# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/255 data_global # REFERENCE : B002885L # ===================== # 1. SUBMISSION DETAILS _publ_contact_author_name ; L\'aszl\'o P\'ark\'anyi Chemical Research Center, Hungarian Academy Sciences Institute of Chemistry, H-1525-Budapest, P.O.Box 17 Hungary ; _publ_contact_author_phone '036 1 212-4790' _publ_contact_author_fax '036 1 212-5020' _publ_contact_author_email 'parka@cric.chemres.hu' _publ_requested_journal 'J.Chem.Soc. Dalton Transactions' _publ_section_title ; Crystallographic characterization of arenesulfonyl azides. Structural and kinetic effects induced by ortho and para substituents ; _publ_contact_letter ; This file contains the cif files of the crystal structures (data_azid4nit; data_azid4ac; data_azid4ome; data_azid2nit; data_ferocn3) discussed in the submitted paper entitled: "Crystallographic characterization of arenesulfonyl azides. Structural and kinetic effects induced by ortho and para substituents" by G. Besenyei*, L. Parkanyi, I. Foch, L.I. Simandi and A. Kalman. Problems related to the crystallographic part of the paper should be addressed to L. Parkanyi. Yours sincerely, L. P\'ark\'anyi ; # 2. DATA # ======= # ------------------------------------------------------------- # azid4nit : 2a data_azid4nit _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4-nitrobenzenesulfonyl azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 N4 O4 S' _chemical_formula_weight 228.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 16.318(1) _cell_length_b 10.782(1) _cell_length_c 10.295(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1811.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.95 _cell_measurement_theta_max 16.90 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 0.9854 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_reflns_number 8512 _diffrn_reflns_av_R_equivalents 0.0040 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 34.98 _reflns_number_total 7933 _reflns_number_gt 5584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0607P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(4) _refine_ls_number_reflns 7933 _refine_ls_number_parameters 271 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.002 _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 S1 S 0.862488(19) 0.64651(3) 0.96869(3) 0.04115(7) Uani 1 1 d . . . O1 O 0.80162(6) 0.73632(10) 0.93517(10) 0.0520(2) Uani 1 1 d . . . O2 O 0.84413(7) 0.51758(10) 0.97216(14) 0.0626(3) Uani 1 1 d . . . O3 O 1.03598(12) 0.71572(18) 1.54246(14) 0.0932(5) Uani 1 1 d . . . O4 O 1.03367(12) 0.90532(17) 1.48244(17) 0.0964(5) Uani 1 1 d . . . N1 N 0.94027(9) 0.65443(12) 0.86233(13) 0.0509(3) Uani 1 1 d . . . N2 N 0.95474(7) 0.76320(12) 0.82503(11) 0.0484(3) Uani 1 1 d . . . N3 N 0.97224(11) 0.85458(15) 0.78623(18) 0.0701(4) Uani 1 1 d . . . N4 N 1.01877(8) 0.79685(16) 1.46588(14) 0.0639(4) Uani 1 1 d . . . C1 C 0.90699(7) 0.69086(11) 1.11734(11) 0.0372(2) Uani 1 1 d . . . C2 C 0.94541(10) 0.60143(13) 1.19254(14) 0.0508(3) Uani 1 1 d . . . H2 H 0.9470 0.5191 1.1656 0.066 Uiso 1 1 calc R . . C3 C 0.98136(11) 0.63685(14) 1.30837(16) 0.0554(4) Uani 1 1 d . . . H3 H 1.0072 0.5790 1.3614 0.072 Uiso 1 1 calc R . . C4 C 0.97786(8) 0.76003(14) 1.34301(12) 0.0455(3) Uani 1 1 d . . . C5 C 0.94033(9) 0.84976(13) 1.27012(14) 0.0478(3) Uani 1 1 d . . . H5 H 0.9396 0.9320 1.2973 0.062 Uiso 1 1 calc R . . C6 C 0.90338(9) 0.81449(11) 1.15452(13) 0.0436(3) Uani 1 1 d . . . H6 H 0.8767 0.8726 1.1029 0.057 Uiso 1 1 calc R . . S1' S 1.30196(2) 0.86683(3) 1.56461(3) 0.04739(8) Uani 1 1 d . . . O1' O 1.33454(7) 0.74754(10) 1.59450(11) 0.0549(2) Uani 1 1 d . . . O2' O 1.35168(9) 0.97478(12) 1.56993(15) 0.0761(4) Uani 1 1 d . . . O3' O 1.13788(11) 0.94153(16) 0.98441(15) 0.0886(5) Uani 1 1 d . . . O4' O 1.09397(9) 0.75749(17) 1.02717(14) 0.0850(5) Uani 1 1 d . . . N1' N 1.22435(12) 0.89903(16) 1.66849(14) 0.0687(4) Uani 1 1 d . . . N2' N 1.18952(10) 0.80159(17) 1.70753(12) 0.0622(4) Uani 1 1 d . . . N3' N 1.15553(10) 0.7221(2) 1.75075(19) 0.0805(5) Uani 1 1 d . . . N4' N 1.13164(8) 0.85103(14) 1.05433(14) 0.0581(3) Uani 1 1 d . . . C1' C 1.25273(8) 0.85982(10) 1.41225(12) 0.0381(2) Uani 1 1 d . . . C2' C 1.23931(10) 0.97037(12) 1.34722(13) 0.0494(3) Uani 1 1 d . . . H2' H 1.2563 1.0453 1.3830 0.064 Uiso 1 1 calc R . . C3' C 1.20012(10) 0.96746(13) 1.22779(14) 0.0507(3) Uani 1 1 d . . . H3' H 1.1911 1.0399 1.1809 0.066 Uiso 1 1 calc R . . C4' C 1.17496(8) 0.85423(13) 1.18062(13) 0.0430(3) Uani 1 1 d . . . C5' C 1.18771(9) 0.74276(13) 1.24491(13) 0.0451(3) Uani 1 1 d . . . H5' H 1.1696 0.6681 1.2099 0.059 Uiso 1 1 calc R . . C6' C 1.22822(8) 0.74645(11) 1.36254(12) 0.0418(2) Uani 1 1 d . . . H6' H 1.2389 0.6736 1.4079 0.054 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 0.04418(14) 0.03974(13) 0.03955(13) -0.00526(12) -0.00809(12) -0.00242(11) O1 0.0460(5) 0.0610(6) 0.0491(5) -0.0019(4) -0.0136(4) 0.0060(4) O2 0.0784(7) 0.0436(5) 0.0659(7) -0.0061(5) -0.0137(6) -0.0167(5) O3 0.1102(12) 0.1170(13) 0.0524(7) -0.0125(8) -0.0369(7) 0.0286(10) O4 0.1132(12) 0.1071(12) 0.0690(9) -0.0246(9) -0.0291(9) -0.0290(10) N1 0.0589(7) 0.0507(6) 0.0431(6) -0.0096(5) 0.0017(5) 0.0045(5) N2 0.0464(6) 0.0588(7) 0.0401(5) -0.0081(5) -0.0036(5) -0.0027(5) N3 0.0751(10) 0.0700(10) 0.0652(10) 0.0037(7) 0.0030(8) -0.0164(7) N4 0.0515(6) 0.0994(11) 0.0410(6) -0.0180(7) -0.0119(6) 0.0072(7) C1 0.0395(5) 0.0357(5) 0.0365(5) -0.0023(4) -0.0036(4) -0.0004(4) C2 0.0659(9) 0.0398(6) 0.0468(7) -0.0006(5) -0.0105(6) 0.0090(6) C3 0.0661(9) 0.0564(8) 0.0437(7) 0.0040(6) -0.0134(6) 0.0138(7) C4 0.0397(5) 0.0608(8) 0.0360(5) -0.0064(5) -0.0050(4) 0.0036(5) C5 0.0542(7) 0.0437(6) 0.0455(6) -0.0100(5) -0.0065(6) 0.0011(5) C6 0.0519(7) 0.0366(5) 0.0423(6) -0.0030(5) -0.0083(5) 0.0051(5) S1' 0.0626(2) 0.04285(14) 0.03672(13) -0.00032(13) -0.00898(14) 0.00040(13) O1' 0.0629(6) 0.0539(5) 0.0481(5) 0.0069(4) -0.0107(4) 0.0100(5) O2' 0.1024(10) 0.0591(7) 0.0669(8) -0.0026(6) -0.0233(8) -0.0250(7) O3' 0.1057(11) 0.1022(11) 0.0580(8) 0.0214(8) -0.0280(7) 0.0147(9) O4' 0.0780(9) 0.1190(12) 0.0580(8) 0.0003(7) -0.0249(7) -0.0258(9) N1' 0.0963(11) 0.0694(9) 0.0406(6) -0.0056(6) 0.0032(7) 0.0245(9) N2' 0.0567(7) 0.0956(12) 0.0342(5) 0.0036(7) -0.0068(5) 0.0155(8) N3' 0.0565(8) 0.1271(17) 0.0579(9) 0.0099(10) -0.0070(7) 0.0015(10) N4' 0.0463(6) 0.0871(10) 0.0407(6) 0.0026(6) -0.0072(5) 0.0101(6) C1' 0.0499(6) 0.0322(5) 0.0323(5) 0.0026(4) 0.0003(4) 0.0011(4) C2' 0.0740(9) 0.0302(5) 0.0441(6) 0.0029(4) -0.0047(6) 0.0024(5) C3' 0.0662(9) 0.0430(6) 0.0430(6) 0.0110(5) -0.0019(6) 0.0105(6) C4' 0.0394(6) 0.0562(7) 0.0336(5) 0.0026(5) -0.0008(4) 0.0068(5) C5' 0.0500(6) 0.0434(6) 0.0421(6) -0.0029(5) -0.0032(5) -0.0037(5) C6' 0.0535(6) 0.0316(5) 0.0402(5) 0.0042(4) -0.0044(5) -0.0019(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 S1 O2 1.4225(11) . ? S1 O1 1.4294(10) . ? S1 N1 1.6784(14) . ? S1 C1 1.7601(12) . ? O3 N4 1.211(2) . ? O4 N4 1.207(2) . ? N1 N2 1.2564(19) . ? N2 N3 1.101(2) . ? N4 C4 1.4844(18) . ? C1 C2 1.3864(18) . ? C1 C6 1.3882(16) . ? C2 C3 1.383(2) . ? C3 C4 1.376(2) . ? C4 C5 1.369(2) . ? C5 C6 1.3873(19) . ? S1' O2' 1.4199(12) . ? S1' O1' 1.4253(11) . ? S1' N1' 1.6935(17) . ? S1' C1' 1.7638(13) . ? O3' N4' 1.217(2) . ? O4' N4' 1.214(2) . ? N1' N2' 1.260(3) . ? N2' N3' 1.114(3) . ? N4' C4' 1.4803(18) . ? C1' C2' 1.3846(16) . ? C1' C6' 1.3843(17) . ? C2' C3' 1.386(2) . ? C3' C4' 1.377(2) . ? C4' C5' 1.388(2) . ? C5' C6' 1.3803(18) . ? 