# ic000810b.cif data_e061 _publ_contact_author_name 'Prof. Thomas M. Klapoetke' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'tmk@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7491' _publ_contact_author_fax '+49 89 2180 7492' _publ_author_name 'Krumm, Burkhard' _publ_author_name 'Ruscitti, Oliver P.' _publ_author_name 'Mayer, Peter' _publ_requested_journal 'Inorg. Chem.' _publ_section_title ; First Synthesis and Structures of Aryltellurium(IV) Diazides ; _audit_author_name 'Mayer, P., Piotrowski, H., Warchtold, M.' _audit_block_code Te_(N3)2_(C6F5)2_e061_klapoetke _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 08-Mar-00 _chemical_name_systematic ? _chemical_compound_source ? _chemical_name_common 'Te(N3)2(C6F5)2' _chemical_formula_moiety 'Te F10 N6 C12' _chemical_formula_sum 'C12 F10 N6 Te' _chemical_formula_weight 545.75 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 15.3104(13) _cell_length_b 6.1035(3) _cell_length_c 18.0152(13) _cell_angle_alpha 90 _cell_angle_beta 113.348(9) _cell_angle_gamma 90 _cell_volume 1545.61(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.9 _cell_special_details 'Monoclinic P (as derived from metrics)' _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.3454(3) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8058 _exptl_absorpt_correction_T_max 0.9092 _exptl_absorpt_process_details 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0320 0 0 -1 0.0210 8 0 -5 0.0400 -8 0 5 0.0550 -7 -5 -4 0.0740 -5 3 7 0.0860 1 1 0 0.1300 0 -1 6 0.0490 -2 -3 -9 0.0660 1 -2 -2 0.0950 3 0 4 0.0380 _diffrn_ambient_temperature 200(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 120.0 _kl_diffrn_detector_area_phi_incr 1.0 _kl_diffrn_detector_area_expos_time 4.00_min _kl_diffrn_detector_area_plate_dist 70.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.005 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 19 _diffrn_special_details ? _diffrn_reflns_number 6923 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.86 _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.86 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.329 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.076 _reflns_number_total 2868 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2868 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0444 _refine_ls_wR_factor_gt 0.0417 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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 Te Te 0.313833(12) 0.00280(4) 0.216243(9) 0.01547(6) Uani 1 1 d . . . N1 N 0.36706(19) -0.2920(4) 0.29179(13) 0.0227(6) Uani 1 1 d . . . N2 N 0.41548(19) -0.4201(4) 0.27363(13) 0.0192(5) Uani 1 1 d . . . N3 N 0.4590(2) -0.5543(4) 0.25993(16) 0.0302(7) Uani 1 1 d . . . N4 N 0.22999(19) 0.2937(4) 0.16107(14) 0.0230(6) Uani 1 1 d . . . N5 N 0.2588(2) 0.4012(4) 0.11861(14) 0.0250(6) Uani 1 1 d . . . N6 N 0.2812(3) 0.5132(7) 0.0783(2) 0.0538(9) Uani 1 1 d . . . C11 C 0.1798(2) -0.1478(5) 0.18245(16) 0.0188(6) Uani 1 1 d . . . C21 C 0.1448(2) -0.2429(5) 0.23537(16) 0.0194(6) Uani 1 1 d . . . C31 C 0.0589(3) -0.3461(5) 0.20777(19) 0.0271(7) Uani 1 1 d . . . C41 C 0.0034(2) -0.3588(5) 0.1257(2) 0.0293(7) Uani 1 1 d . . . C51 C 0.0368(2) -0.2626(5) 0.07228(17) 0.0272(7) Uani 1 1 d . . . C61 C 0.1230(2) -0.1616(5) 0.10058(16) 0.0216(6) Uani 1 1 d . . . F21 F 0.19486(14) -0.2324(3) 0.31528(9) 0.0268(4) Uani 