# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author_name 'Leokadiya Zorina' _publ_contact_author_address ; Institute of Solid State Physics RAS Institutskaya str. 2 Chernogolovka Moscow District 142432 RUSSIAN FEDERATION ; _publ_contact_author_email ZORINA@ISSP.AC.RU # File ET_NP.cif #=================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Molecular conductors with the common and robust building block (BEDT-TTF)~2~NP but different band filling: \b"-(BEDT-TTF)~2~[NP], \b"-(BEDT-TTF)~3~[NP][EG] and \b"-(BEDT-TTF)~4~A[NP]~2~, where A = Na^+^, K^+^, Rb^+^, ...; NP = [FeNO(CN)~5~]^2-^ and EG = C~2~H~4~(OH)~2~ ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Simonov, Sergey V.' ;? ; ; Institute of Solid State Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Zorina, Leokadiya V.' ;? ; ; Institute of Solid State Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Khasanov, Salavat S.' ;? ; ; Institute of Solid State Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Shibaeva, Rimma P.' ;? ; ; Institute of Solid State Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Shevyakova, Irina Yu.' ;? ; ; Institute of Problems of Chemical Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Buravov, Lev I.' ;? ; ; Institute of Problems of Chemical Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Yagubskii, Eduard B.' ;? ; ; Institute of Problems of Chemical Physics, Russian Academy of Sciences 142432 Chernogolovka, MD Russia ; 'Canadell, Enric' ;? ; ; Institut de Ciencia de Materials de Barcelona (CSIC) Campus de la U.A.B. E-08193 Bellaterra Spain ; # File ET_NP.cif #===================================================================== data_(1) _database_code_depnum_ccdc_archive 'CCDC 287001' _vrf_PLAT_241_1 ; PROBLEM: High Ueq as Compared to Neighbours for N13 and O14 RESPONSE: The non-centrosymmetric nitroprusside anion [FeNO(CN)5] occupies an inversion center in the structure of (1). Fe-N-O bonds should be shorter than Fe-C-N ones but it is not possible to separate disordered NO- and opposite CN-groups in this structure, therefore they are defined at the same sites (EXYZ and EADP restraints for corresponding atoms). This is the reason of high Ueq for mixed (C13+N14) and (N13+O14) positions as compared with other ordered CN-ligands of anion. ; _vrf_PLAT_242_1 ; PROBLEM: Low Ueq as Compared to Neighbours for C13 and N14 RESPONSE: Ueq of these atoms are high in comparison with C11 and C12, see response to PLAT_241_1. ; _vrf_PLAT_027_1 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............24.98 Deg. RESPONSE: This value is close to 25.24 degrees required for publication in the IUCr journals in the case of MoKa radiation. Crystals of organic conductors are composed mainly of light atoms and additionally have small size, so it is difficult to obtain reflections with intensities I > 2sigma(I) at higher theta. ; _vrf_PLAT_029_1 ; PROBLEM: _diffrn_measured_fraction_theta_full Low .......0.98 RESPONSE: This value is very close to 1.0. ; _vrf_PLAT_250_1 ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....2.59 RESPONSE: Some intrinsic disorder of S- and C-atoms in the outer cycles of organic donor molecules is typical for the room temperature crystal structures of organic molecular conductors. In the structure of (1) additional disorder of anion exists (described above, see response to PLAT_241_1). ; _vrf_PLAT_301_1 ; PROBLEM: Main Residue Disorder ......................... 9.00 Perc. RESPONSE: This is connected with anion disordering (see response to PLAT_241_1). ; _vrf_PLAT_341_1 ; PROBLEM: Low Bond Precision on C-C bonds (x 1000) Ang ...8 RESPONSE: The bonds between disordered C-atoms of outer ethylene groups of organic donor BEDT-TTF have the lower accuracy (see response to PLAT_250_1). ; _vrf_PLAT_480_1 ; PROBLEM: Long H...A H-Bond Reported....for several H-atoms RESPONSE: In fact these are not real H-bonds but shortened H-contacts with H...A distances < 3.0\%A. Intermolecular contacts of different types shorter than the sum of van-der-Waals radii of corresponding atoms play an important role in the structures of organic molecular conductors. ; # CHEMICAL DATA _chemical_name_systematic ; bis(bis(ethylenedithio)tetrathiafulvalene)(pentacyano-(nitroso)-iron) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_iupac '2(C10 H8 S8), C5 Fe N6 O' _chemical_formula_moiety '2(C10 H8 S8), C5 Fe N6 O' _chemical_formula_sum 'C25 H16 Fe N6 O S16' _chemical_formula_weight 985.25 _chemical_compound_source 'synthesised by authors, see text' _chemical_absolute_configuration ? 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.686(1) _cell_length_b 8.672(1) _cell_length_c 16.095(3) _cell_angle_alpha 99.91(1) _cell_angle_beta 101.54(1) _cell_angle_gamma 94.59(1) _cell_volume 894.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.51 _cell_measurement_theta_max 16.12 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.392 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'WINGX (Farrugia, 1999)' _exptl_absorpt_correction_T_min 0.6059 _exptl_absorpt_correction_T_max 0.9529 #========================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 5 _diffrn_standards_interval_count 500 _diffrn_standards_interval_time 150 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3457 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.978 _reflns_number_total 3079 _reflns_number_gt 2087 _reflns_threshold_expression I>2\sigma(I) _computing_data_collection 'CAD-4 (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD-4 (Enraf-Nonius, 1992)' _computing_data_reduction 'WINGX (Farrugia, 1999)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' #========================================================================= # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+1.0999P] 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_number_reflns 3079 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.547 _refine_diff_density_min -0.566 #========================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.54355(19) 