reflns_number_gt 5715 _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 7481 _refine_ls_number_parameters 424 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.014 _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 Se1 Se -0.05609(3) 0.27015(3) 0.198006(13) 0.02414(9) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.0000 0.01074(11) Uani 1 2 d S . . N4 N 0.2499(2) 0.07884(18) 0.01162(9) 0.0118(4) Uani 1 1 d . . . N2 N 0.0186(2) -0.15492(18) 0.04845(9) 0.0119(4) Uani 1 1 d . . . N1 N -0.0171(2) 0.1060(2) 0.07973(10) 0.0148(4) Uani 1 1 d . . . N8 N 0.0930(3) -0.0017(2) 0.32937(10) 0.0193(5) Uani 1 1 d . . . N7 N 0.3728(2) 0.19814(19) 0.19137(10) 0.0146(4) Uani 1 1 d . . . C5 C 0.1429(3) -0.2410(2) 0.13507(13) 0.0173(5) Uani 1 1 d . . . H5 H 0.2241 -0.2219 0.1715 0.021 Uiso 1 1 calc R . . N3 N 0.2429(2) 0.00488(19) 0.11736(10) 0.0122(4) Uani 1 1 d . . . N6 N 0.3030(2) 0.1903(2) 0.30206(10) 0.0175(4) Uani 1 1 d . . . C8 C 0.5127(3) 0.1318(2) 0.07689(12) 0.0152(5) Uani 1 1 d . . . H8 H 0.5704 0.1274 0.1171 0.018 Uiso 1 1 calc R . . N5 N 0.1682(2) -0.0058(2) 0.22330(10) 0.0159(4) Uani 1 1 d . . . C7 C 0.3368(3) 0.0759(2) 0.06759(12) 0.0129(5) Uani 1 1 d . . . C2 C -0.0803(3) -0.2886(2) 0.02886(12) 0.0157(5) Uani 1 1 d . . . H2 H -0.1558 -0.3065 -0.0093 0.019 Uiso 1 1 calc R . . C6 C 0.1301(3) -0.1336(2) 0.10047(12) 0.0127(5) Uani 1 1 d . . . C11 C 0.3400(3) 0.1355(2) -0.03788(12) 0.0157(5) Uani 1 1 d . . . H11 H 0.2808 0.1345 -0.0786 0.019 Uiso 1 1 calc R . . C12 C 0.2627(3) 0.0690(2) 0.18110(12) 0.0142(5) Uani 1 1 d . A . C1 C -0.0315(3) 0.1714(2) 0.12554(12) 0.0139(5) Uani 1 1 d . . . C4 C 0.0371(3) -0.3756(3) 0.11623(13) 0.0202(5) Uani 1 1 d . . . H4 H 0.0417 -0.4503 0.1400 0.024 Uiso 1 1 calc R . . C10 C 0.5126(3) 0.1942(2) -0.03192(13) 0.0171(5) Uani 1 1 d . . . H10 H 0.5710 0.2350 -0.0674 0.021 Uiso 1 1 calc R . . C3 C -0.0761(3) -0.3994(2) 0.06171(13) 0.0189(5) Uani 1 1 d . . . H3 H -0.1500 -0.4912 0.0472 0.023 Uiso 1 1 calc R . . C9 C 0.6005(3) 0.1931(2) 0.02677(12) 0.0164(5) Uani 1 1 d . . . H9 H 0.7201 0.2342 0.0322 0.020 Uiso 1 1 calc R . . C14 C 0.3912(3) 0.2520(2) 0.25423(12) 0.0151(5) Uani 1 1 d . A . C19 C 0.1021(3) 0.0747(3) 0.39330(13) 0.0249(6) Uani 1 1 d . A . H19A H -0.0075 0.0351 0.4120 0.030 Uiso 1 1 calc R . . H19B H 0.1180 0.1731 0.3869 0.030 Uiso 1 1 calc R . . C13 C 0.1905(3) 0.0632(2) 0.28338(12) 0.0165(5) Uani 1 1 d . A . N9 N 0.5126(2) 0.3790(2) 0.27091(10) 0.0167(4) Uani 1 1 d . . . C23 C 0.5623(3) 0.4261(3) 0.33990(12) 0.0198(5) Uani 1 1 d . A . H23A H 0.4599 0.4079 0.3639 0.024 Uiso 1 1 calc R . . H23B H 0.6238 0.5280 0.3450 0.024 Uiso 1 1 calc R . . C27 C 0.6289(3) 0.4499(2) 0.22456(12) 0.0178(5) Uani 1 1 d . A . H27A H 0.6097 0.3874 0.1836 0.021 Uiso 1 1 calc R . . H27B H 0.7463 0.4690 0.2429 0.021 Uiso 1 1 calc R . . C24 C 0.6745(3) 0.3521(3) 0.36927(13) 0.0223(6) Uani 1 1 d . . . H24A H 0.6107 0.2506 0.3654 0.027 Uiso 1 1 calc R A . H24B H 0.7736 0.3667 0.3436 0.027 Uiso 1 1 calc R . . C20 C 0.2419(4) 0.0722(3) 0.44256(14) 0.0300(6) Uani 1 1 d . . . H20A H 0.2158 -0.0235 0.4555 0.036 Uiso 1 1 calc R A . H20B H 0.3496 0.0970 0.4218 0.036 Uiso 1 1 calc R . . C21 C 0.2624(4) 0.1730(3) 0.50307(14) 0.0372(7) Uani 1 1 d . A . H21A H 0.2985 0.2694 0.4904 0.045 Uiso 1 1 calc R . . H21B H 0.1517 0.1537 0.5213 0.045 Uiso 1 1 calc R . . C25 C 0.7361(3) 0.4018(3) 0.44051(14) 0.0283(6) Uani 1 1 d . A . H25A H 0.7990 0.5035 0.4449 0.034 Uiso 1 1 calc R . . H25B H 0.6377 0.3852 0.4667 0.034 Uiso 1 1 calc R . . C28 C 0.6079(3) 0.5865(2) 0.20911(13) 0.0200(5) Uani 1 1 d . . . H28A H 0.6198 0.6462 0.2506 0.024 Uiso 1 1 calc R A . H28B H 0.6999 0.6358 0.1827 0.024 Uiso 1 1 calc R . . C29 C 0.4394(3) 0.5687(3) 0.17234(13) 0.0237(6) Uani 1 1 d . A . H29A H 0.3472 0.5168 0.1981 0.028 Uiso 1 1 calc R . . H29B H 0.4308 0.6621 0.1686 0.028 Uiso 1 1 calc R . . C30 C 0.4143(4) 0.4922(3) 0.10453(14) 0.0296(7) Uani 1 1 d . . . H30A H 0.5123 0.5358 0.0805 0.044 Uiso 1 1 calc R A . H30B H 0.3124 0.4971 0.0812 0.044 Uiso 1 1 calc R . . H30C H 0.4019 0.3944 0.1080 0.044 Uiso 1 1 calc R . . C26 C 0.8497(4) 0.3271(3) 0.46703(16) 0.0405(8) Uani 1 1 d . . . H26A H 0.7883 0.2263 0.4623 0.061 Uiso 1 1 calc R A . H26B H 0.8842 0.3597 0.5133 0.061 Uiso 1 1 calc R . . H26C H 0.9501 0.3472 0.4426 0.061 Uiso 1 1 calc R . . C22 C 0.3900(4) 0.1632(4) 0.55556(16) 0.0499(9) Uani 1 1 d . . . H22A H 0.3503 0.0703 0.5710 0.075 Uiso 1 1 calc R A . H22B H 0.4030 0.2341 0.5922 0.075 Uiso 1 1 calc R . . H22C H 0.4990 0.1787 0.5375 0.075 Uiso 1 1 calc R . . O1 O 0.6436(4) 0.9458(3) 0.20245(13) 0.0692(9) Uani 1 1 d U . . H1 H 0.7252 1.0167 0.1961 0.083 Uiso 1 1 calc R . . C31 C 0.5998(4) 0.9604(4) 0.26515(19) 0.0491(9) Uani 1 1 d . . . H31A H 0.7021 0.9971 0.2953 0.074 Uiso 1 1 calc R . . H31B H 0.5292 0.8693 0.2770 0.074 Uiso 1 1 calc R . . H31C H 0.5367 1.0251 0.2678 0.074 Uiso 1 1 calc R . . C15A C -0.0370(9) -0.1453(11) 0.3128(5) 0.0207(16) Uani 0.60 1 d P A 1 H15A H -0.0531 -0.1672 0.2647 0.025 Uiso 0.60 1 calc PR A 1 H15B H -0.1461 -0.1452 0.3280 0.025 Uiso 0.60 1 calc PR A 1 C16A C 0.0121(5) -0.2593(4) 0.3435(2) 0.0211(9) Uani 0.60 1 d P A 1 H16A H 0.0378 -0.2329 0.3911 0.025 Uiso 0.60 1 calc PR A 1 H16B H -0.0856 -0.3474 0.3368 0.025 Uiso 0.60 1 calc PR A 1 C15B C 0.0174(14) -0.1475(18) 0.3240(7) 0.022(3) Uani 0.40 1 d P A 2 H15C H -0.0436 -0.1800 0.2802 0.027 Uiso 0.40 1 calc PR A 2 H15D H -0.0666 -0.1730 0.3567 0.027 Uiso 0.40 1 calc PR A 2 C17A C 0.1621(8) -0.2845(7) 0.3159(3) 0.0381(15) Uani 0.60 1 d P A 1 H17A H 0.2623 -0.1989 0.3262 0.046 Uiso 0.60 1 calc PR A 1 H17B H 0.1407 -0.3020 0.2677 0.046 Uiso 0.60 1 calc PR A 1 C17B C 0.0756(10) -0.3785(8) 0.3224(4) 0.0307(17) Uani 0.40 1 d P A 2 H17C H -0.0204 -0.4136 0.3494 0.037 Uiso 0.40 1 calc PR A 2 H17D H 0.0314 -0.4049 0.2760 0.037 Uiso 0.40 1 calc PR A 2 C16B C 0.1460(10) -0.2236(8) 0.3346(4) 0.0225(16) Uani 0.40 1 d P A 2 H16C H 0.2371 -0.1888 0.3054 0.027 Uiso 0.40 1 calc PR A 2 H16D H 0.1978 -0.1980 0.3801 0.027 Uiso 0.40 1 calc PR A 2 C18A C 0.2021(12) -0.4074(10) 0.3418(4) 0.0389(19) Uani 0.60 1 d P A 1 H18A H 0.2271 -0.3898 0.3893 0.058 Uiso 0.60 1 calc PR A 1 H18B H 0.3002 -0.4177 0.3216 0.058 Uiso 0.60 1 calc PR A 1 H18C H 0.1046 -0.4932 0.3310 0.058 Uiso 0.60 1 calc PR A 1 C18B C 0.200(2) -0.4464(15) 0.3373(9) 0.038(4) Uiso 0.40 1 d P A 2 H18D H 0.2923 -0.4159 0.3092 0.057 Uiso 0.40 1 calc PR A 2 H18E H 0.1450 -0.5479 0.3295 0.057 Uiso 0.40 1 calc PR A 2 H18F H 0.2443 -0.4206 0.3832 0.057 Uiso 0.40 1 calc PR 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 Se1 0.03117(16) 0.02322(15) 0.02003(15) -0.00451(11) 0.00372(11) 0.01314(12) Fe1 0.0099(2) 0.0102(2) 0.0117(2) 0.00055(18) 0.00015(18) 0.00319(18) N4 0.0113(9) 0.0106(9) 0.0139(10) 0.0013(8) 0.0003(8) 0.0044(8) N2 0.0106(9) 0.0100(9) 0.0148(10) 0.0004(8) 0.0024(8) 0.0032(8) N1 0.0129(10) 0.0163(10) 0.0161(11) 0.0019(9) -0.0004(8) 0.0063(8) N8 0.0203(11) 0.0199(11) 0.0158(11) 0.0019(9) 0.0036(9) 0.0040(9) N7 0.0135(10) 0.0136(10) 0.0161(11) 0.0022(8) -0.0013(8) 0.0044(8) C5 0.0182(12) 0.0171(12) 0.0200(13) 0.0037(10) 0.0028(10) 0.0101(10) N3 0.0102(9) 0.0117(9) 0.0137(10) 0.0023(8) 0.0001(8) 0.0023(8) N6 0.0176(10) 0.0196(11) 0.0142(11) 0.0011(9) -0.0009(9) 0.0053(9) C8 0.0139(11) 0.0125(11) 0.0191(13) -0.0003(10) -0.0007(10) 0.0052(9) N5 0.0147(10) 0.0166(10) 0.0165(11) 0.0024(8) 0.0024(8) 0.0050(8) C7 0.0135(11) 0.0069(10) 0.0174(12) -0.0017(9) 0.0010(10) 0.0029(9) C2 0.0117(11) 0.0150(12) 0.0182(13) -0.0004(10) 0.0006(10) 0.0020(9) C6 0.0116(11) 0.0123(11) 0.0144(12) 0.0009(9) 0.0030(9) 0.0044(9) C11 0.0189(12) 0.0131(12) 0.0177(13) 0.0030(10) 0.0046(10) 0.0080(10) C12 0.0129(11) 0.0148(12) 0.0168(12) 0.0014(10) -0.0035(10) 0.0080(10) C1 0.0121(11) 0.0134(11) 0.0169(13) 0.0033(10) 0.0006(10) 0.0049(9) C4 0.0227(13) 0.0154(12) 0.0260(15) 0.0062(11) 0.0065(11) 0.0097(11) C10 0.0172(12) 0.0118(11) 0.0238(14) 0.0058(10) 0.0083(10) 0.0051(10) C3 0.0181(12) 0.0108(12) 0.0275(15) 0.0018(10) 0.0049(11) 0.0040(10) C9 0.0129(11) 0.0118(11) 0.0247(14) -0.0002(10) 0.0017(10) 0.0049(9) C14 0.0138(11) 0.0155(12) 0.0167(13) 0.0019(10) -0.0031(10) 0.0066(10) C19 0.0261(14) 0.0273(14) 0.0197(14) 0.0020(11) 0.0095(11) 0.0059(12) C13 0.0147(12) 0.0192(13) 0.0165(13) 0.0046(10) 0.0002(10) 0.0068(10) N9 0.0162(10) 0.0160(10) 0.0157(11) -0.0002(8) -0.0017(8) 0.0035(8) C23 0.0203(13) 0.0164(12) 0.0186(13) -0.0042(10) -0.0037(11) 0.0032(10) C27 0.0151(12) 0.0171(12) 0.0202(13) 0.0005(10) -0.0018(10) 0.0049(10) C24 0.0224(13) 0.0219(13) 0.0196(14) 0.0000(11) -0.0032(11) 0.0051(11) C20 0.0359(16) 0.0293(15) 0.0205(15) 0.0037(12) 0.0017(13) 0.0055(13) C21 0.0384(18) 0.0411(18) 0.0199(15) -0.0009(13) 0.0056(13) -0.0018(14) C25 0.0263(15) 0.0320(15) 0.0223(15) 0.0015(12) -0.0041(12) 0.0055(12) C28 0.0196(13) 0.0153(12) 0.0217(14) 0.0000(11) -0.0001(11) 0.0022(10) C29 0.0245(14) 0.0216(13) 0.0258(15) 0.0050(11) -0.0021(12) 0.0090(11) C30 0.0391(17) 0.0187(14) 0.0293(16) 0.0025(12) -0.0099(13) 0.0097(12) C26 0.0417(18) 0.0455(19) 0.0311(18) 0.0070(15) -0.0130(15) 0.0128(15) C22 0.051(2) 0.057(2) 0.0231(17) -0.0009(16) -0.0035(16) -0.0035(17) O1 0.099(2) 0.0396(14) 0.0407(16) 0.0047(12) 0.0080(15) -0.0132(14) C31 0.045(2) 0.046(2) 0.058(3) 0.0060(18) 0.0138(18) 0.0161(17) C15A 0.018(4) 0.020(3) 0.016(4) 0.003(3) -0.003(3) -0.004(3) C16A 0.017(2) 0.023(2) 0.016(2) 0.0027(18) 0.0011(18) -0.0016(18) C15B 0.017(6) 0.030(5) 0.009(5) 0.000(4) -0.006(4) -0.004(5) C17A 0.042(3) 0.038(4) 0.047(4) 0.021(3) 0.020(3) 0.023(3) C17B 0.036(4) 0.022(4) 0.028(4) 0.005(3) 0.001(3) 0.002(4) C16B 0.023(4) 0.019(4) 0.023(4) 0.005(3) -0.003(3) 0.004(3) C18A 0.047(4) 0.041(6) 0.030(4) -0.003(4) -0.002(3) 0.019(4) _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 Se1 C1 1.799(2) . ? Fe1 N1 1.938(2) . ? Fe1 N1 1.938(2) 2 ? Fe1 N4 1.9820(18) . ? Fe1 N4 1.9820(18) 2 ? Fe1 N2 1.9822(18) . ? Fe1 N2 1.9822(18) 2 ? N4 C7 1.340(3) . ? N4 C11 1.355(3) . ? N2 C6 1.340(3) . ? N2 C2 1.356(3) . ? N1 C1 1.150(3) . ? N8 C13 1.354(3) . ? N8 C15B 1.404(17) . ? N8 C19 1.464(3) . ? N8 C15A 1.508(10) . ? N7 C12 1.328(3) . ? N7 C14 1.347(3) . ? C5 C4 1.376(3) . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? N3 C12 1.397(3) . ? N3 C6 1.419(3) . ? N3 C7 1.424(3) . ? N6 C14 1.337(3) . ? N6 C13 1.339(3) . ? C8 C9 1.373(3) . ? C8 C7 1.396(3) . ? C8 H8 0.9500 . ? N5 C12 1.322(3) . ? N5 C13 1.348(3) . ? C2 C3 1.374(3) . ? C2 H2 0.9500 . ? C11 C10 1.370(3) . ? C11 H11 0.9500 . ? C4 C3 1.384(4) . ? C4 H4 0.9500 . ? C10 C9 1.386(3) . ? C10 H10 0.9500 . ? C3 H3 0.9500 . ? C9 H9 0.9500 . ? C14 N9 1.361(3) . ? C19 C20 1.522(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N9 C23 1.457(3) . ? N9 C27 1.462(3) . ? C23 C24 1.525(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C27 C28 1.522(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C24 C25 1.519(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C20 C21 1.518(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.517(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C25 C26 1.518(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C28 C29 1.521(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.515(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O1 C31 1.375(4) . ? O1 H1 0.8400 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C15A C16A 1.531(10) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.507(7) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C15B C16B 1.550(14) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C17A C18A 1.533(10) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C17B C18B 1.470(16) . ? C17B C16B 1.488(10) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 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 N1 Fe1 N1 180.00(13) . 2 ? N1 Fe1 N4 91.23(8) . . ? N1 Fe1 N4 88.77(8) 2 . ? N1 Fe1 N4 88.77(8) . 2 ? N1 Fe1 N4 91.23(8) 2 2 ? N4 Fe1 N4 180.00(4) . 2 ? N1 Fe1 N2 91.85(8) . . ? N1 Fe1 N2 88.15(8) 2 . ? N4 Fe1 N2 86.74(7) . . ? N4 Fe1 N2 93.26(7) 2 . ? N1 Fe1 N2 88.15(8) . 2 ? N1 Fe1 N2 91.85(8) 2 2 ? N4 Fe1 N2 93.26(7) . 2 ? N4 Fe1 N2 86.74(7) 2 2 ? N2 Fe1 N2 180.00(14) . 2 ? C7 N4 C11 117.31(19) . . ? C7 N4 Fe1 121.94(15) . . ? C11 N4 Fe1 120.74(16) . . ? C6 N2 C2 117.21(19) . . ? C6 N2 Fe1 122.22(15) . . ? C2 N2 Fe1 120.55(16) . . ? C1 N1 Fe1 177.08(19) . . ? C13 N8 C15B 121.3(6) . . ? C13 N8 C19 119.3(2) . . ? C15B N8 C19 117.4(6) . . ? C13 N8 C15A 120.5(4) . . ? C15B N8 C15A 19.8(5) . . ? C19 N8 C15A 120.0(4) . . ? C12 N7 C14 112.8(2) . . ? C4 C5 C6 119.5(2) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C12 N3 C6 120.98(19) . . ? C12 N3 C7 121.01(18) . . ? C6 N3 C7 118.01(19) . . ? C14 N6 C13 114.3(2) . . ? C9 C8 C7 118.7(2) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C12 N5 C13 113.0(2) . . ? N4 C7 C8 122.8(2) . . ? N4 C7 N3 117.20(19) . . ? C8 C7 N3 119.9(2) . . ? N2 C2 C3 123.0(2) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? N2 C6 C5 122.7(2) . . ? N2 C6 N3 116.94(19) . . ? C5 C6 N3 120.3(2) . . ? N4 C11 C10 123.0(2) . . ? N4 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? N5 C12 N7 128.2(2) . . ? N5 C12 N3 116.0(2) . . ? N7 C12 N3 115.7(2) . . ? N1 C1 Se1 178.8(2) . . ? C5 C4 C3 118.4(2) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C11 C10 C9 118.9(2) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C2 C3 C4 119.2(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C8 C9 C10 119.1(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N6 C14 N7 125.7(2) . . ? N6 C14 N9 117.0(2) . . ? N7 C14 N9 117.3(2) . . ? N8 C19 C20 115.2(2) . . ? N8 C19 H19A 108.5 . . ? C20 C19 H19A 108.5 . . ? N8 C19 H19B 108.5 . . ? C20 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? N6 C13 N5 125.6(2) . . ? N6 C13 N8 116.7(2) . . ? N5 C13 N8 117.7(2) . . ? C14 N9 C23 118.6(2) . . ? C14 N9 C27 122.0(2) . . ? C23 N9 C27 116.75(19) . . ? N9 C23 C24 111.6(2) . . ? N9 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N9 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? N9 C27 C28 112.6(2) . . ? N9 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N9 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C25 C24 C23 113.8(2) . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C21 C20 C19 112.0(2) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 113.1(3) . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C26 C25 C24 111.7(2) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C29 C28 C27 114.0(2) . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28B 108.7 . . ? C27 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C28 113.8(2) . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C28 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 O1 H1 109.5 . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C15A C16A 113.1(4) . . ? N8 C15A H15A 109.0 . . ? C16A C15A H15A 109.0 . . ? N8 C15A H15B 109.0 . . ? C16A C15A H15B 109.0 . . ? H15A C15A H15B 107.8 . . ? C17A C16A C15A 113.8(5) . . ? C17A C16A H16A 108.8 . . ? C15A C16A H16A 108.8 . . ? C17A C16A H16B 108.8 . . ? C15A C16A H16B 108.8 . . ? H16A C16A H16B 107.7 . . ? N8 C15B C16B 113.1(8) . . ? N8 C15B H15C 109.0 . . ? C16B C15B H15C 109.0 . . ? N8 C15B H15D 109.0 . . ? C16B C15B H15D 109.0 . . ? H15C C15B H15D 107.8 . . ? C16A C17A C18A 114.1(6) . . ? C16A C17A H17A 108.7 . . ? C18A C17A H17A 108.7 . . ? C16A C17A H17B 108.7 . . ? C18A C17A H17B 108.7 . . ? H17A C17A H17B 107.6 . . ? C18B C17B C16B 113.4(9) . . ? C18B C17B H17C 108.9 . . ? C16B C17B H17C 108.9 . . ? C18B C17B H17D 108.9 . . ? C16B C17B H17D 108.9 . . ? H17C C17B H17D 107.7 . . ? C17B C16B C15B 115.5(8) . . ? C17B C16B H16C 108.4 . . ? C15B C16B H16C 108.4 . . ? C17B C16B H16D 108.4 . . ? C15B C16B H16D 108.4 . . ? H16C C16B H16D 107.5 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.478 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.075 #=END data_5 _database_code_depnum_ccdc_archive 'CCDC 836947' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-[Fe(II)(NCS)2(DDB)2] ; _chemical_name_common cis-[Fe(II)(NCS)2(DDB)2] _chemical_melting_point ? _chemical_formula_moiety '(C60 H88 Fe N18 S2)' _chemical_formula_sum 'C60 H88 Fe N18 S2' _chemical_formula_weight 1181.45 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.614(2) _cell_length_b 14.244(2) _cell_length_c 17.453(2) _cell_angle_alpha 106.404(2) _cell_angle_beta 92.340(10) _cell_angle_gamma 95.281(9) _cell_volume 3225.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36919 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 26.55 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9827 _exptl_absorpt_correction_T_max 0.9827 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77371 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _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 36919 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.55 _reflns_number_total 9473 _reflns_number_gt 7724 _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^)+(0.0848P)^2^+3.3312P] 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 SHELXL _refine_ls_extinction_coef 0.0246(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9473 _refine_ls_number_parameters 759 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _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 0.05981(3) 0.72321(3) 0.23334(2) 0.01586(15) Uani 1 1 d . . . C32 C 0.2720(2) 0.6695(2) 0.41308(17) 0.0183(7) Uani 1 1 d . . . H32 H 0.2736 0.6201 0.4399 0.022 Uiso 1 1 calc R . . N12 N 0.06552(17) 0.88412(19) 0.29565(16) 0.0201(6) Uani 1 1 d . . . N15 N 0.26234(17) 1.00478(18) 0.23674(15) 0.0175(6) Uani 1 1 d . . . N10 N 0.18299(17) 0.74368(18) 0.32783(14) 0.0148(5) Uani 1 1 d . . . N14 N 0.41493(18) 1.02034(18) 0.17405(15) 0.0177(6) Uani 1 1 d . . . C37 C 0.1515(2) 1.0262(2) 0.3916(2) 0.0239(7) Uani 1 1 d . . . H37 H 0.2127 1.0613 0.4162 0.029 Uiso 1 1 calc R . . N11 N 0.24061(17) 0.89595(18) 0.31054(15) 0.0154(5) Uani 1 1 d . . . C31 C 0.1898(2) 0.6736(2) 0.36586(18) 0.0184(7) Uani 1 1 d . . . H31 H 0.1352 0.6249 0.3597 0.022 Uiso 1 1 calc R . . C41 C 0.3037(2) 0.9391(2) 0.26575(18) 0.0155(6) Uani 1 1 d . . . C38 C 0.0634(3) 1.0628(3) 0.4143(2) 0.0315(8) Uani 1 1 d . . . H38 H 0.0627 1.1235 0.4547 0.038 Uiso 1 1 calc R . . N17 N 0.28585(18) 1.10861(19) 0.15674(15) 0.0196(6) Uani 1 1 d . . . C35 C 0.2589(2) 0.8145(2) 0.34000(17) 0.0152(6) Uani 1 1 d . . . N13 N 0.39379(18) 0.91025(18) 0.25635(15) 0.0166(5) Uani 1 1 d . . . C33 C 0.3524(2) 0.7396(2) 0.42041(18) 0.0208(7) Uani 1 1 d . . . H33 H 0.4115 0.7361 0.4498 0.025 Uiso 1 1 calc R . . C34 C 0.3464(2) 0.8147(2) 0.38477(18) 0.0190(7) Uani 1 1 d . . . H34 H 0.4000 0.8645 0.3906 0.023 Uiso 1 1 calc R . . C43 C 0.3221(2) 1.0426(2) 0.19023(17) 0.0159(6) Uani 1 1 d . . . C36 C 0.1492(2) 0.9372(2) 0.33203(18) 0.0187(7) Uani 1 1 d . . . N6 N 0.38040(18) 0.46547(18) 0.32749(15) 0.0179(6) Uani 1 1 d . . . N7 N 0.37099(17) 0.56780(18) 0.23910(15) 0.0164(5) Uani 1 1 d . . . N5 N 0.22788(17) 0.46322(18) 0.25262(14) 0.0160(5) Uani 1 1 d . . . C14 C 0.4203(2) 0.5321(2) 0.29294(17) 0.0157(6) Uani 1 1 d . . . C42 C 0.4460(2) 0.9534(2) 0.20843(17) 0.0162(6) Uani 1 1 d . . . C12 C 0.2773(2) 0.5295(2) 0.22358(17) 0.0160(6) Uani 1 1 d . . . N16 N 0.53874(18) 0.92880(18) 0.19205(16) 0.0194(6) Uani 1 1 d . . . C40 C -0.0203(2) 0.9213(3) 0.3186(2) 0.0303(8) Uani 1 1 d . . . H40 H -0.0807 0.8850 0.2931 0.036 Uiso 1 1 calc R . . C39 C -0.0243(3) 1.0087(3) 0.3766(2) 0.0350(9) Uani 1 1 d . . . H39 H -0.0862 1.0319 0.3909 0.042 Uiso 1 1 calc R . . C13 C 0.2838(2) 0.4359(2) 0.30709(18) 0.0175(7) Uani 1 1 d . . . N8 N 0.23870(18) 0.37531(19) 0.34555(15) 0.0195(6) Uani 1 1 d . . . N4 N 0.18135(18) 0.71275(18) 0.14959(14) 0.0177(6) Uani 1 1 d . . . C54 C 0.4787(2) 1.2921(3) 0.1040(2) 0.0263(7) Uani 1 1 d . . . H54A H 0.5304 1.3398 0.1395 0.032 Uiso 1 1 calc R . . H54B H 0.5124 1.2409 0.0669 0.032 Uiso 1 1 calc R . . C27 C 0.5660(2) 0.6483(2) 0.2902(2) 0.0219(7) Uani 1 1 d . . . H27A H 0.5959 0.6989 0.3390 0.026 Uiso 1 1 calc R . . H27B H 0.5159 0.6785 0.2649 0.026 Uiso 1 1 calc R . . N9 N 0.51636(18) 0.56567(18) 0.31364(15) 0.0184(6) Uani 1 1 d . . . C48 C 0.5925(2) 0.9658(2) 0.13342(19) 0.0204(7) Uani 1 1 d . . . H48A H 0.5454 0.9636 0.0880 0.025 Uiso 1 1 calc R . . H48B H 0.6429 0.9211 0.1123 0.025 Uiso 1 1 calc R . . N2 N 0.04439(17) 0.56300(19) 0.17218(15) 0.0191(6) Uani 1 1 d . . . C44 C 0.5847(2) 0.8574(2) 0.2248(2) 0.0257(8) Uani 1 1 d . B . H44A H 0.6002 0.8017 0.1799 0.031 Uiso 1 1 calc R . . H44B H 0.5368 0.8309 0.2567 0.031 Uiso 1 1 calc R . . C53 C 0.4142(2) 1.2435(2) 0.15524(19) 0.0213(7) Uani 1 1 d . . . H53A H 0.4577 1.2233 0.1933 0.026 Uiso 1 1 calc R . . H53B H 0.3735 1.2926 0.1870 0.026 Uiso 1 1 calc R . . C15 C 0.1321(2) 0.3457(2) 0.3337(2) 0.0218(7) Uani 1 1 d . . . H15A H 0.1192 0.2767 0.3351 0.026 Uiso 1 1 calc R . . H15B H 0.1084 0.3484 0.2800 0.026 Uiso 1 1 calc R . . C6 C 0.1212(2) 0.5142(2) 0.14416(18) 0.0181(7) Uani 1 1 d . . . C11 C 0.1999(2) 0.7851(2) 0.11458(18) 0.0203(7) Uani 1 1 d . . . H11 H 0.1515 0.8294 0.1156 0.024 Uiso 1 1 calc R . . C1 C -0.1022(2) 0.7069(2) 0.36012(19) 0.0196(7) Uani 1 1 d . . . C56 C 0.1860(2) 1.1374(2) 0.1705(2) 0.0228(7) Uani 1 1 d . . . H56A H 0.1857 1.2073 0.1719 0.027 Uiso 1 1 calc R . . H56B H 0.1677 1.1311 0.2233 0.027 Uiso 1 1 calc R . . C23 C 0.5717(2) 0.5286(2) 0.37147(18) 0.0201(7) Uani 1 1 d . . . H23A H 0.5303 0.5279 0.4167 0.024 Uiso 1 1 calc R . . H23B H 0.6318 0.5748 0.3932 0.024 Uiso 1 1 calc R . . C52 C 0.3461(2) 1.1538(2) 0.10613(18) 0.0187(7) Uani 1 1 d . . . H52A H 0.3021 1.1737 0.0684 0.022 Uiso 1 1 calc R . . H52B H 0.3866 1.1045 0.0742 0.022 