data_kr-tebr3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 Br3 N2 Te' _chemical_formula_sum 'C12 H9 Br3 N2 Te' _chemical_formula_weight 548.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9195(4) _cell_length_b 9.7340(5) _cell_length_c 10.4956(4) _cell_angle_alpha 113.570(4) _cell_angle_beta 93.713(3) _cell_angle_gamma 111.227(4) _cell_volume 754.78(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4846 _cell_measurement_theta_min 4.7376 _cell_measurement_theta_max 77.2339 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.5864 _exptl_crystal_size_mid 0.3707 _exptl_crystal_size_min 0.1550 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 24.730 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.008 _exptl_absorpt_correction_T_max 0.164 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5751 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.74 _diffrn_reflns_theta_max 77.45 _reflns_number_total 3144 _reflns_number_gt 3020 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.1482P)^2^+2.5886P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3144 _refine_ls_number_parameters 159 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1984 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.065 _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 Te Te 0.71390(4) 0.62608(4) 0.73878(4) 0.03742(11) Uani 1 1 d . . . Br1 Br 0.69438(10) 0.71687(12) 1.00667(9) 0.0627(2) Uani 1 1 d . A . Br2 Br 0.75429(14) 0.50510(11) 0.47462(9) 0.0679(2) Uani 1 1 d . A . Br3 Br 0.8260(2) 0.91780(14) 0.76781(15) 0.0949(4) Uani 1 1 d . A . N1 N 0.6629(14) 0.3516(14) 0.7249(13) 0.0358(12) Uani 0.530(8) 1 d PU A 1 N2 N 0.7887(13) 0.3327(13) 0.7544(12) 0.0392(13) Uani 0.530(8) 1 d PU A 1 C1 C 0.9431(8) 0.6222(9) 0.8037(9) 0.0339(18) Uani 0.530(8) 1 d PG A 1 C2 C 1.0923(10) 0.7629(9) 0.8558(12) 0.047(3) Uani 0.530(8) 1 d PG A 1 H2A H 1.0944 0.8602 0.8583 0.057 Uiso 0.530(8) 1 calc PR A 1 C3 C 1.2383(9) 0.7582(13) 0.9040(14) 0.065(5) Uani 0.530(8) 1 d PG A 1 H3A H 1.3381 0.8523 0.9388 0.078 Uiso 0.530(8) 1 calc PR A 1 C4 C 1.2352(11) 0.6127(16) 0.9002(14) 0.066(4) Uani 0.530(8) 1 d PG A 1 H4A H 1.3329 0.6096 0.9324 0.079 Uiso 0.530(8) 1 calc PR A 1 C5 C 1.0860(13) 0.4721(13) 0.8481(14) 0.059(3) Uani 0.530(8) 1 d PG A 1 H5A H 1.0839 0.3747 0.8455 0.071 Uiso 0.530(8) 1 calc PR A 1 C6 C 0.9400(10) 0.4768(9) 0.7999(11) 0.0385(16) Uani 0.530(8) 1 d PGU A 1 C7 C 0.5091(10) 0.2199(10) 0.6820(10) 0.0376(15) Uani 0.530(8) 1 d PGU A 1 C8 C 0.3665(12) 0.2378(14) 0.6474(14) 0.054(3) Uani 0.530(8) 1 d PG A 1 H8A H 0.3746 0.3387 0.6543 0.065 Uiso 0.530(8) 1 calc PR A 1 C9 C 0.2119(10) 0.1051(19) 0.6023(18) 0.080(5) Uani 0.530(8) 1 d PG A 1 H9A H 0.1165 0.1171 0.5792 0.097 Uiso 0.530(8) 1 calc PR A 1 C10 C 0.1999(14) -0.0457(16) 0.5919(17) 0.088(5) Uani 0.530(8) 1 d PG A 1 H10A H 0.0965 -0.1345 0.5618 0.105 Uiso 0.530(8) 1 calc PR A 1 C11 C 0.3425(18) -0.0636(11) 0.6265(15) 0.085(5) Uani 0.530(8) 1 d PG A 1 H11A H 0.3345 -0.1644 0.6196 0.102 Uiso 0.530(8) 1 calc PR A 1 C12 C 0.4971(15) 0.0692(12) 0.6716(12) 0.056(3) Uani 0.530(8) 1 d PG A 1 H12A H 0.5925 0.0572 0.6947 0.068 Uiso 0.530(8) 1 calc PR A 1 N1B N 0.6906(17) 0.3750(18) 0.7364(16) 0.0358(12) Uani 0.470(8) 1 d PU A 2 N2B N 0.8261(16) 0.3743(15) 0.7751(15) 0.0392(13) Uani 0.470(8) 1 d PU A 2 C1B C 0.9568(11) 0.6646(12) 0.8113(11) 0.0339(18) Uani 0.470(8) 1 d PG A 2 C2B C 1.1008(13) 0.8096(12) 0.8588(15) 0.047(3) Uani 0.470(8) 1 d PG A 2 H2BA H 1.0958 0.9026 0.8569 0.057 Uiso 0.470(8) 1 calc PR A 2 C3B C 1.2522(11) 0.8157(16) 0.9092(17) 0.065(5) Uani 0.470(8) 1 d PG A 2 H3BA H 1.3486 0.9127 0.9409 0.078 Uiso 0.470(8) 1 calc PR A 2 C4B C 1.2597(12) 0.677(2) 0.9121(17) 0.066(4) Uani 0.470(8) 1 d PG A 2 H4BA H 1.3610 0.6808 0.9458 0.079 Uiso 0.470(8) 1 calc PR A 2 C5B C 1.1157(16) 0.5317(17) 0.8646(17) 0.059(3) Uani 0.470(8) 1 d PG A 2 H5BA H 1.1206 0.4388 0.8665 0.071 Uiso 0.470(8) 1 calc PR A 2 C6B C 0.9642(13) 0.5257(12) 0.8142(13) 0.0385(16) Uani 0.470(8) 1 d PGU A 2 C7B C 0.5469(13) 0.2300(13) 0.6918(12) 0.0376(15) Uani 0.470(8) 1 d PGU A 2 C8B C 0.4024(16) 0.2280(18) 0.6311(17) 0.054(3) Uani 0.470(8) 1 d PG A 2 H8BA H 0.4063 0.3185 0.6187 0.065 Uiso 0.470(8) 1 calc PR A 2 C9B C 0.2521(13) 0.091(2) 0.589(2) 0.080(5) Uani 0.470(8) 1 d PG A 2 H9BA H 0.1554 0.0895 0.5485 0.097 Uiso 0.470(8) 1 calc PR A 2 C10B C 0.2462(18) -0.045(2) 0.608(2) 0.088(5) Uani 0.470(8) 1 d PG A 2 H10B H 0.1456 -0.1363 0.5796 0.105 Uiso 0.470(8) 1 calc PR A 2 C11B C 0.391(2) -0.0425(14) 