0.36869(17) 0.37172(9) 0.0312(3) Uani 1 1 d . . . S2 S 0.1151(2) 0.42030(18) 0.33547(9) 0.0352(4) Uani 1 1 d . . . S3 S 0.4758(2) 0.20983(17) 0.53177(9) 0.0328(4) Uani 1 1 d . . . S4 S 0.0514(2) 0.27731(18) 0.50285(9) 0.0335(4) Uani 1 1 d . . . S5 S 0.6444(2) 0.4937(2) 0.22527(10) 0.0395(4) Uani 1 1 d . . . S6 S 0.1237(2) 0.5488(2) 0.17995(10) 0.0440(4) Uani 1 1 d . . . S7 S 0.4616(2) 0.05278(18) 0.67811(9) 0.0348(4) Uani 1 1 d . . . S8 S -0.0555(2) 0.1278(2) 0.64090(10) 0.0442(4) Uani 1 1 d . . . C1 C 0.3094(8) 0.3524(6) 0.4005(3) 0.0282(12) Uani 1 1 d . . . C2 C 0.2830(7) 0.2880(6) 0.4705(3) 0.0268(12) Uani 1 1 d . . . C3 C 0.4631(8) 0.4548(6) 0.2840(3) 0.0276(12) Uani 1 1 d . . . C4 C 0.2599(8) 0.4772(6) 0.2653(3) 0.0297(12) Uani 1 1 d . . . C5 C 0.3295(7) 0.1456(6) 0.6000(3) 0.0241(11) Uani 1 1 d . . . C6 C 0.1307(8) 0.1763(6) 0.5856(3) 0.0282(12) Uani 1 1 d . . . C7 C 0.4788(9) 0.4840(7) 0.1219(4) 0.0383(14) Uani 1 1 d . . . H7A H 0.5618 0.5065 0.0814 0.046 Uiso 1 1 calc R . . H7B H 0.4099 0.3775 0.1012 0.046 Uiso 1 1 calc R . . C8 C 0.3197(8) 0.5965(7) 0.1229(4) 0.0376(14) Uani 1 1 d . . . H8A H 0.2541 0.5989 0.0638 0.045 Uiso 1 1 calc R . . H8B H 0.3881 0.7014 0.1494 0.045 Uiso 1 1 calc R . . C9 C 0.2553(10) -0.0161(9) 0.7250(5) 0.0541(19) Uani 1 1 d . . . H9A H 0.1868 -0.1143 0.6884 0.065 Uiso 1 1 calc R . . H9B H 0.3164 -0.0400 0.7806 0.065 Uiso 1 1 calc R . . C10 C 0.1001(10) 0.0867(9) 0.7382(4) 0.0543(19) Uani 1 1 d . . . H10A H 0.1673 0.1859 0.7742 0.065 Uiso 1 1 calc R . . H10B H 0.0100 0.0395 0.7696 0.065 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.0000 0.0000 0.0442(4) Uani 1 2 d S . . C11 C 0.1040(9) 0.1881(7) -0.0341(4) 0.0385(14) Uani 1 1 d . A . C12 C 0.1786(9) 0.0651(7) 0.1133(4) 0.0382(14) Uani 1 1 d . A . N11 N 0.1633(9) 0.2984(7) -0.0547(4) 0.0606(17) Uani 1 1 d . . . N12 N 0.2836(10) 0.1002(7) 0.1813(4) 0.0626(17) Uani 1 1 d . . . C13 C -0.1986(9) 0.1009(7) 0.0372(4) 0.0521(16) Uani 0.50 1 d P A 1 N13 N -0.3268(12) 0.1643(9) 0.0609(5) 0.108(3) Uani 0.50 1 d P A 1 N14 N -0.1986(9) 0.1009(7) 0.0372(4) 0.0521(16) Uani 0.50 1 d P A 2 O14 O -0.3268(12) 0.1643(9) 0.0609(5) 0.108(3) Uani 0.50 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 S1 0.0183(7) 0.0417(8) 0.0393(8) 0.0195(7) 0.0069(6) 0.0100(6) S2 0.0197(7) 0.0570(10) 0.0371(8) 0.0261(7) 0.0077(6) 0.0128(6) S3 0.0203(7) 0.0478(9) 0.0380(8) 0.0241(7) 0.0082(6) 0.0110(6) S4 0.0198(7) 0.0508(9) 0.0362(8) 0.0211(7) 0.0072(6) 0.0125(6) S5 0.0199(7) 0.0621(10) 0.0434(9) 0.0237(8) 0.0106(6) 0.0072(7) S6 0.0288(8) 0.0756(12) 0.0420(9) 0.0365(8) 0.0132(7) 0.0229(8) S7 0.0272(7) 0.0484(9) 0.0378(8) 0.0248(7) 0.0104(6) 0.0127(6) S8 0.0229(7) 0.0732(12) 0.0478(9) 0.0295(9) 0.0155(7) 0.0146(7) C1 0.021(3) 0.033(3) 0.033(3) 0.011(2) 0.004(2) 0.007(2) C2 0.018(3) 0.033(3) 0.031(3) 0.014(2) 0.002(2) 0.007(2) C3 0.022(3) 0.028(3) 0.036(3) 0.010(2) 0.009(2) 0.007(2) C4 0.024(3) 0.037(3) 0.034(3) 0.016(3) 0.008(2) 0.012(2) C5 0.019(3) 0.028(3) 0.027(3) 0.009(2) 0.005(2) 0.004(2) C6 0.025(3) 0.035(3) 0.028(3) 0.009(2) 0.010(2) 0.005(2) C7 0.032(3) 0.055(4) 0.030(3) 0.011(3) 0.010(3) 0.004(3) C8 0.028(3) 0.051(4) 0.040(3) 0.022(3) 0.011(3) 0.007(3) C9 0.036(4) 0.074(5) 0.070(5) 0.045(4) 0.020(3) 0.017(3) C10 0.042(4) 0.092(6) 0.046(4) 0.036(4) 0.023(3) 0.026(4) Fe1 0.0509(8) 0.0453(8) 0.0323(7) 0.0165(6) -0.0014(6) -0.0120(6) C11 0.034(3) 0.041(4) 0.037(3) 0.009(3) 0.000(3) -0.001(3) C12 0.043(4) 0.040(3) 0.033(3) 0.012(3) 0.011(3) -0.004(3) N11 0.064(4) 0.060(4) 0.052(4) 0.027(3) -0.007(3) -0.014(3) N12 0.069(4) 0.062(4) 0.047(4) 0.017(3) -0.011(3) -0.006(3) C13 0.039(3) 0.058(4) 0.068(4) 0.017(3) 0.020(3) 0.019(3) N13 0.097(6) 0.116(6) 0.133(7) 0.020(5) 0.066(5) 0.054(5) N14 0.039(3) 0.058(4) 0.068(4) 0.017(3) 0.020(3) 0.019(3) O14 0.097(6) 0.116(6) 0.133(7) 0.020(5) 0.066(5) 0.054(5) #========================================================================= # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.721(5) . no S1 C3 1.721(5) . no S2 C1 1.709(5) . no S2 C4 1.735(5) . no S3 C2 1.720(5) . no S3 C5 1.739(5) . no S4 C2 1.730(5) . no S4 C6 1.737(5) . no S5 C3 1.727(5) . no S5 C7 1.789(6) . no S6 C4 1.727(5) . no S6 C8 1.804(5) . no S7 C5 1.740(5) . no S7 C9 1.808(6) . no S8 C6 1.734(5) . no S8 C10 1.805(6) . no C1 C2 1.375(7) . no C3 C4 1.368(7) . no C5 C6 1.359(7) . no C7 C8 1.500(8) . no C7 H7A 0.97 . no C7 H7B 0.97 . no C8 H8A 0.97 . no C8 H8B 0.97 . no C9 C10 1.445(9) . no C9 H9A 0.97 . no C9 H9B 0.97 . no C10 H10A 0.97 . no C10 H10B 0.97 . no Fe1 N14 1.792(6) 2 no Fe1 C13 1.792(6) 2 no Fe1 C13 1.792(6) . no Fe1 C11 1.929(6) . no Fe1 C11 1.929(6) 2 no Fe1 C12 1.933(6) 2 no Fe1 C12 1.933(6) . no C11 N11 1.133(7) . no C12 N12 1.152(8) . no C13 N13 1.147(8) . no N14 O14 1.147(8) . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 96.1(2) . . no C1 S2 C4 96.5(2) . . no C2 S3 C5 96.5(2) . . no C2 S4 C6 95.9(2) . . no C3 S5 C7 99.7(3) . . no C4 S6 C8 102.6(3) . . no C5 S7 C9 101.2(3) . . no C6 S8 C10 101.4(3) . . no C2 C1 S2 123.2(4) . . no C2 C1 S1 121.8(4) . . no S2 C1 S1 115.0(3) . . no C1 C2 S3 122.8(4) . . no C1 C2 S4 122.5(4) . . no S3 C2 S4 114.8(3) . . no C4 C3 S1 116.8(4) . . no C4 C3 S5 126.7(4) . . no S1 C3 S5 116.4(3) . . no C3 C4 S6 129.5(4) . . no C3 C4 S2 115.6(4) . . no S6 C4 S2 114.9(3) . . no C6 C5 S3 115.9(4) . . no C6 C5 S7 129.3(4) . . no S3 C5 S7 114.7(3) . . no C5 C6 S8 127.7(4) . . no C5 C6 S4 116.9(4) . . no S8 C6 S4 115.4(3) . . no C8 C7 S5 113.6(4) . . no C8 C7 H7A 108.8 . . no S5 C7 H7A 108.8 . . no C8 C7 H7B 108.8 . . no S5 C7 H7B 108.8 . . no H7A C7 H7B 107.7 . . no C7 C8 S6 114.4(4) . . no C7 C8 H8A 108.6 . . no S6 C8 H8A 108.6 . . no C7 C8 H8B 108.7 . . no S6 C8 H8B 108.7 . . no H8A C8 H8B 107.6 . . no C10 C9 S7 118.0(5) . . no C10 C9 H9A 107.8 . . no S7 C9 H9A 107.8 . . no C10 C9 H9B 107.8 . . no S7 C9 H9B 107.8 . . no H9A C9 H9B 107.1 . . no C9 C10 S8 115.3(5) . . no C9 C10 H10A 108.4 . . no S8 C10 H10A 108.4 . . no C9 C10 H10B 108.4 . . no S8 C10 H10B 108.4 . . no H10A C10 H10B 107.5 . . no N14 Fe1 C13 180.0(4) 2 . no C13 Fe1 C13 180.0(4) 2 . no N14 Fe1 C11 89.8(3) 2 . no C13 Fe1 C11 90.2(3) . . no C11 Fe1 C11 180.0(3) . 