Uiso 1 1 calc R . . C49 C 0.6438(2) 1.0706(2) 0.16637(19) 0.0217(7) Uani 1 1 d . . . H49A H 0.5943 1.1157 0.1891 0.026 Uiso 1 1 calc R . . H49B H 0.6935 1.0729 0.2100 0.026 Uiso 1 1 calc R . . C5 C 0.1111(2) 0.4216(2) 0.08910(19) 0.0231(7) Uani 1 1 d . . . H5 H 0.1677 0.3898 0.0710 0.028 Uiso 1 1 calc R . . N1 N -0.0410(2) 0.6968(2) 0.31384(17) 0.0274(6) Uani 1 1 d . . . N3 N 0.21795(17) 0.56467(18) 0.17175(15) 0.0168(6) Uani 1 1 d . . . C60 C -0.1020(2) 0.7736(2) 0.11535(19) 0.0220(7) Uani 1 1 d . . . C4 C 0.0174(2) 0.3763(3) 0.0610(2) 0.0285(8) Uani 1 1 d . . . H4 H 0.0083 0.3128 0.0235 0.034 Uiso 1 1 calc R . . C58 C 0.0041(3) 1.1033(3) 0.1206(3) 0.0457(11) Uani 1 1 d . . . H58A H 0.0050 1.1751 0.1291 0.055 Uiso 1 1 calc R . . H58B H -0.0399 1.0697 0.0722 0.055 Uiso 1 1 calc R . . C8 C 0.3372(2) 0.6561(2) 0.10899(18) 0.0205(7) Uani 1 1 d . . . H8 H 0.3840 0.6102 0.1077 0.025 Uiso 1 1 calc R . . C2 C -0.0473(2) 0.5179(2) 0.1438(2) 0.0259(8) Uani 1 1 d . . . H2 H -0.1029 0.5511 0.1626 0.031 Uiso 1 1 calc R . . C7 C 0.2483(2) 0.6473(2) 0.14389(17) 0.0172(6) Uani 1 1 d . . . C19 C 0.2939(2) 0.3478(2) 0.40908(19) 0.0214(7) Uani 1 1 d . . . H19A H 0.2482 0.3397 0.4500 0.026 Uiso 1 1 calc R . . H19B H 0.3459 0.4020 0.4354 0.026 Uiso 1 1 calc R . . N18 N -0.0401(2) 0.7466(2) 0.14900(17) 0.0281(7) Uani 1 1 d . . . C57 C 0.1087(2) 1.0746(3) 0.1059(2) 0.0341(9) Uani 1 1 d . . . H57A H 0.1097 1.0046 0.1038 0.041 Uiso 1 1 calc R . . H57B H 0.1265 1.0817 0.0532 0.041 Uiso 1 1 calc R . . C50 C 0.6945(3) 1.1056(3) 0.1017(2) 0.0331(8) Uani 1 1 d . . . H50A H 0.6448 1.1017 0.0576 0.040 Uiso 1 1 calc R . . H50B H 0.7446 1.0610 0.0797 0.040 Uiso 1 1 calc R . . C16 C 0.0733(2) 0.4107(3) 0.3968(2) 0.0289(8) Uani 1 1 d . . . H16A H 0.0924 0.4032 0.4499 0.035 Uiso 1 1 calc R . . H16B H 0.0910 0.4805 0.3990 0.035 Uiso 1 1 calc R . . C51 C 0.7450(3) 1.2113(3) 0.1325(2) 0.0395(9) Uani 1 1 d . . . H51A H 0.6956 1.2561 0.1537 0.059 Uiso 1 1 calc R . . H51B H 0.7759 1.2300 0.0885 0.059 Uiso 1 1 calc R . . H51C H 0.7957 1.2153 0.1752 0.059 Uiso 1 1 calc R . . S1 S -0.18662(7) 0.72274(8) 0.42415(5) 0.0399(3) Uani 1 1 d . . . S2 S -0.18762(7) 0.81139(8) 0.06696(6) 0.0433(3) Uani 1 1 d . . . C20 C 0.3418(2) 0.2532(2) 0.37747(19) 0.0213(7) Uani 1 1 d . . . H20A H 0.3851 0.2599 0.3347 0.026 Uiso 1 1 calc R . . H20B H 0.2897 0.1981 0.3538 0.026 Uiso 1 1 calc R . . C21 C 0.4026(2) 0.2298(2) 0.44381(19) 0.0232(7) Uani 1 1 d . . . H21A H 0.4569 0.2833 0.4651 0.028 Uiso 1 1 calc R . . H21B H 0.3600 0.2276 0.4880 0.028 Uiso 1 1 calc R . . C10 C 0.2855(2) 0.7980(2) 0.07727(18) 0.0238(7) Uani 1 1 d . . . H10 H 0.2958 0.8497 0.0531 0.029 Uiso 1 1 calc R . . C55 C 0.4216(3) 1.3453(3) 0.0552(2) 0.0299(8) Uani 1 1 d . . . H55A H 0.3737 1.2977 0.0168 0.045 Uiso 1 1 calc R . . H55B H 0.4677 1.3773 0.0263 0.045 Uiso 1 1 calc R . . H55C H 0.3865 1.3951 0.0912 0.045 Uiso 1 1 calc R . . C45 C 0.6789(3) 0.9016(3) 0.2773(2) 0.0386(10) Uani 1 1 d D . . H45A H 0.7164 0.9531 0.2589 0.046 Uiso 1 1 calc R A 1 H45B H 0.7222 0.8511 0.2819 0.046 Uiso 1 1 calc R A 1 C3 C -0.0636(2) 0.4259(3) 0.0890(2) 0.0302(8) Uani 1 1 d . . . H3 H -0.1290 0.3968 0.0705 0.036 Uiso 1 1 calc R . . C9 C 0.3563(2) 0.7332(2) 0.07605(19) 0.0250(7) Uani 1 1 d . . . H9 H 0.4172 0.7418 0.0528 0.030 Uiso 1 1 calc R . . C25 C 0.6568(2) 0.3901(2) 0.39946(19) 0.0240(7) Uani 1 1 d . . . H25A H 0.7180 0.4349 0.4202 0.029 Uiso 1 1 calc R . . H25B H 0.6145 0.3935 0.4448 0.029 Uiso 1 1 calc R . . C24 C 0.6025(2) 0.4256(2) 0.33637(19) 0.0207(7) Uani 1 1 d . . . H24A H 0.6461 0.4262 0.2924 0.025 Uiso 1 1 calc R . . H24B H 0.5430 0.3791 0.3135 0.025 Uiso 1 1 calc R . . C28 C 0.6461(2) 0.6188(2) 0.2325(2) 0.0252(7) Uani 1 1 d . . . H28A H 0.6886 0.6786 0.2313 0.030 Uiso 1 1 calc R . . H28B H 0.6882 0.5761 0.2521 0.030 Uiso 1 1 calc R . . C29 C 0.6040(2) 0.5645(3) 0.1481(2) 0.0306(8) Uani 1 1 d . . . H29A H 0.5677 0.6096 0.1264 0.037 Uiso 1 1 calc R . . H29B H 0.5560 0.5087 0.1500 0.037 Uiso 1 1 calc R . . C59 C -0.0384(3) 1.0776(3) 0.1920(3) 0.0483(11) Uani 1 1 d . . . H59A H -0.0381 1.0069 0.1848 0.072 Uiso 1 1 calc R . . H59B H -0.1065 1.0947 0.1963 0.072 Uiso 1 1 calc R . . H59C H 0.0017 1.1146 0.2409 0.072 Uiso 1 1 calc R . . C22 C 0.4465(2) 0.1321(2) 0.4151(2) 0.0267(8) Uani 1 1 d . . . H22A H 0.3930 0.0779 0.4008 0.040 Uiso 1 1 calc R . . H22B H 0.4908 0.1242 0.4580 0.040 Uiso 1 1 calc R . . H22C H 0.4837 0.1314 0.3681 0.040 Uiso 1 1 calc R . . C26 C 0.6835(3) 0.2854(3) 0.3673(2) 0.0299(8) Uani 1 1 d . . . H26A H 0.6231 0.2406 0.3470 0.045 Uiso 1 1 calc R . . H26B H 0.7171 0.2662 0.4103 0.045 Uiso 1 1 calc R . . H26C H 0.7275 0.2821 0.3237 0.045 Uiso 1 1 calc R . . C30 C 0.6833(3) 0.5255(3) 0.0920(2) 0.0464(11) Uani 1 1 d . . . H30A H 0.7334 0.5798 0.0925 0.070 Uiso 1 1 calc R . . H30B H 0.6530 0.4964 0.0375 0.070 Uiso 1 1 calc R . . H30C H 0.7146 0.4753 0.1098 0.070 Uiso 1 1 calc R . . C17 C -0.0386(3) 0.3858(3) 0.3800(2) 0.0348(9) Uani 1 1 d . . . H17A H -0.0718 0.4185 0.4283 0.042 Uiso 1 1 calc R . . H17B H -0.0553 0.3139 0.3685 0.042 Uiso 1 1 calc R . . C18 C -0.0777(3) 0.4186(3) 0.3089(3) 0.0468(11) Uani 1 1 d . . . H18A H -0.0610 0.4898 0.3199 0.070 Uiso 1 1 calc R . . H18B H -0.1497 0.4029 0.3012 0.070 Uiso 1 1 calc R . . H18C H -0.0474 0.3841 0.2604 0.070 Uiso 1 1 calc R . . C46A C 0.6767(4) 0.9914(4) 0.3519(3) 0.0372(13) Uani 0.75 1 d PD B 2 H46A H 0.7442 1.0257 0.3678 0.045 Uiso 0.75 1 calc PR B 2 H46B H 0.6338 1.0384 0.3395 0.045 Uiso 0.75 1 calc PR B 2 C47A C 0.6373(5) 0.9549(4) 0.4188(4) 0.0493(15) Uani 0.75 1 d PD B 2 H47A H 0.5737 0.9149 0.4005 0.074 Uiso 0.75 1 calc PR B 2 H47B H 0.6282 1.0113 0.4646 0.074 Uiso 0.75 1 calc PR B 2 H47C H 0.6844 0.9149 0.4351 0.074 Uiso 0.75 1 calc PR B 2 C47B C 0.7074(8) 1.0019(10) 0.4237(7) 0.021(3) Uani 0.25 1 d PDU B 1 H47D H 0.7530 0.9562 0.4329 0.032 Uiso 0.25 1 calc PR B 1 H47E H 0.6762 1.0307 0.4733 0.032 Uiso 0.25 1 calc PR B 1 H47F H 0.7441 1.0544 0.4070 0.032 Uiso 0.25 1 calc PR B 1 C46B C 0.6273(8) 0.9461(10) 0.3577(5) 0.016(3) Uani 0.25 1 d PD B 1 H46C H 0.5799 0.9915 0.3492 0.020 Uiso 0.25 1 calc PR B 1 H46D H 0.5905 0.8924 0.3740 0.020 Uiso 0.25 1 calc PR B 1 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 0.0117(2) 0.0199(3) 0.0170(2) 0.00580(19) -0.00059(17) 0.00559(17) C32 0.0270(17) 0.0146(16) 0.0138(15) 0.0037(13) 0.0006(13) 0.0058(13) N12 0.0116(13) 0.0224(15) 0.0273(14) 0.0083(12) -0.0025(11) 0.0041(11) N15 0.0145(12) 0.0185(14) 0.0221(14) 0.0100(12) -0.0013(11) 0.0023(11) N10 0.0129(12) 0.0177(13) 0.0164(13) 0.0080(11) 0.0026(10) 0.0050(10) N14 0.0191(13) 0.0172(14) 0.0194(13) 0.0085(11) 0.0010(11) 0.0050(11) C37 0.0228(17) 0.0215(18) 0.0257(17) 0.0037(15) 0.0006(14) 0.0046(14) N11 0.0112(12) 0.0172(13) 0.0214(13) 0.0107(11) 0.0020(10) 0.0044(10) C31 0.0206(16) 0.0189(16) 0.0170(15) 0.0055(14) 0.0052(13) 0.0057(13) C41 0.0153(15) 0.0117(15) 0.0194(16) 0.0051(13) -0.0019(12) -0.0002(12) C38 0.0286(19) 0.0245(19) 0.036(2) -0.0015(17) 0.0033(16) 0.0082(16) N17 0.0184(13) 0.0224(14) 0.0227(14) 0.0131(12) 0.0008(11) 0.0059(11) C35 0.0168(15) 0.0171(16) 0.0127(14) 0.0049(13) 0.0037(12) 0.0044(13) N13 0.0158(13) 0.0180(14) 0.0181(13) 0.0078(11) 0.0008(10) 0.0048(11) C33 0.0204(16) 0.0236(18) 0.0176(16) 0.0041(14) -0.0049(13) 0.0062(14) C34 0.0151(15) 0.0226(17) 0.0200(16) 0.0081(14) -0.0016(13) 0.0011(13) C43 0.0165(15) 0.0150(16) 0.0155(15) 0.0035(13) -0.0024(12) 0.0022(12) C36 0.0164(15) 0.0243(17) 0.0214(16) 0.0132(15) 0.0046(13) 0.0108(13) N6 0.0169(13) 0.0196(14) 0.0204(13) 0.0093(12) 0.0025(11) 0.0070(11) N7 0.0142(12) 0.0200(14) 0.0178(13) 0.0087(11) 0.0023(10) 0.0058(11) N5 0.0166(12) 0.0161(13) 0.0166(13) 0.0053(11) 0.0016(10) 0.0057(10) C14 0.0161(15) 0.0157(16) 0.0159(15) 0.0040(13) 0.0024(12) 0.0057(12) C42 0.0165(15) 0.0149(16) 0.0171(15) 0.0045(13) -0.0003(12) 0.0029(13) C12 0.0187(15) 0.0173(16) 0.0139(15) 0.0047(13) 0.0020(12) 0.0110(13) N16 0.0158(13) 0.0201(14) 0.0283(15) 0.0145(12) 0.0063(11) 0.0066(11) C40 0.0171(16) 0.031(2) 0.043(2) 0.0084(17) 0.0021(15) 0.0113(15) C39 0.0219(18) 0.033(2) 0.048(2) 0.0033(18) 0.0078(16) 0.0151(16) C13 0.0186(16) 0.0183(16) 0.0173(15) 0.0055(14) 0.0038(13) 0.0089(13) N8 0.0162(13) 0.0226(14) 0.0239(14) 0.0134(12) 0.0011(11) 0.0035(11) N4 0.0202(13) 0.0208(14) 0.0146(13) 0.0082(11) -0.0017(10) 0.0058(11) C54 0.0277(18) 0.0277(19) 0.0275(18) 0.0134(16) 0.0023(14) 0.0055(15) C27 0.0183(16) 0.0221(17) 0.0282(18) 0.0134(15) -0.0030(13) -0.0001(13) N9 0.0164(13) 0.0192(14) 0.0214(14) 0.0090(12) -0.0026(11) 0.0024(11) C48 0.0187(16) 0.0237(17) 0.0227(17) 0.0107(14) 0.0064(13) 0.0069(13) N2 0.0131(13) 0.0232(14) 0.0204(14) 0.0054(12) -0.0011(11) 0.0029(11) C44 0.0250(17) 0.0238(18) 0.039(2) 0.0216(16) 0.0094(15) 0.0138(14) C53 0.0257(17) 0.0216(17) 0.0210(16) 0.0120(14) 0.0019(13) 0.0061(14) C15 0.0175(16) 0.0208(17) 0.0306(18) 0.0129(15) 0.0026(14) 0.0019(13) C6 0.0172(15) 0.0253(18) 0.0157(15) 0.0104(14) 0.0022(12) 0.0072(13) C11 0.0247(17) 0.0213(17) 0.0155(15) 0.0052(14) -0.0033(13) 0.0074(14) C1 0.0151(15) 0.0203(17) 0.0219(17) 0.0058(14) -0.0010(14) -0.0035(13) C56 0.0191(16) 0.0235(17) 0.0304(18) 0.0143(15) -0.0013(14) 0.0074(13) C23 0.0171(15) 0.0246(18) 0.0203(16) 0.0101(14) -0.0050(13) 0.0030(13) C52 0.0215(16) 0.0210(17) 0.0177(16) 0.0117(14) 0.0001(13) 0.0041(13) C49 0.0193(16) 0.0259(18) 0.0245(17) 0.0136(15) 0.0030(13) 0.0049(14) C5 0.0230(17) 0.0216(18) 0.0246(17) 0.0040(15) 0.0043(14) 0.0086(14) N1 0.0233(15) 0.0269(16) 0.0299(16) 0.0043(13) 0.0025(13) 0.0041(12) N3 0.0126(12) 0.0204(14) 0.0194(13) 0.0083(12) -0.0006(10) 0.0038(11) C60 0.0186(16) 0.0257(18) 0.0209(16) 0.0042(15) 0.0007(14) 0.0058(14) C4 0.0270(18) 0.0263(19) 0.0277(18) 0.0004(16) 0.0001(15) 0.0033(15) C58 0.0221(19) 0.065(3) 0.055(3) 0.028(2) -0.0123(18) 0.0045(19) C8 0.0183(16) 0.0257(18) 0.0190(16) 0.0075(14) 0.0036(13) 0.0062(14) C2 0.0190(16) 0.029(2) 0.0272(18) 0.0026(16) 0.0010(14) 0.0083(14) C7 0.0204(16) 0.0199(16) 0.0131(15) 0.0064(13) 0.0005(12) 0.0070(13) C19 0.0241(17) 0.0245(17) 0.0207(16) 0.0137(14) 0.0023(13) 0.0065(14) N18 0.0237(15) 0.0314(17) 0.0278(15) 0.0056(13) -0.0084(13) 0.0096(13) C57 0.0266(19) 0.045(2) 0.031(2) 0.0124(18) -0.0059(16) 0.0058(17) C50 0.0303(19) 0.043(2) 0.0298(19) 0.0203(18) -0.0018(15) -0.0083(16) C16 0.0253(18) 0.0299(19) 0.034(2) 0.0120(17) 0.0067(15) 0.0077(15) C51 0.040(2) 0.041(2) 0.043(2) 0.028(2) -0.0065(18) -0.0140(18) S1 0.0250(5) 0.0654(7) 0.0250(5) 0.0086(5) 0.0091(4) -0.0062(4) S2 0.0413(6) 0.0562(7) 0.0344(5) 0.0106(5) -0.0123(4) 0.0297(5) C20 0.0219(16) 0.0230(17) 0.0218(17) 0.0102(14) 0.0010(13) 0.0048(14) C21 0.0223(16) 0.0202(17) 0.0248(17) 0.0033(15) -0.0061(14) 0.0036(14) C10 0.0374(19) 0.0223(18) 0.0132(15) 0.0078(14) 0.0026(14) 0.0023(15) C55 0.037(2) 0.0290(19) 0.0292(19) 0.0179(16) 0.0016(16) 