0.6683(18) 0.085(5) Uani 0.470(8) 1 d PG A 2 H11B H 0.3868 -0.1331 0.6808 0.102 Uiso 0.470(8) 1 calc PR A 2 C12B C 0.5410(18) 0.0947(15) 0.7104(15) 0.056(3) Uani 0.470(8) 1 d PG A 2 H12B H 0.6377 0.0960 0.7509 0.068 Uiso 0.470(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te 0.04025(19) 0.03624(17) 0.03950(19) 0.01883(14) 0.00764(14) 0.01865(14) Br1 0.0581(4) 0.0798(5) 0.0565(4) 0.0312(3) 0.0238(3) 0.0340(3) Br2 0.1039(6) 0.0628(4) 0.0488(4) 0.0276(3) 0.0205(4) 0.0447(4) Br3 0.1307(10) 0.0600(5) 0.0969(7) 0.0393(5) 0.0328(7) 0.0383(6) N1 0.036(2) 0.0361(19) 0.0356(19) 0.0185(15) 0.0076(17) 0.0141(16) N2 0.039(2) 0.039(2) 0.041(2) 0.0180(17) 0.0067(18) 0.0186(18) C1 0.033(3) 0.026(4) 0.039(3) 0.014(3) 0.008(2) 0.009(3) C2 0.043(3) 0.031(6) 0.049(4) 0.014(4) 0.012(3) 0.001(4) C3 0.038(4) 0.074(11) 0.054(4) 0.024(6) 0.014(3) -0.001(5) C4 0.038(4) 0.100(11) 0.063(5) 0.036(6) 0.015(3) 0.033(5) C5 0.058(4) 0.086(7) 0.063(4) 0.044(5) 0.020(3) 0.049(4) C6 0.038(2) 0.039(3) 0.040(2) 0.018(2) 0.0091(18) 0.018(2) C7 0.038(3) 0.039(2) 0.035(2) 0.0186(16) 0.012(2) 0.0139(18) C8 0.032(5) 0.059(4) 0.066(5) 0.035(4) 0.010(4) 0.008(4) C9 0.051(7) 0.076(6) 0.087(7) 0.040(5) 0.010(6) -0.003(6) C10 0.100(11) 0.056(5) 0.068(6) 0.028(4) 0.026(7) -0.007(6) C11 0.136(12) 0.038(4) 0.046(7) 0.010(4) 0.038(7) 0.007(6) C12 0.086(7) 0.038(3) 0.053(5) 0.024(3) 0.023(5) 0.029(4) N1B 0.036(2) 0.0361(19) 0.0356(19) 0.0185(15) 0.0076(17) 0.0141(16) N2B 0.039(2) 0.039(2) 0.041(2) 0.0180(17) 0.0067(18) 0.0186(18) C1B 0.033(3) 0.026(4) 0.039(3) 0.014(3) 0.008(2) 0.009(3) C2B 0.043(3) 0.031(6) 0.049(4) 0.014(4) 0.012(3) 0.001(4) C3B 0.038(4) 0.074(11) 0.054(4) 0.024(6) 0.014(3) -0.001(5) C4B 0.038(4) 0.100(11) 0.063(5) 0.036(6) 0.015(3) 0.033(5) C5B 0.058(4) 0.086(7) 0.063(4) 0.044(5) 0.020(3) 0.049(4) C6B 0.038(2) 0.039(3) 0.040(2) 0.018(2) 0.0091(18) 0.018(2) C7B 0.038(3) 0.039(2) 0.035(2) 0.0186(16) 0.012(2) 0.0139(18) C8B 0.032(5) 0.059(4) 0.066(5) 0.035(4) 0.010(4) 0.008(4) C9B 0.051(7) 0.076(6) 0.087(7) 0.040(5) 0.010(6) -0.003(6) C10B 0.100(11) 0.056(5) 0.068(6) 0.028(4) 0.026(7) -0.007(6) C11B 0.136(12) 0.038(4) 0.046(7) 0.010(4) 0.038(7) 0.007(6) C12B 0.086(7) 0.038(3) 0.053(5) 0.024(3) 0.023(5) 0.029(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 Te C1B 2.094(9) . ? Te C1 2.131(8) . ? Te N1B 2.366(17) . ? Te N1 2.483(14) . ? Te Br3 2.5236(13) . ? Te Br1 2.6277(9) . ? Te Br2 2.6512(10) . ? N1 N2 1.241(19) . ? N1 C7 1.383(12) . ? N2 C6 1.423(12) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 H5A 0.9300 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? N1B N2B 1.25(2) . ? N1B C7B 1.393(15) . ? N2B C6B 1.412(14) . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C2B H2BA 0.9300 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B H5BA 0.9300 . ? C7B C8B 1.3900 . ? C7B C12B 1.3900 . ? C8B C9B 1.3900 . ? C8B H8BA 0.9300 . ? C9B C10B 1.3900 . ? C9B H9BA 0.9300 . ? C10B C11B 1.3900 . ? C10B H10B 0.9300 . ? C11B C12B 1.3900 . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? 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 C1B Te C1 9.6(4) . . ? C1B Te N1B 74.5(4) . . ? C1 Te N1B 65.0(4) . . ? C1B Te N1 79.6(4) . . ? C1 Te N1 70.0(3) . . ? N1B Te N1 5.1(5) . . ? C1B Te Br3 88.9(3) . . ? C1 Te Br3 98.5(2) . . ? N1B Te Br3 163.5(3) . . ? N1 Te Br3 168.5(3) . . ? C1B Te Br1 86.4(3) . . ? C1 Te Br1 86.9(2) . . ? N1B Te Br1 85.3(4) . . ? N1 Te Br1 86.3(3) . . ? Br3 Te Br1 93.69(4) . . ? C1B Te Br2 87.4(3) . . ? C1 Te Br2 86.0(2) . . ? N1B Te Br2 86.9(4) . . ? N1 Te Br2 86.2(3) . . ? Br3 Te Br2 92.65(4) . . ? Br1 Te Br2 171.04(4) . . ? N2 N1 C7 118.9(12) . . ? N2 N1 Te 115.6(8) . . ? C7 N1 Te 125.5(10) . . ? N1 N2 C6 114.2(11) . . ? C2 C1 C6 120.0 . . ? C2 C1 Te 121.5(4) . . ? C6 C1 Te 118.4(4) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 N2 118.2(8) . . ? C1 C6 N2 121.7(8) . . ? N1 C7 C8 119.8(9) . . ? N1 C7 C12 120.2(9) . . ? C8 C7 C12 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? N2B N1B C7B 117.9(16) . . ? N2B N1B Te 114.5(10) . . ? C7B N1B Te 127.5(11) . . ? N1B N2B C6B 113.4(14) . . ? C2B C1B C6B 120.0 . . ? C2B C1B Te 127.5(5) . . ? C6B C1B Te 112.4(5) . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2BA 120.0 . . ? C3B C2B H2BA 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3BA 120.0 . . ? C4B C3B H3BA 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4BA 120.0 . . ? C3B C4B H4BA 120.0 . . ? C4B C5B C6B 120.0 . . ? C4B C5B H5BA 120.0 . . ? C6B C5B H5BA 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B N2B 114.8(9) . . ? C1B C6B N2B 125.2(9) . . ? C8B C7B C12B 120.0 . . ? C8B C7B N1B 116.2(11) . . ? C12B C7B N1B 123.7(11) . . ? C7B C8B C9B 120.0 . . ? C7B C8B H8BA 120.0 . . ? C9B C8B H8BA 120.0 . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9BA 120.0 . . ? C8B C9B H9BA 120.0 . . ? C9B C10B C11B 120.0 . . ? C9B C10B H10B 120.0 . . ? C11B C10B H10B 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C7B 120.0 . . ? C11B C12B H12B 120.0 . . ? C7B C12B H12B 120.0 . . ? 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 C1B Te N1 N2 -4.0(10) . . . . ? C1 Te N1 N2 -3.0(9) . . . . ? N1B Te N1 N2 -13(6) . . . . ? Br3 Te N1 N2 -1(2) . . . . ? Br1 Te N1 N2 -91.0(10) . . . . ? Br2 Te N1 N2 84.0(10) . . . . ? C1B Te N1 C7 178.8(11) . . . . ? C1 Te N1 C7 179.8(11) . . . . ? N1B Te N1 C7 170(8) . . . . ? Br3 Te N1 C7 -177.9(8) . . . . ? Br1 Te N1 C7 91.8(10) . . . . ? Br2 Te N1 C7 -93.1(10) . . . . ? C7 N1 N2 C6 -178.9(11) . . . . ? Te N1 N2 C6 3.8(14) . . . . ? C1B Te C1 C2 -1(3) . . . . ? N1B Te C1 C2 -174.4(7) . . . . ? N1 Te C1 C2 -175.3(6) . . . . ? Br3 Te C1 C2 5.1(5) . . . . ? Br1 Te C1 C2 -88.1(4) . . . . ? Br2 Te C1 C2 97.2(4) . . . . ? C1B Te C1 C6 176(3) . . . . ? N1B Te C1 C6 2.4(6) . . . . ? N1 Te C1 C6 1.5(5) . . . . ? Br3 Te C1 C6 -178.1(4) . . . . ? Br1 Te C1 C6 88.7(5) . . . . ? Br2 Te C1 C6 -86.0(5) . . . . ? C6 C1 C2 C3 0.0 . . . . ? Te C1 C2 C3 176.7(5) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C4 C5 C6 N2 -176.8(10) . . . . ? C2 C1 C6 C5 0.0 . . . . ? Te C1 C6 C5 -176.8(5) . . . . ? C2 C1 C6 N2 176.7(10) . . . . ? Te C1 C6 N2 -0.2(10) . . . . ? N1 N2 C6 C5 174.0(9) . . . . ? N1 N2 C6 C1 -2.7(15) . . . . ? N2 N1 C7 C8 -179.5(11) . . . . ? Te N1 C7 C8 -2.5(13) . . . . ? N2 N1 C7 C12 -0.4(16) . . . . ? Te N1 C7 C12 176.7(6) . . . . ? N1 C7 C8 C9 179.1(10) . . . . ? C12 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C7 0.0 . . . . ? N1 C7 C12 C11 -179.1(10) . . . . ? C8 C7 C12 C11 0.0 . . . . ? C1B Te N1B N2B -1.0(12) . . . . ? C1 Te N1B N2B 0.2(11) . . . . ? N1 Te N1B N2B 170(8) . . . . ? Br3 Te N1B N2B -2(2) . . . . ? Br1 Te N1B N2B -88.6(12) . . . . ? Br2 Te N1B N2B 87.2(13) . . . . ? C1B Te N1B C7B -178.0(14) . . . . ? C1 Te N1B C7B -176.8(15) . . . . ? N1 Te N1B C7B -7(6) . . . . ? Br3 Te N1B C7B -178.5(7) . . . . ? Br1 Te N1B C7B 94.4(13) . . . . ? Br2 Te N1B C7B -89.8(13) . . . . ? C7B N1B N2B C6B 178.2(12) . . . . ? Te N1B N2B C6B 0.9(18) . . . . ? C1 Te C1B C2B 177(3) . . . . ? N1B Te C1B C2B -176.7(8) . . . . ? N1 Te C1B C2B -177.5(7) . . . . ? Br3 Te C1B C2B 3.2(6) . . . . ? Br1 Te C1B C2B -90.6(6) . . . . ? Br2 Te C1B C2B 95.9(6) . . . . ? C1 Te C1B C6B -6(3) . . . . ? N1B Te C1B C6B 0.8(6) . . . . ? N1 Te C1B C6B 0.0(6) . . . . ? Br3 Te C1B C6B -179.3(5) . . . . ? Br1 Te C1B C6B 86.9(5) . . . . ? Br2 Te C1B C6B -86.6(5) . . . . ? C6B C1B C2B C3B 0.0 . . . . ? Te C1B C2B C3B 177.3(8) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C1B 0.0 . . . . ? C4B C5B C6B N2B -177.3(11) . . . . ? C2B C1B C6B C5B 0.0 . . . . ? Te C1B C6B C5B -177.7(7) . . . . ? C2B C1B C6B N2B 177.0(13) . . . . ? Te C1B C6B N2B -0.7(12) . . . . ? N1B N2B C6B C5B 176.9(12) . . . . ? N1B N2B C6B C1B -0.2(19) . . . . ? N2B N1B C7B C8B -171.4(14) . . . . ? Te N1B C7B C8B 5.5(16) . . . . ? N2B N1B C7B C12B 11(2) . . . . ? Te N1B C7B C12B -171.7(8) . . . . ? C12B C7B C8B C9B 0.0 . . . . ? N1B C7B C8B C9B -177.3(12) . . . . ? C7B C8B C9B C10B 0.0 . . . . ? C8B C9B C10B C11B 0.0 . . . . ? C9B C10B C11B C12B 0.0 . . . . ? C10B C11B C12B C7B 0.0 . . . . ? C8B C7B C12B C11B 0.0 . . . . ? N1B C7B C12B C11B 177.1(13) . . . . ? 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 C4 H4A Br1 0.93 2.95 3.814(8) 155.9 1_655 C8 H8A Br2 0.93 2.86 3.660(12) 145.0 2_666 C11 H11A Br2 0.93 2.82 3.727(10) 163.9 2_656 C4B H4BA Br1 0.93 2.86 3.777(9) 168.1 1_655 C12B H12B Br3 0.93 2.86 3.686(14) 148.7 1_545 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.845 _refine_diff_density_min -2.310 _refine_diff_density_rms 0.271 #===END data_kr-azote _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N4 Te' _chemical_formula_sum 'C24 H18 N4 Te' _chemical_formula_weight 490.02 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' '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 6.53650(10) _cell_length_b 14.2249(3) _cell_length_c 21.7793(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.7370(17) _cell_angle_gamma 90.00 _cell_volume 2024.13(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 