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 O2 S1 O1 121.45(7) . . ? O2 S1 N1 103.02(7) . . ? O1 S1 N1 109.48(7) . . ? O2 S1 C1 109.30(7) . . ? O1 S1 C1 108.21(6) . . ? N1 S1 C1 103.97(6) . . ? N2 N1 S1 112.89(10) . . ? N3 N2 N1 174.31(17) . . ? O4 N4 O3 124.17(15) . . ? O4 N4 C4 118.06(16) . . ? O3 N4 C4 117.77(16) . . ? C2 C1 C6 122.21(12) . . ? C2 C1 S1 118.89(10) . . ? C6 C1 S1 118.89(9) . . ? C3 C2 C1 118.77(13) . . ? C4 C3 C2 118.19(13) . . ? C5 C4 C3 123.95(12) . . ? C5 C4 N4 118.63(14) . . ? C3 C4 N4 117.41(14) . . ? C4 C5 C6 118.09(12) . . ? C1 C6 C5 118.77(12) . . ? O2' S1' O1' 121.21(9) . . ? O2' S1' N1' 103.58(9) . . ? O1' S1' N1' 109.12(8) . . ? O2' S1' C1' 109.25(7) . . ? O1' S1' C1' 108.86(6) . . ? N1' S1' C1' 103.29(8) . . ? N2' N1' S1' 111.57(13) . . ? N3' N2' N1' 173.5(2) . . ? O4' N4' O3' 124.92(15) . . ? O4' N4' C4' 117.62(14) . . ? O3' N4' C4' 117.44(14) . . ? C2' C1' C6' 122.40(12) . . ? C2' C1' S1' 117.72(9) . . ? C6' C1' S1' 119.88(9) . . ? C1' C2' C3' 118.84(12) . . ? C4' C3' C2' 118.07(12) . . ? C3' C4' C5' 123.72(13) . . ? C3' C4' N4' 118.23(13) . . ? C5' C4' N4' 118.05(13) . . ? C6' C5' C4' 117.73(12) . . ? C5' C6' C1' 119.22(12) . . ? 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 O2 S1 N1 N2 166.24(11) . . . . ? O1 S1 N1 N2 35.70(13) . . . . ? C1 S1 N1 N2 -79.74(12) . . . . ? S1 N1 N2 N3 -179(100) . . . . ? O2 S1 C1 C2 23.45(14) . . . . ? O1 S1 C1 C2 157.65(12) . . . . ? N1 S1 C1 C2 -86.02(13) . . . . ? O2 S1 C1 C6 -157.40(11) . . . . ? O1 S1 C1 C6 -23.20(12) . . . . ? N1 S1 C1 C6 93.14(11) . . . . ? C6 C1 C2 C3 -0.1(2) . . . . ? S1 C1 C2 C3 179.07(13) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C2 C3 C4 N4 -178.35(15) . . . . ? O4 N4 C4 C5 -16.5(2) . . . . ? O3 N4 C4 C5 164.42(17) . . . . ? O4 N4 C4 C3 162.48(17) . . . . ? O3 N4 C4 C3 -16.6(2) . . . . ? C3 C4 C5 C6 0.2(2) . . . . ? N4 C4 C5 C6 179.04(14) . . . . ? C2 C1 C6 C5 0.8(2) . . . . ? S1 C1 C6 C5 -178.37(11) . . . . ? C4 C5 C6 C1 -0.8(2) . . . . ? O2' S1' N1' N2' -158.74(12) . . . . ? O1' S1' N1' N2' -28.34(15) . . . . ? C1' S1' N1' N2' 87.34(13) . . . . ? S1' N1' N2' N3' 165.2(15) . . . . ? O2' S1' C1' C2' -26.17(14) . . . . ? O1' S1' C1' C2' -160.55(12) . . . . ? N1' S1' C1' C2' 83.58(13) . . . . ? O2' S1' C1' C6' 154.53(12) . . . . ? O1' S1' C1' C6' 20.16(14) . . . . ? N1' S1' C1' C6' -95.72(13) . . . . ? C6' C1' C2' C3' -0.2(2) . . . . ? S1' C1' C2' C3' -179.47(12) . . . . ? C1' C2' C3' C4' 1.2(2) . . . . ? C2' C3' C4' C5' -1.0(2) . . . . ? C2' C3' C4' N4' 178.82(13) . . . . ? O4' N4' C4' C3' -163.88(16) . . . . ? O3' N4' C4' C3' 17.6(2) . . . . ? O4' N4' C4' C5' 16.0(2) . . . . ? O3' N4' C4' C5' -162.59(15) . . . . ? C3' C4' C5' C6' -0.2(2) . . . . ? N4' C4' C5' C6' 179.93(12) . . . . ? C4' C5' C6' C1' 1.3(2) . . . . ? C2' C1' C6' C5' -1.1(2) . . . . ? S1' C1' C6' C5' 178.19(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 34.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.297 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.043 # =======================================================END # azid4ac : 2b data_azid4ac _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4-acetylbenzenesulfonyl azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 N3 O3 S' _chemical_formula_weight 225.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.083(1) _cell_length_b 7.309(1) _cell_length_c 10.280(1) _cell_angle_alpha 97.73(1) _cell_angle_beta 108.70(1) _cell_angle_gamma 100.06(1) _cell_volume 485.88(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.04 _cell_measurement_theta_max 20.58 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 232 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7 _diffrn_reflns_number 9019 _diffrn_reflns_av_R_equivalents 0.0095 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 34.96 _reflns_number_total 3507 _reflns_number_gt 2512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0839P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3507 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 S1 S 0.63444(4) 0.82235(4) 0.15236(2) 0.04436(10) Uani 1 1 d . . . O1 O 0.70121(19) 1.02374(13) 0.19717(10) 0.0659(3) Uani 1 1 d . . . O2 O 0.69924(18) 0.72346(17) 0.05152(10) 0.0647(3) Uani 1 1 d . . . O3 O 0.7821(2) 0.27540(14) 0.62908(11) 0.0684(3) Uani 1 1 d . . . N1 N 0.37694(17) 0.76162(15) 0.07691(11) 0.0542(2) Uani 1 1 d . . . N2 N 0.29039(19) 0.88251(17) 0.11560(12) 0.0572(3) Uani 1 1 d . . . N3 N 0.1968(3) 0.9785(3) 0.1394(2) 0.0890(5) Uani 1 1 d . . . C1 C 0.68198(14) 0.71585(13) 0.29901(9) 0.03615(17) Uani 1 1 d . . . C2 C 0.65176(16) 0.51939(14) 0.27807(9) 0.03983(19) Uani 1 1 d . . . H2 H 0.6033 0.4458 0.1878 0.052 Uiso 1 1 calc R . . C3 C 0.69482(15) 0.43561(14) 0.39334(10) 0.03976(19) Uani 1 1 d . . . H3 H 0.6731 0.3042 0.3806 0.052 Uiso 1 1 calc R . . C4 C 0.77066(13) 0.54590(13) 0.52883(9) 0.03532(16) Uani 1 1 d . . . C5 C 0.79862(17) 0.74256(15) 0.54768(10) 0.0424(2) Uani 1 1 d . . . H5 H 0.8485 0.8164 0.6379 0.055 Uiso 1 1 calc R . . C6 C 0.75244(17) 0.82930(14) 0.43233(10) 0.0427(2) Uani 1 1 d . . . H6 H 0.7685 0.9602 0.4444 0.056 Uiso 1 1 calc R . . C41 C 0.82106(16) 0.44756(16) 0.65061(11) 0.0429(2) Uani 1 1 d . . . C42 C 0.91792(19) 0.56329(19) 0.79668(11) 0.0516(3) Uani 1 1 d . . . H42A H 0.8156 0.6100 0.8251 0.072 Uiso 1 1 calc R . . H42B H 1.0225 0.6684 0.7995 0.072 Uiso 1 1 calc R . . H42C H 0.9778 0.4858 0.8593 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 S1 0.05451(16) 0.04255(14) 0.03150(12) 0.00950(9) 0.01167(10) 0.00495(10) O1 0.0872(7) 0.0421(4) 0.0509(5) 0.0126(4) 0.0105(5) -0.0054(4) O2 0.0808(6) 0.0798(7) 0.0448(4) 0.0174(4) 0.0328(5) 0.0234(5) O3 0.0970(8) 0.0471(5) 0.0521(5) 0.0187(4) 0.0147(5) 0.0097(5) N1 0.0588(5) 0.0502(5) 0.0414(5) 0.0058(4) 0.0021(4) 0.0142(4) N2 0.0689(6) 0.0602(6) 0.0494(5) 0.0260(5) 0.0198(5) 0.0234(5) N3 0.1088(13) 0.0925(11) 0.0965(12) 0.0408(10) 0.0522(11) 0.0548(10) C1 0.0382(4) 0.0370(4) 0.0290(3) 0.0048(3) 0.0084(3) 0.0056(3) C2 0.0467(5) 0.0367(4) 0.0297(4) 0.0012(3) 0.0082(3) 0.0076(3) C3 0.0454(4) 0.0343(4) 0.0345(4) 0.0042(3) 0.0090(3) 0.0083(3) C4 0.0334(4) 0.0385(4) 0.0311(4) 0.0066(3) 0.0087(3) 0.0061(3) C5 0.0528(5) 0.0391(4) 0.0281(4) 0.0024(3) 0.0084(3) 0.0066(4) C6 0.0546(5) 0.0344(4) 0.0319(4) 0.0032(3) 0.0091(4) 0.0065(4) C41 0.0441(4) 0.0469(5) 0.0365(4) 0.0128(4) 0.0115(4) 0.0096(4) C42 0.0555(6) 0.0614(7) 0.0334(4) 0.0141(4) 0.0103(4) 0.0088(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 S1 O2 1.4239(10) . ? S1 O1 1.4273(10) . ? S1 N1 1.6860(12) . ? S1 C1 1.7532(9) . ? O3 C41 1.2137(14) . ? N1 N2 1.2514(15) . ? N2 N3 1.1013(19) . ? C1 C6 1.3878(13) . ? C1 C2 1.3906(13) . ? C2 C3 1.3787(14) . ? C3 C4 1.3947(13) . ? C4 C5 1.3942(14) . ? C4 C41 1.5022(14) . ? C5 C6 1.3932(14) . ? C41 C42 1.4953(16) . ? 