1 1 d . . . F31 F 0.02572(15) -0.4328(3) 0.25978(12) 0.0382(5) Uani 1 1 d . . . F41 F -0.07909(15) -0.4631(4) 0.09890(13) 0.0462(6) Uani 1 1 d . . . F51 F -0.01653(15) -0.2722(3) -0.00767(10) 0.0411(5) Uani 1 1 d . . . F61 F 0.15536(14) -0.0767(3) 0.04737(9) 0.0299(4) Uani 1 1 d . . . C12 C 0.3285(2) 0.1446(5) 0.32710(15) 0.0175(6) Uani 1 1 d . . . C22 C 0.4192(2) 0.1559(5) 0.38794(16) 0.0217(6) Uani 1 1 d . . . C32 C 0.4338(3) 0.2521(6) 0.46106(16) 0.0274(7) Uani 1 1 d . . . C42 C 0.3590(3) 0.3364(5) 0.47490(17) 0.0305(8) Uani 1 1 d . . . C52 C 0.2681(3) 0.3298(5) 0.41497(18) 0.0282(7) Uani 1 1 d . . . C62 C 0.2549(2) 0.2353(5) 0.34192(17) 0.0229(6) Uani 1 1 d . . . F22 F 0.49364(13) 0.0753(3) 0.37665(10) 0.0274(4) Uani 1 1 d . . . F32 F 0.52214(15) 0.2611(3) 0.51876(10) 0.0382(5) Uani 1 1 d . . . F42 F 0.37402(19) 0.4297(3) 0.54615(11) 0.0477(6) Uani 1 1 d . . . F52 F 0.19562(18) 0.4149(4) 0.42777(12) 0.0436(5) Uani 1 1 d . . . F62 F 0.16531(13) 0.2289(3) 0.28544(10) 0.0286(4) Uani 1 1 d . . . 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 Te 0.01585(9) 0.01448(9) 0.01776(8) 0.00100(9) 0.00846(6) 0.00131(10) N1 0.0296(15) 0.0189(14) 0.0237(12) 0.0045(10) 0.0149(11) 0.0062(11) N2 0.0170(13) 0.0178(12) 0.0226(11) 0.0031(9) 0.0074(10) -0.0029(11) N3 0.0322(17) 0.0204(18) 0.0464(16) 0.0069(11) 0.0244(13) 0.0104(12) N4 0.0223(14) 0.0184(14) 0.0298(12) 0.0061(10) 0.0119(11) 0.0032(11) N5 0.0248(15) 0.0203(13) 0.0287(13) 0.0023(12) 0.0092(11) 0.0069(12) N6 0.062(2) 0.049(2) 0.0654(19) 0.0374(19) 0.0409(18) 0.020(2) C11 0.0167(15) 0.0130(15) 0.0257(14) 0.0003(11) 0.0073(11) 0.0006(11) C21 0.0188(16) 0.0156(15) 0.0251(14) 0.0002(12) 0.0101(11) 0.0023(12) C31 0.0307(19) 0.0156(15) 0.0433(17) 0.0031(13) 0.0233(14) 0.0027(13) C41 0.0156(17) 0.0217(18) 0.0489(19) -0.0051(14) 0.0110(14) -0.0013(13) C51 0.0226(17) 0.0211(17) 0.0271(15) -0.0045(13) -0.0018(12) 0.0073(13) C61 0.0265(18) 0.0153(15) 0.0238(14) 0.0013(12) 0.0106(12) 0.0049(13) F21 0.0289(12) 0.0304(11) 0.0227(8) 0.0047(8) 0.0121(8) -0.0003(9) F31 0.0316(12) 0.0330(12) 0.0615(12) 0.0077(9) 0.0306(10) -0.0021(8) F41 0.0205(10) 0.0391(15) 0.0722(14) -0.0110(11) 0.0113(9) -0.0097(9) F51 0.0358(15) 0.0348(11) 0.0332(10) -0.0073(9) -0.0071(9) 0.0040(9) F61 0.0389(12) 0.0303(10) 0.0217(8) 0.0033(7) 0.0132(7) 0.0014(8) C12 0.0234(16) 0.0141(15) 0.0165(12) -0.0013(10) 0.0095(11) -0.0023(12) C22 0.0271(17) 0.0156(15) 0.0246(14) 0.0047(12) 0.0125(12) -0.0013(13) C32 0.036(2) 0.0212(17) 0.0202(14) 0.0026(12) 0.0055(13) -0.0099(15) C42 0.052(2) 0.0221(17) 0.0235(14) -0.0033(13) 0.0218(15) -0.0104(16) C52 0.041(2) 0.0195(16) 0.0363(16) -0.0030(13) 0.0284(15) -0.0044(15) C62 0.0271(18) 0.0182(16) 0.0271(14) 0.0002(12) 0.0147(13) -0.0032(13) F22 0.0206(10) 0.0276(10) 0.0315(9) 0.0046(7) 0.0078(7) 0.0027(7) F32 0.0419(14) 0.0349(11) 0.0234(9) 0.0015(8) -0.0023(8) -0.0114(10) F42 0.0815(19) 0.0426(14) 0.0272(9) -0.0165(8) 0.0304(10) -0.0158(11) F52 0.0599(16) 0.0389(12) 0.0513(11) -0.0101(9) 0.0424(11) 0.0026(10) F62 0.0219(11) 0.0300(11) 0.0365(10) -0.0030(8) 0.0145(8) 0.0047(8) 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 Te C12 2.106(3) . ? Te C11 2.106(3) . ? Te N4 2.185(2) . ? Te N1 2.208(2) . ? N1 N2 1.208(4) . ? N2 N3 1.143(4) . ? N4 N5 1.216(4) . ? N5 N6 1.144(4) . ? C11 C61 1.386(4) . ? C11 C21 1.392(4) . ? C21 F21 1.338(3) . ? C21 C31 1.362(5) . ? C31 F31 