2 no N14 Fe1 C12 89.8(3) 2 . no C13 Fe1 C12 90.2(3) . . no C11 Fe1 C12 90.3(2) . . no C12 Fe1 C12 180.0(2) 2 . no N11 C11 Fe1 179.3(6) . . no N12 C12 Fe1 178.2(5) . . no N13 C13 Fe1 179.4(7) . . no O14 N14 Fe1 179.4(7) . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 S2 C1 C2 -179.2(5) . . . . no C4 S2 C1 S1 0.3(4) . . . . no C3 S1 C1 C2 -179.9(5) . . . . no C3 S1 C1 S2 0.6(4) . . . . no S2 C1 C2 S3 176.2(3) . . . . no S1 C1 C2 S3 -3.3(7) . . . . no S2 C1 C2 S4 -3.0(7) . . . . no S1 C1 C2 S4 177.5(3) . . . . no C5 S3 C2 C1 -176.9(5) . . . . no C5 S3 C2 S4 2.3(4) . . . . no C6 S4 C2 C1 176.5(5) . . . . no C6 S4 C2 S3 -2.7(4) . . . . no C1 S1 C3 C4 -1.5(5) . . . . no C1 S1 C3 S5 -177.9(3) . . . . no C7 S5 C3 C4 -23.4(6) . . . . no C7 S5 C3 S1 152.7(3) . . . . no S1 C3 C4 S6 -176.0(4) . . . . no S5 C3 C4 S6 0.1(9) . . . . no S1 C3 C4 S2 1.9(6) . . . . no S5 C3 C4 S2 178.0(3) . . . . no C8 S6 C4 C3 -2.6(6) . . . . no C8 S6 C4 S2 179.5(3) . . . . no C1 S2 C4 C3 -1.3(5) . . . . no C1 S2 C4 S6 176.9(3) . . . . no C2 S3 C5 C6 -0.8(5) . . . . no C2 S3 C5 S7 179.9(3) . . . . no C9 S7 C5 C6 7.6(6) . . . . no C9 S7 C5 S3 -173.2(4) . . . . no S3 C5 C6 S8 179.6(3) . . . . no S7 C5 C6 S8 -1.3(8) . . . . no S3 C5 C6 S4 -1.0(6) . . . . no S7 C5 C6 S4 178.2(3) . . . . no C10 S8 C6 C5 17.2(6) . . . . no C10 S8 C6 S4 -162.3(4) . . . . no C2 S4 C6 C5 2.2(5) . . . . no C2 S4 C6 S8 -178.3(3) . . . . no C3 S5 C7 C8 57.3(4) . . . . no S5 C7 C8 S6 -69.1(5) . . . . no C4 S6 C8 C7 36.7(5) . . . . no C5 S7 C9 C10 -39.9(7) . . . . no S7 C9 C10 S8 64.8(8) . . . . no C6 S8 C10 C9 -47.9(6) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C7 H7B N13 0.97 2.74 3.239(9) 112.6 1_655 n C7 H7B N11 0.97 2.66 3.256(8) 120.4 . n C7 H7B C11 0.97 2.84 3.661(8) 142.8 . n C7 H7A N11 0.97 2.55 3.387(8) 144.7 2_665 n C8 H8A N11 0.97 2.89 3.432(9) 116.1 . n C9 H9B N12 0.97 2.73 3.345(9) 121.5 2_656 n C10 H10B N12 0.97 2.55 3.504(9) 166.9 2_556 n C10 H10A N11 0.97 2.76 3.445(9) 127.8 1_556 n C10 H10B C12 0.97 2.71 3.661(8) 168.0 2_556 n C7 H7B O14 0.97 2.74 3.239(9) 112.6 1_655 n #===END=============================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 287002' #===================================================================== _vrf_PLAT_029_2 ; PROBLEM: _diffrn_measured_fraction_theta_full Low .......0.90 RESPONSE: The experimental data for (2) were obtained on the new Bruker KappaCCD diffractometer X8APEX with uncompleted program software. During first months of work on the new diffractometer we had problems with comleteness of experiments; it was not our mistake but Bruker's fault. This problem was desided only after receiving of new program package. Now we have not crystals of (2) and can not repeat the experiment. ; _vrf_PLAT_094_2 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.84 RESPONSE: The maximum and minimum residual density peaks are associated with disordered outher ethylene groups of organic donors and solvent molecules. ; _vrf_PLAT_155_2 ; PROBLEM: The Triclinic Unitcell is NOT Reduced RESPONSE: Unit cell axes for (2) were chosen in accordance with axes of (1) for comparison of two compounds. b-axis in both (1) and (2) is direction of radical cation stacks in organic layer, c-axis is direction in which cation and anion layers alternate. ; _vrf_PLAT_156_2 ; PROBLEM: Axial System Input Cell not Standard RESPONSE: See response to PLAT_155_2. ; _vrf_PLAT_242_2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for N6A RESPONSE: N6A atom of NO-group is directly connected to Fe-atom of anion while other N1A-N5A atoms are outer atoms of CN-ligands and therefore have higher Ueq. ; _vrf_PLAT_244_2 ; PROBLEM: Low 'Solvent' Ueq as Compared to Neighbors for C1S RESPONSE: Ueq for other solvent atoms are too large because of disorder. See response to PLAT_321_2. ; _vrf_PLAT_250_2 ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....2.28, 2.05, 2.24 RESPONSE: Some intrinsic disorder of S- and C-atoms in the outer cycles of organic donor molecules is typical for the room temperature crystal structures of organic molecular conductors. Outer atoms of anion ligands connected through intermolecular contacts with disordered outer ethylene groups of donors also have higher Ueq. In the structure of (2) additional disorder of solvent exists (see response to PLAT_321_2). ; _vrf_PLAT_301_2 ; PROBLEM: Main Residue Disorder .........................8.00 Perc. RESPONSE: It is connected with disordered outher ethylene groups of donors which have two possible positions in the structure. This type of disorder is typical for our structures. ; _vrf_PLAT_321_2 ; PROBLEM: Check Hybridisation of C2S in Solvent/Ion RESPONSE: Ethyleneglycol molecule of solvent have shortened C(sp3)-C(sp3) bond in the structure of (2) because of its disordering but it is impossible to find two different positions for disordered atoms. ; _vrf_PLAT_360_2 ; PROBLEM: Short C(sp3)-C(sp3) Bond C1S - C2S ... 1.40 Ang. RESPONSE: See response to PLAT_321_2 ; _vrf_PLAT_480_2 ; PROBLEM: Long H...A H-Bond Reported....for several H-atoms RESPONSE: In fact these are not real H-bonds but shortened H-contacts with H...A distances < 3.0\%A. Intermolecular contacts of different types shorter than the sum of van-der-Waals radii of corresponding atoms play an important role in the structures of organic molecular conductors. ; _vrf_PLAT_720_2 ; PROBLEM: Number of Unusual/Non-Standard Label(s) ........ 4 RESPONSE: Labels "s" were used for solvent atoms. ; # CHEMICAL DATA _chemical_name_systematic ; tris(bis(ethylenedithio)tetrathiafulvalene)(pentacyano-(nitroso)-iron) ethylene glycole solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_iupac '3(C10 H8 S8), C5 Fe N6 O, C2 H6 O2' _chemical_formula_moiety '3(C10 H8 S8), C5 Fe N6 O, C2 H6 O2' _chemical_formula_sum 'C37 H30 Fe N6 O3 S24' _chemical_formula_weight 1431.96 _chemical_compound_source 'synthesised by authors, see text' _chemical_absolute_configuration ? 