data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'DIETER LENTZ' _publ_contact_author_address ; Fachbereich Biologie, Chemie, Pharmazie Freie Universitat Berlin Institut fur Chemie und Biochemie Fabeckstrasse, 34-36 Berlin D-14195 GERMANY ; _publ_contact_author_email LENTZ@CHEMIE.FU-BERLIN.DE _publ_section_title ; Pseudopolymorphism as a tool to modify molecular structures: [Te(CN)4] versus [Te(CN)3(u-CN)]n ; loop_ _publ_author_name 'Dieter Lentz' 'Malgorzata Szwak' # Attachment 'deposit.CIF' data_sad _database_code_depnum_ccdc_archive 'CCDC 640797' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tellurium Tetracyanide Bis(2-methoxyethyl)ether Polymere Solvate ; _chemical_name_common ;Tellurium Tetracyanide Bis(2-methoxyethyl)ether Polymere Solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 N4 O3 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' Te Te -0.5308 1.6751 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.202(3) _cell_length_b 10.921(3) _cell_length_c 13.142(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.621(7) _cell_angle_gamma 90.00 _cell_volume 1451.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 688 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 21.1 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 2.056 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9100 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 22.56 _reflns_number_total 1901 _reflns_number_gt 1303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep for Windows ( Farrugia, 1997)' _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^)+(0.0209P)^2^+10.9704P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1901 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Te1 Te 0.36289(6) 0.57654(5) 0.23299(5) 0.0269(2) Uani 1 1 d . . . N1 N 0.5042(10) 0.7731(9) 0.0848(8) 0.069(3) Uani 1 1 d . . . N2 N 0.6364(10) 0.4296(10) 0.2306(9) 0.086(4) Uani 1 1 d . . . N3 N 0.2136(10) 0.4815(8) 0.0146(7) 0.060(3) Uani 1 1 d . . . N4 N 0.2910(7) 0.2782(8) 0.3032(6) 0.035(2) Uani 1 1 d . . . O1L O 0.5308(7) 0.6972(7) 0.3644(6) 0.062(2) Uani 1 1 d . . . O2L O 0.3237(7) 0.5751(8) 0.4403(5) 0.057(2) Uani 1 1 d . . . O3L O 0.1036(6) 0.5467(5) 0.2816(5) 0.0351(17) Uani 1 1 d . . . C1 C 0.4565(10) 0.7053(10) 0.1334(8) 0.045(3) Uani 1 1 d . . . C2 C 0.5387(11) 0.4790(10) 0.2227(9) 0.047(3) Uani 1 1 d . . . C3 C 0.2722(11) 0.5133(9) 0.0909(9) 0.042(3) Uani 1 1 d . . . C4 C 0.3145(9) 0.3745(10) 0.2772(7) 0.031(2) Uani 