1.339(4) . ? C31 C41 1.384(4) . ? C41 F41 1.323(4) . ? C41 C51 1.387(5) . ? C51 F51 1.346(3) . ? C51 C61 1.359(5) . ? C61 F61 1.345(4) . ? C12 C62 1.373(4) . ? C12 C22 1.389(4) . ? C22 F22 1.330(4) . ? C22 C32 1.377(4) . ? C32 F32 1.341(4) . ? C32 C42 1.366(5) . ? C42 F42 1.338(3) . ? C42 C52 1.383(5) . ? C52 F52 1.326(4) . ? C52 C62 1.376(4) . ? C62 F62 1.346(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 C12 Te C11 100.29(11) . . ? C12 Te N4 85.41(10) . . ? C11 Te N4 83.90(10) . . ? C12 Te N1 82.86(10) . . ? C11 Te N1 84.37(10) . . ? N4 Te N1 161.65(9) . . ? N2 N1 Te 118.46(18) . . ? N3 N2 N1 174.2(3) . . ? N5 N4 Te 115.5(2) . . ? N6 N5 N4 175.2(3) . . ? C61 C11 C21 117.0(3) . . ? C61 C11 Te 117.6(2) . . ? C21 C11 Te 125.4(2) . . ? F21 C21 C31 118.2(3) . . ? F21 C21 C11 120.4(3) . . ? C31 C21 C11 121.4(3) . . ? F31 C31 C21 120.4(3) . . ? F31 C31 C41 118.8(3) . . ? C21 C31 C41 120.7(3) . . ? F41 C41 C31 120.7(3) . . ? F41 C41 C51 120.7(3) . . ? C31 C41 C51 118.6(3) . . ? F51 C51 C61 120.5(3) . . ? F51 C51 C41 119.4(3) . . ? C61 C51 C41 120.1(3) . . ? F61 C61 C51 119.0(3) . . ? F61 C61 C11 118.8(3) . . ? C51 C61 C11 122.2(3) . . ? C62 C12 C22 117.9(3) . . ? C62 C12 Te 124.3(2) . . ? C22 C12 Te 117.8(2) . . ? F22 C22 C32 118.7(3) . . ? F22 C22 C12 120.7(2) . . ? C32 C22 C12 120.6(3) . . ? F32 C32 C42 120.3(3) . . ? F32 C32 C22 119.4(3) . . ? C42 C32 C22 120.3(3) . . ? F42 C42 C32 119.9(3) . . ? F42 C42 C52 119.9(3) . . ? C32 C42 C52 120.3(3) . . ? F52 C52 C62 121.0(3) . . ? F52 C52 C42 120.4(3) . . ? C62 C52 C42 118.7(3) . . ? F62 C62 C12 120.7(2) . . ? F62 C62 C52 117.1(3) . . ? C12 C62 C52 122.2(3) . . ? 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 C12 Te N1 N2 -147.5(3) . . . . ? C11 Te N1 N2 111.3(2) . . . . ? N4 Te N1 N2 161.8(3) . . . . ? Te N1 N2 N3 -157(3) . . . . ? C12 Te N4 N5 122.3(2) . . . . ? C11 Te N4 N5 -136.8(2) . . . . ? N1 Te N4 N5 172.7(2) . . . . ? Te N4 N5 N6 -172(4) . . . . ? C12 Te C11 C61 147.7(2) . . . . ? N4 Te C11 C61 63.5(2) . . . . ? N1 Te C11 C61 -130.6(2) . . . . ? C12 Te C11 C21 -35.1(3) . . . . ? N4 Te C11 C21 -119.2(3) . . . . ? N1 Te C11 C21 46.6(3) . . . . ? C61 C11 C21 F21 -178.7(3) . . . . ? Te C11 C21 F21 4.0(4) . . . . ? C61 C11 C21 C31 0.4(4) . . . . ? Te C11 C21 C31 -176.9(2) . . . . ? F21 C21 C31 F31 0.5(4) . . . . ? C11 C21 C31 F31 -178.7(3) . . . . ? F21 C21 C31 C41 178.9(3) . . . . ? C11 C21 C31 C41 -0.2(5) . . . . ? F31 C31 C41 F41 -3.0(5) . . . . ? C21 C31 C41 F41 178.5(3) . . . . ? F31 C31 C41 C51 178.0(3) . . . . ? C21 C31 C41 C51 -0.5(5) . . . . ? F41 C41 C51 F51 1.4(5) . . . . ? C31 C41 C51 F51 -179.6(3) . . . . ? F41 C41 C51 C61 -178.0(3) . . . . ? C31 C41 C51 C61 1.0(5) . . . . ? F51 C51 C61 F61 -1.8(4) . . . . ? C41 C51 C61 F61 177.6(3) . . . . ? F51 C51 C61 C11 179.8(3) . . . . ? C41 C51 C61 C11 -0.8(5) . . . . ? C21 C11 C61 F61 -178.3(3) . . . . ? Te C11 C61 F61 -0.8(4) . . . . ? C21 C11 C61 C51 0.1(5) . . . . ? Te C11 C61 C51 177.6(2) . . . . ? C11 Te C12 C62 -37.1(3) . . . . ? N4 Te C12 C62 45.9(3) . . . . ? N1 Te C12 C62 -120.0(3) . . . . ? C11 Te C12 C22 146.0(2) . . . . ? N4 Te C12 C22 -131.1(2) . . . . ? N1 Te C12 C22 63.1(2) . . . . ? C62 C12 C22 F22 -178.5(3) . . . . ? Te C12 C22 F22 -1.4(4) . . . . ? C62 C12 C22 C32 1.1(4) . . . . ? Te C12 C22 C32 178.2(2) . . . . ? F22 C22 C32 F32 -0.3(4) . . . . ? C12 C22 C32 F32 -179.9(3) . . . . ? F22 