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 O2 S1 O1 120.89(7) . . ? O2 S1 N1 102.91(6) . . ? O1 S1 N1 109.41(6) . . ? O2 S1 C1 109.00(5) . . ? O1 S1 C1 109.69(5) . . ? N1 S1 C1 103.42(5) . . ? N2 N1 S1 113.68(9) . . ? N3 N2 N1 172.95(18) . . ? C6 C1 C2 121.87(9) . . ? C6 C1 S1 119.39(7) . . ? C2 C1 S1 118.73(7) . . ? C3 C2 C1 118.88(8) . . ? C2 C3 C4 120.68(9) . . ? C5 C4 C3 119.59(9) . . ? C5 C4 C41 121.99(8) . . ? C3 C4 C41 118.42(9) . . ? C6 C5 C4 120.48(9) . . ? C1 C6 C5 118.47(9) . . ? O3 C41 C42 120.96(10) . . ? O3 C41 C4 119.55(10) . . ? C42 C41 C4 119.49(10) . . ? _diffrn_measured_fraction_theta_max 0.823 _diffrn_reflns_theta_full 34.96 _diffrn_measured_fraction_theta_full 0.823 _refine_diff_density_max 0.429 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.062 # =======================================================END # azid4ome : 2c data_azid4ome _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4-methoxybenzenesulfonyl azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 N3 O3 S' _chemical_formula_weight 213.22 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' 'O' 'O' 0.0106 0.0060 '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' _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 5.174(1) _cell_length_b 10.727(1) _cell_length_c 16.762(1) _cell_angle_alpha 90.00(1) _cell_angle_beta 94.22(1) _cell_angle_gamma 90.00(1) _cell_volume 927.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21.06 _cell_measurement_theta_max 21.85 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min .9533 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4263 _diffrn_reflns_av_R_equivalents 0.0054 _diffrn_reflns_av_sigmaI/netI 0.0105 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 34.96 _reflns_number_total 4027 _reflns_number_gt 3030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0920P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.016(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4027 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 S1 S 0.47078(4) 0.55895(2) 0.165859(14) 0.04327(9) Uani 1 1 d . . . O1 O 0.28008(18) 0.46583(10) 0.17628(6) 0.0661(2) Uani 1 1 d . . . O2 O 0.39677(17) 0.68216(7) 0.14219(5) 0.0594(2) Uani 1 1 d . . . O3 O 1.24371(19) 0.56039(7) 0.43786(6) 0.0594(2) Uani 1 1 d . . . N1 N 0.6406(2) 0.49678(8) 0.09187(6) 0.0542(2) Uani 1 1 d . . . N2 N 0.76924(18) 0.57671(10) 0.05801(6) 0.0542(2) Uani 1 1 d . . . N3 N 0.8880(3) 0.64030(16) 0.02354(9) 0.0810(4) Uani 1 1 d . . . C1 C 0.69513(17) 0.56450(7) 0.24813(5) 0.03769(16) Uani 1 1 d . . . C2 C 0.83737(18) 0.67256(7) 0.26431(5) 0.04145(17) Uani 1 1 d . . . H2 H 0.8076 0.7428 0.2325 0.054 Uiso 1 1 calc R . . C3 C 1.02414(18) 0.67538(8) 0.32815(5) 0.04277(18) Uani 1 1 d . . . H3 H 1.1199 0.7474 0.3394 0.056 Uiso 1 1 calc R . . C4 C 1.06660(19) 0.56920(8) 0.37514(5) 0.04245(18) Uani 1 1 d . . . C5 C 0.9184(2) 0.46146(9) 0.35891(6) 0.0489(2) Uani 1 1 d . . . H5 H 0.9454 0.3914 0.3912 0.064 Uiso 1 1 calc R . . C6 C 0.7336(2) 0.45862(8) 0.29570(6) 0.04496(19) Uani 1 1 d . . . H6 H 0.6357 0.3871 0.2848 0.058 Uiso 1 1 calc R . . C7 C 1.4130(2) 0.66403(12) 0.45512(7) 0.0581(3) Uani 1 1 d . . . H7A H 1.5031 0.6837 0.4087 0.081 Uiso 1 1 calc R . . H7B H 1.5362 0.6430 0.4987 0.081 Uiso 1 1 calc R . . H7C H 1.3132 0.7349 0.4696 0.081 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 0.04300(13) 0.04243(13) 0.04331(14) -0.00347(7) -0.00403(9) 0.00199(7) O1 0.0522(5) 0.0739(5) 0.0709(6) 0.0001(4) -0.0037(4) -0.0172(4) O2 0.0683(5) 0.0503(4) 0.0570(4) -0.0021(3) -0.0128(3) 0.0198(3) O3 0.0660(5) 0.0589(5) 0.0500(4) 0.0076(3) -0.0184(4) -0.0019(3) N1 0.0680(5) 0.0491(4) 0.0450(4) -0.0119(3) 0.0011(4) 0.0026(4) N2 0.0466(4) 0.0703(5) 0.0448(4) -0.0094(4) -0.0033(3) 0.0021(4) N3 0.0683(7) 0.1040(10) 0.0718(7) 0.0014(7) 0.0119(5) -0.0140(7) C1 0.0433(4) 0.0332(3) 0.0362(3) -0.0006(2) 0.0005(3) 0.0000(3) C2 0.0501(4) 0.0323(3) 0.0411(4) 0.0036(3) -0.0021(3) -0.0013(3) C3 0.0486(4) 0.0355(4) 0.0433(4) 0.0018(3) -0.0025(3) -0.0045(3) C4 0.0478(4) 0.0413(4) 0.0375(4) 0.0015(3) -0.0019(3) 0.0015(3) C5 0.0623(6) 0.0376(4) 0.0456(5) 0.0097(3) -0.0038(4) -0.0035(4) C6 0.0555(5) 0.0343(3) 0.0447(4) 0.0043(3) 0.0006(3) -0.0055(3) C7 0.0544(5) 0.0620(6) 0.0555(6) -0.0064(4) -0.0120(4) 0.0019(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 S1 O1 1.4238(9) . ? S1 O2 1.4243(8) . ? S1 N1 1.7073(10) . ? S1 C1 1.7370(9) . ? O3 C4 1.3462(13) . ? O3 C7 1.4315(14) . ? N1 N2 1.2474(15) . ? N2 N3 1.1086(18) . ? C1 C2 1.3890(11) . ? C1 C6 1.3937(12) . ? C2 C3 1.3884(13) . ? C3 C4 1.3930(12) . ? C4 C5 1.4025(13) . ? C5 C6 1.3743(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 S1 O2 120.71(6) . . ? O1 S1 N1 102.32(6) . . ? O2 S1 N1 107.59(5) . . ? O1 S1 C1 110.81(5) . . ? O2 S1 C1 109.85(4) . . ? N1 S1 C1 103.92(5) . . ? C4 O3 C7 118.32(8) . . ? N2 N1 S1 112.48(7) . . ? N3 N2 N1 174.21(14) . . ? C2 C1 C6 121.14(8) . . ? C2 C1 S1 119.81(6) . . ? C6 C1 S1 119.03(6) . . ? C3 C2 C1 119.82(7) . . ? C2 C3 C4 119.34(8) . . ? O3 C4 C3 124.68(8) . . ? O3 C4 C5 115.13(8) . . ? C3 C4 C5 120.19(9) . . ? C6 C5 C4 120.48(8) . . ? C5 C6 C1 119.01(8) . . ? 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 O1 S1 N1 N2 161.16(9) . . . . ? O2 S1 N1 N2 33.02(10) . . . . ? C1 S1 N1 N2 -83.45(9) . . . . ? S1 N1 N2 N3 -172.4(13) . . . . ? O1 S1 C1 C2 -157.05(9) . . . . ? O2 S1 C1 C2 -21.15(10) . . . . ? N1 S1 C1 C2 93.72(8) . . . . ? O1 S1 C1 C6 24.57(10) . . . . ? O2 S1 C1 C6 160.46(8) . . . . ? N1 S1 C1 C6 -84.67(9) . . . . ? C6 C1 C2 C3 0.96(14) . . . . ? S1 C1 C2 C3 -177.39(7) . . . . ? C1 C2 C3 C4 0.12(14) . . . . ? C7 O3 C4 C3 -4.18(16) . . . . ? C7 O3 C4 C5 176.27(10) . . . . ? C2 C3 C4 O3 179.26(10) . . . . ? C2 C3 C4 C5 -1.22(15) . . . . ? O3 C4 C5 C6 -179.17(10) . . . . ? C3 C4 C5 C6 1.26(16) . . . . ? C4 C5 C6 C1 -0.19(16) . . . . ? C2 C1 C6 C5 -0.92(15) . . . . ? S1 C1 C6 C5 177.45(8) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 34.96 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.354 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.068 # =======================================================END # azid2nit : 2d data_azid2nit _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-nitrobenzenesulfonyl azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 N4 O4 S' _chemical_formula_weight 228.