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #========================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.481(3) _cell_length_b 8.6405(10) _cell_length_c 16.441(2) _cell_angle_alpha 98.894(10) _cell_angle_beta 93.169(10) _cell_angle_gamma 100.273(10) _cell_volume 2680.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5872 _cell_measurement_theta_min 2.382 _cell_measurement_theta_max 31.557 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; based on intensities of measured equivalent reflections, SADABS (Sheldrick, 1996) ; _exptl_absorpt_correction_T_min 0.6664 _exptl_absorpt_correction_T_max 0.9691 #========================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator OSMIC _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined \w- and \f-scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27538 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 32.71 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_max 0.752 _diffrn_measured_fraction_theta_full 0.906 _reflns_number_total 14818 _reflns_number_gt 8731 _reflns_threshold_expression I>2\sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction ; Apex2 V.1.27 (Bruker, 2005), WINGX (Farrugia, 1999) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' #========================================================================= # REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^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_number_reflns 14818 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.581 _refine_diff_density_min -0.557 #========================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.13376(3) 0.40256(8) 0.35903(4) 0.03700(16) Uani 1 1 d . . . S2 S 0.01276(3) 0.37284(7) 0.36956(4) 0.03274(15) Uani 1 1 d . . . S3 S -0.15458(3) 0.25281(8) 0.52692(4) 0.03426(15) Uani 1 1 d . . . S4 S -0.00923(3) 0.20948(8) 0.53203(4) 0.03369(15) Uani 1 1 d . . . S5 S -0.13117(4) 0.53793(10) 0.20648(4) 0.0475(2) Uani 1 1 d . . . S6 S 0.04563(3) 0.50745(8) 0.21933(4) 0.03980(17) Uani 1 1 d . . . S7 S -0.19033(4) 0.09835(9) 0.66937(4) 0.04572(19) Uani 1 1 d . . . S8 S -0.01385(3) 0.05255(8) 0.67848(4) 0.03622(16) Uani 1 1 d . . . C1 C -0.06637(12) 0.3447(3) 0.41238(14) 0.0292(5) Uani 1 1 d . . . C2 C -0.07578(12) 0.2773(3) 0.48294(14) 0.0274(5) Uani 1 1 d . . . C3 C -0.08465(12) 0.4696(3) 0.28199(14) 0.0306(5) Uani 1 1 d . . . C4 C -0.01574(12) 0.4569(3) 0.28809(14) 0.0285(5) Uani 1 1 d . . . C5 C -0.12634(12) 0.1566(3) 0.60509(14) 0.0287(5) Uani 1 1 d . A . C6 C -0.05865(12) 0.1384(3) 0.60851(13) 0.0271(5) Uani 1 1 d . A . C7 C -0.06619(13) 0.5877(3) 0.13575(17) 0.0423(7) Uani 1 1 d . . . H7A H -0.0900 0.5820 0.0816 0.051 Uiso 1 1 calc R . . H7B H -0.0423 0.6972 0.1540 0.051 Uiso 1 1 calc R . . C8 C -0.01223(13) 0.4829(3) 0.12742(15) 0.0388(6) Uani 1 1 d . . . H8A H 0.0153 0.5068 0.0820 0.047 Uiso 1 1 calc R . . H8B H -0.0359 0.3723 0.1140 0.047 Uiso 1 1 calc R . . C9 C -0.1376(2) 0.0628(5) 0.7557(3) 0.0366(10) Uani 0.80 1 d P A 1 H9A H -0.1126 0.1644 0.7860 0.044 Uiso 0.80 1 calc PR A 1 H9B H -0.1681 0.0125 0.7927 0.044 Uiso 0.80 1 calc PR A 1 C10 C -0.0849(2) -0.0423(5) 0.7301(3) 0.0352(10) Uani 0.80 1 d P A 1 H10A H -0.1093 -0.1378 0.6938 0.042 Uiso 0.80 1 calc PR A 1 H10B H -0.0656 -0.0749 0.7790 0.042 Uiso 0.80 1 calc PR A 1 C9B C -0.1505(11) -0.019(2) 0.7294(14) 0.056(6) Uani 0.20 1 d P A 2 H9C H -0.1772 -0.0303 0.7769 0.068 Uiso 0.20 1 calc PR A 2 H9D H -0.1549 -0.1242 0.6968 0.068 Uiso 0.20 1 calc PR A 2 C10B C -0.0773(9) 0.037(2) 0.7595(10) 0.038(4) Uani 0.20 1 d P A 2 H10C H -0.0641 -0.0353 0.7947 0.045 Uiso 0.20 1 calc PR A 2 H10D H -0.0726 0.1409 0.7936 0.045 Uiso 0.20 1 calc PR A 2 S11 S 0.20742(3) 0.46000(8) 0.30365(4) 0.03888(16) Uani 1 1 d . . . S12 S 0.35451(3) 0.43477(8) 0.31264(4) 0.03531(15) Uani 1 1 d . . . S13 S 0.18744(3) 0.31292(8) 0.47044(4) 0.03549(16) Uani 1 1 d . . . S14 S 0.33322(3) 0.27205(8) 0.47817(4) 0.03403(15) Uani 1 1 d . . . S15 S 0.20538(4) 0.58011(10) 0.14663(4) 0.0497(2) Uani 1 1 d . . . S16 S 0.38393(3) 0.55679(9) 0.15758(4) 0.04126(17) Uani 1 1 d . . . S17 S 0.14989(3) 0.15305(9) 0.61154(4) 0.04445(18) Uani 1 1 d . . . S18 S 0.32608(3) 0.11392(9) 0.62381(4) 0.04159(17) Uani 1 1 d . . . C11 C 0.27584(12) 0.4044(3) 0.35630(14) 0.0301(5) Uani 1 1 d . . . C12 C 0.26678(12) 0.3375(3) 0.42666(14) 0.0296(5) Uani 1 1 d . . . C13 C 0.25470(13) 0.5200(3) 0.22314(14) 0.0325(5) Uani 1 1 d . . . C14 C 0.32356(12) 0.5090(3) 0.22813(14) 0.0294(5) Uani 1 1 d . . . C15 C 0.21411(12) 0.2153(3) 0.54822(14) 0.0291(5) Uani 1 1 d . B . C16 C 0.28243(12) 0.1988(3) 0.55258(14) 0.0283(5) Uani 1 1 d . B . C17 C 0.27070(14) 0.6488(4) 0.08096(17) 0.0501(7) Uani 1 1 d . . . H17A H 0.2477 0.6532 0.0278 0.060 Uiso 1 1 calc R . . H17B H 0.2937 0.7565 0.1050 0.060 Uiso 1 1 calc R . . C18 C 0.32553(14) 0.5474(4) 0.06732(16) 0.0472(7) Uani 1 1 d . . . H18A H 0.3529 0.5809 0.0235 0.057 Uiso 1 1 calc R . . H18B H 0.3024 0.4374 0.0489 0.057 Uiso 1 1 calc R . . C19 C 0.2019(2) 0.1224(5) 0.7001(3) 0.0412(11) Uani 0.80 1 d P B 1 H19A H 0.2253 0.2254 0.7304 0.049 Uiso 0.80 1 calc PR B 1 H19B H 0.1710 0.0711 0.7364 0.049 Uiso 0.80 1 calc PR B 1 C20 C 0.2563(2) 0.0215(5) 0.6773(2) 0.0399(9) Uani 0.80 1 d P B 1 H20A H 0.2331 -0.0775 0.6428 0.048 Uiso 0.80 1 calc PR B 1 H20B H 0.2763 -0.0053 0.7274 0.048 Uiso 0.80 1 calc PR B 1 C19B C 0.1901(10) 0.040(2) 0.6710(12) 0.047(5) Uani 0.20 1 d P B 2 H19C H 0.1624 0.0216 0.7171 0.056 Uiso 0.20 1 calc PR B 2 H19D H 0.1898 -0.0635 0.6377 0.056 Uiso 0.20 1 calc PR B 2 C20B C 0.2647(8) 0.1129(19) 0.7047(10) 0.040(4) Uani 0.20 1 d P B 2 H20C H 0.2794 0.0533 0.7457 0.048 Uiso 0.20 1 calc PR B 2 H20D H 0.2664 0.2216 0.7319 0.048 Uiso 0.20 1 calc PR B 2 S21 S 0.52522(3) 0.35751(8) 0.41409(4) 0.03511(15) Uani 1 1 d . . . S22 S 0.67071(3) 0.30974(8) 0.42291(4) 0.03530(16) Uani 1 1 d . . . S23 S 0.50195(3) 0.18751(8) 0.57899(4) 0.03812(16) Uani 1 1 d . . . S24 S 0.64844(3) 0.14773(8) 0.58229(4) 0.03707(16) Uani 1 1 d . . . S25 S 0.53420(4) 0.50309(9) 0.26392(4) 0.04323(18) Uani 1 1 d . . . S26 S 0.70558(4) 0.43942(10) 