C22 C32 C42 -179.9(3) . . . . ? C12 C22 C32 C42 0.5(5) . . . . ? F32 C32 C42 F42 0.5(5) . . . . ? C22 C32 C42 F42 -180.0(3) . . . . ? F32 C32 C42 C52 179.1(3) . . . . ? C22 C32 C42 C52 -1.3(5) . . . . ? F42 C42 C52 F52 -0.1(5) . . . . ? C32 C42 C52 F52 -178.8(3) . . . . ? F42 C42 C52 C62 179.2(3) . . . . ? C32 C42 C52 C62 0.5(5) . . . . ? C22 C12 C62 F62 -179.8(3) . . . . ? Te C12 C62 F62 3.3(4) . . . . ? C22 C12 C62 C52 -1.9(4) . . . . ? Te C12 C62 C52 -178.8(2) . . . . ? F52 C52 C62 F62 -1.6(4) . . . . ? C42 C52 C62 F62 179.1(3) . . . . ? F52 C52 C62 C12 -179.6(3) . . . . ? C42 C52 C62 C12 1.1(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e061 in P21/c (14, sir97 CELL 0.71073 15.3104 6.1035 18.0152 90.000 113.348 90.000 ZERR 4 0.0013 0.0003 0.0013 0.000 0.009 0.000 LATT 1 SYMM -X, .50000+Y, .50000-Z SFAC C N F TE UNIT 48 24 40 4 L.S. 8 BOND CONF TEMP -73 ACTA FMAP 2 PLAN -25 WGHT 0.024300 FVAR 0.34434 TE 4 0.313833 0.002796 0.216243 11.00000 0.01585 0.01448 = 0.01776 0.00100 0.00846 0.00131 N1 2 0.367063 -0.291974 0.291787 11.00000 0.02964 0.01887 = 0.02372 0.00449 0.01491 0.00619 N2 2 0.415483 -0.420065 0.273626 11.00000 0.01698 0.01776 = 0.02262 0.00315 0.00744 -0.00293 N3 2 0.459005 -0.554272 0.259926 11.00000 0.03217 0.02037 = 0.04640 0.00689 0.02442 0.01040 N4 2 0.229992 0.293655 0.161067 11.00000 0.02226 0.01842 = 0.02984 0.00605 0.01190 0.00323 N5 2 0.258779 0.401231 0.118611 11.00000 0.02479 0.02034 = 0.02870 0.00233 0.00920 0.00687 N6 2 0.281211 0.513224 0.078335 11.00000 0.06160 0.04926 = 0.06536 0.03742 0.04095 0.02021 C11 1 0.179787 -0.147818 0.182449 11.00000 0.01670 0.01295 = 0.02570 0.00031 0.00727 0.00063 C21 1 0.144840 -0.242939 0.235369 11.00000 0.01877 0.01560 = 0.02509 0.00017 0.01012 0.00230 C31 1 0.058904 -0.346069 0.207771 11.00000 0.03066 0.01564 = 0.04329 0.00311 0.02331 0.00272 C41 1 0.003396 -0.358768 0.125750 11.00000 0.01563 0.02174 = 0.04892 -0.00512 0.01101 -0.00129 C51 1 0.036788 -0.262629 0.072285 11.00000 0.02257 0.02107 = 0.02707 -0.00445 -0.00181 0.00726 C61 1 0.122986 -0.161639 0.100581 11.00000 0.02649 0.01530 = 0.02375 0.00130 0.01060 0.00485 F21 3 0.194856 -0.232414 0.315280 11.00000 0.02893 0.03044 = 0.02267 0.00468 0.01206 -0.00030 F31 3 0.025724 -0.432751 0.259778 11.00000 0.03156 0.03295 = 0.06146 0.00765 0.03060 -0.00210 F41 3 -0.079088 -0.463091 0.098903 11.00000 0.02050 0.03913 = 0.07219 -0.01098 0.01130 -0.00974 F51 3 -0.016533 -0.272219 -0.007675 11.00000 0.03581 0.03484 = 0.03323 -0.00735 -0.00707 0.00400 F61 3 0.155363 -0.076657 0.047374 11.00000 0.03886 0.03034 = 0.02169 0.00333 0.01317 0.00139 C12 1 0.328459 0.144588 0.327102 11.00000 0.02343 0.01406 = 0.01653 -0.00128 0.00953 -0.00225 C22 1 0.419165 0.155909 0.387941 11.00000 0.02705 0.01563 = 0.02460 0.00468 0.01251 -0.00131 C32 1 0.433837 0.252141 0.461057 11.00000 0.03557 0.02124 = 0.02017 0.00255 0.00550 -0.00991 C42 1 0.359021 0.336431 0.474897 11.00000 0.05233 0.02208 = 0.02349 -0.00333 0.02185 -0.01036 C52 1 0.268099 0.329765 0.414970 11.00000 0.04098 0.01951 = 0.03630 -0.00300 0.02838 -0.00441 C62 1 0.254867 0.235326 0.341916 11.00000 0.02714 0.01817 = 0.02714 0.00021 0.01466 -0.00319 F22 3 0.493642 0.075271 0.376653 11.00000 0.02064 0.02759 = 0.03152 0.00456 0.00780 0.00272 F32 3 0.522140 0.261110 0.518757 11.00000 0.04195 0.03488 = 0.02340 0.00147 -0.00230 -0.01139 F42 3 0.374023 0.429687 