1 1 d . . . C1L C 0.6625(10) 0.7289(12) 0.3493(9) 0.065(4) Uani 1 1 d . . . H1L1 H 0.6889 0.8042 0.3871 0.097 Uiso 1 1 calc R . . H1L2 H 0.6664 0.7418 0.2760 0.097 Uiso 1 1 calc R . . H1L3 H 0.7228 0.6624 0.3745 0.097 Uiso 1 1 calc R . . C2L C 0.5065(11) 0.7090(11) 0.4653(8) 0.057(3) Uani 1 1 d . . . H2L1 H 0.5289 0.7934 0.4892 0.068 Uiso 1 1 calc R . . H2L2 H 0.5647 0.6520 0.5090 0.068 Uiso 1 1 calc R . . C3L C 0.3676(13) 0.6833(10) 0.4777(10) 0.069(4) Uani 1 1 d . . . H3L1 H 0.3583 0.6864 0.5517 0.083 Uiso 1 1 calc R . . H3L2 H 0.3111 0.7486 0.4429 0.083 Uiso 1 1 calc R . . C4L C 0.1950(10) 0.5418(10) 0.4580(8) 0.046(3) Uani 1 1 d . . . H4L1 H 0.1807 0.5711 0.5270 0.056 Uiso 1 1 calc R . . H4L2 H 0.1886 0.4513 0.4582 0.056 Uiso 1 1 calc R . . C5L C 0.0881(9) 0.5913(10) 0.3811(7) 0.038(2) Uani 1 1 d . . . H5L1 H 0.0009 0.5659 0.3992 0.046 Uiso 1 1 calc R . . H5L2 H 0.0917 0.6818 0.3814 0.046 Uiso 1 1 calc R . . C6L C -0.0127(9) 0.5622(10) 0.2106(8) 0.051(3) Uani 1 1 d . . . H6L1 H -0.0861 0.5181 0.2351 0.076 Uiso 1 1 calc R . . H6L2 H 0.0021 0.5298 0.1435 0.076 Uiso 1 1 calc R . . H6L3 H -0.0344 0.6495 0.2041 0.076 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 Te1 0.0309(3) 0.0223(3) 0.0271(3) 0.0009(3) 0.0032(2) 0.0014(4) N1 0.075(7) 0.058(7) 0.079(8) 0.027(6) 0.033(6) 0.003(6) N2 0.049(7) 0.069(8) 0.143(11) 0.022(8) 0.029(7) 0.015(7) N3 0.089(8) 0.043(6) 0.045(6) -0.006(5) -0.006(6) -0.009(5) N4 0.034(5) 0.030(5) 0.039(5) -0.001(4) 0.013(4) -0.007(4) O1L 0.065(5) 0.077(6) 0.046(5) -0.015(4) 0.012(4) -0.041(5) O2L 0.046(4) 0.081(6) 0.046(4) -0.023(5) 0.011(3) -0.015(5) O3L 0.030(4) 0.038(4) 0.037(4) 0.002(3) 0.006(3) 0.005(3) C1 0.046(7) 0.043(7) 0.049(7) 0.007(6) 0.021(6) 0.009(6) C2 0.040(7) 0.041(7) 0.060(8) 0.012(6) 0.006(6) -0.007(6) C3 0.054(7) 0.024(6) 0.047(7) 0.003(5) 0.004(6) -0.002(5) C4 0.032(6) 0.040(7) 0.024(5) -0.007(5) 0.009(4) -0.005(5) C1L 0.046(7) 0.079(9) 0.066(8) 0.011(7) -0.005(6) -0.029(7) C2L 0.067(8) 0.056(8) 0.042(7) -0.020(6) -0.013(6) 0.008(7) C3L 0.101(11) 0.036(7) 0.079(10) -0.018(7) 0.045(8) -0.028(7) C4L 0.049(7) 0.058(8) 0.035(6) 0.001(5) 0.015(5) 0.008(6) C5L 0.038(6) 0.040(6) 0.039(6) 0.003(5) 0.014(5) -0.003(5) C6L 0.028(6) 0.055(8) 0.068(8) 0.008(7) 0.006(5) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 C3 2.088(11) . ? Te1 C2 2.106(12) . ? Te1 C1 2.221(11) . ? Te1 C4 2.350(11) . ? Te1 O1L 2.621(7) . ? Te1 N4 2.710(8) . ? Te1 O2L 2.805(7) . ? Te1 O3L 2.822(6) . ? N1 C1 1.130(12) . ? N2 C2 1.126(12) . ? N3 C3 1.151(12) . ? N4 C4 1.142(11) 2 ? O1L C2L 1.387(12) . ? O1L C1L 1.427(12) . ? O2L C3L 1.334(12) . ? O2L C4L 1.412(11) . ? O3L C6L 1.419(10) . ? O3L C5L 1.424(10) . ? C4 N4 1.142(11) 2_545 ? C2L C3L 1.474(15) . ? C4L C5L 1.487(13) . ? 