12252 _cell_measurement_theta_min 4.5858 _cell_measurement_theta_max 34.6792 _exptl_crystal_description needle _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83383 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 23174 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 34.75 _reflns_number_total 8223 _reflns_number_gt 6366 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0301P)^2^+0.5979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8223 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _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 Te Te 0.325185(15) 0.672692(8) 0.012234(4) 0.02560(4) Uani 1 1 d . . . N1A N 0.3406(2) 0.65933(10) 0.16471(6) 0.0248(3) Uani 1 1 d . . . N2A N 0.21459(19) 0.63187(10) 0.12361(6) 0.0218(2) Uani 1 1 d . . . N1B N 0.2577(2) 0.82482(11) -0.09504(6) 0.0264(3) Uani 1 1 d . . . N2B N 0.1773(2) 0.86899(12) -0.13871(7) 0.0283(3) Uani 1 1 d . . . C1A C 0.5342(2) 0.72632(11) 0.07829(7) 0.0212(3) Uani 1 1 d . . . C2A C 0.7062(2) 0.77788(12) 0.06181(8) 0.0259(3) Uani 1 1 d . . . H2AA H 0.7288 0.7898 0.0196 0.031 Uiso 1 1 calc R . . C3A C 0.8440(3) 0.81186(13) 0.10583(9) 0.0308(4) Uani 1 1 d . . . H3AA H 0.9596 0.8468 0.0935 0.037 Uiso 1 1 calc R . . C4A C 0.8152(3) 0.79539(14) 0.16783(9) 0.0322(4) Uani 1 1 d . . . H4AA H 0.9106 0.8189 0.1978 0.039 Uiso 1 1 calc R . . C5A C 0.6467(3) 0.74449(14) 0.18560(8) 0.0297(3) Uani 1 1 d . . . H5AA H 0.6269 0.7323 0.2279 0.036 Uiso 1 1 calc R . . C6A C 0.5053(2) 0.71094(12) 0.14126(7) 0.0225(3) Uani 1 1 d . . . C7A C 0.0479(2) 0.57693(11) 0.14407(7) 0.0207(3) Uani 1 1 d . . . C8A C 0.0309(2) 0.54610(13) 0.20430(7) 0.0263(3) Uani 1 1 d . . . H8AA H 0.1340 0.5613 0.2344 0.032 Uiso 1 1 calc R . . C9A C -0.1372(3) 0.49318(14) 0.22016(8) 0.0316(4) Uani 1 1 d . . . H9AA H -0.1489 0.4715 0.2612 0.038 Uiso 1 1 calc R . . C10A C -0.2887(3) 0.47159(13) 0.17636(9) 0.0307(3) Uani 1 1 d . . . H10A H -0.4041 0.4355 0.1875 0.037 Uiso 1 1 calc R . . C11A C -0.2721(2) 0.50256(13) 0.11657(8) 0.0280(3) Uani 1 1 d . . . H11A H -0.3765 0.4881 0.0868 0.034 Uiso 1 1 calc R . . C12A C -0.1032(2) 0.55481(12) 0.09995(7) 0.0254(3) Uani 1 1 d . . . H12A H -0.0907 0.5754 0.0587 0.031 Uiso 1 1 calc R . . C1B C 0.5082(2) 0.70824(12) -0.06546(7) 0.0226(3) Uani 1 1 d . . . C2B C 0.6871(3) 0.65828(13) -0.07688(8) 0.0283(3) Uani 1 1 d . . . H2BA H 0.7380 0.6141 -0.0475 0.034 Uiso 1 1 calc R . . C3B C 0.7913(3) 0.67250(14) -0.13078(9) 0.0311(3) Uani 1 1 d . . . H3BA H 0.9147 0.6393 -0.1376 0.037 Uiso 1 1 calc R . . C4B C 0.7154(3) 0.73506(14) -0.17450(8) 0.0315(4) Uani 1 1 d . . . H4BA H 0.7863 0.7442 -0.2115 0.038 Uiso 1 1 calc R . . C5B C 0.5378(3) 0.78416(13) -0.16474(8) 0.0279(3) Uani 1 1 d . . . H5BA H 0.4849 0.8262 -0.1952 0.033 Uiso 1 1 calc R . . C6B C 0.4351(2) 0.77185(11) -0.10968(7) 0.0220(3) Uani 1 1 d . . . C7B C 0.0037(2) 0.92389(12) -0.12234(8) 0.0256(3) Uani 1 1 d . . . C8B C -0.0821(3) 0.97880(14) -0.16898(9) 0.0314(4) Uani 1 1 d . . . H8BA H -0.0258 0.9782 -0.2087 0.038 Uiso 1 1 calc R . . C9B C -0.2509(3) 1.03471(14) -0.15729(10) 0.0365(4) Uani 1 1 d . . . H9BA H -0.3082 1.0738 -0.1887 0.044 Uiso 1 1 calc R . . C10B C -0.3347(3) 1.03348(15) -0.10031(11) 0.0420(5) Uani 1 1 d . . . H10B H -0.4523 1.0705 -0.0927 0.050 Uiso 1 1 calc R . . C11B C -0.2482(3) 0.97828(17) -0.05356(11) 0.0440(5) Uani 1 1 d . . . H11B H -0.3062 0.9783 -0.0141 0.053 Uiso 1 1 calc R . . C12B C -0.0785(3) 0.92358(15) -0.06422(9) 0.0346(4) Uani 1 1 d . . . H12B H -0.0188 0.8862 -0.0323 0.041 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 Te 0.02502(5) 0.03328(6) 0.01852(5) 0.00370(5) 0.00117(3) -0.00376(4) N1A 0.0252(6) 0.0298(7) 0.0197(6) -0.0019(5) 0.0041(5) -0.0021(5) N2A 0.0244(6) 0.0222(6) 0.0191(5) 0.0007(5) 0.0029(4) -0.0011(5) N1B 0.0271(6) 0.0283(7) 0.0242(6) 0.0045(6) 0.0050(5) 0.0043(6) N2B 0.0251(6) 0.0342(8) 0.0256(6) 0.0029(6) 0.0015(5) 0.0040(6) C1A 0.0237(7) 0.0179(6) 0.0221(6) -0.0002(6) 0.0031(5) 0.0020(5) C2A 0.0293(7) 0.0230(7) 0.0257(7) 0.0017(6) 0.0066(6) -0.0021(6) C3A 0.0291(8) 0.0278(9) 0.0359(9) -0.0041(7) 0.0064(7) -0.0067(6) C4A 0.0296(8) 0.0359(9) 0.0310(8) -0.0097(8) 0.0000(6) -0.0054(7) C5A 0.0316(8) 0.0355(9) 0.0221(7) -0.0060(7) 0.0033(6) -0.0028(7) C6A 0.0231(7) 0.0228(7) 0.0217(6) -0.0025(6) 0.0035(5) -0.0006(6) C7A 0.0232(6) 0.0206(7) 0.0186(6) -0.0010(5) 0.0032(5) 0.0008(5) C8A 0.0279(7) 0.0320(8) 0.0193(6) -0.0002(6) 0.0027(5) -0.0037(6) C9A 0.0333(8) 0.0374(10) 0.0244(7) 0.0058(7) 