0.546147 11.00000 0.08148 0.04261 = 0.02723 -0.01653 0.03039 -0.01583 F52 3 0.195622 0.414916 0.427768 11.00000 0.05985 0.03887 = 0.05132 -0.01009 0.04242 0.00258 F62 3 0.165307 0.228920 0.285442 11.00000 0.02190 0.03004 = 0.03652 -0.00303 0.01455 0.00469 HKLF 4 REM e061 in P21/c (14, sir97 REM R1 = 0.0204 for 2060 Fo > 4sig(Fo) and 0.0361 for all 2868 data REM 262 parameters refined using 0 restraints #===END WGHT 0.0243 0.0000 REM Highest difference peak 0.329, deepest hole -0.372, 1-sigma level 0.076 Q1 1 0.2399 0.4802 0.0486 11.00000 0.05 0.33 Q2 1 0.3787 0.0029 0.2332 11.00000 0.05 0.30 Q3 1 0.2400 -0.0033 0.1944 11.00000 0.05 0.30 Q4 1 0.3125 -0.0644 0.1755 11.00000 0.05 0.28 ; _kl_archive_SCHAKAL_comment ? _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ? #===END data_e082 _publ_contact_author_name 'Prof. Thomas M. Klapoetke' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians-University Butenandtstr. 5-13 (Haus D) D-81377 Munich, Germany ; _publ_contact_author_email 'tmk@cup.uni-muenchen.de' _publ_contact_author_phone '+49 89 2180 7491' _publ_contact_author_fax '+49 89 2180 7492' _publ_author_name 'Krumm, Burkhard' _publ_author_name 'Ruscitti, Oliver P.' _publ_author_name 'Mayer, Peter' _publ_requested_journal 'Inorg. Chem.' _publ_section_title ; First Synthesis and Structures of Aryltellurium(IV) Diazides ; _audit_author_name 'Mayer, P.' _audit_block_code Te_(N3)2_(C6H5)2_e082_klapoetke _audit_creation_method 'form98_1/compatible with shelxl97-2' _audit_creation_date 04-Apr-00 _chemical_name_systematic ? _chemical_compound_source ? _chemical_name_common 'Te(N3)2(C6H5)2' _chemical_formula_moiety 'Te N6 C12 H10' _chemical_formula_sum 'C12 H10 N6 Te' _chemical_formula_weight 365.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5801(4) _cell_length_b 14.9046(9) _cell_length_c 23.0845(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2608.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(3) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.8 _cell_special_details 'Orthorhombic P (as derived from metrics)' _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.8635(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.277 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5440 _exptl_absorpt_correction_T_max 0.7794 _exptl_absorpt_process_details ; shape of the crystal calculated with X-Shape, absorption correction with XRed, rev. 1.09, Stoe (Darmstadt, Germany) ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.5738 -1 2 -10 0.1022 -1 -1 10 0.1023 1 -1 6 0.1629 0 1 0 0.0480 0 -1 0 0.0720 _diffrn_ambient_temperature 150(3) _diffrn_source_type 'Spellman DF4 Series' _diffrn_source_power 2.75_kW _diffrn_source_voltage 55_kV _diffrn_source_current 50_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'image-plate area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_detector_area_resol_mean ? _kl_diffrn_detector_area_phi_start 0.0 _kl_diffrn_detector_area_phi_end 120.0 _kl_diffrn_detector_area_phi_incr 0.8 _kl_diffrn_detector_area_expos_time 6.00_min _kl_diffrn_detector_area_plate_dist 70.0_mm _kl_diffrn_detector_area_eff_mos_spread 0.007 _kl_diffrn_detector_area_profile_funct dynamic _kl_diffrn_detector_area_profile_min 11 _kl_diffrn_detector_area_profile_max 21 _diffrn_special_details ? _diffrn_reflns_number 8285 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.83 _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.426 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.086 _reflns_number_total 2295 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution 'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2295 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_special_details ; 1 common U for all H atoms ; 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 Te Te 0.35651(2) 0.071923(12) 0.190156(6) 0.00917(7) Uani 1 1 d . . . N1 N 0.0706(3) 0.03165(19) 0.19627(9) 0.0146(5) Uani 1 1 d . . . N2 N 0.0226(3) -0.0288(2) 0.16436(9) 0.0139(6) Uani 1 1 d . . . N3 N -0.0270(4) -0.0855(2) 0.13528(10) 0.0276(8) Uani 1 1 d . . . N4 N 0.6396(3) 0.0990(2) 0.17727(9) 0.0182(6) Uani 1 1 d . . . N5 N 0.6939(3) 0.1069(2) 0.12794(10) 0.0167(6) Uani 1 1 d . . . N6 N 0.7532(4) 0.1153(3) 0.08298(10) 0.0306(8) Uani 1 1 d . . . C11 C 0.4129(4) -0.0660(2) 0.18438(10) 0.0105(6) Uani 1 1 d . . . C21 C 0.5228(4) -0.1008(2) 0.14181(12) 0.0159(7) Uani 1 1 d . . . H21 H 0.577(5) -0.060(3) 0.1111(14) 0.032(3) Uiso 1 1 d . . . C31 C 0.5644(5) -0.1900(2) 0.14324(12) 0.0197(7) Uani 1 1 d . . . H31 H 0.645(5) -0.212(3) 0.1163(14) 0.032(3) Uiso 1 1 d . . . C41 C 0.5009(4) -0.2459(2) 0.18695(13) 0.0176(6) Uani 1 1 d . . . H41 H 0.526(5) -0.301(3) 0.1853(14) 0.032(3) Uiso 1 1 d . . . C51 C 0.3910(4) -0.2103(2) 0.22925(11) 0.0163(7) Uani 1 1 d . . . H51 H 0.344(5) -0.253(3) 0.2592(14) 0.032(3) Uiso 1 1 d . . . C61 C 0.3447(4) -0.1210(2) 0.22779(10) 0.0114(6) Uani 1 1 d . . . H61 H 0.263(5) -0.099(3) 0.2553(14) 0.032(3) Uiso 1 1 d . . . C12 C 0.3083(4) 0.1073(2) 0.10296(10) 0.0131(7) Uani 1 1 d . . . C22 C 0.3182(4) 0.1973(3) 0.09041(12) 0.0194(7) Uani 1 1 d . . . H22 H 0.359(5) 0.238(3) 0.1167(14) 0.032(3) Uiso 1 1 d . . . C32 C 0.2659(5) 0.2271(3) 0.03593(13) 0.0287(9) Uani 1 1 d . . . H32 H 0.265(5) 0.281(3) 0.0295(14) 0.032(3) Uiso 1 1 d . . . C42 C 0.2048(5) 0.1664(3) -0.00455(12) 0.0288(9) Uani 1 1 d . . . H42 H 0.158(5) 0.185(3) -0.0398(14) 0.032(3) Uiso 1 1 d . . . C52 C 0.2007(5) 0.0773(3) 0.00786(12) 0.0286(9) Uani 1 1 d . . . H52 H 0.163(5) 0.037(3) -0.0160(15) 0.032(3) Uiso 1 1 d . . . C62 C 0.2549(5) 0.0453(3) 0.06197(11) 0.0192(7) Uani 1 1 d . . . H62 H 0.249(5) -0.013(3) 0.0668(14) 0.032(3) Uiso 1 1 d . . . 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 Te 0.01143(10) 0.00486(11) 0.01122(9) -0.00063(6) 0.00011(6) -0.00023(9) N1 0.0127(12) 0.0113(15) 0.0198(10) 0.0011(10) 0.0027(9) -0.0027(12) N2 0.0140(13) 0.0132(16) 0.0144(10) 0.0024(10) 0.0005(9) 0.0004(12) N3 0.0234(16) 0.035(2) 0.0242(13) -0.0068(12) 0.0014(10) -0.0125(15) N4 0.0118(12) 0.0226(18) 0.0202(11) -0.0008(9) -0.0013(9) -0.0051(13) N5 0.0154(14) 0.0084(17) 0.0263(13) -0.0002(10) -0.0004(10) -0.0051(12) N6 0.0312(17) 0.033(2) 0.0279(15) 0.0012(12) 0.0105(12) -0.0083(16) C11 0.0107(13) 0.0033(16) 0.0176(11) -0.0003(11) -0.0023(10) 0.0003(12) C21 0.0173(17) 0.0098(18) 0.0208(13) -0.0009(11) 0.0044(11) -0.0018(14) C31 0.0188(17) 0.013(2) 0.0272(14) -0.0050(12) 0.0071(13) 0.0041(15) C41 0.0175(16) 0.0054(17) 0.0300(15) -0.0010(12) -0.0033(12) 0.0012(14) C51 0.0108(16) 0.0141(19) 0.0239(13) 0.0046(12) -0.0027(10) -0.0022(14) C61 0.0106(14) 0.0072(17) 0.0163(12) 0.0013(10) -0.0009(11) -0.0001(14) C12 0.0128(15) 0.0156(18) 0.0110(11) 0.0025(10) 0.0007(10) 0.0033(13) C22 0.0220(19) 0.013(2) 0.0228(14) 0.0014(11) 0.0041(11) -0.0007(15) C32 