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 C3 Te1 C2 93.1(4) . . ? C3 Te1 C1 81.8(4) . . ? C2 Te1 C1 81.1(4) . . ? C3 Te1 C4 80.1(3) . . ? C2 Te1 C4 75.5(3) . . ? C1 Te1 C4 149.4(3) . . ? C3 Te1 O1L 158.3(3) . . ? C2 Te1 O1L 79.0(4) . . ? C1 Te1 O1L 77.0(3) . . ? C4 Te1 O1L 116.7(3) . . ? C3 Te1 N4 86.2(3) . . ? C2 Te1 N4 151.5(3) . . ? C1 Te1 N4 70.5(3) . . ? C4 Te1 N4 132.1(3) . . ? O1L Te1 N4 91.1(3) . . ? C3 Te1 O2L 139.8(3) . . ? C2 Te1 O2L 107.0(3) . . ? C1 Te1 O2L 134.7(3) . . ? C4 Te1 O2L 72.1(3) . . ? O1L Te1 O2L 61.8(2) . . ? N4 Te1 O2L 91.2(2) . . ? C3 Te1 O3L 81.2(3) . . ? C2 Te1 O3L 142.0(3) . . ? C1 Te1 O3L 134.1(3) . . ? C4 Te1 O3L 66.5(2) . . ? O1L Te1 O3L 117.4(2) . . ? N4 Te1 O3L 66.1(2) . . ? O2L Te1 O3L 61.39(18) . . ? C4 N4 Te1 146.7(7) 2 . ? C2L O1L C1L 113.7(8) . . ? C2L O1L Te1 119.5(6) . . ? C1L O1L Te1 125.1(6) . . ? C3L O2L C4L 116.2(9) . . ? C3L O2L Te1 105.6(7) . . ? C4L O2L Te1 114.7(5) . . ? C6L O3L C5L 112.2(7) . . ? C6L O3L Te1 124.4(5) . . ? C5L O3L Te1 112.9(5) . . ? N1 C1 Te1 178.1(10) . . ? N2 C2 Te1 170.9(11) . . ? N3 C3 Te1 175.0(10) . . ? N4 C4 Te1 176.9(8) 2_545 . ? O1L C2L C3L 112.6(9) . . ? O2L C3L C2L 114.1(10) . . ? O2L C4L C5L 114.1(8) . . ? O3L C5L C4L 109.9(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 C3 Te1 N4 C4 -172.0(13) . . . 2 ? C2 Te1 N4 C4 -82.4(15) . . . 2 ? C1 Te1 N4 C4 -89.4(13) . . . 2 ? C4 Te1 N4 C4 115.0(12) . . . 2 ? O1L Te1 N4 C4 -13.6(13) . . . 2 ? O2L Te1 N4 C4 48.2(13) . . . 2 ? O3L Te1 N4 C4 106.0(13) . . . 2 ? C3 Te1 O1L C2L 166.7(9) . . . . ? C2 Te1 O1L C2L -123.0(8) . . . . ? C1 Te1 O1L C2L 153.7(8) . . . . ? C4 Te1 O1L C2L -55.5(8) . . . . ? N4 Te1 O1L C2L 84.0(8) . . . . ? O2L Te1 O1L C2L -6.7(7) . . . . ? O3L Te1 O1L C2L 20.5(8) . . . . ? C3 Te1 O1L C1L -29.0(14) . . . . ? C2 Te1 O1L C1L 41.4(9) . . . . ? C1 Te1 O1L C1L -41.9(8) . . . . ? C4 Te1 O1L C1L 108.9(8) . . . . ? N4 Te1 O1L C1L -111.6(8) . . . . ? O2L Te1 O1L C1L 157.6(9) . . . . ? O3L Te1 O1L C1L -175.1(8) . . . . ? C3 Te1 O2L C3L -144.2(8) . . . . ? C2 Te1 O2L C3L 99.1(8) . . . . ? C1 Te1 O2L C3L 4.8(9) . . . . ? C4 Te1 O2L C3L 167.2(8) . . . . ? O1L Te1 O2L C3L 32.1(7) . . . . ? N4 Te1 O2L C3L -58.6(8) . . . . ? O3L Te1 O2L C3L -120.3(8) . . . . ? C3 Te1 O2L C4L -14.9(9) . . . . ? C2 Te1 O2L C4L -131.6(7) . . . . ? C1 Te1 O2L C4L 134.1(7) . . . . ? C4 Te1 O2L C4L -63.5(7) . . . . ? O1L Te1 O2L C4L 161.4(8) . . . . ? N4 Te1 O2L C4L 70.7(7) . . . . ? O3L Te1 O2L C4L 9.0(6) . . . . ? C3 Te1 O3L C6L -31.7(7) . . . . ? C2 Te1 O3L C6L -115.4(8) . . . . ? C1 Te1 O3L C6L 37.7(8) . . . . ? C4 Te1 O3L C6L -114.6(7) . . . . ? O1L Te1 O3L C6L 136.3(7) . . . . ? N4 Te1 O3L C6L 58.1(7) . . . . ? O2L Te1 O3L C6L 163.7(8) . . . . ? C3 Te1 O3L C5L -173.6(6) . . . . ? C2 Te1 O3L C5L 102.6(8) . . . . ? C1 Te1 O3L C5L -104.2(7) . . . . ? C4 Te1 O3L C5L 103.5(6) . . . . ? O1L Te1 O3L C5L -5.6(6) . . . . ? N4 Te1 O3L C5L -83.8(6) . . . . ? O2L Te1 O3L C5L 21.7(6) . . . . ? C3 Te1 C1 N1 148(31) . . . . ? C2 Te1 C1 N1 -117(31) . . . . ? C4 Te1 C1 N1 -158(31) . . . . ? O1L Te1 C1 N1 -37(31) . . . . ? N4 Te1 C1 N1 59(31) . . . . ? O2L Te1 C1 N1 -12(31) . . . . ? O3L Te1 C1 N1 79(31) . . . . ? C3 Te1 C2 N2 -164(6) . . . . ? C1 Te1 C2 N2 115(6) . . . . ? C4 Te1 C2 N2 -85(6) . . . . ? O1L Te1 C2 N2 36(6) . . . . ? N4 Te1 C2 N2 108(6) . . . . ? O2L Te1 C2 N2 -20(6) . . . . ? O3L Te1 C2 N2 -85(6) . . . . ? C2 Te1 C3 N3 166(11) . . . . ? C1 Te1 C3 N3 -113(11) . . . . ? C4 Te1 C3 N3 91(11) . . . . ? O1L Te1 C3 N3 -126(10) . . . . ? N4 Te1 C3 N3 -42(11) . . . . ? O2L Te1 C3 N3 45(11) . . . . ? O3L Te1 C3 N3 24(11) . . . . ? C3 Te1 C4 N4 -156(15) . . . 2_545 ? C2 Te1 C4 N4 109(15) . . . 2_545 ? C1 Te1 C4 N4 150(15) . . . 2_545 ? O1L Te1 C4 N4 39(15) . . . 2_545 ? N4 Te1 C4 N4 -80(15) . . . 2_545 ? O2L Te1 C4 N4 -5(15) . . . 2_545 ? O3L Te1 C4 N4 -71(15) . . . 2_545 ? C1L O1L C2L C3L 176.4(10) . . . . ? Te1 O1L C2L C3L -17.6(13) . . . . ? C4L O2L C3L C2L 174.8(10) . . . . ? Te1 O2L C3L C2L -56.8(12) . . . . ? O1L C2L C3L O2L 53.8(15) . . . . ? C3L O2L C4L C5L 85.0(12) . . . . ? Te1 O2L C4L C5L -38.8(11) . . . . ? C6L O3L C5L C4L 163.8(8) . . . . ? Te1 O3L C5L C4L -49.6(9) . . . . ? O2L C4L C5L O3L 60.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.56 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.887 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.142 # Attachment 'deposit.CIF' data_c2c _database_code_depnum_ccdc_archive 'CCDC 640798' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tellurium Tetracyanide Bis(2-methoxyethyl)ether Monomere Solvate ; _chemical_name_common ;Tellurium Tetracyanide Bis(2-methoxyethyl)ether Monomere Solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 N4 O6 Te' _chemical_formula_weight 500.02 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' Te Te -0.5308 1.6751 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 17.596(5) _cell_length_b 7.664(5) _cell_length_c 18.360(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.657(5) _cell_angle_gamma 90.000(5) _cell_volume 2231.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 30.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13443 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 30.52 _reflns_number_total 3364 _reflns_number_gt 3168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep for windows ( Farrugia, 1997)' _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^)+(0.0196P)^2^+0.8273P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3364 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0145 _refine_ls_wR_factor_ref 0.0370 _refine_ls_wR_factor_gt 0.0359 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Te1 Te 0.0000 0.142510(11) 0.7500 0.02075(3) Uani 1 2 d S . . N1 N -0.20806(8) 0.03237(18) 0.67404(8) 0.0464(3) Uani 1 1 d . . . N2 N 0.00914(10) -0.15038(14) 0.88078(8) 0.0440(3) Uani 1 1 d . . . C1 C -0.13866(8) 0.06755(16) 0.69716(7) 0.0304(2) Uani 1 1 d . . . C2 C 0.00483(8) -0.04973(14) 0.83346(7) 0.0296(2) Uani 1 1 d . . . O1L O -0.12133(6) 0.26437(13) 0.55415(6) 0.0398(2) Uani 1 1 d . . . O2L O -0.11821(5) 0.46537(11) 0.68424(5) 0.03221(17) Uani 1 1 d . . . O3L O -0.06985(5) 0.28734(11) 0.83876(5) 0.02780(16) Uani 1 1 d . . . C1L C -0.09013(10) 0.2247(2) 0.49655(8) 0.0469(3) Uani 1 1 d . . . H1L1 H -0.0696 0.1069 0.5043 0.070 Uiso 1 1 calc R . . H1L2 H -0.0450 0.3033 0.5033 0.070 Uiso 1 1 calc R . . H1L3 H -0.1347 0.2371 0.4430 0.070 Uiso 1 1 calc R . . C2L C -0.15217(9) 0.4382(2) 0.54383(8) 0.0426(3) Uani 1 1 d . . . H2L1 H -0.1969 0.4528 0.4898 0.051 Uiso 1 1 calc R . . H2L2 H -0.1072 0.5190 0.5506 0.051 Uiso 1 1 calc R . . C3L C -0.18506(9) 0.4762(2) 0.60484(9) 0.0440(3) Uani 1 1 d . . . H3L1 H -0.2095 0.5921 0.5958 0.053 Uiso 1 1 calc R . . H3L2 H -0.2288 0.3929 0.5991 0.053 Uiso 1 1 calc R . . C4L C -0.14550(8) 0.51860(17) 0.74367(9) 0.0368(3) Uani 1 1 d . . . H4L1 H -0.1976 0.4597 0.7347 0.044 Uiso 1 1 calc R . . H4L2 H -0.1556 0.6434 0.7402 0.044 Uiso 1 1 calc R . . C5L C -0.07784(8) 0.47230(15) 0.82541(8) 0.0336(2) Uani 1 1 d . . . H5L1 H -0.0245 0.5189 0.8307 0.040 Uiso 1 1 calc R . . H5L2 H -0.0906 0.5264 0.8666 0.040 