0.0072(6) -0.0049(7) C10A 0.0280(8) 0.0288(8) 0.0357(9) -0.0018(7) 0.0078(6) -0.0051(7) C11A 0.0259(7) 0.0276(8) 0.0302(8) -0.0032(7) -0.0006(6) -0.0012(6) C12A 0.0283(7) 0.0275(8) 0.0205(6) 0.0002(6) 0.0001(6) 0.0003(6) C1B 0.0247(7) 0.0253(7) 0.0179(6) 0.0007(6) 0.0027(5) -0.0012(6) C2B 0.0273(7) 0.0301(9) 0.0276(7) 0.0024(7) 0.0013(6) 0.0040(6) C3B 0.0261(7) 0.0316(8) 0.0362(9) -0.0044(8) 0.0085(6) 0.0016(7) C4B 0.0322(8) 0.0350(9) 0.0281(8) -0.0003(7) 0.0122(7) -0.0029(7) C5B 0.0307(8) 0.0302(9) 0.0231(7) 0.0037(7) 0.0049(6) -0.0001(7) C6B 0.0237(7) 0.0229(7) 0.0195(6) 0.0007(6) 0.0030(5) -0.0017(6) C7B 0.0226(7) 0.0252(8) 0.0291(8) 0.0006(6) 0.0003(6) -0.0008(6) C8B 0.0291(8) 0.0324(9) 0.0325(8) 0.0025(8) -0.0045(6) 0.0006(7) C9B 0.0314(8) 0.0289(9) 0.0486(11) 0.0002(8) -0.0104(8) 0.0034(7) C10B 0.0297(9) 0.0332(10) 0.0631(14) -0.0092(10) 0.0011(9) 0.0069(8) C11B 0.0390(10) 0.0465(12) 0.0474(11) -0.0017(10) 0.0150(9) 0.0090(9) C12B 0.0327(8) 0.0378(10) 0.0336(9) 0.0053(8) 0.0070(7) 0.0052(7) _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 Te C1A 2.0973(16) . ? Te C1B 2.1616(15) . ? N1A N2A 1.2601(19) . ? N1A C6A 1.411(2) . ? N2A C7A 1.423(2) . ? N1B N2B 1.243(2) . ? N1B C6B 1.427(2) . ? N2B C7B 1.431(2) . ? C1A C2A 1.399(2) . ? C1A C6A 1.407(2) . ? C2A C3A 1.383(3) . ? C2A H2AA 0.9500 . ? C3A C4A 1.389(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.383(3) . ? C4A H4AA 0.9500 . ? C5A C6A 1.400(2) . ? C5A H5AA 0.9500 . ? C7A C8A 1.391(2) . ? C7A C12A 1.393(2) . ? C8A C9A 1.384(2) . ? C8A H8AA 0.9500 . ? C9A C10A 1.389(3) . ? C9A H9AA 0.9500 . ? C10A C11A 1.382(2) . ? C10A H10A 0.9500 . ? C11A C12A 1.388(2) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C6B 1.395(2) . ? C1B C2B 1.397(2) . ? C2B C3B 1.390(2) . ? C2B H2BA 0.9500 . ? C3B C4B 1.384(3) . ? C3B H3BA 0.9500 . ? C4B C5B 1.377(2) . ? C4B H4BA 0.9500 . ? C5B C6B 1.403(2) . ? C5B H5BA 0.9500 . ? C7B C8B 1.386(2) . ? C7B C12B 1.390(2) . ? C8B C9B 1.390(3) . ? C8B H8BA 0.9500 . ? C9B C10B 1.372(3) . ? C9B H9BA 0.9500 . ? C10B C11B 1.392(3) . ? C10B H10B 0.9500 . ? C11B C12B 1.380(3) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Te C1B 95.02(6) . . ? N2A N1A C6A 113.19(13) . . ? N1A N2A C7A 115.99(13) . . ? N2B N1B C6B 115.05(13) . . ? N1B N2B C7B 113.90(14) . . ? C2A C1A C6A 117.67(14) . . ? C2A C1A Te 121.78(11) . . ? C6A C1A Te 120.54(11) . . ? C3A C2A C1A 121.15(15) . . ? C3A C2A H2AA 119.4 . . ? C1A C2A H2AA 119.4 . . ? C2A C3A C4A 120.71(16) . . ? C2A C3A H3AA 119.6 . . ? C4A C3A H3AA 119.6 . . ? C5A C4A C3A 119.52(16) . . ? C5A C4A H4AA 120.2 . . ? C3A C4A H4AA 120.2 . . ? C4A C5A C6A 120.00(16) . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C1A 120.93(15) . . ? C5A C6A N1A 114.99(14) . . ? C1A C6A N1A 124.05(14) . . ? C8A C7A C12A 120.28(14) . . ? C8A C7A N2A 123.51(14) . . ? C12A C7A N2A 116.21(13) . . ? C9A C8A C7A 119.56(15) . . ? C9A C8A H8AA 120.2 . . ? C7A C8A H8AA 120.2 . . ? C8A C9A C10A 120.27(16) . . ? C8A C9A H9AA 119.9 . . ? C10A C9A H9AA 119.9 . . ? C11A C10A C9A 120.11(15) . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C10A C11A C12A 120.15(15) . . ? C10A C11A H11A 119.9 . . ? C12A C11A H11A 119.9 . . ? C11A C12A C7A 119.61(15) . . ? C11A C12A H12A 120.2 . . ? C7A C12A H12A 120.2 . . ? C6B C1B C2B 118.54(14) . . ? C6B C1B Te 120.40(11) . . ? C2B C1B Te 120.43(12) . . ? C3B C2B C1B 120.72(16) . . ? C3B C2B H2BA 119.6 . . ? C1B C2B H2BA 119.6 . . ? C4B C3B C2B 119.98(16) . . ? C4B C3B H3BA 120.0 . . ? C2B C3B H3BA 120.0 . . ? C5B C4B C3B 120.42(15) . . ? C5B C4B H4BA 119.8 . . ? C3B C4B H4BA 119.8 . . ? C4B C5B C6B 119.74(16) . . ? C4B C5B H5BA 120.1 . . ? C6B C5B H5BA 120.1 . . ? C1B C6B C5B 120.57(15) . . ? C1B C6B N1B 116.85(13) . . ? C5B C6B N1B 122.55(15) . . ? C8B C7B C12B 120.66(16) . . ? C8B C7B N2B 115.54(15) . . ? C12B C7B N2B 123.80(16) . . ? C7B C8B C9B 119.60(18) . . ? C7B C8B H8BA 120.2 . . ? C9B C8B H8BA 120.2 . . ? C10B C9B C8B 119.96(19) . . ? C10B C9B H9BA 120.0 . . ? C8B C9B H9BA 120.0 . . ? C9B C10B C11B 120.28(18) . . ? C9B C10B H10B 119.9 . . ? C11B C10B H10B 119.9 . . ? C12B C11B C10B 120.37(19) . . ? C12B C11B H11B 119.8 . . ? C10B C11B H11B 119.8 . . ? C11B C12B C7B 119.10(18) . . ? C11B C12B H12B 120.4 . . ? C7B C12B H12B 120.4 . . ? 