0.035(2) 0.023(3) 0.0281(15) 0.0130(15) 0.0068(14) 0.0104(19) C42 0.0257(19) 0.046(3) 0.0149(13) 0.0117(14) 0.0024(11) 0.0022(19) C52 0.0260(18) 0.046(3) 0.0134(12) -0.0026(15) -0.0010(11) -0.008(2) C62 0.0178(16) 0.018(2) 0.0216(14) -0.0012(12) 0.0028(11) -0.0035(14) 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 Te C11 2.104(3) . ? Te C12 2.113(2) . ? Te N4 2.204(3) . ? Te N1 2.253(3) . ? N1 N2 1.220(4) . ? N2 N3 1.143(4) . ? N4 N5 1.217(3) . ? N5 N6 1.138(3) . ? C11 C21 1.388(4) . ? C11 C61 1.394(4) . ? C21 C31 1.367(5) . ? C21 H21 1.02(4) . ? C31 C41 1.394(5) . ? C31 H31 0.93(4) . ? C41 C51 1.389(4) . ? C41 H41 0.85(5) . ? C51 C61 1.378(5) . ? C51 H51 1.01(4) . ? C61 H61 0.94(4) . ? C12 C22 1.375(5) . ? C12 C62 1.384(5) . ? C22 C32 1.391(5) . ? C22 H22 0.91(4) . ? C32 C42 1.381(6) . ? C32 H32 0.81(5) . ? C42 C52 1.359(6) . ? C42 H42 0.93(4) . ? C52 C62 1.399(4) . ? C52 H52 0.86(4) . ? C62 H62 0.88(5) . ? 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 C11 Te C12 102.64(11) . . ? C11 Te N4 88.41(11) . . ? C12 Te N4 89.66(10) . . ? C11 Te N1 86.51(10) . . ? C12 Te N1 87.71(10) . . ? N4 Te N1 173.64(9) . . ? N2 N1 Te 116.49(19) . . ? N3 N2 N1 178.0(3) . . ? N5 N4 Te 118.25(19) . . ? N6 N5 N4 176.4(3) . . ? C21 C11 C61 120.8(3) . . ? C21 C11 Te 122.1(2) . . ? C61 C11 Te 116.9(2) . . ? C31 C21 C11 119.0(3) . . ? C31 C21 H21 120(2) . . ? C11 C21 H21 121(2) . . ? C21 C31 C41 121.3(3) . . ? C21 C31 H31 119(3) . . ? C41 C31 H31 120(3) . . ? C51 C41 C31 119.2(3) . . ? C51 C41 H41 123(2) . . ? C31 C41 H41 118(2) . . ? C61 C51 C41 120.3(3) . . ? C61 C51 H51 123(2) . . ? C41 C51 H51 117(2) . . ? C51 C61 C11 119.4(3) . . ? C51 C61 H61 119(3) . . ? C11 C61 H61 122(3) . . ? C22 C12 C62 121.6(3) . . ? C22 C12 Te 115.8(2) . . ? C62 C12 Te 122.3(2) . . ? C12 C22 C32 119.1(3) . . ? C12 C22 H22 122(3) . . ? C32 C22 H22 119(3) . . ? C42 C32 C22 119.9(4) . . ? C42 C32 H32 121(3) . . ? C22 C32 H32 119(3) . . ? C52 C42 C32 120.4(3) . . ? C52 C42 H42 118(3) . . ? C32 C42 H42 121(3) . . ? C42 C52 C62 121.0(4) . . ? C42 C52 H52 123(3) . . ? C62 C52 H52 116(3) . . ? C12 C62 C52 117.9(4) . . ? C12 C62 H62 126(2) . . ? C52 C62 H62 116(2) . . ? 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 C11 Te N1 N2 -41.2(2) . . . . ? C12 Te N1 N2 61.7(2) . . . . ? N4 Te N1 N2 -4.0(9) . . . . ? Te N1 N2 N3 172(100) . . . . ? C11 Te N4 N5 88.7(3) . . . . ? C12 Te N4 N5 -14.0(3) . . . . ? N1 Te N4 N5 51.6(9) . . . . ? Te N4 N5 N6 177(100) . . . . ? C12 Te C11 C21 44.1(2) . . . . ? N4 Te C11 C21 -45.2(2) . . . . ? N1 Te C11 C21 130.9(2) . . . . ? C12 Te C11 C61 -140.2(2) . . . . ? N4 Te C11 C61 130.5(2) . . . . ? N1 Te C11 C61 -53.3(2) . . . . ? C61 C11 C21 C31 -0.5(4) . . . . ? Te C11 C21 C31 175.1(2) . . . . ? C11 C21 C31 C41 -0.9(5) . . . . ? C21 C31 C41 C51 1.0(5) . . . . ? C31 C41 C51 C61 0.4(5) . . . . ? C41 C51 C61 C11 -1.7(4) . . . . ? C21 C11 C61 C51 1.8(4) . . . . ? Te C11 C61 C51 -174.0(2) . . . . ? C11 Te C12 C22 -161.7(2) . . . . ? N4 Te C12 C22 -73.4(2) . . . . ? N1 Te C12 C22 112.4(2) . . . . ? C11 Te C12 C62 23.8(3) . . . . ? N4 Te C12 C62 112.1(3) . . . . ? N1 Te C12 C62 -62.1(3) . . . . ? C62 C12 C22 C32 2.8(5) . . . . ? Te C12 C22 C32 -171.7(2) . . . . ? C12 C22 C32 C42 0.2(5) . . . . ? C22 C32 C42 C52 -2.2(5) . . . . ? C32 C42 C52 C62 1.2(5) . . . . ? C22 C12 C62 C52 -3.7(5) . . . . ? Te C12 C62 C52 170.5(2) . . . . ? C42 