0.0035(16) C45 0.050(2) 0.033(2) 0.034(2) 0.0063(17) -0.0071(18) 0.0283(19) C3 0.0216(17) 0.031(2) 0.036(2) 0.0075(17) -0.0026(15) 0.0010(15) C9 0.0246(17) 0.033(2) 0.0189(17) 0.0097(15) 0.0068(14) 0.0021(15) C25 0.0253(17) 0.0288(19) 0.0208(17) 0.0095(15) 0.0009(14) 0.0107(15) C24 0.0176(15) 0.0247(18) 0.0212(16) 0.0082(15) -0.0023(13) 0.0057(13) C28 0.0206(16) 0.0285(19) 0.0306(19) 0.0145(16) -0.0002(14) 0.0058(14) C29 0.0245(18) 0.034(2) 0.033(2) 0.0073(17) 0.0019(15) 0.0080(16) C59 0.025(2) 0.059(3) 0.064(3) 0.025(2) -0.0033(19) 0.0012(19) C22 0.0252(17) 0.0233(18) 0.0320(19) 0.0076(16) -0.0037(15) 0.0079(14) C26 0.0311(19) 0.031(2) 0.0321(19) 0.0136(16) 0.0052(15) 0.0121(16) C30 0.037(2) 0.059(3) 0.039(2) 0.003(2) 0.0053(18) 0.017(2) C17 0.0256(18) 0.037(2) 0.046(2) 0.0162(19) 0.0138(17) 0.0087(16) C18 0.029(2) 0.054(3) 0.064(3) 0.027(2) 0.0008(19) 0.0074(19) C46A 0.036(3) 0.029(3) 0.050(4) 0.015(3) 0.000(3) 0.010(2) C47A 0.066(4) 0.038(3) 0.046(4) 0.012(3) 0.005(3) 0.018(3) C47B 0.012(5) 0.031(6) 0.012(5) -0.009(5) -0.002(5) 0.005(5) C46B 0.018(7) 0.025(8) 0.006(7) 0.005(6) -0.003(5) 0.003(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 N18 2.080(3) . ? Fe1 N1 2.088(3) . ? Fe1 N2 2.216(3) . ? Fe1 N12 2.235(3) . ? Fe1 N4 2.240(3) . ? Fe1 N10 2.243(2) . ? C32 C31 1.378(4) . ? C32 C33 1.387(4) . ? C32 H32 0.9500 . ? N12 C36 1.335(4) . ? N12 C40 1.355(4) . ? N15 C41 1.338(4) . ? N15 C43 1.353(4) . ? N10 C35 1.342(4) . ? N10 C31 1.353(4) . ? N14 C42 1.351(4) . ? N14 C43 1.353(4) . ? C37 C38 1.379(5) . ? C37 C36 1.392(5) . ? C37 H37 0.9500 . ? N11 C41 1.398(4) . ? N11 C35 1.432(4) . ? N11 C36 1.443(4) . ? C31 H31 0.9500 . ? C41 N13 1.331(4) . ? C38 C39 1.390(5) . ? C38 H38 0.9500 . ? N17 C43 1.357(4) . ? N17 C56 1.466(4) . ? N17 C52 1.466(4) . ? C35 C34 1.397(4) . ? N13 C42 1.357(4) . ? C33 C34 1.387(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? N6 C13 1.346(4) . ? N6 C14 1.347(4) . ? N7 C12 1.326(4) . ? N7 C14 1.369(4) . ? N5 C12 1.335(4) . ? N5 C13 1.356(4) . ? C14 N9 1.348(4) . ? C42 N16 1.361(4) . ? C12 N3 1.411(4) . ? N16 C48 1.468(4) . ? N16 C44 1.473(4) . ? C40 C39 1.373(5) . ? C40 H40 0.9500 . ? C39 H39 0.9500 . ? C13 N8 1.354(4) . ? N8 C15 1.463(4) . ? N8 C19 1.476(4) . ? N4 C11 1.349(4) . ? N4 C7 1.350(4) . ? C54 C55 1.525(4) . ? C54 C53 1.533(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C27 N9 1.469(4) . ? C27 C28 1.523(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N9 C23 1.476(4) . ? C48 C49 1.529(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? N2 C6 1.342(4) . ? N2 C2 1.356(4) . ? C44 C45 1.519(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C53 C52 1.525(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C15 C16 1.530(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C6 C5 1.386(5) . ? C6 N3 1.436(4) . ? C11 C10 1.381(5) . ? C11 H11 0.9500 . ? C1 N1 1.174(4) . ? C1 S1 1.622(3) . ? C56 C57 1.529(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C23 C24 1.526(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C49 C50 1.522(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C5 C4 1.379(5) . ? C5 H5 0.9500 . ? N3 C7 1.430(4) . ? C60 N18 1.162(4) . ? C60 S2 1.629(3) . ? C4 C3 1.395(5) . ? C4 H4 0.9500 . ? C58 C59 1.515(6) . ? C58 C57 1.529(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C8 C9 1.386(4) . ? C8 C7 1.388(4) . ? C8 H8 0.9500 . ? C2 C3 1.379(5) . ? C2 H2 0.9500 . ? C19 C20 1.522(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C50 C51 1.533(5) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C16 C17 1.530(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C20 C21 1.526(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.526(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C10 C9 1.391(5) . ? C10 H10 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C45 C46A 1.549(6) . ? C45 C46B 1.589(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C3 H3 0.9500 . ? C9 H9 0.9500 . ? C25 C26 1.522(4) . ? C25 C24 1.527(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C28 C29 1.517(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.525(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C17 C18 1.535(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C46A C47A 1.506(7) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C47B C46B 1.540(10) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? 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 N18 Fe1 N1 98.26(11) . . ? N18 Fe1 N2 91.29(10) . . ? N1 Fe1 N2 88.82(10) . . ? N18 Fe1 N12 86.82(10) . . ? N1 Fe1 N12 88.60(10) . . ? N2 Fe1 N12 176.55(9) . . ? N18 Fe1 N4 91.54(10) . . ? N1 Fe1 N4 164.34(10) . . ? N2 Fe1 N4 78.72(9) . . ? N12 Fe1 N4 104.20(9) . . ? N18 Fe1 N10 163.33(10) . . ? N1 Fe1 N10 89.31(10) . . ? N2 Fe1 N10 103.76(9) . . ? N12 Fe1 N10 78.50(9) . . ? N4 Fe1 N10 84.54(9) . . ? C31 C32 C33 118.2(3) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C36 N12 C40 116.9(3) . . ? C36 N12 Fe1 121.74(18) . . ? C40 N12 Fe1 118.2(2) . . ? C41 N15 C43 112.9(2) . . ? C35 N10 C31 117.6(2) . . ? C35 N10 Fe1 122.62(18) . . ? C31 N10 Fe1 119.0(2) . . ? C42 N14 C43 114.0(3) . . ? C38 C37 C36 119.0(3) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C41 N11 C35 126.0(2) . . ? C41 N11 C36 118.6(2) . . ? C35 N11 C36 115.3(2) . . ? N10 C31 C32 123.2(3) . . ? N10 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? N13 C41 N15 128.6(3) . . ? N13 C41 N11 118.1(2) . . ? N15 C41 N11 113.3(2) . . ? C37 C38 C39 118.4(3) . . ? C37 C38 H38 120.8 . . ? C39 C38 H38 120.8 . . ? C43 N17 C56 121.1(3) . . ? C43 N17 C52 120.7(2) . . ? C56 N17 C52 118.1(2) . . ? N10 C35 C34 123.0(3) . . ? N10 C35 N11 115.2(2) . . ? C34 C35 N11 121.5(3) . . ? C41 N13 C42 112.6(2) . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 117.7(3) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? N14 C43 N15 125.8(3) . . ? N14 C43 N17 117.0(3) . . ? N15 C43 N17 117.3(3) . . ? N12 C36 C37 123.3(3) . . ? N12 C36 N11 117.2(3) . . ? C37 C36 N11 119.4(3) . . ? C13 N6 C14 115.0(2) . . ? C12 N7 C14 112.6(2) . . ? C12 N5 C13 112.8(3) . . ? N6 C14 N9 116.7(2) . . ? N6 C14 N7 125.1(3) . . ? N9 C14 N7 118.1(3) . . ? N14 C42 N13 126.1(3) . . ? N14 C42 N16 115.0(3) . . ? N13 C42 N16 118.9(2) . . ? N7 C12 N5 129.1(3) . . ? N7 C12 N3 117.5(3) . . ? N5 C12 N3 113.4(3) . . ? C42 N16 C48 119.9(2) . . ? C42 N16 C44 122.4(2) . . ? C48 N16 C44 117.4(2) . . ? N12 C40 C39 123.3(3) . . ? N12 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? C40 C39 C38 119.1(3) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N6 C13 N8 116.9(3) . . ? N6 C13 N5 125.4(3) . . ? N8 C13 N5 117.7(3) . . ? C13 N8 C15 121.6(2) . . ? C13 N8 C19 120.3(3) . . ? C15 N8 C19 117.5(2) . . ? C11 N4 C7 117.6(3) . . ? C11 N4 Fe1 118.88(19) . . ? C7 N4 Fe1 122.41(19) . . ? C55 C54 C53 114.0(3) . . ? C55 C54 H54A 108.8 . . ? C53 C54 H54A 108.8 . . ? C55 C54 H54B 108.8 . . ? C53 C54 H54B 108.8 . . ? H54A C54 H54B 107.6 . . ? N9 C27 C28 113.6(3) . . ? N9 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? N9 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C14 N9 C27 122.9(2) . . ? C14 N9 C23 119.5(2) . . ? C27 N9 C23 117.1(2) . . ? N16 C48 C49 114.6(3) . . ? N16 C48 H48A 108.6 . . ? C49 C48 H48A 108.6 . . ? N16 C48 H48B 108.6 . . ? C49 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? C6 N2 C2 117.0(3) . . ? C6 N2 Fe1 122.8(2) . . ? C2 N2 Fe1 118.00(19) . . ? N16 C44 C45 113.1(3) . . ? N16 C44 H44A 109.0 . . ? C45 C44 H44A 109.0 . . ? N16 C44 H44B 109.0 . . ? C45 C44 H44B 109.0 . . ? H44A C44 H44B 107.8 . . ? C52 C53 C54 113.4(3) . . ? C52 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? C52 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? N8 C15 C16 113.1(3) . . ? N8 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N8 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N2 C6 C5 123.5(3) . . ? N2 C6 N3 116.4(3) . . ? C5 C6 N3 120.0(3) . . ? N4 C11 C10 123.3(3) . . ? N4 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N1 C1 S1 179.1(3) . . ? N17 C56 C57 112.6(3) . . ? N17 C56 H56A 109.1 . . ? C57 C56 H56A 109.1 . . ? N17 C56 H56B 109.1 . . ? C57 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? N9 C23 C24 114.2(2) . . ? N9 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? N9 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N17 C52 C53 112.1(2) . . ? N17 C52 H52A 109.2 . . ? C53 C52 H52A 109.2 . . ? N17 C52 H52B 109.2 . . ? C53 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C50 C49 C48 111.7(3) . . ? C50 C49 H49A 109.3 . . ? C48 C49 H49A 109.3 . . ? C50 C49 H49B 109.3 . . ? C48 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 N1 Fe1 162.2(3) . . ? C12 N3 C7 124.1(2) . . ? C12 N3 C6 118.5(2) . . ? C7 N3 C6 117.4(2) . . ? N18 C60 S2 179.0(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C59 C58 C57 113.7(3) . . ? C59 C58 H58A 108.8 . . ? C57 C58 H58A 108.8 . . ? C59 C58 H58B 108.8 . . ? C57 C58 H58B 108.8 . . ? H58A C58 H58B 107.7 . . ? C9 C8 C7 118.6(3) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? N2 C2 C3 123.0(3) . . ? N2 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? N4 C7 C8 122.7(3) . . ? N4 C7 N3 114.8(3) . . ? C8 C7 N3 122.4(3) . . ? N8 C19 C20 112.8(3) . . ? N8 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N8 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C60 N18 Fe1 166.0(3) . . ? C56 C57 C58 112.8(3) . . ? C56 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? C56 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C49 C50 C51 113.0(3) . . ? C49 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C17 C16 C15 113.0(3) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C19 C20 C21 111.5(3) . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 112.7(3) . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C11 C10 C9 118.3(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C44 C45 C46A 120.1(3) . . ? C44 C45 C46B 96.9(5) . . ? C46A C45 C46B 34.0(5) . . ? C44 C45 H45A 112.4 . . ? C46A C45 H45A 80.0 . . ? C46B C45 H45A 112.4 . . ? C44 C45 H45B 112.4 . . ? C46A C45 H45B 117.2 . . ? C46B C45 H45B 112.4 . . ? H45A C45 H45B 109.9 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C26 C25 C24 113.0(3) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C23 C24 C25 111.8(3) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C29 C28 C27 112.5(3) . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C30 112.8(3) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C16 C17 C18 112.2(3) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C47A C46A C45 108.3(4) . . ? C47A C46A H46A 110.0 . . ? C45 C46A H46A 110.0 . . ? C47A C46A H46B 110.0 . . ? C45 C46A H46B 110.0 . . ? H46A C46A H46B 108.4 . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C47B C46B C45 108.9(8) . . ? C47B C46B H46C 109.9 . . ? C45 C46B H46C 109.9 . . ? C47B C46B H46D 109.9 . . ? C45 C46B H46D 109.9 . . ? H46C C46B H46D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.654 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.083 #=END data_6 _database_code_depnum_ccdc_archive 'CCDC 836948' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCSe)2(DDCCl)].2CH3OH ; _chemical_name_common trans-[Fe(II)(NCSe)2(DDCCl)].2CH3OH _chemical_melting_point ? _chemical_formula_moiety '(C52 H60 Cl2 Fe N16 Se2), 2(C H4 O)' _chemical_formula_sum 'C54 H68 Cl2 Fe N16 O2 Se2' _chemical_formula_weight 1257.91 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' Cl Cl 0.1484 0.1585 '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' Se Se -0.0929 2.2259 '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 8.5210(6) _cell_length_b 11.7421(7) _cell_length_c 15.3839(9) _cell_angle_alpha 79.359(2) _cell_angle_beta 86.745(2) _cell_angle_gamma 72.678(3) _cell_volume 1444.15(16) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 15746 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.669 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7313 _exptl_absorpt_correction_T_max 0.8508 _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 15746 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6921 _reflns_number_gt 6021 _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 6921 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _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 1.0000 0.0000 0.5000 0.01106(7) Uani 1 2 d S . . Se1 Se 0.83694(2) -0.248061(17) 0.760344(12) 0.02341(6) Uani 1 1 d . . . N1 N 0.94978(17) -0.10174(12) 0.60586(10) 0.0151(3) Uani 1 1 d . . . C1 C 0.90497(19) -0.15886(14) 0.66652(11) 0.0148(3) Uani 1 1 d . . . C5 C 0.6196(2) 0.32465(14) 0.52267(11) 0.0162(3) Uani 1 1 d . . . H5 H 0.5350 0.3795 0.4850 0.019 Uiso 1 1 calc R . . N2 N 0.84725(16) 0.14237(12) 0.54444(9) 0.0131(3) Uani 1 1 d . . . C2 C 0.8594(2) 0.15980(15) 0.62822(11) 0.0172(3) Uani 1 1 d . . . H2 H 0.9399 0.1012 0.6663 0.021 Uiso 1 1 calc R . . C3 C 0.7599(2) 0.25902(16) 0.66050(12) 0.0207(4) Uani 1 1 d . . . H3 H 0.7738 0.2691 0.7192 0.025 Uiso 1 1 calc R . . C6 C 0.72613(19) 0.22321(14) 0.49422(11) 0.0133(3) Uani 1 1 d . . . Cl1 Cl 0.73554(6) 0.60120(4) 0.27013(3) 0.02497(10) Uani 1 1 d . . . N3 N 0.70461(16) 0.19723(11) 0.40987(9) 0.0125(3) Uani 1 1 d . . . N4 N 0.80474(16) -0.01555(12) 0.44484(9) 0.0132(3) Uani 1 1 d . . . C4 C 0.6392(2) 0.34401(15) 0.60648(12) 0.0192(3) Uani 1 1 d . . . H4 H 0.5714 0.4142 0.6269 0.023 Uiso 1 1 calc R . . C11 C 0.7811(2) -0.12543(14) 0.44865(11) 0.0165(3) Uani 1 1 d . . . H11 H 0.8621 -0.1951 0.4770 0.020 Uiso 1 1 calc R . . N5 N 0.72167(17) 0.38722(12) 0.34252(10) 0.0163(3) Uani 1 1 d . . . N7 N 0.70207(17) 0.24053(12) 0.25772(9) 0.0153(3) Uani 1 1 d . . . C7 C 0.68534(19) 0.08167(14) 0.40751(11) 0.0130(3) Uani 1 1 d . . . C8 C 0.5438(2) 0.07343(15) 0.37209(11) 0.0169(3) Uani 1 1 d . . . H8 H 0.4615 0.1445 0.3468 0.020 Uiso 1 1 calc R . . C12 C 0.70789(19) 0.27902(14) 0.33271(11) 0.0139(3) Uani 1 1 d . . . C14 C 0.7190(2) 0.31869(14) 0.18380(11) 0.0156(3) Uani 1 1 d . . . C10 C 0.6459(2) -0.14132(15) 0.41356(12) 0.0192(3) Uani 1 1 d . . . H10 H 0.6357 -0.2203 0.4162 0.023 Uiso 1 1 calc R . . C9 C 0.5245(2) -0.03957(16) 0.37414(12) 0.0204(4) Uani 1 1 d . . . H9 H 0.4299 -0.0477 0.3491 0.025 Uiso 1 1 calc R . . N6 N 0.72630(18) 0.43299(12) 0.18454(10) 0.0171(3) Uani 1 1 d . . . N8 N 0.72928(18) 0.28204(12) 0.10532(10) 0.0180(3) Uani 1 1 d . . . C13 C 0.7273(2) 0.45585(14) 0.26451(12) 0.0170(3) Uani 1 1 d . . . O1 O 0.2958(2) 0.38563(16) 0.38684(13) 0.0472(4) Uani 1 1 d . . . H1 H 0.2773 0.3536 0.3455 0.057 Uiso 1 1 calc R . . C21 C 0.7525(2) 0.15338(15) 0.09943(12) 0.0208(4) Uani 1 1 d . . . H21 H 0.7751 0.1478 0.0356 0.025 Uiso 1 1 calc R . . C15 C 0.7574(2) 0.36228(15) 0.02367(11) 0.0197(4) Uani 1 1 d . . . H15 H 0.7265 0.4463 0.0371 0.024 Uiso 1 1 calc R . . C16 C 0.9386(2) 0.32953(16) -0.00207(12) 0.0202(4) Uani 1 1 d . . . H16A H 0.9745 0.2463 -0.0154 0.024 Uiso 1 1 calc R . . H16B H 1.0052 0.3316 0.0480 0.024 Uiso 1 1 calc R . . C18 C 0.8623(2) 0.41985(16) -0.16048(12) 0.0220(4) Uani 1 1 d . . . H18A H 0.8792 0.4801 -0.2115 0.026 Uiso 1 1 calc R . . H18B H 0.8969 0.3392 -0.1783 0.026 Uiso 1 1 calc R . . C17 C 0.9665(3) 0.41856(18) -0.08303(12) 0.0265(4) Uani 1 1 d . . . H17A H 0.9377 0.5009 -0.0683 0.032 Uiso 1 1 calc R . . H17B H 1.0841 0.3951 -0.0999 0.032 Uiso 1 1 calc R . . C26 C 0.9041(3) 0.06598(16) 0.14963(13) 0.0264(4) Uani 1 1 d . . . H26A H 1.0022 0.0932 0.1310 0.032 Uiso 1 1 calc R . . H26B H 0.8882 0.0654 0.2139 0.032 Uiso 1 1 calc R . . C20 C 0.6492(2) 0.36525(18) -0.05334(13) 0.0268(4) Uani 1 1 d . . . H20A H 0.5320 0.3924 -0.0362 0.032 Uiso 1 1 calc R . . H20B H 0.6730 0.2827 -0.0672 0.032 Uiso 1 1 calc R . . C19 C 0.6815(3) 0.45158(18) -0.13532(13) 0.0293(4) Uani 1 1 d . . . H19A H 0.6166 0.4479 -0.1855 0.035 Uiso 1 1 calc R . . H19B H 0.6446 0.5356 -0.1235 0.035 Uiso 1 1 calc R . . C25 C 0.9308(3) -0.06165(17) 0.13042(14) 0.0351(5) Uani 1 1 d . . . H25A H 0.9555 -0.0620 0.0668 0.042 Uiso 1 1 calc R . . H25B H 1.0263 -0.1185 0.1647 0.042 Uiso 1 1 calc R . . C22 C 0.5986(3) 0.1136(2) 0.12215(14) 0.0315(4) Uani 1 1 d . . . H22A H 0.5061 0.1687 0.0848 0.038 Uiso 1 1 calc R . . H22B H 0.5687 0.1179 0.1848 0.038 Uiso 1 1 calc R . . C23 C 0.6290(3) -0.0168(2) 0.10659(17) 0.0456(6) Uani 1 1 d . . . H23A H 0.5319 -0.0443 0.1270 0.055 Uiso 1 1 calc R . . H23B H 0.6424 -0.0181 0.0424 0.055 Uiso 1 1 calc R . . C24 C 0.7802(4) -0.1035(2) 0.15471(16) 0.0446(6) Uani 1 1 d . . . H24A H 0.7615 -0.1101 0.2193 0.053 Uiso 1 1 calc R . . H24B H 0.7990 -0.1850 0.1396 0.053 Uiso 1 1 calc R . . C27 C 0.1457(3) 0.4432(2) 0.42515(18) 0.0427(6) Uani 1 1 d . . . H27A H 0.1654 0.4519 0.4854 0.064 Uiso 1 1 calc R . . H27B H 0.0700 0.3942 0.4270 0.064 Uiso 1 1 calc R . . H27C H 0.0973 0.5234 0.3896 0.064 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 0.01120(15) 0.01111(14) 0.01090(16) -0.00055(12) -0.00045(11) -0.00409(11) Se1 0.02108(10) 0.02949(10) 0.01838(11) 0.00789(7) -0.00207(7) -0.01239(7) N1 0.0138(6) 0.0151(6) 0.0169(7) -0.0031(5) -0.0018(5) -0.0047(5) C1 0.0125(7) 0.0152(7) 0.0165(8) -0.0021(6) -0.0018(6) -0.0036(6) C5 0.0154(8) 0.0150(7) 0.0180(9) -0.0010(6) 0.0017(6) -0.0057(6) N2 0.0131(6) 0.0139(6) 0.0126(7) -0.0009(5) -0.0005(5) -0.0054(5) C2 0.0182(8) 0.0193(8) 0.0145(8) -0.0020(6) -0.0017(6) -0.0067(6) C3 0.0252(9) 0.0242(8) 0.0159(9) -0.0084(7) 0.0014(7) -0.0093(7) C6 0.0135(7) 0.0146(7) 0.0131(8) -0.0012(6) 0.0013(6) -0.0071(6) Cl1 0.0362(2) 0.01526(18) 0.0252(2) -0.00429(16) 0.01019(19) -0.01155(17) N3 0.0141(6) 0.0123(6) 0.0112(7) -0.0014(5) -0.0008(5) -0.0040(5) N4 0.0130(6) 0.0146(6) 0.0126(7) -0.0018(5) 0.0000(5) -0.0053(5) C4 0.0199(8) 0.0186(8) 0.0205(9) -0.0069(7) 0.0053(7) -0.0065(6) C11 0.0171(8) 0.0144(7) 0.0182(9) -0.0017(6) 0.0008(6) -0.0058(6) N5 0.0171(7) 0.0147(6) 0.0169(7) -0.0020(5) 0.0029(5) -0.0054(5) N7 0.0167(7) 0.0149(6) 0.0138(7) -0.0014(5) 0.0001(5) -0.0044(5) C7 0.0146(7) 0.0141(7) 0.0106(8) -0.0018(6) 0.0020(6) -0.0053(6) C8 0.0145(8) 0.0206(8) 0.0154(9) -0.0005(6) -0.0016(6) -0.0060(6) C12 0.0101(7) 0.0148(7) 0.0148(8) -0.0002(6) 0.0008(6) -0.0021(6) C14 0.0135(7) 0.0157(7) 0.0150(8) -0.0002(6) 0.0010(6) -0.0019(6) C10 0.0220(8) 0.0191(8) 0.0204(9) -0.0040(7) 0.0016(7) -0.0116(7) C9 0.0178(8) 0.0267(9) 0.0203(9) -0.0023(7) -0.0021(7) -0.0126(7) N6 0.0193(7) 0.0139(6) 0.0154(7) -0.0006(5) 0.0033(5) -0.0027(5) N8 0.0237(7) 0.0145(6) 0.0132(7) -0.0010(5) 0.0014(6) -0.0027(6) C13 0.0164(8) 0.0125(7) 0.0215(9) -0.0028(6) 0.0037(6) -0.0040(6) O1 0.0384(9) 0.0448(9) 0.0594(12) -0.0187(9) -0.0160(8) -0.0051(7) C21 0.0317(10) 0.0173(8) 0.0144(9) -0.0029(7) -0.0006(7) -0.0084(7) C15 0.0283(9) 0.0142(7) 0.0126(9) -0.0002(6) 0.0037(7) -0.0020(7) C16 0.0263(9) 0.0227(8) 0.0136(9) -0.0026(7) -0.0016(7) -0.0100(7) C18 0.0319(10) 0.0196(8) 0.0137(9) -0.0017(7) -0.0001(7) -0.0070(7) C17 0.0378(11) 0.0307(10) 0.0165(9) -0.0032(8) 0.0011(8) -0.0192(8) C26 0.0379(11) 0.0163(8) 0.0223(10) -0.0046(7) -0.0028(8) -0.0025(8) C20 0.0211(9) 0.0322(10) 0.0191(10) 0.0044(8) -0.0005(7) -0.0012(8) C19 0.0316(10) 0.0266(9) 0.0185(10) 0.0042(8) -0.0018(8) 0.0037(8) C25 0.0584(15) 0.0180(9) 0.0254(11) -0.0046(8) 0.0067(10) -0.0070(9) C22 0.0369(11) 0.0388(11) 0.0249(11) -0.0062(9) 0.0017(8) -0.0203(9) C23 0.0645(17) 0.0493(14) 0.0409(14) -0.0190(12) 0.0112(12) -0.0390(13) C24 0.0783(19) 0.0265(10) 0.0340(13) -0.0106(9) 0.0161(12) -0.0229(11) C27 0.0448(14) 0.0337(11) 0.0490(15) 0.0010(11) -0.0050(11) -0.0146(10) _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 1.9415(15) 2_756 ? Fe1 N1 1.9415(15) . ? Fe1 N4 1.9799(14) . ? Fe1 N4 1.9799(14) 2_756 ? Fe1 N2 1.9954(13) 2_756 ? Fe1 N2 1.9954(13) . ? Se1 C1 1.7957(17) . ? N1 C1 1.161(2) . ? C5 C4 1.377(2) . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? N2 C6 1.341(2) . ? N2 C2 1.356(2) . ? C2 C3 1.379(2) . ? C2 H2 0.9500 . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C6 N3 1.420(2) . ? Cl1 C13 1.7469(17) . ? N3 C12 1.387(2) . ? N3 C7 1.422(2) . ? N4 C7 1.342(2) . ? N4 C11 1.354(2) . ? C4 H4 0.9500 . ? C11 C10 1.374(2) . ? C11 H11 0.9500 . ? N5 C13 1.323(2) . ? N5 C12 1.346(2) . ? N7 C12 1.323(2) . ? N7 C14 1.353(2) . ? C7 C8 1.387(2) . ? C8 C9 1.379(2) . ? C8 H8 0.9500 . ? C14 N8 1.345(2) . ? C14 N6 1.364(2) . ? C10 C9 1.391(2) . ? C10 H10 0.9500 . ? C9 H9 0.9500 . ? N6 C13 1.308(2) . ? N8 C15 1.479(2) . ? N8 C21 1.483(2) . ? O1 C27 1.410(3) . ? O1 H1 0.8400 . ? C21 C22 1.520(3) . ? C21 C26 1.533(3) . ? C21 H21 1.0000 . ? C15 C16 1.524(3) . ? C15 C20 1.531(3) . ? C15 H15 1.0000 . ? C16 C17 1.528(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C19 1.518(3) . ? C18 C17 1.521(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C26 C25 1.529(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C20 C19 1.532(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C25 C24 1.511(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C22 C23 1.536(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.515(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 N1 Fe1 N1 180.000(1) 2_756 . ? N1 Fe1 N4 92.42(6) 2_756 . ? N1 Fe1 N4 87.58(6) . . ? N1 Fe1 N4 87.58(6) 2_756 2_756 ? N1 Fe1 N4 92.42(6) . 2_756 ? N4 Fe1 N4 180.000(1) . 2_756 ? N1 Fe1 N2 87.96(6) 2_756 2_756 ? N1 Fe1 N2 92.04(6) . 2_756 ? N4 Fe1 N2 93.43(5) . 