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.908(1) _cell_length_b 14.572(1) _cell_length_c 8.238(1) _cell_angle_alpha 90.00 _cell_angle_beta 106.59(1) _cell_angle_gamma 90.00 _cell_volume 909.79(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.96 _cell_measurement_theta_max 16.73 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9714 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_reflns_number 4292 _diffrn_reflns_av_R_equivalents 0.0094 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 36.49 _reflns_number_total 3940 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0577P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3940 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _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 S1 S 0.26147(4) 0.060569(19) 0.81671(4) 0.03769(9) Uani 1 1 d . . . O1 O 0.37962(12) 0.09672(7) 0.97056(11) 0.0471(2) Uani 1 1 d . . . O2 O 0.14734(13) -0.00970(7) 0.83148(18) 0.0667(3) Uani 1 1 d . . . O3 O 0.37915(15) 0.34279(7) 0.87455(14) 0.0606(3) Uani 1 1 d . . . O4 O 0.47232(11) 0.22775(7) 0.75783(15) 0.0560(3) Uani 1 1 d . . . N1 N 0.36063(13) 0.01599(7) 0.67853(15) 0.0471(3) Uani 1 1 d . . . N2 N 0.51350(15) 0.03673(7) 0.71241(14) 0.0421(2) Uani 1 1 d . . . N3 N 0.65009(18) 0.04875(10) 0.7304(2) 0.0630(3) Uani 1 1 d . . . N4 N 0.35873(13) 0.27277(6) 0.78720(13) 0.0382(2) Uani 1 1 d . . . C1 C 0.13683(13) 0.15026(7) 0.69433(14) 0.0332(2) Uani 1 1 d . . . C2 C 0.18391(13) 0.24285(7) 0.70353(14) 0.0329(2) Uani 1 1 d . . . C3 C 0.06915(16) 0.31017(8) 0.62735(17) 0.0441(3) Uani 1 1 d . . . H3 H 0.1022 0.3716 0.6401 0.057 Uiso 1 1 calc R . . C4 C -0.09365(17) 0.28551(10) 0.5328(2) 0.0553(4) Uani 1 1 d . . . H4 H -0.1744 0.3303 0.4798 0.072 Uiso 1 1 calc R . . C5 C -0.14045(16) 0.19458(11) 0.5147(2) 0.0556(4) Uani 1 1 d . . . H5 H -0.2508 0.1783 0.4443 0.072 Uiso 1 1 calc R . . C6 C -0.02735(15) 0.12694(9) 0.59874(18) 0.0454(3) Uani 1 1 d . . . H6 H -0.0632 0.0659 0.5900 0.059 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 0.03673(13) 0.02967(12) 0.04568(17) 0.00642(11) 0.01019(11) 0.00076(10) O1 0.0497(5) 0.0491(5) 0.0381(4) 0.0027(4) 0.0057(4) 0.0084(4) O2 0.0559(6) 0.0422(5) 0.1026(10) 0.0224(6) 0.0238(6) -0.0079(4) O3 0.0671(6) 0.0431(5) 0.0633(6) -0.0152(5) 0.0053(5) -0.0139(5) O4 0.0327(4) 0.0534(6) 0.0786(7) -0.0082(5) 0.0107(4) -0.0049(4) N1 0.0408(5) 0.0399(5) 0.0552(7) -0.0111(5) 0.0051(5) 0.0057(4) N2 0.0463(6) 0.0369(5) 0.0441(6) 0.0000(4) 0.0148(4) 0.0058(4) N3 0.0521(7) 0.0652(8) 0.0792(10) -0.0053(7) 0.0307(7) -0.0005(6) N4 0.0392(5) 0.0319(4) 0.0407(5) 0.0009(4) 0.0067(4) -0.0081(4) C1 0.0290(4) 0.0302(5) 0.0394(5) 0.0005(4) 0.0081(4) 0.0001(4) C2 0.0325(5) 0.0285(4) 0.0369(5) 0.0000(4) 0.0085(4) 0.0001(4) C3 0.0448(6) 0.0332(5) 0.0538(7) 0.0051(5) 0.0134(5) 0.0076(5) C4 0.0408(6) 0.0525(8) 0.0675(9) 0.0107(7) 0.0072(6) 0.0174(6) C5 0.0310(5) 0.0574(8) 0.0701(9) 0.0001(7) 0.0012(5) 0.0054(5) C6 0.0296(5) 0.0411(6) 0.0617(8) -0.0040(5) 0.0069(5) -0.0021(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 S1 O2 1.3931(9) . ? S1 O1 1.4424(10) . ? S1 N1 1.6859(12) . ? S1 C1 1.7688(11) . ? O3 N4 1.2323(13) . ? O4 N4 1.1916(14) . ? N1 N2 1.1992(15) . ? N2 N3 1.0621(16) . ? N4 C2 1.4256(14) . ? C1 C6 1.3555(15) . ? C1 C2 1.3960(15) . ? C2 C3 1.3617(15) . ? C3 C4 1.3492(18) . ? C4 C5 1.372(2) . ? C5 C6 1.3774(19) . ? 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 O2 S1 O1 117.71(7) . . ? O2 S1 N1 102.33(7) . . ? O1 S1 N1 115.12(5) . . ? O2 S1 C1 108.87(6) . . ? O1 S1 C1 110.29(5) . . ? N1 S1 C1 101.00(6) . . ? N2 N1 S1 112.21(9) . . ? N3 N2 N1 172.55(14) . . ? O4 N4 O3 126.43(11) . . ? O4 N4 C2 114.62(10) . . ? O3 N4 C2 118.87(11) . . ? C6 C1 C2 118.05(10) . . ? C6 C1 S1 115.55(9) . . ? C2 C1 S1 125.92(8) . . ? C3 C2 C1 122.61(10) . . ? C3 C2 N4 115.42(10) . . ? C1 C2 N4 121.91(9) . . ? C4 C3 C2 118.34(12) . . ? C3 C4 C5 120.21(12) . . ? C4 C5 C6 121.33(12) . . ? C1 C6 C5 119.30(12) . . ? 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 O2 S1 N1 N2 -142.69(10) . . . . y O1 S1 N1 N2 -13.77(12) . . . . y C1 S1 N1 N2 104.99(10) . . . . y S1 N1 N2 N3 169.8(11) . . . . y O2 S1 C1 C6 -18.41(12) . . . . y O1 S1 C1 C6 -148.97(10) . . . . y N1 S1 C1 C6 88.83(10) . . . . y O2 S1 C1 C2 153.43(11) . . . . y O1 S1 C1 C2 22.87(12) . . . . y N1 S1 C1 C2 -99.33(11) . . . . y C6 C1 C2 C3 3.21(19) . . . . ? S1 C1 C2 C3 -168.45(10) . . . . y C6 C1 C2 N4 -173.79(12) . . . . y S1 C1 C2 N4 14.55(17) . . . . y O4 N4 C2 C3 -133.58(12) . . . . y O3 N4 C2 C3 43.31(16) . . . . y O4 N4 C2 C1 43.62(16) . . . . y O3 N4 C2 C1 -139.49(12) . . . . y C1 C2 C3 C4 -3.21(19) . . . . ? N4 C2 C3 C4 173.97(12) . . . . y C2 C3 C4 C5 -0.2(2) . . . . ? C3 C4 C5 C6 3.5(3) . . . . ? C2 C1 C6 C5 0.2(2) . . . . ? S1 C1 C6 C5 172.68(12) . . . . y C4 C5 C6 C1 -3.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 36.49 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.332 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.048 # ========================================================END # ferocn3 : 2f data_ferocn3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ferrocenesulfonyl azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H9 Fe N3 O2 S' _chemical_formula_weight 291.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 5.984(1) _cell_length_b 35.194(1) _cell_length_c 10.795(1) _cell_angle_alpha 90.00 _cell_angle_beta 92.29(1) _cell_angle_gamma 90.00 _cell_volume 2271.