0.27202(5) 0.0507(2) Uani 1 1 d . . . S27 S 0.47223(4) 0.04955(10) 0.73002(5) 0.0487(2) Uani 1 1 d . . . S28 S 0.64843(3) 0.00240(8) 0.73173(4) 0.04233(18) Uani 1 1 d . . . C21 C 0.59077(12) 0.2876(3) 0.46598(14) 0.0302(5) Uani 1 1 d . . . C22 C 0.58054(12) 0.2160(3) 0.53384(14) 0.0290(5) Uani 1 1 d . . . C23 C 0.57707(12) 0.4218(3) 0.33788(14) 0.0290(5) Uani 1 1 d . . . C24 C 0.64422(12) 0.3991(3) 0.34238(14) 0.0292(5) Uani 1 1 d . . . C25 C 0.53295(13) 0.1025(3) 0.66042(15) 0.0328(6) Uani 1 1 d . C . C26 C 0.60050(12) 0.0842(3) 0.66188(14) 0.0303(5) Uani 1 1 d . C . C27 C 0.59777(14) 0.5358(3) 0.19002(16) 0.0444(7) Uani 1 1 d . . . H27A H 0.5730 0.5305 0.1365 0.053 Uiso 1 1 calc R . . H27B H 0.6250 0.6430 0.2058 0.053 Uiso 1 1 calc R . . C28 C 0.64766(14) 0.4203(3) 0.18095(15) 0.0428(7) Uani 1 1 d . . . H28A H 0.6752 0.4384 0.1347 0.051 Uiso 1 1 calc R . . H28B H 0.6209 0.3122 0.1686 0.051 Uiso 1 1 calc R . . C29 C 0.5287(3) 0.0106(6) 0.8121(4) 0.0387(13) Uani 0.67 1 d P C 1 H29A H 0.5549 0.1116 0.8417 0.046 Uiso 0.67 1 calc PR C 1 H29B H 0.4999 -0.0393 0.8507 0.046 Uiso 0.67 1 calc PR C 1 C30 C 0.5804(2) -0.0957(6) 0.7836(3) 0.0388(12) Uani 0.67 1 d P C 1 H30A H 0.5553 -0.1900 0.7468 0.047 Uiso 0.67 1 calc PR C 1 H30B H 0.6008 -0.1302 0.8312 0.047 Uiso 0.67 1 calc PR C 1 C29B C 0.5136(6) -0.0653(13) 0.7880(8) 0.042(3) Uani 0.33 1 d P C 2 H29C H 0.4885 -0.0774 0.8366 0.051 Uiso 0.33 1 calc PR C 2 H29D H 0.5095 -0.1707 0.7555 0.051 Uiso 0.33 1 calc PR C 2 C30B C 0.5884(5) -0.0034(14) 0.8154(6) 0.045(3) Uani 0.33 1 d P C 2 H30C H 0.6034 -0.0689 0.8532 0.053 Uiso 0.33 1 calc PR C 2 H30D H 0.5930 0.1039 0.8459 0.053 Uiso 0.33 1 calc PR C 2 Fe1 Fe 0.160831(17) 0.03926(4) -0.02384(2) 0.03006(10) Uani 1 1 d . . . C1A C 0.20969(13) 0.2146(3) -0.07195(15) 0.0370(6) Uani 1 1 d . . . C2A C 0.12366(13) -0.1561(3) 0.01642(16) 0.0407(6) Uani 1 1 d . . . C3A C 0.22827(13) 0.0995(3) 0.07265(16) 0.0358(6) Uani 1 1 d . . . C4A C 0.10332(13) -0.0389(3) -0.12752(16) 0.0356(6) Uani 1 1 d . . . C5A C 0.22901(14) -0.0767(3) -0.07190(17) 0.0391(6) Uani 1 1 d . . . N1A N 0.23910(14) 0.3171(3) -0.10031(15) 0.0585(7) Uani 1 1 d . . . N2A N 0.10120(14) -0.2703(3) 0.04060(16) 0.0648(8) Uani 1 1 d . . . N3A N 0.26704(13) 0.1347(3) 0.13005(15) 0.0538(6) Uani 1 1 d . . . N4A N 0.06928(13) -0.0835(3) -0.18860(15) 0.0545(7) Uani 1 1 d . . . N5A N 0.27167(14) -0.1415(3) -0.09686(18) 0.0699(8) Uani 1 1 d . . . N6A N 0.10352(12) 0.1376(3) 0.01882(14) 0.0470(6) Uani 1 1 d . . . O1A O 0.06362(14) 0.2033(3) 0.04843(17) 0.0966(10) Uani 1 1 d . . . C1S C 0.40618(18) 0.1587(4) -0.0337(3) 0.0758(11) Uani 1 1 d . . . H1S1 H 0.3654 0.1793 -0.0057 0.091 Uiso 1 1 calc R . . H1S2 H 0.3990 0.1773 -0.0900 0.091 Uiso 1 1 calc R . . C2S C 0.4650(2) 0.2686(4) 0.0057(3) 0.1002(15) Uani 1 1 d . . . H2S1 H 0.4619 0.3683 -0.0132 0.120 Uiso 1 1 calc R . . H2S2 H 0.4570 0.2850 0.0639 0.120 Uiso 1 1 calc R . . O1S O 0.41023(11) -0.0021(3) -0.03595(17) 0.0836(8) Uani 1 1 d . . . H1S H 0.3738 -0.0585 -0.0587 0.100 Uiso 1 1 calc R . . O2S O 0.52989(13) 0.2564(3) 0.00361(19) 0.0993(9) Uani 1 1 d . . . H2S H 0.5348 0.1694 0.0146 0.119 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 S1 0.0262(3) 0.0583(4) 0.0351(4) 0.0261(3) 0.0062(3) 0.0144(3) S2 0.0259(3) 0.0439(3) 0.0344(4) 0.0176(3) 0.0047(3) 0.0124(3) S3 0.0278(3) 0.0503(4) 0.0314(3) 0.0183(3) 0.0046(3) 0.0149(3) S4 0.0263(3) 0.0489(4) 0.0331(3) 0.0217(3) 0.0059(3) 0.0128(3) S5 0.0361(4) 0.0825(5) 0.0384(4) 0.0349(4) 0.0095(3) 0.0264(4) S6 0.0276(3) 0.0589(4) 0.0364(4) 0.0184(3) 0.0083(3) 0.0069(3) S7 0.0301(4) 0.0744(5) 0.0433(4) 0.0314(4) 0.0131(3) 0.0167(3) S8 0.0315(3) 0.0507(4) 0.0340(4) 0.0226(3) 0.0043(3) 0.0139(3) C1 0.0264(12) 0.0355(12) 0.0293(13) 0.0139(11) 0.0028(10) 0.0080(9) C2 0.0250(12) 0.0356(12) 0.0238(12) 0.0093(10) 0.0028(9) 0.0076(9) C3 0.0312(13) 0.0399(13) 0.0261(13) 0.0157(11) 0.0056(10) 0.0113(10) C4 0.0290(13) 0.0329(12) 0.0253(13) 0.0093(10) 0.0029(10) 0.0062(9) C5 0.0291(13) 0.0374(13) 0.0224(12) 0.0106(10) 0.0030(9) 0.0090(10) C6 0.0300(13) 0.0323(12) 0.0221(12) 0.0099(10) 0.0018(9) 0.0093(9) C7 0.0368(15) 0.0551(16) 0.0429(16) 0.0269(14) 0.0096(12) 0.0123(12) C8 0.0380(15) 0.0522(16) 0.0280(14) 0.0104(12) 0.0087(11) 0.0085(12) C9 0.038(2) 0.050(3) 0.027(3) 0.016(2) 0.0083(18) 0.012(2) C10 0.035(2) 0.040(2) 0.033(3) 0.015(2) 0.0043(18) 0.0059(19) C9B 0.058(12) 0.062(13) 0.052(15) 0.032(12) -0.003(10) 0.004(11) C10B 0.034(8) 0.059(11) 0.022(10) 0.014(9) 0.005(7) 0.006(9) S11 0.0305(3) 0.0586(4) 0.0365(4) 0.0253(3) 0.0072(3) 0.0161(3) S12 0.0290(3) 0.0467(4) 0.0357(4) 0.0182(3) 0.0052(3) 0.0111(3) S13 0.0288(3) 0.0524(4) 0.0322(4) 0.0191(3) 0.0045(3) 0.0149(3) S14 0.0263(3) 0.0484(4) 0.0340(4) 0.0204(3) 0.0062(3) 0.0121(3) S15 0.0394(4) 0.0844(5) 0.0396(4) 0.0342(4) 0.0096(3) 0.0271(4) S16 0.0314(4) 0.0613(4) 0.0356(4) 0.0190(3) 0.0084(3) 0.0096(3) S17 0.0300(4) 0.0702(5) 0.0417(4) 0.0265(4) 0.0125(3) 0.0147(3) S18 0.0334(4) 0.0601(4) 0.0412(4) 0.0276(3) 0.0042(3) 0.0184(3) C11 0.0263(12) 0.0370(13) 0.0311(13) 0.0138(11) 0.0044(10) 0.0095(10) C12 0.0287(13) 0.0356(13) 0.0274(13) 0.0105(11) 0.0033(10) 0.0091(10) C13 0.0323(13) 0.0412(14) 0.0283(13) 0.0130(11) 0.0044(10) 0.0118(10) C14 0.0355(14) 0.0307(12) 0.0241(13) 0.0091(10) 0.0054(10) 0.0073(10) C15 0.0284(13) 0.0369(13) 0.0247(13) 0.0103(11) 0.0034(10) 0.0088(10) C16 0.0268(12) 0.0334(12) 0.0273(13) 0.0103(10) 0.0036(10) 0.0080(9) C17 0.0447(17) 0.0683(19) 0.0439(17) 0.0318(15) 0.0025(13) 0.0092(14) C18 0.0409(16) 0.0701(19) 0.0310(15) 0.0115(14) 0.0051(12) 0.0086(14) C19 0.045(3) 0.056(3) 0.029(3) 0.012(2) 0.0079(19) 0.019(2) C20 0.043(2) 0.047(2) 0.036(2) 0.020(2) 0.0114(17) 0.0129(19) C19B 0.058(12) 0.055(12) 0.034(12) 0.015(9) 0.008(9) 0.019(10) C20B 0.045(9) 0.034(8) 0.038(10) -0.001(8) 0.018(7) -0.002(7) S21 0.0280(3) 0.0548(4) 0.0295(3) 0.0181(3) 0.0073(3) 0.0156(3) S22 0.0282(3) 0.0503(4) 0.0353(4) 0.0206(3) 0.0066(3) 0.0159(3) S23 0.0310(3) 0.0572(4) 0.0336(4) 0.0204(3) 0.0077(3) 0.0156(3) S24 0.0308(3) 0.0548(4) 0.0344(4) 0.0227(3) 0.0083(3) 0.0168(3) S25 