Uiso 1 1 calc R . . C6L C -0.12980(9) 0.21843(19) 0.86433(9) 0.0380(3) Uani 1 1 d . . . H6L1 H -0.1218 0.0947 0.8721 0.057 Uiso 1 1 calc R . . H6L2 H -0.1858 0.2417 0.8238 0.057 Uiso 1 1 calc R . . H6L3 H -0.1220 0.2726 0.9142 0.057 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 Te1 0.02195(5) 0.01693(4) 0.02528(5) 0.000 0.01203(4) 0.000 N1 0.0354(6) 0.0622(8) 0.0394(6) -0.0005(5) 0.0142(5) -0.0176(6) N2 0.0660(9) 0.0285(5) 0.0428(6) 0.0045(4) 0.0286(6) -0.0024(5) C1 0.0317(6) 0.0303(5) 0.0302(5) -0.0017(4) 0.0145(5) -0.0074(5) C2 0.0368(6) 0.0221(5) 0.0329(6) -0.0002(4) 0.0180(5) -0.0007(4) O1L 0.0401(5) 0.0464(5) 0.0356(5) 0.0090(4) 0.0190(4) 0.0014(4) O2L 0.0251(4) 0.0358(4) 0.0339(4) 0.0055(3) 0.0110(3) 0.0054(3) O3L 0.0257(4) 0.0302(4) 0.0298(4) -0.0019(3) 0.0142(3) 0.0012(3) C1L 0.0465(8) 0.0645(9) 0.0294(6) 0.0037(6) 0.0163(6) -0.0015(7) C2L 0.0401(7) 0.0457(7) 0.0316(6) 0.0107(5) 0.0058(5) -0.0007(6) C3L 0.0300(7) 0.0494(8) 0.0418(7) 0.0092(6) 0.0053(6) 0.0100(6) C4L 0.0324(6) 0.0317(6) 0.0500(7) 0.0026(5) 0.0213(6) 0.0100(5) C5L 0.0362(6) 0.0285(5) 0.0383(6) -0.0090(4) 0.0182(5) -0.0007(4) C6L 0.0362(7) 0.0446(7) 0.0424(7) 0.0005(5) 0.0256(6) 0.0003(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 Te1 C2 2.1007(13) 2_556 ? Te1 C2 2.1007(13) . ? Te1 C1 2.2748(14) . ? Te1 C1 2.2748(14) 2_556 ? Te1 O3L 2.6707(9) . ? Te1 O2L 3.1196(16) . ? Te1 O1L 3.4224(12) . ? N1 C1 1.1380(17) . ? N2 C2 1.1397(16) . ? O1L C1L 1.4195(17) . ? O1L C2L 1.420(2) . ? O2L C3L 1.4251(16) . ? O2L C4L 1.4289(16) . ? O3L C6L 1.4288(15) . ? O3L C5L 1.4351(17) . ? C2L C3L 1.495(2) . ? C4L C5L 1.4993(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 C2 Te1 C2 90.93(7) 2_556 . ? C2 Te1 C1 79.32(5) 2_556 . ? C2 Te1 C1 80.28(5) . . ? C2 Te1 C1 80.28(5) 2_556 2_556 ? C2 Te1 C1 79.32(5) . 2_556 ? C1 Te1 C1 150.74(7) . 2_556 ? C2 Te1 O3L 148.49(4) 2_556 . ? C2 Te1 O3L 74.36(5) . . ? C1 Te1 O3L 70.92(4) . . ? C1 Te1 O3L 122.47(4) 2_556 . ? C2 Te1 O2L 117.67(5) 2_556 . ? C2 Te1 O2L 130.41(4) . . ? C1 Te1 O2L 67.85(5) . . ? C1 Te1 O2L 141.05(4) 2_556 . ? O3L Te1 O2L 60.04(3) . . ? C2 Te1 O1L 67.37(5) 2_556 . ? C2 Te1 O1L 140.14(4) . . ? C1 Te1 O1L 63.57(3) . . ? C1 Te1 O1L 125.66(3) 2_556 . ? O3L Te1 O1L 106.57(3) . . ? O2L Te1 O1L 50.86(2) . . ? N1 C1 Te1 176.81(11) . . ? N2 C2 Te1 177.69(12) . . ? C1L O1L C2L 110.50(11) . . ? C1L O1L Te1 117.24(8) . . ? C2L O1L Te1 115.14(7) . . ? C3L O2L C4L 111.29(10) . . ? C3L O2L Te1 123.97(8) . . ? C4L O2L Te1 108.61(7) . . ? C6L O3L C5L 112.93(9) . . ? C6L O3L Te1 130.34(8) . . ? C5L O3L Te1 110.08(7) . . ? O1L C2L C3L 109.42(11) . . ? O2L C3L C2L 109.82(11) . . ? O2L C4L C5L 108.24(10) . . ? O3L C5L C4L 112.42(10) . . ? 