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.32 _cell_measurement_theta_max 16.99 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.503 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.607 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_process_details 'PLATON (Spek, 1982)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710730 _diffrn_radiation_type 'MO k\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 41.1 _diffrn_reflns_number 5791 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.97 _reflns_number_total 5175 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0584P)^2^+0.0959P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5175 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.08376(5) 0.297269(9) 0.42807(3) 0.03751(11) Uani 1 1 d . . . S1 S 0.14877(10) 0.203849(18) 0.40497(5) 0.04469(16) Uani 1 1 d . . . O1 O 0.3852(3) 0.20337(6) 0.40289(19) 0.0628(5) Uani 1 1 d . . . O2 O 0.0144(3) 0.19842(6) 0.29455(16) 0.0571(5) Uani 1 1 d . . . N1 N 0.0928(4) 0.16727(7) 0.5053(2) 0.0597(6) Uani 1 1 d . . . N2 N -0.0962(5) 0.15478(7) 0.4906(2) 0.0603(6) Uani 1 1 d . . . N3 N -0.2662(5) 0.14089(9) 0.4853(3) 0.0920(9) Uani 1 1 d . . . C1 C 0.0619(4) 0.24307(7) 0.4835(2) 0.0403(5) Uani 1 1 d . . . C2 C 0.1938(4) 0.26402(7) 0.5727(2) 0.0461(6) Uani 1 1 d . . . H2 H 0.3425 0.2595 0.5964 0.060 Uiso 1 1 calc R . . C3 C 0.0568(5) 0.29276(8) 0.6177(2) 0.0528(6) Uani 1 1 d . . . H3 H 0.0994 0.3106 0.6775 0.069 Uiso 1 1 calc R . . C4 C -0.1561(4) 0.29017(8) 0.5575(2) 0.0536(6) Uani 1 1 d . . . H4 H -0.2763 0.3062 0.5710 0.070 Uiso 1 1 calc R . . C5 C -0.1578(4) 0.25940(7) 0.4734(2) 0.0461(6) Uani 1 1 d . . . H5 H -0.2771 0.2514 0.4221 0.060 Uiso 1 1 calc R . . C6 C 0.3501(5) 0.31776(13) 0.3403(4) 0.0920(14) Uani 1 1 d . . . H6 H 0.4978 0.3105 0.3566 0.120 Uiso 1 1 calc R . . C7 C 0.1940(8) 0.30098(10) 0.2537(3) 0.0823(12) Uani 1 1 d . . . H7 H 0.2199 0.2804 0.2023 0.107 Uiso 1 1 calc R . . C8 C -0.0013(6) 0.32090(12) 0.2603(3) 0.0782(10) Uani 1 1 d . . . H8 H -0.1313 0.3161 0.2128 0.102 Uiso 1 1 calc R . . C9 C 0.0231(7) 0.34820(10) 0.3452(4) 0.0835(11) Uani 1 1 d . . . H9 H -0.0880 0.3652 0.3666 0.109 Uiso 1 1 calc R . . C10 C 0.2341(7) 0.34754(11) 0.3959(3) 0.0839(11) Uani 1 1 d . . . H10 H 0.2918 0.3639 0.4567 0.109 Uiso 1 1 calc R . . Fe1' Fe 0.25099(5) 0.062714(10) 0.25569(3) 0.04114(11) Uani 1 1 d . . . S1' S 0.34288(11) -0.02895(2) 0.22643(6) 0.05160(17) Uani 1 1 d . . . O1' O 0.5798(3) -0.02796(7) 0.2244(2) 0.0790(7) Uani 1 1 d . . . O2' O 0.2115(4) -0.03286(6) 0.11526(17) 0.0671(5) Uani 1 1 d . . . N1' N 0.2901(5) -0.06717(7) 0.3191(3) 0.0709(7) Uani 1 1 d . . . N2' N 0.1051(5) -0.08125(7) 0.2929(2) 0.0626(6) Uani 1 1 d . . . N3' N -0.0579(5) -0.09659(9) 0.2780(3) 0.0903(9) Uani 1 1 d . . . C1' C 0.2501(4) 0.00865(7) 0.3120(2) 0.0441(5) Uani 1 1 d . . . C2' C 0.3860(4) 0.03084(8) 0.3966(2) 0.0505(6) Uani 1 1 d . . . H2' H 0.5374 0.0272 0.4158 0.066 Uiso 1 1 calc R . . C3' C 0.2487(5) 0.05910(8) 0.4456(2) 0.0579(7) Uani 1 1 d . . . H3' H 0.2942 0.0778 0.5021 0.075 Uiso 1 1 calc R . . C4' C 0.0292(5) 0.05429(9) 0.3939(3) 0.0599(7) Uani 1 1 d . . . H4' H -0.0940 0.0691 0.4120 0.078 Uiso 1 1 calc R . . C5' C 0.0273(4) 0.02302(8) 0.3096(2) 0.0515(6) Uani 1 1 d . . . H5' H -0.0947 0.0139 0.2626 0.067 Uiso 1 1 calc R . . C6' C 0.5062(6) 0.08729(12) 0.1679(3) 0.0819(11) Uani 1 1 d . . . H6' H 0.6573 0.0835 0.1876 0.106 Uiso 1 1 calc R . . C7' C 0.3706(8) 0.06541(10) 0.0827(3) 0.0871(13) Uani 1 1 d . . . H7' H 0.4162 0.0448 0.0362 0.113 Uiso 1 1 calc R . . C8' C 0.1537(6) 0.08127(10) 0.0828(3) 0.0716(9) Uani 1 1 d . . . H8' H 0.0297 0.0729 0.0358 0.093 Uiso 1 1 calc R . . C9' C 0.1582(5) 0.11139(9) 0.1648(3) 0.0679(8) Uani 1 1 d . . . H9' H 0.0364 0.1266 0.1825 0.088 Uiso 1 1 calc R . . C10' C 0.3705(6) 0.11535(9) 0.2162(3) 0.0729(9) Uani 1 1 d . . . H10' H 0.4162 0.1337 0.2737 0.095 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 0.03458(17) 0.0414(2) 0.03646(17) -0.00013(13) 0.00007(12) 0.00100(13) S1 0.0461(3) 0.0456(4) 0.0422(3) -0.0012(2) 0.0002(2) 0.0050(3) O1 0.0448(10) 0.0697(14) 0.0744(12) -0.0091(10) 0.0081(9) 0.0096(9) O2 0.0698(12) 0.0580(12) 0.0427(9) -0.0063(8) -0.0056(8) 0.0034(9) N1 0.0660(15) 0.0500(14) 0.0617(14) 0.0103(11) -0.0148(11) 0.0010(12) N2 0.0773(18) 0.0402(13) 0.0631(14) 0.0055(11) -0.0015(13) 0.0048(12) N3 0.080(2) 0.079(2) 0.116(2) 0.0197(18) -0.0039(18) -0.0137(17) C1 0.0383(11) 0.0454(13) 0.0372(11) 0.0032(10) 0.0021(9) 0.0024(10) C2 0.0484(13) 0.0540(15) 0.0356(11) 0.0030(10) -0.0035(10) 0.0024(11) C3 0.0675(17) 0.0567(17) 0.0342(12) -0.0064(11) 0.0014(11) 0.0014(13) C4 0.0482(14) 0.0572(17) 0.0571(15) 0.0001(12) 0.0221(12) 0.0094(12) C5 0.0360(12) 0.0485(14) 0.0540(14) 0.0024(11) 0.0047(10) -0.0018(10) C6 0.0417(16) 0.119(3) 0.116(3) 0.072(3) 0.0168(18) 0.0039(18) C7 0.132(4) 0.0566(19) 0.0614(19) -0.0042(15) 0.046(2) -0.013(2) C8 0.072(2) 0.110(3) 0.0517(17) 0.0288(19) -0.0156(15) -0.014(2) C9 0.099(3) 0.060(2) 0.093(3) 0.0297(19) 0.023(2) 0.0234(19) C10 0.118(3) 0.066(2) 0.068(2) 0.0060(17) -0.004(2) -0.046(2) Fe1' 0.04177(19) 0.0420(2) 0.03980(18) -0.00029(14) 0.00305(13) -0.00315(14) S1' 0.0497(4) 0.0495(4) 0.0561(4) -0.0071(3) 0.0067(3) -0.0032(3) O1' 0.0488(11) 0.0773(16) 0.1118(18) -0.0249(13) 0.0160(11) 0.0001(10) O2' 0.0806(14) 0.0686(14) 0.0518(11) -0.0127(9) 0.0004(10) -0.0093(11) N1' 0.0808(19) 0.0518(15) 0.0789(17) 0.0053(13) -0.0120(14) -0.0023(13) N2' 0.0797(18) 0.0450(14) 0.0642(15) -0.0032(11) 0.0150(13) -0.0018(13) N3' 0.090(2) 0.072(2) 0.111(2) -0.0044(17) 0.0260(18) -0.0224(17) C1' 0.0436(13) 0.0449(14) 0.0440(12) 0.0021(10) 0.0071(10) -0.0054(10) C2' 0.0547(15) 0.0558(16) 0.0408(12) 0.0045(11) -0.0016(11) -0.0034(12) C3' 0.0760(19) 0.0567(18) 0.0415(13) -0.0064(12) 0.0084(12) -0.0052(14) C4' 0.0584(17) 0.0599(18) 0.0631(17) -0.0047(14) 0.0230(14) 0.0007(14) C5' 0.0437(13) 0.0536(16) 0.0578(15) 0.0009(12) 0.0081(11) -0.0071(11) C6' 0.0571(18) 0.098(3) 0.091(2) 0.043(2) 0.0158(17) -0.0100(18) C7' 0.147(4) 0.060(2) 0.0580(18) 0.0110(15) 0.052(2) 0.013(2) C8' 0.092(2) 0.074(2) 0.0476(15) 0.0104(15) -0.0122(15) -0.0131(18) C9' 0.077(2) 0.0569(18) 0.0694(19) 0.0137(15) -0.0035(15) 0.0084(15) C10' 0.088(2) 0.0547(19) 0.075(2) 0.0120(15) -0.0015(18) -0.0192(17) _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 C1 2.005(2) . ? Fe1 C6 2.020(3) . ? Fe1 C10 2.021(3) . ? Fe1 C7 2.024(3) . ? Fe1 C9 2.029(3) . ? Fe1 C8 2.038(3) . ? Fe1 C2 2.039(2) . ? Fe1 C5 2.040(2) . ? Fe1 C4 2.058(2) . ? Fe1 C3 2.066(2) . ? S1 O1 1.4162(19) . ? S1 O2 1.4238(18) . ? S1 C1 1.712(2) . ? S1 N1 1.724(2) . ? N1 N2 1.218(3) . ? N2 N3 1.128(4) . ? C1 C2 1.425(3) . ? C1 C5 1.435(3) . ? C2 C3 1.401(4) . ? C3 C4 1.410(4) . ? C4 C5 1.413(4) . ? C6 C10 1.405(5) . ? C6 C7 1.423(6) . ? C7 C8 1.367(5) . ? C8 C9 1.332(5) . ? C9 C10 1.356(5) . ? Fe1' C1' 1.997(2) . ? Fe1' C6' 2.023(3) . ? Fe1' C7' 2.029(3) . ? Fe1' C2' 2.032(2) . ? Fe1' C5' 2.036(3) . ? Fe1' C10' 2.037(3) . ? Fe1' C9' 2.040(3) . ? Fe1' C8' 2.040(3) . ? Fe1' C3' 2.054(3) . ? Fe1' C4' 2.058(3) . ? S1' O2' 1.415(2) . ? S1' O1' 1.419(2) . ? S1' N1' 1.713(3) . ? S1' C1' 1.718(3) . ? N1' N2' 1.236(4) . ? N2' N3' 1.121(4) . ? C1' C5' 1.425(3) . ? C1' C2' 1.431(3) . ? C2' C3' 1.407(4) . ? C3' C4' 1.416(4) . ? C4' C5' 1.428(4) . ? C6' C10' 1.393(5) . ? C6' C7' 1.428(5) . ? C7' C8' 1.413(5) . ? C8' C9' 