0.0362(4) 0.0624(4) 0.0415(4) 0.0277(4) 0.0051(3) 0.0202(3) S26 0.0313(4) 0.0851(5) 0.0446(4) 0.0320(4) 0.0137(3) 0.0133(4) S27 0.0348(4) 0.0784(5) 0.0450(4) 0.0341(4) 0.0145(3) 0.0195(3) S28 0.0343(4) 0.0621(4) 0.0404(4) 0.0294(3) 0.0071(3) 0.0163(3) C21 0.0292(13) 0.0361(13) 0.0280(13) 0.0086(11) 0.0028(10) 0.0104(10) C22 0.0277(12) 0.0370(13) 0.0256(12) 0.0097(11) 0.0025(10) 0.0105(10) C23 0.0274(13) 0.0345(12) 0.0284(13) 0.0114(11) 0.0040(10) 0.0091(9) C24 0.0277(13) 0.0365(13) 0.0280(13) 0.0130(11) 0.0072(10) 0.0103(10) C25 0.0321(14) 0.0417(14) 0.0289(13) 0.0140(11) 0.0061(10) 0.0103(10) C26 0.0304(13) 0.0368(13) 0.0270(13) 0.0133(11) 0.0050(10) 0.0078(10) C27 0.0487(17) 0.0551(17) 0.0354(15) 0.0215(13) 0.0099(13) 0.0120(13) C28 0.0481(17) 0.0519(16) 0.0309(15) 0.0110(13) 0.0080(12) 0.0111(13) C29 0.041(3) 0.050(3) 0.029(3) 0.013(3) 0.009(2) 0.010(3) C30 0.039(3) 0.044(3) 0.038(3) 0.020(2) 0.004(2) 0.008(2) C29B 0.036(6) 0.050(7) 0.044(8) 0.018(7) 0.006(5) 0.007(5) C30B 0.035(5) 0.076(7) 0.024(6) 0.024(5) 0.004(4) 0.000(5) Fe1 0.0280(2) 0.0351(2) 0.0287(2) 0.01039(16) 0.00090(14) 0.00641(14) C1A 0.0408(15) 0.0392(14) 0.0306(14) 0.0096(12) -0.0039(11) 0.0052(11) C2A 0.0375(15) 0.0496(16) 0.0340(15) 0.0149(13) -0.0049(11) 0.0008(12) C3A 0.0382(15) 0.0370(14) 0.0334(15) 0.0115(12) 0.0013(12) 0.0058(11) C4A 0.0344(14) 0.0373(13) 0.0361(15) 0.0134(12) -0.0001(11) 0.0043(10) C5A 0.0342(15) 0.0389(14) 0.0413(16) 0.0009(12) -0.0038(12) 0.0065(11) N1A 0.0665(18) 0.0529(15) 0.0516(16) 0.0227(13) -0.0094(13) -0.0081(12) N2A 0.0722(19) 0.0601(16) 0.0557(16) 0.0295(14) -0.0134(14) -0.0155(13) N3A 0.0508(16) 0.0616(16) 0.0469(16) 0.0151(13) -0.0089(12) 0.0037(12) N4A 0.0546(16) 0.0587(16) 0.0472(16) 0.0145(13) -0.0124(13) 0.0030(12) N5A 0.0491(18) 0.0650(19) 0.092(2) -0.0114(16) 0.0088(16) 0.0203(14) N6A 0.0426(14) 0.0588(15) 0.0461(15) 0.0101(12) 0.0114(11) 0.0234(12) O1A 0.081(2) 0.113(2) 0.110(2) 0.0068(18) 0.0355(18) 0.0589(18) C1S 0.055(2) 0.062(2) 0.119(3) 0.030(2) 0.006(2) 0.0213(17) C2S 0.065(3) 0.059(2) 0.173(5) 0.008(3) 0.010(3) 0.013(2) O1S 0.0422(13) 0.0520(14) 0.157(2) 0.0215(14) -0.0052(14) 0.0104(10) O2S 0.0503(16) 0.0685(17) 0.175(3) 0.0232(17) -0.0100(17) 0.0054(12) #========================================================================= # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.728(2) . no S1 C3 1.737(2) . no S2 C1 1.724(2) . no S2 C4 1.730(2) . no S3 C2 1.726(2) . no S3 C5 1.749(2) . no S4 C2 1.726(2) . no S4 C6 1.745(2) . no S5 C3 1.733(2) . no S5 C7 1.806(2) . no S6 C4 1.736(2) . no S6 C8 1.796(3) . no S7 C5 1.735(2) . no S7 C9B 1.760(19) . no S7 C9 1.804(4) . no S8 C6 1.738(2) . no S8 C10 1.803(4) . no S8 C10B 1.870(16) . no C1 C2 1.383(3) . no C3 C4 1.366(3) . no C5 C6 1.355(3) . no C7 C8 1.504(3) . no C7 H7A 0.9700 . no C7 H7B 0.9700 . no C8 H8A 0.9700 . no C8 H8B 0.9700 . no C9 C10 1.522(6) . no C9 H9A 0.9700 . no C9 H9B 0.9700 . no C10 H10A 0.9700 . no C10 H10B 0.9700 . no C9B C10B 1.46(2) . no C9B H9C 0.9700 . no C9B H9D 0.9700 . no C10B H10C 0.9700 . no C10B H10D 0.9700 . no S11 C11 1.728(2) . no S11 C13 1.745(2) . no S12 C11 1.723(2) . no S12 C14 1.740(2) . no S13 C12 1.733(2) . no S13 C15 1.742(2) . no S14 C12 1.732(2) . no S14 C16 1.740(2) . no S15 C13 1.738(2) . no S15 C17 1.794(3) . no S16 C14 1.739(2) . no S16 C18 1.802(3) . no S17 C19B 1.735(17) . no S17 C15 1.736(2) . no S17 C19 1.808(4) . no S18 C16 1.735(2) . no S18 C20 1.795(3) . no S18 C20B 1.836(14) . no C11 C12 1.377(3) . no C13 C14 1.360(3) . no C15 C16 1.363(3) . no C17 C18 1.503(4) . no C17 H17A 0.9700 . no C17 H17B 0.9700 . no C18 H18A 0.9700 . no C18 H18B 0.9700 . no C19 C20 1.516(5) . no C19 H19A 0.9700 . no C19 H19B 0.9700 . no C20 H20A 0.9700 . no C20 H20B 0.9700 . no C19B C20B 1.52(2) . no C19B H19C 0.9700 . no C19B H19D 0.9700 . no C20B H20C 0.9700 . no C20B H20D 0.9700 . no S21 C21 1.743(2) . no S21 C23 1.747(2) . no S22 C24 1.732(2) . no S22 C21 1.738(2) . no S23 C22 1.733(2) . no S23 C25 1.752(2) . no S24 C22 1.743(2) . no S24 C26 1.749(2) . no S25 C23 1.741(2) . no S25 C27 1.799(3) . no S26 C24 1.737(2) . no S26 C28 1.792(3) . no S27 C29B 1.743(11) . no S27 C25 1.742(2) . no S27 C29 1.804(6) . no S28 C26 1.749(2) . no S28 C30 1.775(4) . no S28 C30B 1.854(9) . no C21 C22 1.364(3) . no C23 C24 1.357(3) . no C25 C26 1.352(3) . no C27 C28 1.510(3) . no C27 H27A 0.9700 . no C27 H27B 0.9700 . no C28 H28A 0.9700 . no C28 H28B 0.9700 . no C29 C30 1.525(7) . no C29 H29A 0.9700 . no C29 H29B 0.9700 . no C30 H30A 0.9700 . no C30 H30B 0.9700 . no C29B C30B 1.478(14) . no C29B H29C 0.9700 . no C29B H29D 0.9700 . no C30B H30C 0.9700 . no C30B H30D 0.9700 . no Fe1 N6A 1.644(2) . no Fe1 C5A 1.933(3) . no Fe1 C1A 1.940(2) . no Fe1 C2A 1.943(2) . no Fe1 C3A 1.945(3) . no Fe1 C4A 1.944(3) . no C1A N1A 1.143(3) . no C2A N2A 1.145(3) . no C3A N3A 1.142(3) . no C4A N4A 1.145(3) . no C5A N5A 1.143(3) . no N6A O1A 1.130(3) . no C1S O1S 1.400(3) . no C1S C2S 1.406(5) . no C1S H1S1 0.9700 . no C1S H1S2 0.9700 . no C2S O2S 1.288(4) . no C2S H2S1 0.9700 . no C2S H2S2 0.9700 . no O1S H1S 0.8200 . no O2S H2S 0.8200 . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 96.24(11) . . no C1 S2 C4 95.97(10) . . no C2 S3 C5 95.25(10) . . no C2 S4 C6 95.93(10) . . no C3 S5 C7 103.00(11) . . no C4 S6 C8 99.14(11) . . no C5 S7 C9B 103.1(7) . . no C5 S7 C9 100.98(16) . . no C6 S8 C10 101.27(16) . . no C6 S8 C10B 100.7(5) . . no C2 C1 S2 122.65(18) . . no C2 C1 S1 122.43(18) . . no S2 C1 S1 114.90(12) . . no C1 C2 S3 122.61(18) . . no C1 C2 S4 121.82(18) . . no S3 C2 S4 115.57(12) . . no C4 C3 S5 129.27(17) . . no C4 C3 S1 115.76(16) . . no S5 C3 S1 114.94(13) . . no C3 C4 S2 117.10(16) . . no C3 C4 S6 126.58(17) . . no S2 C4 S6 116.24(13) . . no C6 C5 S7 128.54(16) . . no C6 C5 S3 117.18(17) . . no S7 C5 S3 114.28(13) . . no C5 C6 S8 128.93(17) . . no C5 C6 S4 116.03(16) . . no S8 C6 S4 115.04(13) . . no C8 C7 S5 114.99(16) . . no C8 C7 H7A 108.5 . . no S5 C7 H7A 108.5 . . no C8 C7 H7B 108.5 . . no S5 C7 H7B 108.5 . . no H7A C7 H7B 107.5 . . no C7 C8 S6 113.21(19) . . no