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 C2 Te1 C1 N1 153(2) 2_556 . . . ? C2 Te1 C1 N1 60(2) . . . . ? C1 Te1 C1 N1 106(2) 2_556 . . . ? O3L Te1 C1 N1 -17(2) . . . . ? O2L Te1 C1 N1 -81(2) . . . . ? O1L Te1 C1 N1 -137(2) . . . . ? C2 Te1 C2 N2 146(3) 2_556 . . . ? C1 Te1 C2 N2 -135(3) . . . . ? C1 Te1 C2 N2 66(3) 2_556 . . . ? O3L Te1 C2 N2 -62(3) . . . . ? O2L Te1 C2 N2 -85(3) . . . . ? O1L Te1 C2 N2 -159(3) . . . . ? C2 Te1 O1L C1L -41.89(10) 2_556 . . . ? C2 Te1 O1L C1L -103.73(11) . . . . ? C1 Te1 O1L C1L -130.92(11) . . . . ? C1 Te1 O1L C1L 16.49(11) 2_556 . . . ? O3L Te1 O1L C1L 171.00(10) . . . . ? O2L Te1 O1L C1L 147.04(11) . . . . ? C2 Te1 O1L C2L -174.48(9) 2_556 . . . ? C2 Te1 O1L C2L 123.68(10) . . . . ? C1 Te1 O1L C2L 96.49(10) . . . . ? C1 Te1 O1L C2L -116.10(9) 2_556 . . . ? O3L Te1 O1L C2L 38.41(9) . . . . ? O2L Te1 O1L C2L 14.45(8) . . . . ? C2 Te1 O2L C3L 11.55(10) 2_556 . . . ? C2 Te1 O2L C3L -106.51(10) . . . . ? C1 Te1 O2L C3L -52.39(10) . . . . ? C1 Te1 O2L C3L 121.74(10) 2_556 . . . ? O3L Te1 O2L C3L -132.44(10) . . . . ? O1L Te1 O2L C3L 20.86(9) . . . . ? C2 Te1 O2L C4L 145.09(8) 2_556 . . . ? C2 Te1 O2L C4L 27.02(9) . . . . ? C1 Te1 O2L C4L 81.15(8) . . . . ? C1 Te1 O2L C4L -104.72(9) 2_556 . . . ? O3L Te1 O2L C4L 1.10(7) . . . . ? O1L Te1 O2L C4L 154.39(9) . . . . ? C2 Te1 O3L C6L 20.22(13) 2_556 . . . ? C2 Te1 O3L C6L -44.67(10) . . . . ? C1 Te1 O3L C6L 40.24(10) . . . . ? C1 Te1 O3L C6L -110.70(10) 2_556 . . . ? O2L Te1 O3L C6L 115.11(11) . . . . ? O1L Te1 O3L C6L 93.78(10) . . . . ? C2 Te1 O3L C5L -128.49(9) 2_556 . . . ? C2 Te1 O3L C5L 166.63(8) . . . . ? C1 Te1 O3L C5L -108.46(8) . . . . ? C1 Te1 O3L C5L 100.60(8) 2_556 . . . ? O2L Te1 O3L C5L -33.60(7) . . . . ? O1L Te1 O3L C5L -54.92(7) . . . . ? C1L O1L C2L C3L 179.68(12) . . . . ? Te1 O1L C2L C3L -44.66(13) . . . . ? C4L O2L C3L C2L 173.96(11) . . . . ? Te1 O2L C3L C2L -53.54(14) . . . . ? O1L C2L C3L O2L 63.04(15) . . . . ? C3L O2L C4L C5L 169.45(11) . . . . ? Te1 O2L C4L C5L 29.63(11) . . . . ? C6L O3L C5L C4L -82.48(13) . . . . ? Te1 O3L C5L C4L 72.06(10) . . . . ? O2L C4L C5L O3L -69.22(13) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.419 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.049