1.381(5) . ? C9' C10' 1.373(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 C1 Fe1 C6 122.82(14) . . ? C1 Fe1 C10 156.77(15) . . ? C6 Fe1 C10 40.68(16) . . ? C1 Fe1 C7 111.51(12) . . ? C6 Fe1 C7 41.22(17) . . ? C10 Fe1 C7 67.65(14) . . ? C1 Fe1 C9 163.58(15) . . ? C6 Fe1 C9 66.94(15) . . ? C10 Fe1 C9 39.10(16) . . ? C7 Fe1 C9 65.95(15) . . ? C1 Fe1 C8 129.52(14) . . ? C6 Fe1 C8 67.11(14) . . ? C10 Fe1 C8 65.61(14) . . ? C7 Fe1 C8 39.33(15) . . ? C9 Fe1 C8 38.22(15) . . ? C1 Fe1 C2 41.27(9) . . ? C6 Fe1 C2 109.12(12) . . ? C10 Fe1 C2 120.12(13) . . ? C7 Fe1 C2 129.93(15) . . ? C9 Fe1 C2 152.98(15) . . ? C8 Fe1 C2 167.34(15) . . ? C1 Fe1 C5 41.55(10) . . ? C6 Fe1 C5 157.81(17) . . ? C10 Fe1 C5 159.65(16) . . ? C7 Fe1 C5 121.72(14) . . ? C9 Fe1 C5 124.53(13) . . ? C8 Fe1 C5 109.00(12) . . ? C2 Fe1 C5 69.61(10) . . ? C1 Fe1 C4 68.05(10) . . ? C6 Fe1 C4 161.23(18) . . ? C10 Fe1 C4 123.39(15) . . ? C7 Fe1 C4 154.36(16) . . ? C9 Fe1 C4 106.80(13) . . ? C8 Fe1 C4 119.77(13) . . ? C2 Fe1 C4 67.86(11) . . ? C5 Fe1 C4 40.33(10) . . ? C1 Fe1 C3 67.82(10) . . ? C6 Fe1 C3 125.93(15) . . ? C10 Fe1 C3 106.90(12) . . ? C7 Fe1 C3 165.46(16) . . ? C9 Fe1 C3 118.99(14) . . ? C8 Fe1 C3 152.23(15) . . ? C2 Fe1 C3 39.91(10) . . ? C5 Fe1 C3 68.15(10) . . ? C4 Fe1 C3 39.97(11) . . ? O1 S1 O2 121.09(12) . . ? O1 S1 C1 109.92(12) . . ? O2 S1 C1 110.51(11) . . ? O1 S1 N1 102.74(12) . . ? O2 S1 N1 107.96(12) . . ? C1 S1 N1 102.74(12) . . ? N2 N1 S1 112.99(18) . . ? N3 N2 N1 173.7(3) . . ? C2 C1 C5 109.0(2) . . ? C2 C1 S1 125.50(18) . . ? C5 C1 S1 125.50(19) . . ? C2 C1 Fe1 70.65(14) . . ? C5 C1 Fe1 70.55(14) . . ? S1 C1 Fe1 126.49(12) . . ? C3 C2 C1 107.0(2) . . ? C3 C2 Fe1 71.08(14) . . ? C1 C2 Fe1 68.09(13) . . ? C2 C3 C4 108.9(2) . . ? C2 C3 Fe1 69.01(13) . . ? C4 C3 Fe1 69.71(14) . . ? C3 C4 C5 109.2(2) . . ? C3 C4 Fe1 70.32(15) . . ? C5 C4 Fe1 69.17(13) . . ? C4 C5 C1 106.0(2) . . ? C4 C5 Fe1 70.50(15) . . ? C1 C5 Fe1 67.90(13) . . ? C10 C6 C7 105.5(3) . . ? C10 C6 Fe1 69.72(18) . . ? C7 C6 Fe1 69.54(18) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 Fe1 70.92(18) . . ? C6 C7 Fe1 69.24(18) . . ? C9 C8 C7 109.6(3) . . ? C9 C8 Fe1 70.52(18) . . ? C7 C8 Fe1 69.75(18) . . ? C8 C9 C10 109.9(3) . . ? C8 C9 Fe1 71.3(2) . . ? C10 C9 Fe1 70.12(19) . . ? C9 C10 C6 108.0(3) . . ? C9 C10 Fe1 70.77(19) . . ? C6 C10 Fe1 69.60(19) . . ? C1' Fe1' C6' 124.13(13) . . ? C1' Fe1' C7' 109.27(12) . . ? C6' Fe1' C7' 41.26(16) . . ? C1' Fe1' C2' 41.59(10) . . ? C6' Fe1' C2' 107.57(13) . . ? C7' Fe1' C2' 124.81(14) . . ? C1' Fe1' C5' 41.36(10) . . ? C6' Fe1' C5' 160.82(15) . . ? C7' Fe1' C5' 123.75(15) . . ? C2' Fe1' C5' 69.71(11) . . ? C1' Fe1' C10' 159.26(12) . . ? C6' Fe1' C10' 40.12(14) . . ? C7' Fe1' C10' 67.98(15) . . ? C2' Fe1' C10' 121.76(12) . . ? C5' Fe1' C10' 157.57(14) . . ? C1' Fe1' C9' 160.42(12) . . ? C6' Fe1' C9' 67.16(14) . . ? C7' Fe1' C9' 67.50(14) . . ? C2' Fe1' C9' 156.38(12) . . ? C5' Fe1' C9' 122.98(12) . . ? C10' Fe1' C9' 39.37(12) . . ? C1' Fe1' C8' 125.39(12) . . ? C6' Fe1' C8' 68.14(14) . . ? C7' Fe1' C8' 40.63(15) . . ? C2' Fe1' C8' 162.22(13) . . ? C5' Fe1' C8' 108.33(12) . . ? C10' Fe1' C8' 66.87(13) . . ? C9' Fe1' C8' 39.56(13) . . ? C1' Fe1' C3' 68.73(11) . . ? C6' Fe1' C3' 121.94(14) . . ? C7' Fe1' C3' 159.73(17) . . ? C2' Fe1' C3' 40.27(11) . . ? C5' Fe1' C3' 68.99(11) . . ? C10' Fe1' C3' 106.35(13) . . ? C9' Fe1' C3' 121.28(12) . . ? C8' Fe1' C3' 156.87(14) . . ? C1' Fe1' C4' 68.44(11) . . ? C6' Fe1' C4' 157.21(16) . . ? C7' Fe1' C4' 159.35(17) . . ? C2' Fe1' C4' 68.04(12) . . ? C5' Fe1' C4' 40.82(11) . . ? C10' Fe1' C4' 121.66(14) . . ? C9' Fe1' C4' 107.38(13) . . ? C8' Fe1' C4' 122.74(14) . . ? C3' Fe1' C4' 40.29(12) . . ? O2' S1' O1' 120.70(14) . . ? O2' S1' N1' 108.06(13) . . ? O1' S1' N1' 103.65(15) . . ? O2' S1' C1' 110.50(12) . . ? O1' S1' C1' 109.52(13) . . ? N1' S1' C1' 102.68(13) . . ? N2' N1' S1' 111.4(2) . . ? N3' N2' N1' 173.1(4) . . ? C5' C1' C2' 109.0(2) . . ? C5' C1' S1' 125.86(19) . . ? C2' C1' S1' 125.2(2) . . ? C5' C1' Fe1' 70.75(15) . . ? C2' C1' Fe1' 70.49(15) . . ? S1' C1' Fe1' 124.41(13) . . ? C3' C2' C1' 107.5(2) . . ? C3' C2' Fe1' 70.73(15) . . ? C1' C2' Fe1' 67.92(14) . . ? C2' C3' C4' 108.3(2) . . ? C2' C3' Fe1' 69.01(14) . . ? C4' C3' Fe1' 69.98(15) . . ? C3' C4' C5' 109.1(2) . . ? C3' C4' Fe1' 69.72(15) . . ? C5' C4' Fe1' 68.75(15) . . ? C1' C5' C4' 106.2(2) . . ? C1' C5' Fe1' 67.89(14) . . ? C4' C5' Fe1' 70.42(16) . . ? C10' C6' C7' 107.4(3) . . ? C10' C6' Fe1' 70.48(18) . . ? C7' C6' Fe1' 69.57(18) . . ? C8' C7' C6' 106.6(3) . . ? C8' C7' Fe1' 70.13(18) . . ? C6' C7' Fe1' 69.17(18) . . ? C9' C8' C7' 108.0(3) . . ? C9' C8' Fe1' 70.21(17) . . ? C7' C8' Fe1' 69.24(17) . . ? C10' C9' C8' 109.3(3) . . ? C10' C9' Fe1' 70.20(18) . . ? C8' C9' Fe1' 70.23(18) . . ? C9' C10' C6' 108.7(3) . . ? C9' C10' Fe1' 70.44(18) . . ? C6' C10' Fe1' 69.41(19) . . ? 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 O1 S1 N1 N2 -157.7(2) . . . . ? O2 S1 N1 N2 -28.7(2) . . . . ? C1 S1 N1 N2 88.1(2) . . . . ? S1 N1 N2 N3 178(100) . . . . ? O1 S1 C1 C2 -22.4(2) . . . . ? O2 S1 C1 C2 -158.6(2) . . . . ? N1 S1 C1 C2 86.4(2) . . . . ? O1 S1 C1 C5 159.9(2) . . . . ? O2 S1 C1 C5 23.7(2) . . . . ? N1 S1 C1 C5 -91.3(2) . . . . ? O1 S1 C1 Fe1 68.81(18) . . . . ? O2 S1 C1 Fe1 -67.41(18) . . . . ? N1 S1 C1 Fe1 177.62(14) . . . . ? C6 Fe1 C1 C2 81.7(2) . . . . ? C10 Fe1 C1 C2 43.5(4) . . . . ? C7 Fe1 C1 C2 126.66(19) . . . . ? C9 Fe1 C1 C2 -155.6(4) . . . . ? C8 Fe1 C1 C2 167.83(18) . . . . ? C5 Fe1 C1 C2 -119.3(2) . . . . ? C4 Fe1 C1 C2 -80.98(16) . . . . ? C3 Fe1 C1 C2 -37.69(15) . . . . ? C6 Fe1 C1 C5 -159.0(2) . . . . ? C10 Fe1 C1 C5 162.8(3) . . . . ? C7 Fe1 C1 C5 -114.0(2) . . . . ? C9 Fe1 C1 C5 -36.3(5) . . . . ? C8 Fe1 C1 C5 -72.9(2) . . . . ? C2 Fe1 C1 C5 119.3(2) . . . . ? C4 Fe1 C1 C5 38.32(15) . . . . ? C3 Fe1 C1 C5 81.61(15) . . . . ? C6 Fe1 C1 S1 -38.7(2) . . . . ? C10 Fe1 C1 S1 -76.9(3) . . . . ? C7 Fe1 C1 S1 6.3(2) . . . . ? C9 Fe1 C1 S1 84.0(5) . . . . ? C8 Fe1 C1 S1 47.4(2) . . . . ? C2 Fe1 C1 S1 -120.4(2) . . . . ? C5 Fe1 C1 S1 120.3(2) . . . . ? C4 Fe1 C1 S1 158.64(19) . . . . ? C3 Fe1 C1 S1 -158.08(19) . . . . ? C5 C1 C2 C3 0.4(3) . . . . ? S1 C1 C2 C3 -177.64(18) . . . . ? Fe1 C1 C2 C3 60.78(17) . . . . ? C5 C1 C2 Fe1 -60.40(16) . . . . ? S1 C1 C2 Fe1 121.58(19) . . . . ? C1 Fe1 C2 C3 -118.1(2) . . . . ? C6 Fe1 C2 C3 123.6(2) . . . . ? C10 Fe1 C2 C3 80.2(2) . . . . ? C7 Fe1 C2 C3 165.2(2) . . . . ? C9 Fe1 C2 C3 47.1(3) . . . . ? C8 Fe1 C2 C3 -165.9(5) . . . . ? C5 Fe1 C2 C3 -79.96(17) . . . . ? C4 Fe1 C2 C3 -36.58(17) . . . . ? C6 Fe1 C2 C1 -118.3(2) . . . . ? C10 Fe1 C2 C1 -161.72(18) . . . . ? C7 Fe1 C2 C1 -76.8(2) . . . . ? C9 Fe1 