C7 C8 H8A 108.9 . . no S6 C8 H8A 108.9 . . no C7 C8 H8B 108.9 . . no S6 C8 H8B 108.9 . . no H8A C8 H8B 107.7 . . no C10 C9 S7 113.2(3) . . no C10 C9 H9A 108.9 . . no S7 C9 H9A 108.9 . . no C10 C9 H9B 108.9 . . no S7 C9 H9B 108.9 . . no H9A C9 H9B 107.7 . . no C9 C10 S8 114.1(3) . . no C9 C10 H10A 108.7 . . no S8 C10 H10A 108.7 . . no C9 C10 H10B 108.7 . . no S8 C10 H10B 108.7 . . no H10A C10 H10B 107.6 . . no C10B C9B S7 118.1(13) . . no C10B C9B H9C 107.8 . . no S7 C9B H9C 107.8 . . no C10B C9B H9D 107.8 . . no S7 C9B H9D 107.8 . . no H9C C9B H9D 107.1 . . no C9B C10B S8 115.9(14) . . no C9B C10B H10C 108.3 . . no S8 C10B H10C 108.3 . . no C9B C10B H10D 108.3 . . no S8 C10B H10D 108.3 . . no H10C C10B H10D 107.4 . . no C11 S11 C13 96.20(11) . . no C11 S12 C14 96.04(11) . . no C12 S13 C15 95.86(10) . . no C12 S14 C16 95.87(11) . . no C13 S15 C17 102.23(12) . . no C14 S16 C18 100.19(12) . . no C19B S17 C15 103.1(6) . . no C15 S17 C19 101.70(17) . . no C16 S18 C20 102.87(14) . . no C16 S18 C20B 100.1(5) . . no C12 C11 S12 123.28(17) . . no C12 C11 S11 121.76(18) . . no S12 C11 S11 114.94(12) . . no C11 C12 S14 122.91(18) . . no C11 C12 S13 122.14(17) . . no S14 C12 S13 114.95(12) . . no C14 C13 S15 129.67(18) . . no C14 C13 S11 115.90(16) . . no S15 C13 S11 114.40(14) . . no C13 C14 S12 116.89(17) . . no C13 C14 S16 126.96(17) . . no S12 C14 S16 116.13(13) . . no C16 C15 S17 128.12(17) . . no C16 C15 S13 116.47(17) . . no S17 C15 S13 115.41(13) . . no C15 C16 S18 128.14(17) . . no C15 C16 S14 116.72(16) . . no S18 C16 S14 115.14(13) . . no C18 C17 S15 114.56(18) . . no C18 C17 H17A 108.6 . . no S15 C17 H17A 108.6 . . no C18 C17 H17B 108.6 . . no S15 C17 H17B 108.6 . . no H17A C17 H17B 107.6 . . no C17 C18 S16 114.1(2) . . no C17 C18 H18A 108.7 . . no S16 C18 H18A 108.7 . . no C17 C18 H18B 108.7 . . no S16 C18 H18B 108.7 . . no H18A C18 H18B 107.6 . . no C20 C19 S17 113.2(3) . . no C20 C19 H19A 108.9 . . no S17 C19 H19A 108.9 . . no C20 C19 H19B 108.9 . . no S17 C19 H19B 108.9 . . no H19A C19 H19B 107.7 . . no C19 C20 S18 114.8(3) . . no C19 C20 H20A 108.6 . . no S18 C20 H20A 108.6 . . no C19 C20 H20B 108.6 . . no S18 C20 H20B 108.6 . . no H20A C20 H20B 107.5 . . no C20B C19B S17 115.0(13) . . no C20B C19B H19C 108.5 . . no S17 C19B H19C 108.5 . . no C20B C19B H19D 108.5 . . no S17 C19B H19D 108.5 . . no H19C C19B H19D 107.5 . . no C19B C20B S18 112.6(12) . . no C19B C20B H20C 109.1 . . no S18 C20B H20C 109.1 . . no C19B C20B H20D 109.1 . . no S18 C20B H20D 109.1 . . no H20C C20B H20D 107.8 . . no C21 S21 C23 95.31(11) . . no C24 S22 C21 95.76(11) . . no C22 S23 C25 95.67(11) . . no C22 S24 C26 95.54(11) . . no C23 S25 C27 103.68(12) . . no C24 S26 C28 99.40(12) . . no C29B S27 C25 103.3(4) . . no C25 S27 C29 100.8(2) . . no C26 S28 C30 101.13(16) . . no C26 S28 C30B 99.7(3) . . no C22 C21 S22 121.66(18) . . no C22 C21 S21 123.34(18) . . no S22 C21 S21 114.97(12) . . no C21 C22 S23 124.06(18) . . no C21 C22 S24 120.86(18) . . no S23 C22 S24 115.07(12) . . no C24 C23 S25 128.40(18) . . no C24 C23 S21 116.75(16) . . no S25 C23 S21 114.82(13) . . no C23 C24 S22 117.20(17) . . no C23 C24 S26 126.75(17) . . no S22 C24 S26 115.93(13) . . no C26 C25 S27 127.52(17) . . no C26 C25 S23 116.83(17) . . no S27 C25 S23 115.65(13) . . no C25 C26 S24 116.84(16) . . no C25 C26 S28 129.55(17) . . no S24 C26 S28 113.60(13) . . no C28 C27 S25 115.48(17) . . no C28 C27 H27A 108.4 . . no S25 C27 H27A 108.4 . . no C28 C27 H27B 108.4 . . no S25 C27 H27B 108.4 . . no H27A C27 H27B 107.5 . . no C27 C28 S26 112.70(19) . . no C27 C28 H28A 109.1 . . no S26 C28 H28A 109.1 . . no C27 C28 H28B 109.1 . . no S26 C28 H28B 109.1 . . no H28A C28 H28B 107.8 . . no C30 C29 S27 114.6(4) . . no C30 C29 H29A 108.6 . . no S27 C29 H29A 108.6 . . no C30 C29 H29B 108.6 . . no S27 C29 H29B 108.6 . . no H29A C29 H29B 107.6 . . no C29 C30 S28 112.6(3) . . no C29 C30 H30A 109.1 . . no S28 C30 H30A 109.1 . . no C29 C30 H30B 109.1 . . no S28 C30 H30B 109.1 . . no H30A C30 H30B 107.8 . . no C30B C29B S27 116.4(8) . . no C30B C29B H29C 108.2 . . no S27 C29B H29C 108.2 . . no C30B C29B H29D 108.2 . . no S27 C29B H29D 108.2 . . no H29C C29B H29D 107.3 . . no C29B C30B S28 115.5(8) . . no C29B C30B H30C 108.4 . . no S28 C30B H30C 108.4 . . no C29B C30B H30D 108.4 . . no S28 C30B H30D 108.4 . . no H30C C30B H30D 107.5 . . no N6A Fe1 C5A 178.88(10) . . no N6A Fe1 C1A 95.74(11) . . no C5A Fe1 C1A 84.73(11) . . no N6A Fe1 C2A 94.00(12) . . no C5A Fe1 C2A 85.53(11) . . no C1A Fe1 C2A 170.26(10) . . no N6A Fe1 C3A 94.04(11) . . no C5A Fe1 C3A 84.94(11) . . no C1A Fe1 C3A 89.89(10) . . no C2A Fe1 C3A 89.10(10) . . no N6A Fe1 C4A 94.45(11) . . no C5A Fe1 C4A 86.57(11) . . no C1A Fe1 C4A 89.50(10) . . no C2A Fe1 C4A 90.06(10) . . no C3A Fe1 C4A 171.51(10) . . no N1A C1A Fe1 179.3(3) . . no N2A C2A Fe1 179.2(3) . . no N3A C3A Fe1 179.0(2) . . no N4A C4A Fe1 179.3(2) . . no N5A C5A Fe1 176.5(3) . . no O1A N6A Fe1 179.0(3) . . no O1S C1S C2S 115.2(3) . . no O1S C1S H1S1 108.5 . . no C2S C1S H1S1 108.5 . . no O1S C1S H1S2 108.5 . . no C2S C1S H1S2 108.5 . . no H1S1 C1S H1S2 107.5 . . no O2S C2S C1S 127.6(4) . . no O2S C2S H2S1 105.4 . . no C1S C2S H2S1 105.4 . . no O2S C2S H2S2 105.4 . . no C1S C2S H2S2 105.4 . . no H2S1 C2S H2S2 106.0 . . no C1S O1S H1S 109.5 . . no C2S O2S H2S 109.5 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 S2 C1 C2 179.9(2) . . . . no C4 S2 C1 S1 1.37(16) . . . . no C3 S1 C1 C2 -179.4(2) . . . . no C3 S1 C1 S2 -0.84(17) . . . . no S2 C1 C2 S3 178.68(13) . . . . no S1 C1 C2 S3 -2.9(3) . . . . no S2 C1 C2 S4 -2.3(3) . . . . no S1 C1 C2 S4 176.13(13) . . . . no C5 S3 C2 C1 177.2(2) . . . . no C5 S3 C2 S4 -1.89(16) . . . . no C6 S4 C2 C1 -177.9(2) . . . . no C6 S4 C2 S3 1.21(16) . . . . no C7 S5 C3 C4 0.5(3) . . . . no C7 S5 C3 S1 -177.37(14) . . . . no C1 S1 C3 C4 -0.2(2) . . . . no C1 S1 C3 S5 177.92(15) . . . . no S5 C3 C4 S2 -176.58(15) . . . . no S1 C3 C4 S2 1.3(3) . . . . no S5 C3 C4 S6 0.0(4) . . . . no S1 C3 C4 S6 177.83(14) . . . . no C1 S2 C4 C3 -1.6(2) . . . . no C1 S2 C4 S6 -178.52(15) . . . . no C8 S6 C4 C3 -25.9(3) . . . . no C8 S6 C4 S2 150.65(15) . . . . no C9B S7 C5 C6 -9.3(8) . . . . no C9 S7 C5 C6 15.8(3) . . . . no C9B S7 C5 S3 171.4(7) . . . . no C9 S7 C5 S3 -163.58(18) . . . . no C2 S3 C5 C6 2.1(2) . . . . no C2 S3 C5 S7 -178.46(14) . . . . no S7 C5 C6 S8 -0.5(4) . . . . no S3 C5 C6 S8 178.80(14) . . . . no S7 C5 C6 S4 179.03(15) . . . . no S3 C5 C6 S4 -1.6(3) . . . . no C10 S8 C6 C5 11.8(3) . . . . no C10B S8 C6 C5 -12.4(6) . . . . no C10 S8 C6 S4 -167.81(17) . . . . no C10B S8 C6 S4 168.0(6) . . . . no C2 S4 C6 C5 0.3(2) . . . . no C2 S4 C6 S8 179.88(14) . . . . no C3 S5 C7 C8 33.6(2) . . . . no S5 C7 C8 S6 -68.1(2) . . . . no C4 S6 C8 C7 59.12(19) . . . . no C5 S7 C9 C10 -49.5(3) . . . . no C9B S7 C9 C10 48.1(19) . . . . no S7 C9 C10 S8 70.4(4) . . . . no C6 S8 C10 C9 -46.1(4) . . . . no C10B S8 C10 C9 45.0(14) . . . . no C5 S7 C9B C10B 42(2) . . . . no C9 S7 C9B C10B -46.1(14) . . . . no S7 C9B C10B S8 -62(2) . . . . no C6 S8 C10B C9B 42.9(15) . . . . no C10 S8 C10B C9B -50.7(14) . . . . no C14 S12 C11 C12 177.1(2) . . . . no C14 S12 C11 S11 -1.37(16) . . . . no C13 S11 C11 C12 -176.8(2) . . . . no C13 S11 C11 S12 1.72(16) . . . . no S12 C11 C12 S14 -1.4(3) . . . . no S11 C11 C12 S14 176.93(14) . . . . no S12 C11 C12 S13 178.43(13) . . . . no S11 C11 C12 S13 -3.2(3) . . . . no C16 S14 C12 C11 -177.3(2) . . . . no C16 S14 C12 S13 2.79(16) . . . . no C15 S13 C12 C11 176.6(2) . . . . no C15 S13 C12 S14 -3.56(16) . . . . no C17 S15 C13 C14 -7.0(3) . . . . no C17 S15 C13 S11 175.02(15) . . . . no C11 S11 C13 C14 -1.5(2) . . . . no C11 S11 C13 S15 176.79(15) . . . . no S15 C13 C14 S12 -177.17(16) . . . . no S11 C13 C14 S12 0.8(3) . . . . no S15 C13 C14 S16 1.1(4) . . . . no S11 C13 C14 S16 179.15(14) . . . . no C11 S12 C14 C13 0.3(2) . . . . no C11 S12 C14 S16 -178.18(14) . . . . no C18 S16 C14 C13 -20.4(3) . . . . no C18 S16 C14 S12 157.89(15) . . . . no C19B S17 C15 C16 -8.6(7) . . . . no C19 S17 C15 C16 17.5(3) . . . . no C19B S17 C15 S13 172.2(7) . . . . no C19 S17 C15 S13 -161.66(18) . . . . no C12 S13 C15 C16 3.2(2) . . . . no C12 S13 C15 S17 -177.50(15) . . . . no S17 C15 C16 S18 -1.3(4) . . . . no S13 C15 C16 S18 177.89(14) . . . . no S17 C15 C16 S14 179.01(14) . . . . no S13 C15 C16 S14 -1.8(3) . . . . no C20 S18 C16 C15 10.3(3) . . . . no C20B S18 C16 C15 -16.5(6) . . . . no C20 S18 C16 S14 -169.99(18) . . . . no C20B S18 C16 S14 163.2(5) . . . . no C12 S14 C16 C15 -0.6(2) . . . . no C12 S14 C16 S18 179.65(14) . . . . no C13 S15 C17 C18 40.4(2) . . . . no S15 C17 C18 S16 -69.2(3) . . . . no C14 S16 C18 C17 53.8(2) . . . . no C19B S17 C19 C20 46.2(15) . . . . no C15 S17 C19 C20 -49.8(4) . . . . no S17 C19 C20 S18 68.1(4) . . . . no C16 S18 C20 C19 -43.7(4) . . . . no C20B S18 C20 C19 43.2(12) . . . . no C15 S17 C19B C20B 44.5(15) . . . . no C19 S17 C19B C20B -45.2(13) . . . . no S17 C19B C20B S18 -70.4(17) . . . . no C16 S18 C20B C19B 50.4(13) . . . . no C20 S18 C20B C19B -48.2(11) . . . . no C24 S22 C21 C22 178.3(2) . . . . no C24 S22 C21 S21 0.22(16) . . . . no C23 S21 C21 C22 -178.3(2) . . . . no C23 S21 C21 S22 -0.28(16) . . . . no S22 C21 C22 S23 -179.03(13) . . . . no S21 C21 C22 S23 -1.1(3) . . . . no S22 C21 C22 S24 1.7(3) . . . . no S21 C21 C22 S24 179.57(13) . . . . no C25 S23 C22 C21 -177.3(2) . . . . no C25 S23 C22 S24 2.03(16) . . . . no C26 S24 C22 C21 177.3(2) . . . . no C26 S24 C22 S23 -2.04(16) . . . . no C27 S25 C23 C24 4.3(3) . . . . no C27 S25 C23 S21 -173.89(14) . . . . no C21 S21 C23 C24 0.3(2) . . . . no C21 S21 C23 S25 178.70(14) . . . . no S25 C23 C24 S22 -178.34(14) . . . . no S21 C23 C24 S22 -0.1(3) . . . . no S25 C23 C24 S26 -2.5(4) . . . . no S21 C23 C24 S26 175.70(14) . . . . no C21 S22 C24 C23 -0.1(2) . . . . no C21 S22 C24 S26 -176.34(15) . . . . no C28 S26 C24 C23 -26.3(3) . . . . no C28 S26 C24 S22 149.60(15) . . . . no C29B S27 C25 C26 -11.2(5) . . . . no C29 S27 C25 C26 12.4(3) . . . . no C29B S27 C25 S23 168.3(4) . . . . no C29 S27 C25 S23 -168.2(2) . . . . no C22 S23 C25 C26 -1.2(2) . . . . no C22 S23 C25 S27 179.28(15) . . . . no S27 C25 C26 S24 179.41(15) . . . . no S23 C25 C26 S24 0.0(3) . . . . no S27 C25 C26 S28 0.5(4) . . . . no S23 C25 C26 S28 -178.96(15) . . . . no C22 S24 C26 C25 1.2(2) . . . . no C22 S24 C26 S28 -179.65(14) . . . . no C30 S28 C26 C25 14.3(3) . . . . no C30B S28 C26 C25 -13.6(5) . . . . no C30 S28 C26 S24 -164.6(2) . . . . no C30B S28 C26 S24 167.4(4) . . . . no C23 S25 C27 C28 30.7(2) . . . . no S25 C27 C28 S26 -66.6(3) . . . . no C24 S26 C28 C27 59.7(2) . . . . no C29B S27 C29 C30 50.8(13) . . . . no C25 S27 C29 C30 -47.9(4) . . . . no S27 C29 C30 S28 71.7(5) . . . . no C26 S28 C30 C29 -48.5(4) . . . . no C30B S28 C30 C29 41.2(7) . . . . no C25 S27 C29B C30B 44.1(11) . . . . no C29 S27 C29B C30B -42.2(10) . . . . no S27 C29B C30B S28 -66.2(12) . . . . no C26 S28 C30B C29B 45.3(9) . . . . no C30 S28 C30B C29B -50.2(8) . . . . no O1S C1S C2S O2S 37.4(7) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C8 H8B N2A 0.97 2.72 3.282(4) 117.4 2 n C8 H8A N2A 0.97 2.52 3.328(3) 140.6 1_565 n C9 H9B N3A 0.97 2.62 3.575(5) 169.9 2_556 n C10 H10B N4A 0.97 2.67 3.319(5) 124.8 1_556 n C9B H9C N3A 0.97 2.53 3.46(2) 162.2 2_556 n C10B H10C N4A 0.97 2.71 3.319(18) 121.4 1_556 n C18 H18B N1A 0.97 2.65 3.315(4) 125.7 . n C19 H19B N4A 0.97 2.66 3.615(5) 169.3 1_556 n C19B H19C N4A 0.97 2.58 3.530(19) 165.1 1_556 n C28 H28A N1A 0.97 2.61 3.353(3) 134.0 2_665 n C30 H30B N3A 0.97 2.63 3.317(5) 128.5 2_656 n C29B H29D S25 0.97 2.81 3.683(11) 150.3 2_656 n C30B H30C N3A 0.97 2.69 3.347(11) 125.2 2_656 n C18 H18A O2S 0.97 2.56 3.382(4) 142.7 2_665 n C27 H27A O2S 0.97 2.93 3.619(4) 129.1 . n C29 H29A O2S 0.97 2.87 3.512(7) 124.8 1_556 n C29 H29B O1S 0.97 2.65 3.495(7) 146.2 1_556 n C29B H29C O1S 0.97 2.72 3.645(14) 158.5 1_556 n O1S H1S N5A 0.82 2.02 2.812(4) 162.4 . n O2S H2S O1S 0.82 2.01 2.772(3) 154.9 2_655 n #################################################################### # END of CIF ####################################################################