2_756 ? N4 Fe1 N2 86.57(5) 2_756 2_756 ? N1 Fe1 N2 92.04(6) 2_756 . ? N1 Fe1 N2 87.96(6) . . ? N4 Fe1 N2 86.57(5) . . ? N4 Fe1 N2 93.43(5) 2_756 . ? N2 Fe1 N2 180.00(7) 2_756 . ? C1 N1 Fe1 173.74(13) . . ? N1 C1 Se1 179.60(16) . . ? C4 C5 C6 118.69(16) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C6 N2 C2 116.98(14) . . ? C6 N2 Fe1 122.02(11) . . ? C2 N2 Fe1 120.99(11) . . ? N2 C2 C3 122.77(16) . . ? N2 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C2 C3 C4 119.34(16) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? N2 C6 C5 123.40(15) . . ? N2 C6 N3 116.30(13) . . ? C5 C6 N3 120.22(15) . . ? C12 N3 C6 121.68(13) . . ? C12 N3 C7 121.19(13) . . ? C6 N3 C7 117.10(13) . . ? C7 N4 C11 117.04(14) . . ? C7 N4 Fe1 121.93(11) . . ? C11 N4 Fe1 120.88(11) . . ? C5 C4 C3 118.69(15) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N4 C11 C10 123.39(15) . . ? N4 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C13 N5 C12 110.65(14) . . ? C12 N7 C14 114.78(14) . . ? N4 C7 C8 123.05(15) . . ? N4 C7 N3 116.87(14) . . ? C8 C7 N3 119.99(14) . . ? C9 C8 C7 118.97(15) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? N7 C12 N5 127.33(15) . . ? N7 C12 N3 116.27(14) . . ? N5 C12 N3 116.36(14) . . ? N8 C14 N7 118.44(15) . . ? N8 C14 N6 118.07(15) . . ? N7 C14 N6 123.49(15) . . ? C11 C10 C9 118.69(16) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C8 C9 C10 118.80(16) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C13 N6 C14 112.86(14) . . ? C14 N8 C15 119.96(14) . . ? C14 N8 C21 121.50(14) . . ? C15 N8 C21 116.99(13) . . ? N6 C13 N5 130.65(15) . . ? N6 C13 Cl1 115.18(13) . . ? N5 C13 Cl1 114.17(13) . . ? C27 O1 H1 109.5 . . ? N8 C21 C22 113.47(15) . . ? N8 C21 C26 113.26(15) . . ? C22 C21 C26 112.41(16) . . ? N8 C21 H21 105.6 . . ? C22 C21 H21 105.6 . . ? C26 C21 H21 105.6 . . ? N8 C15 C16 111.23(14) . . ? N8 C15 C20 112.85(15) . . ? C16 C15 C20 111.31(14) . . ? N8 C15 H15 107.0 . . ? C16 C15 H15 107.0 . . ? C20 C15 H15 107.0 . . ? C15 C16 C17 110.32(15) . . ? C15 C16 H16A 109.6 . . ? C17 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? C17 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C19 C18 C17 110.55(16) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C17 C16 110.85(16) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C25 C26 C21 109.65(17) . . ? C25 C26 H26A 109.7 . . ? C21 C26 H26A 109.7 . . ? C25 C26 H26B 109.7 . . ? C21 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C15 C20 C19 110.40(17) . . ? C15 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C15 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C18 C19 C20 111.88(15) . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C24 C25 C26 110.89(18) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.0 . . ? C21 C22 C23 110.00(18) . . ? C21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C22 112.2(2) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 111.53(19) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.467 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.062 #=END data_7 _database_code_depnum_ccdc_archive 'CCDC 836949' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCS)2(DDT)2].4CH2Cl2 ; _chemical_name_common trans-[Fe(II)(NCS)2(DDT)2].4CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety '(C76 H56 Fe N18 S2), 4(C H2 Cl2)' _chemical_formula_sum 'C80 H64 Cl8 Fe N18 S2' _chemical_formula_weight 1681.06 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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 '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 9.4833(6) _cell_length_b 11.3020(6) _cell_length_c 18.8225(11) _cell_angle_alpha 82.031(3) _cell_angle_beta 85.455(3) _cell_angle_gamma 72.293(4) _cell_volume 1901.80(19) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 22155 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8420 _exptl_absorpt_correction_T_max 0.9941 _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 22155 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8626 _reflns_number_gt 4916 _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 8626 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _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 0.5000 0.5000 0.5000 0.01404(16) Uani 1 2 d S . . S1 S 0.56314(10) 0.21327(8) 0.31906(5) 0.0225(2) Uani 1 1 d . . . N5 N 0.9191(3) 0.2618(2) 0.35765(13) 0.0113(6) Uani 1 1 d . . . N7 N 0.9231(3) 0.2264(2) 0.23542(14) 0.0143(6) Uani 1 1 d . . . N6 N 0.7828(3) 0.4249(2) 0.27252(13) 0.0131(6) Uani 1 1 d . . . N3 N 0.7903(3) 0.4551(2) 0.39144(13) 0.0113(6) Uani 1 1 d . . . N8 N 1.0530(3) 0.0717(2) 0.32190(14) 0.0134(6) Uani 1 1 d . . . N2 N 0.5863(3) 0.6242(2) 0.41902(13) 0.0138(6) Uani 1 1 d . . . N9 N 0.7813(3) 0.3816(2) 0.15590(14) 0.0169(6) Uani 1 1 d . . . N4 N 0.7389(3) 0.4176(2) 0.51604(14) 0.0149(6) Uani 1 1 d . . . C13 C 0.8310(3) 0.3434(3) 0.22379(17) 0.0143(7) Uani 1 1 d . . . C12 C 0.8345(3) 0.3776(3) 0.33713(16) 0.0114(7) Uani 1 1 d . . . N1 N 0.5094(3) 0.3771(2) 0.42329(14) 0.0192(6) Uani 1 1 d . . . C16 C 1.1248(3) -0.0458(3) 0.43905(17) 0.0149(7) Uani 1 1 d . . . H16 H 1.0615 -0.0947 0.4338 0.018 Uiso 1 1 calc R . . C14 C 0.9608(3) 0.1914(3) 0.30334(17) 0.0128(7) Uani 1 1 d . . . C8 C 0.9926(3) 0.3616(3) 0.47308(17) 0.0139(7) Uani 1 1 d . . . H8 H 1.0626 0.3585 0.4338 0.017 Uiso 1 1 calc R . . C9 C 1.0388(3) 0.3190(3) 0.54191(17) 0.0158(7) Uani 1 1 d . . . H9 H 1.1413 0.2835 0.5506 0.019 Uiso 1 1 calc R . . C7 C 0.8419(3) 0.4093(3) 0.46203(17) 0.0132(7) Uani 1 1 d . . . C6 C 0.7067(3) 0.5840(3) 0.37599(16) 0.0132(7) Uani 1 1 d . . . C22 C 1.2106(4) -0.1182(3) 0.27605(17) 0.0182(7) Uani 1 1 d . . . H22 H 1.2889 -0.1144 0.3033 0.022 Uiso 1 1 calc R . . C5 C 0.7539(4) 0.6612(3) 0.32331(17) 0.0165(7) Uani 1 1 d . . . H5 H 0.8370 0.6282 0.2927 0.020 Uiso 1 1 calc R . . C17 C 1.2048(3) -0.0675(3) 0.50128(17) 0.0164(7) Uani 1 1 d . . . H17 H 1.1963 -0.1313 0.5384 0.020 Uiso 1 1 calc R . . C2 C 0.5165(4) 0.7488(3) 0.41094(18) 0.0184(7) Uani 1 1 d . . . H2 H 0.4330 0.7798 0.4418 0.022 Uiso 1 1 calc R . . C19 C 1.3103(3) 0.0963(3) 0.45400(17) 0.0181(7) Uani 1 1 d . . . H19 H 1.3734 0.1453 0.4593 0.022 Uiso 1 1 calc R . . C1 C 0.5312(3) 0.3093(3) 0.37949(17) 0.0169(7) Uani 1 1 d . . . C15 C 1.1381(3) 0.0476(3) 0.38512(17) 0.0139(7) Uani 1 1 d . . . C33 C 0.6924(3) 0.5073(3) 0.13320(17) 0.0179(7) Uani 1 1 d . . . C11 C 0.7871(3) 0.3795(3) 0.58323(17) 0.0160(7) Uani 1 1 d . . . H11 H 0.7158 0.3885 0.6220 0.019 Uiso 1 1 calc R . . C26 C 0.9590(4) -0.0357(3) 0.23972(18) 0.0199(8) Uani 1 1 d . . . H26 H 0.8640 0.0243 0.2418 0.024 Uiso 1 1 calc R . . C21 C 1.0726(4) -0.0268(3) 0.27884(16) 0.0146(7) Uani 1 1 d . . . C34 C 0.5644(4) 0.5249(3) 0.09679(18) 0.0209(8) Uani 1 1 d . . . H34 H 0.5365 0.4548 0.0875 0.025 Uiso 1 1 calc R . . C18 C 1.2962(3) 0.0043(3) 0.50846(17) 0.0182(8) Uani 1 1 d . . . H18 H 1.3496 -0.0095 0.5509 0.022 Uiso 1 1 calc R . . C3 C 0.5589(4) 0.8320(3) 0.36127(18) 0.0192(8) Uani 1 1 d . . . H3 H 0.5072 0.9188 0.3582 0.023 Uiso 1 1 calc R . . C23 C 1.2336(4) -0.2138(3) 0.23390(18) 0.0224(8) Uani 1 1 d . . . H23 H 1.3277 -0.2751 0.2323 0.027 Uiso 1 1 calc R . . C10 C 0.9345(3) 0.3281(3) 0.59862(18) 0.0175(7) Uani 1 1 d . . . H10 H 0.9639 0.2998 0.6466 0.021 Uiso 1 1 calc R . . C37 C 0.6456(4) 0.7290(3) 0.12294(19) 0.0301(9) Uani 1 1 d . . . H37 H 0.6733 0.7993 0.1321 0.036 Uiso 1 1 calc R . . C27 C 0.8055(4) 0.2908(3) 0.10612(17) 0.0192(8) Uani 1 1 d . . . C20 C 1.2327(3) 0.1172(3) 0.39177(17) 0.0159(7) Uani 1 1 d . . . H20 H 1.2445 0.1789 0.3539 0.019 Uiso 1 1 calc R . . C25 C 0.9837(4) -0.1318(3) 0.19761(18) 0.0242(8) Uani 1 1 d . . . H25 H 0.9055 -0.1368 0.1707 0.029 Uiso 1 1 calc R . . C32 C 0.9045(4) 0.2949(3) 0.04838(18) 0.0253(8) Uani 1 1 d . . . H32 H 0.9577 0.3548 0.0423 0.030 Uiso 1 1 calc R . . C24 C 1.1208(4) -0.2207(3) 0.19425(19) 0.0256(9) Uani 1 1 d . . . H24 H 1.1371 -0.2858 0.1649 0.031 Uiso 1 1 calc R . . C4 C 0.6792(4) 0.7876(3) 0.31518(18) 0.0194(8) Uani 1 1 d . . . H4 H 0.7096 0.8430 0.2788 0.023 Uiso 1 1 calc R . . C35 C 0.4775(4) 0.6451(3) 0.07406(18) 0.0257(9) Uani 1 1 d . . . H35 H 0.3904 0.6570 0.0488 0.031 Uiso 1 1 calc R . . C36 C 0.5164(4) 0.7472(3) 0.08779(19) 0.0290(9) Uani 1 1 d . . . H36 H 0.4553 0.8295 0.0733 0.035 Uiso 1 1 calc R . . C29 C 0.7459(4) 0.1212(3) 0.0649(2) 0.0327(10) Uani 1 1 d . . . H29 H 0.6923 0.0617 0.0706 0.039 Uiso 1 1 calc R . . C38 C 0.7347(4) 0.6095(3) 0.14491(18) 0.0236(8) Uani 1 1 d . . . H38 H 0.8244 0.5978 0.1679 0.028 Uiso 1 1 calc R . . C28 C 0.7255(4) 0.2060(3) 0.11455(19) 0.0247(8) Uani 1 1 d . . . H28 H 0.6568 0.2055 0.1541 0.030 Uiso 1 1 calc R . . C31 C 0.9240(4) 0.2088(4) -0.0007(2) 0.0343(10) Uani 1 1 d . . . H31 H 0.9929 0.2088 -0.0402 0.041 Uiso 1 1 calc R . . C30 C 0.8451(4) 0.1246(4) 0.0073(2) 0.0362(11) Uani 1 1 d . . . H30 H 0.8586 0.0676 -0.0271 0.043 Uiso 1 1 calc R . . Cl3 Cl 0.61965(12) 0.90374(10) 0.80071(5) 0.0439(3) Uani 1 1 d . . . Cl2 Cl 0.85163(11) 0.55401(10) 0.72651(6) 0.0459(3) Uani 1 1 d . . . Cl1 Cl 0.79780(14) 0.55176(11) 0.88090(7) 0.0579(3) Uani 1 1 d . . . C39 C 0.7191(4) 0.5670(4) 0.7976(2) 0.0353(10) Uani 1 1 d . . . H39A H 0.6695 0.5014 0.7982 0.042 Uiso 1 1 calc R . . H39B H 0.6429 0.6494 0.7899 0.042 Uiso 1 1 calc R . . Cl4 Cl 0.68384(11) 0.87515(10) 0.95153(5) 0.0379(3) Uani 1 1 d . . . C40 C 0.7469(4) 0.9090(4) 0.86316(19) 0.0297(9) Uani 1 1 d . . . H40A H 0.8441 0.8476 0.8539 0.036 Uiso 1 1 calc R . . H40B H 0.7606 0.9933 0.8569 0.036 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 0.0133(3) 0.0151(4) 0.0130(4) -0.0041(3) 0.0007(3) -0.0024(3) S1 0.0262(5) 0.0252(5) 0.0197(5) -0.0108(4) 0.0022(4) -0.0103(4) N5 0.0134(14) 0.0105(14) 0.0093(14) -0.0013(11) -0.0005(11) -0.0023(11) N7 0.0143(14) 0.0145(14) 0.0133(14) -0.0027(11) -0.0015(11) -0.0025(12) N6 0.0134(14) 0.0153(14) 0.0095(14) -0.0024(11) -0.0007(11) -0.0022(12) N3 0.0132(14) 0.0092(13) 0.0091(14) -0.0017(11) -0.0014(11) 0.0009(11) N8 0.0162(14) 0.0085(13) 0.0133(14) -0.0026(11) -0.0046(11) 0.0014(12) N2 0.0146(14) 0.0135(14) 0.0116(14) -0.0027(11) 0.0000(11) -0.0010(12) N9 0.0209(15) 0.0146(14) 0.0110(14) -0.0026(11) -0.0041(11) 0.0023(12) N4 0.0176(15) 0.0155(14) 0.0112(14) -0.0026(11) -0.0014(11) -0.0036(12) C13 0.0140(17) 0.0146(17) 0.0131(17) 0.0000(14) 0.0015(13) -0.0039(14) C12 0.0089(15) 0.0144(17) 0.0117(17) -0.0032(13) 0.0007(12) -0.0042(13) N1 0.0200(16) 0.0218(16) 0.0165(16) -0.0065(13) 0.0016(12) -0.0059(13) C16 0.0141(17) 0.0110(17) 0.0191(18) -0.0054(14) 0.0037(13) -0.0026(14) C14 0.0101(16) 0.0140(17) 0.0138(17) 0.0018(13) -0.0014(13) -0.0041(14) C8 0.0145(17) 0.0118(16) 0.0156(17) -0.0057(13) 0.0011(13) -0.0029(14) C9 0.0135(17) 0.0130(17) 0.0204(19) -0.0066(14) -0.0042(14) -0.0001(14) C7 0.0161(17) 0.0093(16) 0.0133(17) -0.0036(13) -0.0042(13) -0.0006(14) C6 0.0133(16) 0.0130(17) 0.0129(17) -0.0033(13) -0.0028(13) -0.0021(14) C22 0.0208(18) 0.0190(18) 0.0130(17) -0.0005(14) 0.0010(14) -0.0045(15) C5 0.0174(17) 0.0181(18) 0.0121(17) 0.0000(14) 0.0001(13) -0.0035(14) C17 0.0156(17) 0.0129(17) 0.0155(18) -0.0020(14) 0.0026(13) 0.0029(14) C2 0.0169(18) 0.0150(18) 0.0210(19) -0.0038(15) -0.0016(14) -0.0002(15) C19 0.0145(17) 0.0195(18) 