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 C6A N1A N2A C7A 178.19(13) . . . . ? C6B N1B N2B C7B -178.08(14) . . . . ? C1B Te C1A C2A 8.22(14) . . . . ? C1B Te C1A C6A -171.54(13) . . . . ? C6A C1A C2A C3A 0.5(2) . . . . ? Te C1A C2A C3A -179.22(13) . . . . ? C1A C2A C3A C4A 0.1(3) . . . . ? C2A C3A C4A C5A 0.0(3) . . . . ? C3A C4A C5A C6A -0.8(3) . . . . ? C4A C5A C6A C1A 1.5(3) . . . . ? C4A C5A C6A N1A 179.49(16) . . . . ? C2A C1A C6A C5A -1.4(2) . . . . ? Te C1A C6A C5A 178.41(13) . . . . ? C2A C1A C6A N1A -179.17(15) . . . . ? Te C1A C6A N1A 0.6(2) . . . . ? N2A N1A C6A C5A 178.70(15) . . . . ? N2A N1A C6A C1A -3.4(2) . . . . ? N1A N2A C7A C8A -6.3(2) . . . . ? N1A N2A C7A C12A 173.44(14) . . . . ? C12A C7A C8A C9A 0.0(3) . . . . ? N2A C7A C8A C9A 179.77(16) . . . . ? C7A C8A C9A C10A -0.5(3) . . . . ? C8A C9A C10A C11A 0.3(3) . . . . ? C9A C10A C11A C12A 0.5(3) . . . . ? C10A C11A C12A C7A -0.9(3) . . . . ? C8A C7A C12A C11A 0.7(2) . . . . ? N2A C7A C12A C11A -179.09(15) . . . . ? C1A Te C1B C6B -117.41(13) . . . . ? C1A Te C1B C2B 71.80(14) . . . . ? C6B C1B C2B C3B 0.8(3) . . . . ? Te C1B C2B C3B 171.75(14) . . . . ? C1B C2B C3B C4B -1.6(3) . . . . ? C2B C3B C4B C5B 0.6(3) . . . . ? C3B C4B C5B C6B 1.1(3) . . . . ? C2B C1B C6B C5B 0.9(2) . . . . ? Te C1B C6B C5B -170.03(13) . . . . ? C2B C1B C6B N1B -177.05(15) . . . . ? Te C1B C6B N1B 12.0(2) . . . . ? C4B C5B C6B C1B -1.9(3) . . . . ? C4B C5B C6B N1B 175.98(16) . . . . ? N2B N1B C6B C1B -168.72(15) . . . . ? N2B N1B C6B C5B 13.3(2) . . . . ? N1B N2B C7B C8B 176.05(16) . . . . ? N1B N2B C7B C12B -4.3(3) . . . . ? C12B C7B C8B C9B 0.6(3) . . . . ? N2B C7B C8B C9B -179.82(16) . . . . ? C7B C8B C9B C10B -1.6(3) . . . . ? C8B C9B C10B C11B 1.7(3) . . . . ? C9B C10B C11B C12B -0.6(3) . . . . ? C10B C11B C12B C7B -0.4(3) . . . . ? C8B C7B C12B C11B 0.5(3) . . . . ? N2B C7B C12B C11B -179.11(18) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.474 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.081 #===END data_ups802 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 I N2 Te' _chemical_formula_sum 'C12 H9 I N2 Te' _chemical_formula_weight 435.71 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' 'I' 'I' -0.4742 1.8119 '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 9.2451(6) _cell_length_b 12.6258(10) _cell_length_c 10.7974(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.882(4) _cell_angle_gamma 90.00 _cell_volume 1241.65(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5819 _cell_measurement_theta_min 2.537 _cell_measurement_theta_max 30.435 _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 4.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22840 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 35.05 _reflns_number_total 5446 _reflns_number_gt 4751 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0199P)^2^+0.5630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5446 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _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 Te Te 0.460720(12) 0.675668(9) 0.599706(10) 0.01136(3) Uani 1 1 d . . . I I 0.280939(14) 0.604375(10) 0.781631(12) 0.01892(3) Uani 1 1 d . . . N1 N 0.53488(17) 0.65254(12) 0.33801(14) 0.0131(3) Uani 1 1 d . . . N2 N 0.58298(16) 0.69818(11) 0.44281(13) 0.0118(2) Uani 1 1 d . . . C1 C 0.34384(19) 0.59175(13) 0.45022(16) 0.0122(3) Uani 1 1 d . . . C2 C 0.21746(19) 0.53105(14) 0.44962(18) 0.0154(3) Uani 1 1 d . . . H2A H 0.1751 0.5255 0.5235 0.018 Uiso 1 1 calc R . . C3 C 0.1542(2) 0.47909(15) 0.34098(18) 0.0179(3) Uani 1 1 d . . . H3A H 0.0692 0.4369 0.3413 0.021 Uiso 1 1 calc R . . C4 C 0.2137(2) 0.48772(15) 0.23032(18) 0.0185(3) Uani 1 1 d . . . H4A H 0.1680 0.4524 0.1562 0.022 Uiso 1 1 calc R . . C5 C 0.3385(2) 0.54738(14) 0.22892(17) 0.0160(3) Uani 1 1 d . . . H5A H 0.3790 0.5534 0.1541 0.019 Uiso 1 1 calc R . . C6 C 0.40480(19) 0.59903(13) 0.33939(16) 0.0127(3) Uani 1 1 d . . . C7 C 0.72564(18) 0.74363(13) 0.45906(15) 0.0121(3) Uani 1 1 d . . . C8 C 0.8297(2) 0.70640(14) 0.39055(17) 0.0141(3) Uani 1 1 d . . . H8A H 0.8037 0.6543 0.3271 0.017 Uiso 1 1 calc R . . C9 C 0.9714(2) 0.74583(15) 0.41554(17) 0.0167(3) Uani 1 1 d . . . H9A H 1.0426 0.7215 0.3684 0.020 Uiso 1 1 calc R . . C10 C 1.0098(2) 0.82123(15) 0.50988(18) 0.0176(3) Uani 1 1 d . . . H10A H 1.1077 0.8470 0.5282 0.021 Uiso 1 1 calc R . . C11 C 0.9051(2) 0.85863(16) 0.57709(17) 0.0172(3) Uani 1 1 d . . . H11A H 0.9313 0.9104 0.6408 0.021 Uiso 1 1 calc R . . C12 C 0.7617(2) 0.82037(15) 0.55129(17) 0.0163(3) Uani 1 1 d . . . H12A H 0.6894 0.8465 0.5963 0.020 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 Te 0.01168(5) 0.01093(5) 0.01182(5) -0.00119(4) 0.00300(3) -0.00127(3) I 0.01955(6) 0.01925(6) 