C2 C1 165.1(3) . . . . ? C8 Fe1 C2 C1 -47.9(6) . . . . ? C5 Fe1 C2 C1 38.10(14) . . . . ? C4 Fe1 C2 C1 81.48(15) . . . . ? C3 Fe1 C2 C1 118.1(2) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? Fe1 C2 C3 C4 58.40(19) . . . . ? C1 C2 C3 Fe1 -58.86(16) . . . . ? C1 Fe1 C3 C2 38.94(15) . . . . ? C6 Fe1 C3 C2 -76.4(2) . . . . ? C10 Fe1 C3 C2 -117.0(2) . . . . ? C7 Fe1 C3 C2 -51.4(5) . . . . ? C9 Fe1 C3 C2 -157.65(19) . . . . ? C8 Fe1 C3 C2 173.4(3) . . . . ? C5 Fe1 C3 C2 83.93(17) . . . . ? C4 Fe1 C3 C2 120.8(2) . . . . ? C1 Fe1 C3 C4 -81.83(17) . . . . ? C6 Fe1 C3 C4 162.9(2) . . . . ? C10 Fe1 C3 C4 122.2(2) . . . . ? C7 Fe1 C3 C4 -172.1(5) . . . . ? C9 Fe1 C3 C4 81.6(2) . . . . ? C8 Fe1 C3 C4 52.7(3) . . . . ? C2 Fe1 C3 C4 -120.8(2) . . . . ? C5 Fe1 C3 C4 -36.85(16) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? Fe1 C3 C4 C5 58.36(18) . . . . ? C2 C3 C4 Fe1 -57.98(18) . . . . ? C1 Fe1 C4 C3 81.21(16) . . . . ? C6 Fe1 C4 C3 -47.9(4) . . . . ? C10 Fe1 C4 C3 -75.9(2) . . . . ? C7 Fe1 C4 C3 175.4(3) . . . . ? C9 Fe1 C4 C3 -115.3(2) . . . . ? C8 Fe1 C4 C3 -154.7(2) . . . . ? C2 Fe1 C4 C3 36.52(16) . . . . ? C5 Fe1 C4 C3 120.7(2) . . . . ? C1 Fe1 C4 C5 -39.46(15) . . . . ? C6 Fe1 C4 C5 -168.5(3) . . . . ? C10 Fe1 C4 C5 163.48(18) . . . . ? C7 Fe1 C4 C5 54.8(3) . . . . ? C9 Fe1 C4 C5 123.99(19) . . . . ? C8 Fe1 C4 C5 84.6(2) . . . . ? C2 Fe1 C4 C5 -84.15(16) . . . . ? C3 Fe1 C4 C5 -120.7(2) . . . . ? C3 C4 C5 C1 -0.1(3) . . . . ? Fe1 C4 C5 C1 58.91(16) . . . . ? C3 C4 C5 Fe1 -59.05(19) . . . . ? C2 C1 C5 C4 -0.1(3) . . . . ? S1 C1 C5 C4 177.87(18) . . . . ? Fe1 C1 C5 C4 -60.61(17) . . . . ? C2 C1 C5 Fe1 60.46(16) . . . . ? S1 C1 C5 Fe1 -121.52(18) . . . . ? C1 Fe1 C5 C4 117.3(2) . . . . ? C6 Fe1 C5 C4 170.2(3) . . . . ? C10 Fe1 C5 C4 -43.1(4) . . . . ? C7 Fe1 C5 C4 -155.4(2) . . . . ? C9 Fe1 C5 C4 -74.4(2) . . . . ? C8 Fe1 C5 C4 -113.94(19) . . . . ? C2 Fe1 C5 C4 79.43(16) . . . . ? C3 Fe1 C5 C4 36.54(16) . . . . ? C6 Fe1 C5 C1 53.0(4) . . . . ? C10 Fe1 C5 C1 -160.3(3) . . . . ? C7 Fe1 C5 C1 87.3(2) . . . . ? C9 Fe1 C5 C1 168.27(18) . . . . ? C8 Fe1 C5 C1 128.77(18) . . . . ? C2 Fe1 C5 C1 -37.86(14) . . . . ? C4 Fe1 C5 C1 -117.3(2) . . . . ? C3 Fe1 C5 C1 -80.75(15) . . . . ? C1 Fe1 C6 C10 -157.99(19) . . . . ? C7 Fe1 C6 C10 116.3(3) . . . . ? C9 Fe1 C6 C10 37.0(2) . . . . ? C8 Fe1 C6 C10 78.7(2) . . . . ? C2 Fe1 C6 C10 -114.3(2) . . . . ? C5 Fe1 C6 C10 163.0(3) . . . . ? C4 Fe1 C6 C10 -37.0(5) . . . . ? C3 Fe1 C6 C10 -73.0(2) . . . . ? C1 Fe1 C6 C7 85.7(2) . . . . ? C10 Fe1 C6 C7 -116.3(3) . . . . ? C9 Fe1 C6 C7 -79.3(2) . . . . ? C8 Fe1 C6 C7 -37.6(2) . . . . ? C2 Fe1 C6 C7 129.4(2) . . . . ? C5 Fe1 C6 C7 46.7(4) . . . . ? C4 Fe1 C6 C7 -153.2(4) . . . . ? C3 Fe1 C6 C7 170.7(2) . . . . ? C10 C6 C7 C8 0.4(4) . . . . ? Fe1 C6 C7 C8 61.2(2) . . . . ? C10 C6 C7 Fe1 -60.8(2) . . . . ? C1 Fe1 C7 C8 126.8(2) . . . . ? C6 Fe1 C7 C8 -117.5(3) . . . . ? C10 Fe1 C7 C8 -78.3(3) . . . . ? C9 Fe1 C7 C8 -35.6(2) . . . . ? C2 Fe1 C7 C8 170.4(2) . . . . ? C5 Fe1 C7 C8 81.3(2) . . . . ? C4 Fe1 C7 C8 42.9(4) . . . . ? C3 Fe1 C7 C8 -148.8(5) . . . . ? C1 Fe1 C7 C6 -115.7(2) . . . . ? C10 Fe1 C7 C6 39.2(2) . . . . ? C9 Fe1 C7 C6 81.9(2) . . . . ? C8 Fe1 C7 C6 117.5(3) . . . . ? C2 Fe1 C7 C6 -72.1(3) . . . . ? C5 Fe1 C7 C6 -161.1(2) . . . . ? C4 Fe1 C7 C6 160.4(3) . . . . ? C3 Fe1 C7 C6 -31.3(6) . . . . ? C6 C7 C8 C9 -0.7(4) . . . . ? Fe1 C7 C8 C9 59.4(2) . . . . ? C6 C7 C8 Fe1 -60.1(2) . . . . ? C1 Fe1 C8 C9 164.2(2) . . . . ? C6 Fe1 C8 C9 -81.3(3) . . . . ? C10 Fe1 C8 C9 -36.7(2) . . . . ? C7 Fe1 C8 C9 -120.7(3) . . . . ? C2 Fe1 C8 C9 -156.4(5) . . . . ? C5 Fe1 C8 C9 122.1(2) . . . . ? C4 Fe1 C8 C9 79.2(2) . . . . ? C3 Fe1 C8 C9 43.1(4) . . . . ? C1 Fe1 C8 C7 -75.1(3) . . . . ? C6 Fe1 C8 C7 39.4(2) . . . . ? C10 Fe1 C8 C7 83.9(3) . . . . ? C9 Fe1 C8 C7 120.7(3) . . . . ? C2 Fe1 C8 C7 -35.7(7) . . . . ? C5 Fe1 C8 C7 -117.2(2) . . . . ? C4 Fe1 C8 C7 -160.2(2) . . . . ? C3 Fe1 C8 C7 163.8(3) . . . . ? C7 C8 C9 C10 0.8(4) . . . . ? Fe1 C8 C9 C10 59.7(2) . . . . ? C7 C8 C9 Fe1 -58.9(2) . . . . ? C1 Fe1 C9 C8 -47.9(5) . . . . ? C6 Fe1 C9 C8 81.8(3) . . . . ? C10 Fe1 C9 C8 120.3(3) . . . . ? C7 Fe1 C9 C8 36.6(2) . . . . ? C2 Fe1 C9 C8 168.9(2) . . . . ? C5 Fe1 C9 C8 -76.4(2) . . . . ? C4 Fe1 C9 C8 -117.1(2) . . . . ? C3 Fe1 C9 C8 -158.6(2) . . . . ? C1 Fe1 C9 C10 -168.2(4) . . . . ? C6 Fe1 C9 C10 -38.5(2) . . . . ? C7 Fe1 C9 C10 -83.6(3) . . . . ? C8 Fe1 C9 C10 -120.3(3) . . . . ? C2 Fe1 C9 C10 48.6(4) . . . . ? C5 Fe1 C9 C10 163.3(2) . . . . ? C4 Fe1 C9 C10 122.7(2) . . . . ? C3 Fe1 C9 C10 81.1(2) . . . . ? C8 C9 C10 C6 -0.5(4) . . . . ? Fe1 C9 C10 C6 59.9(2) . . . . ? C8 C9 C10 Fe1 -60.4(3) . . . . ? C7 C6 C10 C9 0.0(4) . . . . ? Fe1 C6 C10 C9 -60.7(2) . . . . ? C7 C6 C10 Fe1 60.7(2) . . . . ? C1 Fe1 C10 C9 171.6(3) . . . . ? C6 Fe1 C10 C9 118.6(3) . . . . ? C7 Fe1 C10 C9 78.9(3) . . . . ? C8 Fe1 C10 C9 35.9(2) . . . . ? C2 Fe1 C10 C9 -156.8(2) . . . . ? C5 Fe1 C10 C9 -42.9(4) . . . . ? C4 Fe1 C10 C9 -74.8(2) . . . . ? C3 Fe1 C10 C9 -115.4(2) . . . . ? C1 Fe1 C10 C6 53.0(4) . . . . ? C7 Fe1 C10 C6 -39.7(2) . . . . ? C9 Fe1 C10 C6 -118.6(3) . . . . ? C8 Fe1 C10 C6 -82.7(2) . . . . ? C2 Fe1 C10 C6 84.6(2) . . . . ? C5 Fe1 C10 C6 -161.5(3) . . . . ? C4 Fe1 C10 C6 166.6(2) . . . . ? C3 Fe1 C10 C6 126.0(2) . . . . ? O2' S1' N1' N2' -23.9(3) . . . . ? O1' S1' N1' N2' -153.1(2) . . . . ? C1' S1' N1' N2' 92.9(2) . . . . ? S1' N1' N2' N3' 179(100) . . . . ? O2' S1' C1' C5' 27.5(3) . . . . ? O1' S1' C1' C5' 162.8(2) . . . . ? N1' S1' C1' C5' -87.6(2) . . . . ? O2' S1' C1' C2' -151.9(2) . . . . ? O1' S1' C1' C2' -16.6(3) . . . . ? N1' S1' C1' C2' 93.0(2) . . . . ? O2' S1' C1' Fe1' -62.64(18) . . . . ? O1' S1' C1' Fe1' 72.65(19) . . . . ? N1' S1' C1' Fe1' -177.69(15) . . . . ? C6' Fe1' C1' C5' -163.10(19) . . . . ? C7' Fe1' C1' C5' -119.6(2) . . . . ? C2' Fe1' C1' C5' 119.3(2) . . . . ? C10' Fe1' C1' C5' 161.9(3) . . . . ? C9' Fe1' C1' C5' -42.7(4) . . . . ? C8' Fe1' C1' C5' -77.1(2) . . . . ? C3' Fe1' C1' C5' 81.94(16) . . . . ? C4' Fe1' C1' C5' 38.51(15) . . . . ? C6' Fe1' C1' C2' 77.6(2) . . . . ? C7' Fe1' C1' C2' 121.1(2) . . . . ? C5' Fe1' C1' C2' -119.3(2) . . . . ? C10' Fe1' C1' C2' 42.6(4) . . . . ? C9' Fe1' C1' C2' -162.0(3) . . . . ? C8' Fe1' C1' C2' 163.59(18) . . . . ? C3' Fe1' C1' C2' -37.34(16) . . . . ? C4' Fe1' C1' C2' -80.77(17) . . . . ? C6' Fe1' C1' S1' -42.2(2) . . . . ? C7' Fe1' C1' S1' 1.3(2) . . . . ? C2' Fe1' C1' S1' -119.9(2) . . . . ? C5' Fe1' C1' S1' 120.9(2) . . . . ? C10' Fe1' C1' S1' -77.3(4) . . . . ? C9' Fe1' C1' S1' 78.2(4) . . . . ? C8' Fe1' C1' S1' 43.7(2) . . . . ? C3' Fe1' C1' S1' -157.20(19) . . . . ? C4' Fe1' C1' S1' 