0.0199(19) -0.0090(15) 0.0005(14) -0.0018(15) C1 0.0155(17) 0.0184(18) 0.0150(18) -0.0005(15) -0.0002(14) -0.0033(15) C15 0.0101(16) 0.0107(16) 0.0180(18) -0.0049(14) 0.0007(13) 0.0025(13) C33 0.0184(18) 0.0181(18) 0.0134(18) -0.0010(14) 0.0000(14) -0.0002(15) C11 0.0188(18) 0.0182(18) 0.0117(17) -0.0027(14) 0.0002(13) -0.0060(15) C26 0.0195(19) 0.0140(18) 0.023(2) -0.0016(15) -0.0010(15) -0.0008(15) C21 0.0222(18) 0.0108(16) 0.0104(17) -0.0007(13) 0.0027(13) -0.0051(14) C34 0.0227(19) 0.0194(19) 0.0190(19) -0.0039(15) 0.0013(15) -0.0035(16) C18 0.0134(17) 0.0221(19) 0.0138(18) -0.0064(15) -0.0007(13) 0.0043(15) C3 0.0184(18) 0.0115(17) 0.027(2) -0.0067(15) -0.0053(15) -0.0004(15) C23 0.027(2) 0.0180(19) 0.0167(19) -0.0038(15) 0.0011(15) 0.0011(16) C10 0.0221(19) 0.0142(18) 0.0145(18) -0.0018(14) -0.0073(14) -0.0012(15) C37 0.046(3) 0.019(2) 0.024(2) 0.0019(16) -0.0034(18) -0.0104(18) C27 0.0195(18) 0.0184(19) 0.0153(18) -0.0061(15) -0.0043(14) 0.0033(15) C20 0.0149(17) 0.0142(17) 0.0159(18) -0.0049(14) 0.0005(14) 0.0009(14) C25 0.034(2) 0.023(2) 0.0176(19) -0.0044(16) -0.0044(16) -0.0098(17) C32 0.023(2) 0.028(2) 0.020(2) -0.0056(16) -0.0048(15) 0.0024(17) C24 0.043(2) 0.0131(18) 0.020(2) -0.0089(15) 0.0020(17) -0.0047(17) C4 0.0241(19) 0.0131(17) 0.0192(19) 0.0027(14) -0.0046(15) -0.0038(15) C35 0.024(2) 0.025(2) 0.021(2) 0.0016(16) -0.0022(16) 0.0025(17) C36 0.033(2) 0.020(2) 0.024(2) 0.0027(16) 0.0003(17) 0.0052(17) C29 0.045(3) 0.016(2) 0.035(2) -0.0026(17) -0.019(2) -0.0035(18) C38 0.030(2) 0.022(2) 0.0185(19) 0.0017(15) -0.0061(15) -0.0073(17) C28 0.030(2) 0.0184(19) 0.021(2) -0.0007(15) -0.0073(16) 0.0006(17) C31 0.025(2) 0.048(3) 0.020(2) -0.0176(19) -0.0052(16) 0.009(2) C30 0.039(2) 0.027(2) 0.033(2) -0.0162(19) -0.021(2) 0.014(2) Cl3 0.0580(7) 0.0555(7) 0.0302(6) 0.0048(5) -0.0126(5) -0.0362(6) Cl2 0.0368(6) 0.0373(6) 0.0554(7) 0.0003(5) 0.0173(5) -0.0061(5) Cl1 0.0749(9) 0.0555(8) 0.0481(8) -0.0087(6) -0.0211(6) -0.0210(7) C39 0.035(2) 0.030(2) 0.038(3) -0.0027(19) 0.0011(19) -0.0054(19) Cl4 0.0436(6) 0.0499(6) 0.0228(5) -0.0025(5) 0.0049(4) -0.0200(5) C40 0.036(2) 0.034(2) 0.022(2) -0.0008(17) 0.0004(17) -0.0158(19) _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 2.117(3) 2_666 ? Fe1 N1 2.117(3) . ? Fe1 N4 2.200(2) . ? Fe1 N4 2.200(2) 2_666 ? Fe1 N2 2.207(3) . ? Fe1 N2 2.207(3) 2_666 ? S1 C1 1.629(3) . ? N5 C12 1.332(4) . ? N5 C14 1.344(4) . ? N7 C14 1.329(4) . ? N7 C13 1.344(4) . ? N6 C12 1.327(4) . ? N6 C13 1.346(4) . ? N3 C12 1.395(4) . ? N3 C7 1.425(4) . ? N3 C6 1.432(4) . ? N8 C14 1.383(4) . ? N8 C21 1.425(4) . ? N8 C15 1.439(4) . ? N2 C6 1.344(4) . ? N2 C2 1.354(4) . ? N9 C13 1.364(4) . ? N9 C33 1.439(4) . ? N9 C27 1.440(4) . ? N4 C7 1.345(4) . ? N4 C11 1.347(4) . ? N1 C1 1.167(4) . ? C16 C15 1.387(4) . ? C16 C17 1.399(4) . ? C8 C9 1.375(4) . ? C8 C7 1.387(4) . ? C9 C10 1.389(4) . ? C6 C5 1.368(4) . ? C22 C23 1.383(4) . ? C22 C21 1.401(4) . ? C5 C4 1.381(4) . ? C17 C18 1.379(4) . ? C2 C3 1.359(4) . ? C19 C18 1.384(4) . ? C19 C20 1.387(4) . ? C15 C20 1.384(4) . ? C33 C38 1.382(5) . ? C33 C34 1.389(4) . ? C11 C10 1.377(4) . ? C26 C25 1.385(4) . ? C26 C21 1.388(4) . ? C34 C35 1.385(4) . ? C3 C4 1.386(4) . ? C23 C24 1.378(5) . ? C37 C38 1.384(5) . ? C37 C36 1.385(5) . ? C27 C28 1.378(5) . ? C27 C32 1.384(5) . ? C25 C24 1.383(5) . ? C32 C31 1.396(5) . ? C35 C36 1.376(5) . ? C29 C30 1.383(6) . ? C29 C28 1.391(5) . ? C31 C30 1.365(6) . ? Cl3 C40 1.769(4) . ? Cl2 C39 1.752(4) . ? Cl1 C39 1.754(4) . ? Cl4 C40 1.754(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 N1 Fe1 N1 180.000(1) 2_666 . ? N1 Fe1 N4 89.36(10) 2_666 . ? N1 Fe1 N4 90.64(10) . . ? N1 Fe1 N4 90.64(10) 2_666 2_666 ? N1 Fe1 N4 89.36(10) . 2_666 ? N4 Fe1 N4 180.00(13) . 2_666 ? N1 Fe1 N2 89.08(10) 2_666 . ? N1 Fe1 N2 90.92(10) . . ? N4 Fe1 N2 80.23(9) . . ? N4 Fe1 N2 99.77(9) 2_666 . ? N1 Fe1 N2 90.92(10) 2_666 2_666 ? N1 Fe1 N2 89.08(10) . 2_666 ? N4 Fe1 N2 99.77(9) . 2_666 ? N4 Fe1 N2 80.23(9) 2_666 2_666 ? N2 Fe1 N2 180.000(1) . 2_666 ? C12 N5 C14 113.1(3) . . ? C14 N7 C13 113.6(3) . . ? C12 N6 C13 112.7(3) . . ? C12 N3 C7 119.5(2) . . ? C12 N3 C6 121.1(2) . . ? C7 N3 C6 119.1(2) . . ? C14 N8 C21 122.5(3) . . ? C14 N8 C15 118.6(2) . . ? C21 N8 C15 118.7(2) . . ? C6 N2 C2 116.5(3) . . ? C6 N2 Fe1 123.9(2) . . ? C2 N2 Fe1 119.6(2) . . ? C13 N9 C33 122.9(3) . . ? C13 N9 C27 119.3(3) . . ? C33 N9 C27 117.5(3) . . ? C7 N4 C11 117.4(3) . . ? C7 N4 Fe1 123.2(2) . . ? C11 N4 Fe1 119.3(2) . . ? N7 C13 N6 126.4(3) . . ? N7 C13 N9 116.1(3) . . ? N6 C13 N9 117.5(3) . . ? N6 C12 N5 127.6(3) . . ? N6 C12 N3 117.0(3) . . ? N5 C12 N3 115.3(3) . . ? C1 N1 Fe1 172.2(3) . . ? C15 C16 C17 119.7(3) . . ? N7 C14 N5 126.4(3) . . ? N7 C14 N8 118.7(3) . . ? N5 C14 N8 115.0(3) . . ? C9 C8 C7 118.7(3) . . ? C8 C9 C10 119.5(3) . . ? N4 C7 C8 122.7(3) . . ? N4 C7 N3 117.1(3) . . ? C8 C7 N3 120.2(3) . . ? N2 C6 C5 123.1(3) . . ? N2 C6 N3 115.7(3) . . ? C5 C6 N3 121.0(3) . . ? C23 C22 C21 120.5(3) . . ? C6 C5 C4 119.3(3) . . ? C18 C17 C16 119.7(3) . . ? N2 C2 C3 123.8(3) . . ? C18 C19 C20 120.3(3) . . ? N1 C1 S1 179.2(3) . . ? C20 C15 C16 120.4(3) . . ? C20 C15 N8 120.0(3) . . ? C16 C15 N8 119.6(3) . . ? C38 C33 C34 119.9(3) . . ? C38 C33 N9 121.3(3) . . ? C34 C33 N9 118.8(3) . . ? N4 C11 C10 123.5(3) . . ? C25 C26 C21 120.1(3) . . ? C26 C21 C22 118.8(3) . . ? C26 C21 N8 122.0(3) . . ? C22 C21 N8 119.2(3) . . ? C35 C34 C33 119.9(3) . . ? C17 C18 C19 120.3(3) . . ? C2 C3 C4 118.7(3) . . ? C24 C23 C22 120.4(3) . . ? C11 C10 C9 118.1(3) . . ? C38 C37 C36 120.7(4) . . ? C28 C27 C32 121.3(3) . . ? C28 C27 N9 120.0(3) . . ? C32 C27 N9 118.6(3) . . ? C15 C20 C19 119.5(3) . . ? C24 C25 C26 120.8(3) . . ? C27 C32 C31 118.2(4) . . ? C23 C24 C25 119.4(3) . . ? C5 C4 C3 118.5(3) . . ? C36 C35 C34 120.5(3) . . ? C35 C36 C37 119.4(3) . . ? C30 C29 C28 119.2(4) . . ? C33 C38 C37 119.6(3) . . ? C27 C28 C29 119.7(4) . . ? C30 C31 C32 120.8(4) . . ? C31 C30 C29 120.8(4) . . ? Cl2 C39 Cl1 112.1(2) . . ? Cl4 C40 Cl3 111.0(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.368 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.088 #=END data_8 _database_code_depnum_ccdc_archive 'CCDC 836950' #TrackingRef 'MegaCIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[Fe(II)(NCSe)2(DDT)2].4CH2Cl2 ; _chemical_name_common trans-[Fe(II)(NCSe)2(DDT)2].4CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety (C76 _chemical_formula_sum 'C80 H64 Cl8 Fe N18 Se2' _chemical_formula_weight 1774.86 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' Cl Cl 0.1484 0.1585 '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' Se Se -0.0929 2.2259 '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 9.5165(5) _cell_length_b 11.3385(7) _cell_length_c 18.8082(10) _cell_angle_alpha 82.509(2) _cell_angle_beta 85.500(3) _cell_angle_gamma 72.142(2) _cell_volume 1913.60(19) _cell_formula_units_Z 1 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 15932 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6640 _exptl_absorpt_correction_T_max 0.9853 _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 15932 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6659 _reflns_number_gt 4484 _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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 6659 _refine_ls_number_parameters 493 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.5000 0.5000 0.5000 0.0108(2) Uani 1 2 d S . . Se1 Se 0.55927(5) 0.20788(5) 0.31557(3) 0.02087(14) Uani 1 1 d . . . N5 N 0.9148(4) 0.2634(3) 0.35905(18) 0.0110(8) Uani 1 1 d . . . N1 N 0.5125(4) 0.3805(4) 0.42547(19) 0.0165(9) Uani 1 1 d . . . C1 C 0.5296(4) 0.3134(4) 0.3824(2) 0.0151(11) Uani 1 1 d . . . N7 N 0.9213(4) 0.2282(3) 0.23615(18) 0.0103(8) Uani 1 1 d . . . N6 N 0.7794(4) 0.4256(3) 0.27401(18) 0.0118(8) Uani 1 1 d . . . N3 N 0.7826(4) 0.4551(3) 0.39381(17) 0.0099(8) Uani 1 1 d . . . C13 C 0.8280(4) 0.3448(4) 0.2247(2) 0.0114(10) Uani 1 1 d . . . C14 C 0.9575(4) 0.1934(4) 0.3041(2) 0.0110(10) Uani 1 1 d . . . C5 C 0.7438(5) 0.6614(4) 0.3276(2) 0.0193(11) Uani 1 1 d . . . H5 H 0.8275 0.6298 0.2970 0.023 Uiso 1 1 calc R . . N9 N 0.7805(4) 0.3827(3) 0.15708(18) 0.0147(9) Uani 1 1 d . . . C17 C 1.2040(5) -0.0642(4) 0.5006(2) 0.0150(10) Uani 1 1 d . . . H17 H 1.1969 -0.1285 0.5373 0.018 Uiso 1 1 calc R . . C8 C 0.9806(5) 0.3625(4) 0.4768(2) 0.0170(11) Uani 1 1 d . . . H8 H 1.0519 0.3573 0.4381 0.020 Uiso 1 1 calc R . . C21 C 1.0703(5) -0.0245(4) 0.2789(2) 0.0146(10) Uani 1 1 d . . . N4 N 0.7263(4) 0.4214(3) 0.51762(18) 0.0163(9) Uani 1 1 d . . . N2 N 0.5767(4) 0.6200(3) 0.42293(19) 0.0149(9) Uani 1 1 d . . . C2 C 0.5055(5) 0.7443(4) 0.4163(3) 0.0202(11) Uani 1 1 d . . . H2 H 0.4225 0.7741 0.4477 0.024 Uiso 1 1 calc R . . C9 C 1.0242(5) 0.3217(4) 0.5464(3) 0.0224(12) Uani 1 1 d . . . H9 H 1.1259 0.2855 0.5559 0.027 Uiso 1 1 calc R . . C11 C 0.7737(5) 0.3847(4) 0.5856(2) 0.0200(11) Uani 1 1 d . . . H11 H 0.7016 0.3950 0.6241 0.024 Uiso 1 1 calc R . . C4 C 0.6673(5) 0.7867(4) 0.3210(2) 0.0213(12) Uani 1 1 d . . . H4 H 0.6969 0.8432 0.2857 0.026 Uiso 1 1 calc R . . C15 C 1.1337(4) 0.0510(4) 0.3861(2) 0.0112(10) Uani 1 1 d . . . C34 C 0.5644(5) 0.5242(4) 0.0976(2) 0.0207(11) Uani 1 1 d . . . H34 H 0.5369 0.4540 0.0886 0.025 Uiso 1 1 calc R . . C3 C 0.5458(5) 0.8287(5) 0.3673(3) 0.0251(12) Uani 1 1 d . . . H3 H 0.4918 0.9147 0.3648 0.030 Uiso 1 1 calc R . . N8 N 1.0500(4) 0.0743(3) 0.32230(18) 0.0119(8) Uani 1 1 d . . . C20 C 1.2262(4) 0.1220(4) 0.3934(2) 0.0129(10) Uani 1 1 d . . . H20 H 1.2359 0.1846 0.3563 0.015 Uiso 1 1 calc R . . C16 C 1.1245(4) -0.0441(4) 0.4389(2) 0.0128(10) Uani 1 1 d . . . H16 H 1.0644 -0.0951 0.4330 0.015 Uiso 1 1 calc R . . C38 C 0.7327(5) 0.6107(4) 0.1465(2) 0.0212(11) Uani 1 1 d . . . H38 H 0.8211 0.5997 0.1702 0.025 Uiso 1 1 calc R . . C12 C 0.8299(4) 0.3778(4) 0.3385(2) 0.0112(10) Uani 1 1 d . . . C35 C 0.4777(5) 0.6443(4) 0.0746(2) 0.0234(12) Uani 1 1 d . . . H35 H 0.3912 0.6564 0.0491 0.028 Uiso 1 1 calc R . . C19 C 1.3041(5) 0.1009(4) 0.4552(2) 0.0159(10) Uani 1 1 d . . . H19 H 1.3660 0.1506 0.4607 0.019 Uiso 1 1 calc R . . C25 C 0.9776(6) -0.1300(4) 0.1994(2) 0.0252(12) Uani 1 1 d . . . H25 H 0.8987 -0.1353 0.1733 0.030 Uiso 1 1 calc R . . C24 C 1.1151(6) -0.2184(4) 0.1945(2) 0.0276(13) Uani 1 1 d . . . H24 H 1.1302 -0.2841 0.1654 0.033 Uiso 1 1 calc R . . C33 C 0.6915(5) 0.5080(4) 0.1340(2) 0.0164(11) Uani 1 1 d . . . C7 C 0.8315(5) 0.4111(4) 0.4646(2) 0.0144(10) Uani 1 1 d U . . C23 C 1.2291(5) -0.2100(4) 0.2320(2) 0.0218(11) Uani 1 1 d . . . H23 H 1.3233 -0.2704 0.2289 0.026 Uiso 1 1 calc R . . C18 C 1.2929(5) 0.0084(4) 0.5091(2) 0.0165(11) Uani 1 1 d . . . H18 H 1.3461 -0.0050 0.5515 0.020 Uiso 1 1 calc R . . C26 C 0.9541(5) -0.0347(4) 0.2418(2) 0.0184(11) Uani 1 1 d . . . H26 H 0.8589 0.0240 0.2457 0.022 