0.02062(6) -0.00312(4) 0.01093(5) -0.00484(4) N1 0.0157(7) 0.0111(6) 0.0121(6) 0.0004(5) 0.0012(5) 0.0005(5) N2 0.0129(6) 0.0111(6) 0.0113(6) 0.0000(5) 0.0016(5) -0.0010(5) C1 0.0122(7) 0.0094(7) 0.0143(7) -0.0007(5) 0.0005(5) 0.0007(5) C2 0.0117(7) 0.0135(8) 0.0206(8) -0.0005(6) 0.0020(6) -0.0007(6) C3 0.0137(8) 0.0139(8) 0.0245(9) -0.0009(7) -0.0013(6) -0.0012(6) C4 0.0183(8) 0.0128(8) 0.0214(8) -0.0023(6) -0.0045(7) 0.0006(6) C5 0.0187(8) 0.0137(8) 0.0143(7) -0.0010(6) -0.0014(6) 0.0010(6) C6 0.0130(7) 0.0101(7) 0.0141(7) 0.0012(6) 0.0000(6) 0.0005(5) C7 0.0116(7) 0.0122(7) 0.0126(7) 0.0018(6) 0.0026(5) -0.0008(5) C8 0.0155(7) 0.0124(7) 0.0151(7) -0.0005(6) 0.0045(6) -0.0003(6) C9 0.0164(8) 0.0160(8) 0.0192(8) 0.0018(6) 0.0072(6) 0.0013(6) C10 0.0146(8) 0.0198(9) 0.0184(8) 0.0027(7) 0.0025(6) -0.0025(6) C11 0.0157(8) 0.0209(9) 0.0147(7) -0.0023(6) 0.0017(6) -0.0056(6) C12 0.0159(8) 0.0180(8) 0.0159(7) -0.0027(6) 0.0054(6) -0.0036(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 Te C1 2.0729(17) . ? Te N2 2.2103(14) . ? Te I 2.9244(2) . ? N1 N2 1.280(2) . ? N1 C6 1.382(2) . ? N2 C7 1.421(2) . ? C1 C2 1.396(2) . ? C1 C6 1.411(2) . ? C2 C3 1.383(3) . ? C2 H2A 0.9500 . ? C3 C4 1.403(3) . ? C3 H3A 0.9500 . ? C4 C5 1.380(3) . ? C4 H4A 0.9500 . ? C5 C6 1.405(2) . ? C5 H5A 0.9500 . ? C7 C12 1.389(2) . ? C7 C8 1.392(2) . ? C8 C9 1.384(3) . ? C8 H8A 0.9500 . ? C9 C10 1.395(3) . ? C9 H9A 0.9500 . ? C10 C11 1.388(3) . ? C10 H10A 0.9500 . ? C11 C12 1.393(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te N2 74.68(6) . . ? C1 Te I 94.89(5) . . ? N2 Te I 168.17(4) . . ? N2 N1 C6 112.44(14) . . ? N1 N2 C7 117.72(14) . . ? N1 N2 Te 118.30(11) . . ? C7 N2 Te 122.90(11) . . ? C2 C1 C6 119.19(16) . . ? C2 C1 Te 127.45(13) . . ? C6 C1 Te 113.36(12) . . ? C3 C2 C1 119.73(17) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.99(17) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 120.17(17) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.22(17) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? N1 C6 C5 118.15(16) . . ? N1 C6 C1 121.08(15) . . ? C5 C6 C1 120.69(16) . . ? C12 C7 C8 120.93(16) . . ? C12 C7 N2 118.28(15) . . ? C8 C7 N2 120.63(15) . . ? C9 C8 C7 119.48(16) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 120.13(16) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.04(17) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.16(17) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C7 C12 C11 119.24(16) . . ? C7 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? 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 C6 N1 N2 C7 171.63(14) . . . . ? C6 N1 N2 Te 3.19(19) . . . . ? C1 Te N2 N1 -1.09(12) . . . . ? I Te N2 N1 27.7(3) . . . . ? C1 Te N2 C7 -168.89(14) . . . . ? I Te N2 C7 -140.15(15) . . . . ? N2 Te C1 C2 178.14(17) . . . . ? I Te C1 C2 3.82(16) . . . . ? N2 Te C1 C6 -1.30(11) . . . . ? I Te C1 C6 -175.62(11) . . . . ? C6 C1 C2 C3 0.1(3) . . . . ? Te C1 C2 C3 -179.34(13) . . . . ? C1 C2 C3 C4 -1.0(3) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? N2 N1 C6 C5 178.59(15) . . . . ? N2 N1 C6 C1 -4.6(2) . . . . ? C4 C5 C6 N1 175.83(16) . . . . ? C4 C5 C6 C1 -1.0(3) . . . . ? C2 C1 C6 N1 -175.79(16) . . . . ? Te C1 C6 N1 3.7(2) . . . . ? C2 C1 C6 C5 1.0(2) . . . . ? Te C1 C6 C5 -179.55(13) . . . . ? N1 N2 C7 C12 159.95(16) . . . . ? Te N2 C7 C12 -32.2(2) . . . . ? N1 N2 C7 C8 -24.7(2) . . . . ? Te N2 C7 C8 143.14(14) . . . . ? C12 C7 C8 C9 0.6(3) . . . . ? N2 C7 C8 C9 -174.64(16) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C8 C9 C10 C11 -1.4(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C8 C7 C12 C11 -1.4(3) . . . . ? N2 C7 C12 C11 173.88(16) . . . . ? C10 C11 C12 C7 0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.107 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.137 #===END data_azotecl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cl2 N4 Te' _chemical_formula_sum 'C24 H18 Cl2 N4 Te' _chemical_formula_weight 560.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 29.6142(9) _cell_length_b 12.8389(3) _cell_length_c 12.4737(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4742.