C52 C62 C12 1.6(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? _geom_special_details ? _kl_archive_SHELXL_comment 'release 97-2' _kl_archive_SHELXL_res ; TITL e082 in Pbca (61), sir97 CELL 0.71073 7.5801 14.9046 23.0845 90.000 90.000 90.000 ZERR 8 0.0004 0.0009 0.0014 0.000 0.000 0.000 LATT 1 SYMM .50000-X,-Y, .50000+Z SYMM .50000+X, .50000-Y,-Z SYMM -X, .50000+Y, .50000-Z SFAC C H N TE UNIT 96 80 48 8 L.S. 8 TEMP -123 BOND $H CONF ACTA FMAP 2 PLAN -30 WGHT 0.024800 FVAR 0.25682 0.03199 TE 4 0.356514 0.071923 0.190156 11.00000 0.01143 0.00486 = 0.01122 -0.00063 0.00011 -0.00023 N1 3 0.070601 0.031645 0.196270 11.00000 0.01267 0.01133 = 0.01977 0.00111 0.00271 -0.00267 N2 3 0.022590 -0.028826 0.164357 11.00000 0.01399 0.01324 = 0.01445 0.00244 0.00047 0.00039 N3 3 -0.027047 -0.085546 0.135281 11.00000 0.02344 0.03515 = 0.02422 -0.00676 0.00137 -0.01250 N4 3 0.639619 0.098983 0.177274 11.00000 0.01175 0.02257 = 0.02021 -0.00080 -0.00128 -0.00509 N5 3 0.693894 0.106925 0.127936 11.00000 0.01538 0.00842 = 0.02627 -0.00020 -0.00042 -0.00514 N6 3 0.753244 0.115328 0.082979 11.00000 0.03119 0.03274 = 0.02793 0.00125 0.01051 -0.00825 C11 1 0.412949 -0.066036 0.184381 11.00000 0.01072 0.00326 = 0.01759 -0.00031 -0.00229 0.00033 C21 1 0.522757 -0.100793 0.141808 11.00000 0.01731 0.00977 = 0.02077 -0.00091 0.00436 -0.00179 H21 2 0.577432 -0.059923 0.111134 11.00000 21.00000 C31 1 0.564449 -0.190011 0.143244 11.00000 0.01878 0.01310 = 0.02715 -0.00500 0.00711 0.00408 H31 2 0.644500 -0.212302 0.116313 11.00000 21.00000 C41 1 0.500897 -0.245915 0.186954 11.00000 0.01749 0.00537 = 0.03005 -0.00100 -0.00331 0.00119 H41 2 0.526353 -0.301058 0.185327 11.00000 21.00000 C51 1 0.390987 -0.210329 0.229250 11.00000 0.01082 0.01415 = 0.02390 0.00462 -0.00274 -0.00220 H51 2 0.344172 -0.253102 0.259212 11.00000 21.00000 C61 1 0.344659 -0.120982 0.227787 11.00000 0.01062 0.00725 = 0.01630 0.00133 -0.00091 -0.00014 H61 2 0.263076 -0.099445 0.255311 11.00000 21.00000 C12 1 0.308339 0.107334 0.102962 11.00000 0.01281 0.01558 = 0.01102 0.00250 0.00073 0.00326 C22 1 0.318160 0.197348 0.090413 11.00000 0.02202 0.01346 = 0.02283 0.00143 0.00405 -0.00074 H22 2 0.358512 0.238143 0.116710 11.00000 21.00000 C32 1 0.265907 0.227088 0.035925 11.00000 0.03542 0.02272 = 0.02805 0.01299 0.00680 0.01041 H32 2 0.265359 0.280735 0.029544 11.00000 21.00000 C42 1 0.204762 0.166372 -0.004550 11.00000 0.02568 0.04589 = 0.01495 0.01175 0.00244 0.00219 H42 2 0.158383 0.185298 -0.039775 11.00000 21.00000 C52 1 0.200687 0.077266 0.007855 11.00000 0.02601 0.04624 = 0.01344 -0.00262 -0.00102 -0.00846 H52 2 0.163169 0.037397 -0.015998 11.00000 21.00000 C62 1 0.254854 0.045252 0.061969 11.00000 0.01775 0.01836 = 0.02156 -0.00118 0.00276 -0.00347 H62 2 0.249238 -0.013478 0.066824 11.00000 21.00000 HKLF 4 REM e082 in Pbca (61), sir97 REM R1 = 0.0209 for 1798 Fo > 4sig(Fo) and 0.0319 for all 2295 data REM 203 parameters refined using 0 restraints #===END WGHT 0.0249 0.0000 REM Highest difference peak 0.426, deepest hole -0.459, 1-sigma level 0.086 Q1 1 0.3503 0.0653 0.1503 11.00000 0.05 0.43 Q2 1 0.3572 0.0726 0.2287 11.00000 0.05 0.40 Q3 1 0.5747 0.0146 0.1733 11.00000 0.05 0.40 Q4 1 0.4281 0.0227 0.2305 11.00000 0.05 0.37 ; _kl_archive_SCHAKAL_comment ? _kl_archive_SCHAKAL_dat ? _kl_archive_ORTEP_comment ? _kl_archive_ORTEP_ins ? _kl_archive_rtf_text ? #===END