159.38(19) . . . . ? C5' C1' C2' C3' -0.6(3) . . . . ? S1' C1' C2' C3' 178.86(19) . . . . ? Fe1' C1' C2' C3' 59.93(18) . . . . ? C5' C1' C2' Fe1' -60.55(18) . . . . ? S1' C1' C2' Fe1' 118.93(19) . . . . ? C1' Fe1' C2' C3' -119.0(2) . . . . ? C6' Fe1' C2' C3' 119.0(2) . . . . ? C7' Fe1' C2' C3' 161.2(2) . . . . ? C5' Fe1' C2' C3' -81.09(18) . . . . ? C10' Fe1' C2' C3' 77.4(2) . . . . ? C9' Fe1' C2' C3' 46.0(4) . . . . ? C8' Fe1' C2' C3' -167.9(4) . . . . ? C4' Fe1' C2' C3' -37.21(17) . . . . ? C6' Fe1' C2' C1' -122.00(19) . . . . ? C7' Fe1' C2' C1' -79.8(2) . . . . ? C5' Fe1' C2' C1' 37.92(15) . . . . ? C10' Fe1' C2' C1' -163.63(16) . . . . ? C9' Fe1' C2' C1' 165.0(3) . . . . ? C8' Fe1' C2' C1' -48.9(5) . . . . ? C3' Fe1' C2' C1' 119.0(2) . . . . ? C4' Fe1' C2' C1' 81.79(16) . . . . ? C1' C2' C3' C4' 1.0(3) . . . . ? Fe1' C2' C3' C4' 59.13(19) . . . . ? C1' C2' C3' Fe1' -58.17(17) . . . . ? C1' Fe1' C3' C2' 38.53(16) . . . . ? C6' Fe1' C3' C2' -79.3(2) . . . . ? C7' Fe1' C3' C2' -49.7(4) . . . . ? C5' Fe1' C3' C2' 83.03(17) . . . . ? C10' Fe1' C3' C2' -120.16(18) . . . . ? C9' Fe1' C3' C2' -160.29(17) . . . . ? C8' Fe1' C3' C2' 170.7(3) . . . . ? C4' Fe1' C3' C2' 119.9(2) . . . . ? C1' Fe1' C3' C4' -81.33(18) . . . . ? C6' Fe1' C3' C4' 160.8(2) . . . . ? C7' Fe1' C3' C4' -169.5(3) . . . . ? C2' Fe1' C3' C4' -119.9(2) . . . . ? C5' Fe1' C3' C4' -36.83(17) . . . . ? C10' Fe1' C3' C4' 119.98(19) . . . . ? C9' Fe1' C3' C4' 79.8(2) . . . . ? C8' Fe1' C3' C4' 50.8(4) . . . . ? C2' C3' C4' C5' -1.0(3) . . . . ? Fe1' C3' C4' C5' 57.56(19) . . . . ? C2' C3' C4' Fe1' -58.53(18) . . . . ? C1' Fe1' C4' C3' 82.13(18) . . . . ? C6' Fe1' C4' C3' -46.0(4) . . . . ? C7' Fe1' C4' C3' 169.7(3) . . . . ? C2' Fe1' C4' C3' 37.19(17) . . . . ? C5' Fe1' C4' C3' 121.1(2) . . . . ? C10' Fe1' C4' C3' -77.5(2) . . . . ? C9' Fe1' C4' C3' -118.18(18) . . . . ? C8' Fe1' C4' C3' -158.78(18) . . . . ? C1' Fe1' C4' C5' -39.01(16) . . . . ? C6' Fe1' C4' C5' -167.1(3) . . . . ? C7' Fe1' C4' C5' 48.6(4) . . . . ? C2' Fe1' C4' C5' -83.95(17) . . . . ? C10' Fe1' C4' C5' 161.33(17) . . . . ? C9' Fe1' C4' C5' 120.68(18) . . . . ? C8' Fe1' C4' C5' 80.1(2) . . . . ? C3' Fe1' C4' C5' -121.1(2) . . . . ? C2' C1' C5' C4' 0.0(3) . . . . ? S1' C1' C5' C4' -179.4(2) . . . . ? Fe1' C1' C5' C4' -60.36(18) . . . . ? C2' C1' C5' Fe1' 60.39(17) . . . . ? S1' C1' C5' Fe1' -119.1(2) . . . . ? C3' C4' C5' C1' 0.6(3) . . . . ? Fe1' C4' C5' C1' 58.71(17) . . . . ? C3' C4' C5' Fe1' -58.1(2) . . . . ? C6' Fe1' C5' C1' 47.1(4) . . . . ? C7' Fe1' C5' C1' 80.9(2) . . . . ? C2' Fe1' C5' C1' -38.11(14) . . . . ? C10' Fe1' C5' C1' -163.2(3) . . . . ? C9' Fe1' C5' C1' 164.28(16) . . . . ? C8' Fe1' C5' C1' 123.15(17) . . . . ? C3' Fe1' C5' C1' -81.27(16) . . . . ? C4' Fe1' C5' C1' -117.6(2) . . . . ? C1' Fe1' C5' C4' 117.6(2) . . . . ? C6' Fe1' C5' C4' 164.7(4) . . . . ? C7' Fe1' C5' C4' -161.5(2) . . . . ? C2' Fe1' C5' C4' 79.53(18) . . . . ? C10' Fe1' C5' C4' -45.6(4) . . . . ? C9' Fe1' C5' C4' -78.1(2) . . . . ? C8' Fe1' C5' C4' -119.2(2) . . . . ? C3' Fe1' C5' C4' 36.37(17) . . . . ? C1' Fe1' C6' C10' -161.61(18) . . . . ? C7' Fe1' C6' C10' 118.1(3) . . . . ? C2' Fe1' C6' C10' -118.8(2) . . . . ? C5' Fe1' C6' C10' 162.6(3) . . . . ? C9' Fe1' C6' C10' 36.68(19) . . . . ? C8' Fe1' C6' C10' 79.6(2) . . . . ? C3' Fe1' C6' C10' -77.0(2) . . . . ? C4' Fe1' C6' C10' -43.8(4) . . . . ? C1' Fe1' C6' C7' 80.3(2) . . . . ? C2' Fe1' C6' C7' 123.2(2) . . . . ? C5' Fe1' C6' C7' 44.5(5) . . . . ? C10' Fe1' C6' C7' -118.1(3) . . . . ? C9' Fe1' C6' C7' -81.4(2) . . . . ? C8' Fe1' C6' C7' -38.5(2) . . . . ? C3' Fe1' C6' C7' 164.9(2) . . . . ? C4' Fe1' C6' C7' -161.8(3) . . . . ? C10' C6' C7' C8' -0.1(3) . . . . ? Fe1' C6' C7' C8' 60.5(2) . . . . ? C10' C6' C7' Fe1' -60.6(2) . . . . ? C1' Fe1' C7' C8' 122.3(2) . . . . ? C6' Fe1' C7' C8' -117.5(3) . . . . ? C2' Fe1' C7' C8' 166.10(19) . . . . ? C5' Fe1' C7' C8' 78.6(2) . . . . ? C10' Fe1' C7' C8' -79.7(2) . . . . ? C9' Fe1' C7' C8' -37.0(2) . . . . ? C3' Fe1' C7' C8' -157.0(3) . . . . ? C4' Fe1' C7' C8' 42.5(5) . . . . ? C1' Fe1' C7' C6' -120.2(2) . . . . ? C2' Fe1' C7' C6' -76.4(2) . . . . ? C5' Fe1' C7' C6' -163.9(2) . . . . ? C10' Fe1' C7' C6' 37.8(2) . . . . ? C9' Fe1' C7' C6' 80.5(2) . . . . ? C8' Fe1' C7' C6' 117.5(3) . . . . ? C3' Fe1' C7' C6' -39.5(5) . . . . ? C4' Fe1' C7' C6' 160.0(3) . . . . ? C6' C7' C8' C9' -0.1(4) . . . . ? Fe1' C7' C8' C9' 59.7(2) . . . . ? C6' C7' C8' Fe1' -59.9(2) . . . . ? C1' Fe1' C8' C9' 162.69(18) . . . . ? C6' Fe1' C8' C9' -80.1(2) . . . . ? C7' Fe1' C8' C9' -119.2(3) . . . . ? C2' Fe1' C8' C9' -159.4(3) . . . . ? C5' Fe1' C8' C9' 120.0(2) . . . . ? C10' Fe1' C8' C9' -36.6(2) . . . . ? C3' Fe1' C8' C9' 40.7(4) . . . . ? C4' Fe1' C8' C9' 77.2(2) . . . . ? C1' Fe1' C8' C7' -78.1(2) . . . . ? C6' Fe1' C8' C7' 39.1(2) . . . . ? C2' Fe1' C8' C7' -40.2(5) . . . . ? C5' Fe1' C8' C7' -120.8(2) . . . . ? C10' Fe1' C8' C7' 82.6(2) . . . . ? C9' Fe1' C8' C7' 119.2(3) . . . . ? C3' Fe1' C8' C7' 159.9(3) . . . . ? C4' Fe1' C8' C7' -163.6(2) . . . . ? C7' C8' C9' C10' 0.4(4) . . . . ? Fe1' C8' C9' C10' 59.5(2) . . . . ? C7' C8' C9' Fe1' -59.1(2) . . . . ? C1' Fe1' C9' C10' -166.6(3) . . . . ? C6' Fe1' C9' C10' -37.4(2) . . . . ? C7' Fe1' C9' C10' -82.2(2) . . . . ? C2' Fe1' C9' C10' 44.3(4) . . . . ? C5' Fe1' C9' C10' 161.1(2) . . . . ? C8' Fe1' C9' C10' -120.2(3) . . . . ? C3' Fe1' C9' C10' 77.2(2) . . . . ? C4' Fe1' C9' C10' 119.1(2) . . . . ? C1' Fe1' C9' C8' -46.4(4) . . . . ? C6' Fe1' C9' C8' 82.9(2) . . . . ? C7' Fe1' C9' C8' 38.0(2) . . . . ? C2' Fe1' C9' C8' 164.5(3) . . . . ? C5' Fe1' C9' C8' -78.7(2) . . . . ? C10' Fe1' C9' C8' 120.2(3) . . . . ? C3' Fe1' C9' C8' -162.6(2) . . . . ? C4' Fe1' C9' C8' -120.7(2) . . . . ? C8' C9' C10' C6' -0.5(4) . . . . ? Fe1' C9' C10' C6' 59.1(2) . . . . ? C8' C9' C10' Fe1' -59.5(2) . . . . ? C7' C6' C10' C9' 0.4(4) . . . . ? Fe1' C6' C10' C9' -59.7(2) . . . . ? C7' C6' C10' Fe1' 60.1(2) . . . . ? C1' Fe1' C10' C9' 167.3(3) . . . . ? C6' Fe1' C10' C9' 119.8(3) . . . . ? C7' Fe1' C10' C9' 80.9(2) . . . . ? C2' Fe1' C10' C9' -160.80(18) . . . . ? C5' Fe1' C10' C9' -45.3(4) . . . . ? C8' Fe1' C10' C9' 36.8(2) . . . . ? C3' Fe1' C10' C9' -119.7(2) . . . . ? C4' Fe1' C10' C9' -78.6(2) . . . . ? C1' Fe1' C10' C6' 47.5(4) . . . . ? C7' Fe1' C10' C6' -38.9(2) . . . . ? C2' Fe1' C10' C6' 79.4(2) . . . . ? C5' Fe1' C10' C6' -165.1(3) . . . . ? C9' Fe1' C10' C6' -119.8(3) . . . . ? C8' Fe1' C10' C6' -83.0(2) . . . . ? C3' Fe1' C10' C6' 120.5(2) . . . . ? C4' Fe1' C10' C6' 161.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.421 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.069 #==========================================================END