Uiso 1 1 calc R . . C22 C 1.2076(5) -0.1140(4) 0.2744(2) 0.0171(11) Uani 1 1 d . . . H22 H 1.2870 -0.1094 0.3005 0.021 Uiso 1 1 calc R . . C10 C 0.9185(5) 0.3340(4) 0.6019(3) 0.0240(12) Uani 1 1 d . . . H10 H 0.9461 0.3078 0.6502 0.029 Uiso 1 1 calc R . . C37 C 0.6434(6) 0.7291(5) 0.1241(2) 0.0289(13) Uani 1 1 d . . . H37 H 0.6701 0.7996 0.1335 0.035 Uiso 1 1 calc R . . C36 C 0.5174(5) 0.7463(5) 0.0887(3) 0.0266(12) Uani 1 1 d . . . H36 H 0.4571 0.8283 0.0738 0.032 Uiso 1 1 calc R . . C6 C 0.6966(5) 0.5822(4) 0.3798(2) 0.0134(10) Uani 1 1 d . . . C27 C 0.8070(5) 0.2924(4) 0.1056(2) 0.0169(11) Uani 1 1 d . . . C28 C 0.7284(5) 0.2073(4) 0.1137(2) 0.0243(12) Uani 1 1 d . . . H28 H 0.6603 0.2057 0.1533 0.029 Uiso 1 1 calc R . . C32 C 0.9048(5) 0.2972(5) 0.0486(2) 0.0257(12) Uani 1 1 d . . . H32 H 0.9572 0.3571 0.0437 0.031 Uiso 1 1 calc R . . C29 C 0.7507(6) 0.1241(5) 0.0629(3) 0.0332(14) Uani 1 1 d . . . H29 H 0.6978 0.0645 0.0678 0.040 Uiso 1 1 calc R . . C31 C 0.9262(6) 0.2133(5) -0.0018(3) 0.0350(14) Uani 1 1 d . . . H31 H 0.9944 0.2153 -0.0413 0.042 Uiso 1 1 calc R . . Cl4 Cl 0.68505(15) 0.87780(13) 0.95342(7) 0.0379(4) Uani 1 1 d . . . Cl2 Cl 0.86279(15) 0.55260(13) 0.73200(8) 0.0462(4) Uani 1 1 d . . . Cl3 Cl 0.63118(17) 0.89838(15) 0.80202(8) 0.0498(4) Uani 1 1 d . . . Cl1 Cl 0.79895(19) 0.54765(15) 0.88602(9) 0.0582(5) Uani 1 1 d . . . C39 C 0.7266(6) 0.5639(5) 0.8013(3) 0.0381(14) Uani 1 1 d . . . H39A H 0.6503 0.6459 0.7935 0.046 Uiso 1 1 calc R . . H39B H 0.6783 0.4985 0.7997 0.046 Uiso 1 1 calc R . . C40 C 0.7521(5) 0.9078(5) 0.8656(2) 0.0296(13) Uani 1 1 d . . . H40B H 0.8501 0.8466 0.8579 0.036 Uiso 1 1 calc R . . H40A H 0.7646 0.9921 0.8589 0.036 Uiso 1 1 calc R . . C30 C 0.8493(6) 0.1276(5) 0.0053(3) 0.0380(15) Uani 1 1 d . . . H30 H 0.8640 0.0706 -0.0293 0.046 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 0.0119(5) 0.0095(5) 0.0100(5) -0.0030(4) 0.0002(4) -0.0011(4) Se1 0.0243(3) 0.0234(3) 0.0191(3) -0.0057(2) -0.0004(2) -0.0120(2) N5 0.013(2) 0.006(2) 0.013(2) -0.0037(16) -0.0011(16) -0.0010(16) N1 0.013(2) 0.023(2) 0.014(2) -0.0020(18) 0.0039(17) -0.0071(18) C1 0.008(2) 0.021(3) 0.017(3) 0.004(2) -0.004(2) -0.006(2) N7 0.013(2) 0.007(2) 0.011(2) -0.0006(15) -0.0037(15) -0.0022(16) N6 0.014(2) 0.011(2) 0.009(2) 0.0002(16) -0.0038(16) -0.0015(17) N3 0.015(2) 0.007(2) 0.0057(18) -0.0001(15) -0.0046(15) 0.0011(16) C13 0.010(2) 0.011(3) 0.013(2) -0.003(2) 0.0003(19) -0.003(2) C14 0.007(2) 0.011(3) 0.015(2) -0.002(2) 0.0005(19) -0.004(2) C5 0.027(3) 0.015(3) 0.016(3) -0.001(2) -0.008(2) -0.006(2) N9 0.018(2) 0.013(2) 0.011(2) -0.0030(16) -0.0032(16) -0.0003(17) C17 0.016(2) 0.013(3) 0.010(2) 0.0018(19) 0.0046(19) 0.001(2) C8 0.023(3) 0.008(3) 0.020(3) -0.008(2) -0.009(2) -0.001(2) C21 0.024(3) 0.011(3) 0.010(2) 0.0000(19) -0.001(2) -0.006(2) N4 0.031(2) 0.008(2) 0.011(2) 0.0011(16) -0.0091(17) -0.0070(18) N2 0.015(2) 0.009(2) 0.018(2) -0.0038(16) -0.0029(17) 0.0028(17) C2 0.020(3) 0.012(3) 0.028(3) -0.007(2) -0.010(2) 0.002(2) C9 0.025(3) 0.011(3) 0.031(3) -0.005(2) -0.016(2) 0.000(2) C11 0.039(3) 0.008(3) 0.014(3) 0.001(2) -0.004(2) -0.009(2) C4 0.035(3) 0.009(3) 0.022(3) 0.003(2) -0.016(2) -0.008(2) C15 0.008(2) 0.012(3) 0.010(2) -0.0026(19) -0.0010(18) 0.003(2) C34 0.024(3) 0.019(3) 0.019(3) -0.001(2) 0.001(2) -0.007(2) C3 0.026(3) 0.014(3) 0.032(3) -0.008(2) -0.015(2) 0.004(2) N8 0.015(2) 0.007(2) 0.011(2) -0.0039(16) -0.0039(16) 0.0008(17) C20 0.010(2) 0.006(2) 0.018(3) 0.0017(19) -0.0009(19) 0.003(2) C16 0.010(2) 0.007(2) 0.018(3) -0.005(2) 0.0018(19) 0.0034(19) C38 0.022(3) 0.019(3) 0.020(3) 0.003(2) -0.007(2) -0.003(2) C12 0.007(2) 0.013(3) 0.015(2) -0.002(2) 0.0030(19) -0.006(2) C35 0.018(3) 0.023(3) 0.019(3) 0.007(2) -0.002(2) 0.004(2) C19 0.017(3) 0.017(3) 0.014(3) -0.005(2) -0.002(2) -0.004(2) C25 0.039(3) 0.019(3) 0.022(3) -0.005(2) -0.011(2) -0.011(3) C24 0.054(4) 0.010(3) 0.017(3) -0.004(2) -0.005(3) -0.006(3) C33 0.021(3) 0.015(3) 0.007(2) 0.0039(19) -0.002(2) 0.002(2) C7 0.0162(13) 0.0130(13) 0.0142(13) -0.0028(9) -0.0017(9) -0.0038(9) C23 0.030(3) 0.011(3) 0.019(3) -0.005(2) 0.001(2) 0.002(2) C18 0.013(2) 0.024(3) 0.008(2) -0.006(2) -0.0012(19) 0.001(2) C26 0.024(3) 0.013(3) 0.019(3) -0.001(2) -0.002(2) -0.007(2) C22 0.021(3) 0.012(3) 0.016(3) -0.003(2) -0.002(2) 0.000(2) C10 0.040(3) 0.015(3) 0.019(3) -0.003(2) -0.012(2) -0.007(2) C37 0.049(4) 0.020(3) 0.016(3) 0.001(2) -0.005(3) -0.009(3) C36 0.032(3) 0.017(3) 0.021(3) 0.004(2) 0.000(2) 0.003(2) C6 0.019(3) 0.010(3) 0.013(2) -0.005(2) -0.008(2) -0.003(2) C27 0.025(3) 0.014(3) 0.006(2) -0.0006(19) -0.007(2) 0.003(2) C28 0.030(3) 0.022(3) 0.019(3) -0.002(2) -0.004(2) -0.003(2) C32 0.020(3) 0.034(3) 0.019(3) -0.006(2) -0.003(2) 0.000(2) C29 0.053(4) 0.018(3) 0.025(3) 0.000(2) -0.023(3) 0.000(3) C31 0.025(3) 0.052(4) 0.017(3) -0.011(3) -0.003(2) 0.007(3) Cl4 0.0438(9) 0.0510(10) 0.0218(7) -0.0026(6) 0.0059(6) -0.0211(8) Cl2 0.0375(9) 0.0329(9) 0.0620(11) -0.0027(7) 0.0173(7) -0.0071(7) Cl3 0.0709(11) 0.0629(11) 0.0331(8) 0.0076(7) -0.0182(7) -0.0472(9) Cl1 0.0753(12) 0.0562(11) 0.0487(10) -0.0068(8) -0.0219(9) -0.0228(9) C39 0.036(3) 0.039(4) 0.034(3) -0.002(3) 0.002(3) -0.006(3) C40 0.033(3) 0.034(3) 0.024(3) -0.001(2) -0.004(2) -0.014(3) C30 0.044(4) 0.031(4) 0.027(3) -0.016(3) -0.025(3) 0.018(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 2.045(4) 2_666 ? Fe1 N1 2.045(4) . ? Fe1 N4 2.098(4) 2_666 ? Fe1 N4 2.098(4) . ? Fe1 N2 2.101(4) 2_666 ? Fe1 N2 2.101(4) . ? Se1 C1 1.795(5) . ? N5 C12 1.326(5) . ? N5 C14 1.347(5) . ? N1 C1 1.151(5) . ? N7 C14 1.327(5) . ? N7 C13 1.348(5) . ? N6 C12 1.326(5) . ? N6 C13 1.344(5) . ? N3 C12 1.405(5) . ? N3 C7 1.420(5) . ? N3 C6 1.425(5) . ? C13 N9 1.355(5) . ? C14 N8 1.383(5) . ? C5 C4 1.378(6) . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? N9 C33 1.443(5) . ? N9 C27 1.453(5) . ? C17 C18 1.379(6) . ? C17 C16 1.390(6) . ? C17 H17 0.9500 . ? C8 C9 1.381(6) . ? C8 C7 1.382(6) . ? C8 H8 0.9500 . ? C21 C22 1.391(6) . ? C21 C26 1.394(6) . ? C21 N8 1.428(5) . ? N4 C7 1.347(5) . ? N4 C11 1.360(5) . ? N2 C6 1.337(5) . ? N2 C2 1.357(5) . ? C2 C3 1.360(7) . ? C2 H2 0.9500 . ? C9 C10 1.382(6) . ? C9 H9 0.9500 . ? C11 C10 1.362(6) . ? C11 H11 0.9500 . ? C4 C3 1.391(7) . ? C4 H4 0.9500 . ? C15 C16 1.387(6) . ? C15 C20 1.387(6) . ? C15 N8 1.443(5) . ? C34 C33 1.387(6) . ? C34 C35 1.392(6) . ? C34 H34 0.9500 . ? C3 H3 0.9500 . ? C20 C19 1.381(6) . ? C20 H20 0.9500 . ? C16 H16 0.9500 . ? C38 C37 1.382(6) . ? C38 C33 1.390(6) . ? C38 H38 0.9500 . ? C35 C36 1.383(6) . ? C35 H35 0.9500 . ? C19 C18 1.383(6) . ? C19 H19 0.9500 . ? C25 C26 1.379(6) . ? C25 C24 1.388(6) . ? C25 H25 0.9500 . ? C24 C23 1.372(6) . ? C24 H24 0.9500 . ? C23 C22 1.389(6) . ? C23 H23 0.9500 . ? C18 H18 0.9500 . ? C26 H26 0.9500 . ? C22 H22 0.9500 . ? C10 H10 0.9500 . ? C37 C36 1.366(6) . ? C37 H37 0.9500 . ? C36 H36 0.9500 . ? C27 C32 1.369(6) . ? C27 C28 1.378(6) . ? C28 C29 1.389(6) . ? C28 H28 0.9500 . ? C32 C31 1.390(7) . ? C32 H32 0.9500 . ? C29 C30 1.381(7) . ? C29 H29 0.9500 . ? C31 C30 1.373(7) . ? C31 H31 0.9500 . ? Cl4 C40 1.752(5) . ? Cl2 C39 1.752(5) . ? Cl3 C40 1.758(5) . ? Cl1 C39 1.751(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40B 0.9900 . ? C40 H40A 0.9900 . ? C30 H30 0.9500 . ? 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 180.000(1) 2_666 . ? N1 Fe1 N4 90.76(13) 2_666 2_666 ? N1 Fe1 N4 89.24(13) . 2_666 ? N1 Fe1 N4 89.24(13) 2_666 . ? N1 Fe1 N4 90.76(13) . . ? N4 Fe1 N4 180.0 2_666 . ? N1 Fe1 N2 90.85(14) 2_666 2_666 ? N1 Fe1 N2 89.15(14) . 2_666 ? N4 Fe1 N2 82.45(13) 2_666 2_666 ? N4 Fe1 N2 97.55(13) . 2_666 ? N1 Fe1 N2 89.15(14) 2_666 . ? N1 Fe1 N2 90.85(14) . . ? N4 Fe1 N2 97.55(13) 2_666 . ? N4 Fe1 N2 82.45(13) . . ? N2 Fe1 N2 180.000(1) 2_666 . ? C12 N5 C14 112.5(4) . . ? C1 N1 Fe1 175.2(3) . . ? N1 C1 Se1 179.1(4) . . ? C14 N7 C13 113.7(3) . . ? C12 N6 C13 112.7(4) . . ? C12 N3 C7 120.3(3) . . ? C12 N3 C6 121.5(3) . . ? C7 N3 C6 117.9(3) . . ? N6 C13 N7 125.9(4) . . ? N6 C13 N9 117.8(4) . . ? N7 C13 N9 116.3(4) . . ? N7 C14 N5 126.6(4) . . ? N7 C14 N8 118.6(4) . . ? N5 C14 N8 114.7(4) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C13 N9 C33 123.4(4) . . ? C13 N9 C27 119.8(4) . . ? C33 N9 C27 116.5(3) . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C22 C21 C26 119.1(4) . . ? C22 C21 N8 119.7(4) . . ? C26 C21 N8 121.2(4) . . ? C7 N4 C11 116.6(4) . . ? C7 N4 Fe1 123.2(3) . . ? C11 N4 Fe1 120.1(3) . . ? C6 N2 C2 116.3(4) . . ? C6 N2 Fe1 123.9(3) . . ? C2 N2 Fe1 119.8(3) . . ? N2 C2 C3 124.0(4) . . ? N2 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N4 C11 C10 123.9(4) . . ? N4 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C16 C15 C20 120.2(4) . . ? C16 C15 N8 120.1(4) . . ? C20 C15 N8 119.7(4) . . ? C33 C34 C35 119.3(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C2 C3 C4 118.8(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C14 N8 C21 122.6(3) . . ? C14 N8 C15 118.4(3) . . ? C21 N8 C15 119.0(3) . . ? C19 C20 C15 119.5(4) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C37 C38 C33 119.2(4) . . ? C37 C38 H38 120.4 . . ? C33 C38 H38 120.4 . . ? N6 C12 N5 128.4(4) . . ? N6 C12 N3 116.7(4) . . ? N5 C12 N3 114.8(4) . . ? C36 C35 C34 120.1(5) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C20 C19 C18 120.8(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C26 C25 C24 120.9(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C34 C33 C38 120.3(4) . . ? C34 C33 N9 118.5(4) . . ? C38 C33 N9 121.2(4) . . ? N4 C7 C8 122.9(4) . . ? N4 C7 N3 116.8(4) . . ? C8 C7 N3 120.4(4) . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C17 C18 C19 119.5(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C25 C26 C21 119.9(4) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C11 C10 C9 118.4(4) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C36 C37 C38 121.0(5) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C36 C35 120.0(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? N2 C6 C5 123.5(4) . . ? N2 C6 N3 116.0(4) . . ? C5 C6 N3 120.3(4) . . ? C32 C27 C28 121.7(4) . . ? C32 C27 N9 119.2(4) . . ? C28 C27 N9 119.0(4) . . ? C27 C28 C29 118.7(5) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C27 C32 C31 119.1(5) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C30 C31 C32 120.2(5) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? Cl1 C39 Cl2 112.3(3) . . ? Cl1 C39 H39A 109.1 . . ? Cl2 C39 H39A 109.1 . . ? Cl1 C39 H39B 109.1 . . ? Cl2 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? Cl4 C40 Cl3 111.4(3) . . ? Cl4 C40 H40B 109.4 . . ? Cl3 C40 H40B 109.4 . . ? Cl4 C40 H40A 109.4 . . ? Cl3 C40 H40A 109.4 . . ? H40B C40 H40A 108.0 . . ? C31 C30 C29 120.1(5) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.606 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.097 #=END OF CIF