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19374 _cell_measurement_theta_min 4.5988 _cell_measurement_theta_max 32.5541 _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69929 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 51040 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 32.61 _reflns_number_total 8161 _reflns_number_gt 5978 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0074P)^2^+13.9927P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8161 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_restrained_S_all 1.252 _refine_ls_shift/su_max 0.003 _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 Te Te 0.615205(8) 0.779680(18) 0.45683(2) 0.03264(7) Uani 1 1 d . . . Cl1 Cl 0.66802(4) 0.81215(9) 0.30118(9) 0.0463(3) Uani 1 1 d . A . Cl2 Cl 0.57005(4) 0.76711(9) 0.62512(9) 0.0474(3) Uani 1 1 d . A . N1A N 0.52628(17) 0.8326(4) 0.3965(4) 0.0324(10) Uani 0.744(6) 1 d P A 1 N2A N 0.48482(17) 0.8306(4) 0.3767(4) 0.0374(11) Uani 0.744(6) 1 d P A 1 C7A C 0.46631(18) 0.7283(3) 0.3741(4) 0.0398(14) Uani 0.744(6) 1 d PG A 1 C8A C 0.42011(18) 0.7233(4) 0.3552(5) 0.0544(17) Uani 0.744(6) 1 d PG A 1 H8AA H 0.4032 0.7855 0.3455 0.065 Uiso 0.744(6) 1 calc PR A 1 C9A C 0.39858(19) 0.6272(5) 0.3505(9) 0.069(2) Uani 0.744(6) 1 d PG A 1 H9AA H 0.3670 0.6237 0.3376 0.083 Uiso 0.744(6) 1 calc PR A 1 C10A C 0.4233(3) 0.5361(4) 0.3647(13) 0.0682(17) Uani 0.744(6) 1 d PG A 1 H10A H 0.4085 0.4704 0.3615 0.082 Uiso 0.744(6) 1 calc PR A 1 C11A C 0.4695(3) 0.5412(3) 0.3837(11) 0.0643(17) Uani 0.744(6) 1 d PG A 1 H11A H 0.4863 0.4789 0.3934 0.077 Uiso 0.744(6) 1 calc PR A 1 C12A C 0.49099(18) 0.6372(4) 0.3884(6) 0.0537(17) Uani 0.744(6) 1 d PG A 1 H12A H 0.5226 0.6407 0.4013 0.064 Uiso 0.744(6) 1 calc PR A 1 N1C N 0.5073(5) 0.8731(12) 0.3842(11) 0.0324(10) Uani 0.256(6) 1 d P A 2 N2C N 0.5215(5) 0.7813(14) 0.3912(12) 0.0374(11) Uani 0.256(6) 1 d P A 2 C7C C 0.4881(5) 0.7025(11) 0.3794(12) 0.0398(14) Uani 0.256(6) 1 d PG A 2 C8C C 0.4425(6) 0.7253(11) 0.3664(15) 0.0544(17) Uani 0.256(6) 1 d PG A 2 H8CA H 0.4329 0.7957 0.3608 0.065 Uiso 0.256(6) 1 calc PR A 2 C9C C 0.4111(5) 0.6451(18) 0.362(3) 0.069(2) Uani 0.256(6) 1 d PG A 2 H9CA H 0.3799 0.6607 0.3526 0.083 Uiso 0.256(6) 1 calc PR A 2 C10C C 0.4251(9) 0.5422(14) 0.370(4) 0.0682(17) Uani 0.256(6) 1 d PG A 2 H10C H 0.4036 0.4874 0.3664 0.082 Uiso 0.256(6) 1 calc PR A 2 C11C C 0.4707(9) 0.5194(10) 0.383(4) 0.0643(17) Uani 0.256(6) 1 d PG A 2 H11C H 0.4803 0.4490 0.3884 0.077 Uiso 0.256(6) 1 calc PR A 2 C12C C 0.5022(6) 0.5996(14) 0.388(2) 0.0537(17) Uani 0.256(6) 1 d PG A 2 H12C H 0.5333 0.5840 0.3965 0.064 Uiso 0.256(6) 1 calc PR A 2 N1B N 0.71414(12) 0.6555(3) 0.5076(3) 0.0385(8) Uani 1 1 d . . . N2B N 0.67733(12) 0.6198(3) 0.4789(3) 0.0385(8) Uani 1 1 d . A . C1A C 0.59050(14) 0.9329(3) 0.4275(3) 0.0342(8) Uani 1 1 d . A . C2A C 0.61582(16) 1.0228(3) 0.4287(4) 0.0441(10) Uani 1 1 d . . . H2AA H 0.6472 1.0200 0.4448 0.053 Uiso 1 1 calc R A . C3A C 0.59542(18) 1.1175(3) 0.4064(4) 0.0503(12) Uani 1 1 d . A . H3AA H 0.6128 1.1797 0.4074 0.060 Uiso 1 1 calc R . . C4A C 0.54965(18) 1.1217(4) 0.3827(4) 0.0525(13) Uani 1 1 d . . . H4AA H 0.5357 1.1870 0.3694 0.063 Uiso 1 1 calc R A . C5A C 0.52457(16) 1.0324(4) 0.3782(3) 0.0442(10) Uani 1 1 d . A . H5AA H 0.4934 1.0355 0.3601 0.053 Uiso 1 1 calc R . . C6A C 0.54476(14) 0.9375(3) 0.4002(3) 0.0356(9) Uani 1 1 d . . . C1B C 0.67105(14) 0.8187(3) 0.5577(3) 0.0363(8) Uani 1 1 d . A . C2B C 0.67005(16) 0.9065(3) 0.6217(4) 0.0444(10) Uani 1 1 d . . . H2BA H 0.6437 0.9487 0.6238 0.053 Uiso 1 1 calc R A . C3B C 0.70750(18) 0.9335(4) 0.6831(4) 0.0501(12) Uani 1 1 d . A . H3BA H 0.7066 0.9940 0.7270 0.060 Uiso 1 1 calc R . . C4B C 0.74587(18) 0.8732(4) 0.6808(4) 0.0509(12) Uani 1 1 d . . . H4BA H 0.7717 0.8932 0.7209 0.061 Uiso 1 1 calc R A . C5B C 0.74673(15) 0.7834(4) 0.6198(3) 0.0436(9) Uani 1 1 d . A . H5BA H 0.7731 0.7414 0.6187 0.052 Uiso 1 1 calc R . . C6B C 0.70929(14) 0.7541(3) 0.5602(3) 0.0364(9) Uani 1 1 d . A . C7B C 0.67837(14) 0.5207(3) 0.4257(3) 0.0351(8) Uani 1 1 d . . . C8B C 0.71722(15) 0.4616(3) 0.4108(4) 0.0426(10) Uani 1 1 d . A . H8BA H 0.7456 0.4857 0.4362 0.051 Uiso 1 1 calc R . . C9B C 0.71372(17) 0.3667(4) 0.3582(4) 0.0502(11) Uani 1 1 d . . . H9BA H 0.7398 0.3246 0.3489 0.060 Uiso 1 1 calc R A . C10B C 0.67245(17) 0.3328(3) 0.3191(4) 0.0464(11) Uani 1 1 d . A . H10B H 0.6704 0.2684 0.2819 0.056 Uiso 1 1 calc R . . C11B C 0.63461(17) 0.3921(4) 0.3342(4) 0.0510(12) Uani 1 1 d . . . H11B H 0.6063 0.3689 0.3072 0.061 Uiso 1 1 calc R A . C12B C 0.63731(15) 0.4855(3) 0.3882(4) 0.0485(11) Uani 1 1 d . A . H12B H 0.6108 0.5257 0.3998 0.058 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 Te 0.03330(12) 0.02982(11) 0.03481(12) -0.00057(11) 0.00176(11) 0.00460(10) Cl1 0.0428(6) 0.0568(6) 0.0391(5) -0.0012(5) 0.0095(4) 0.0062(5) Cl2 0.0475(6) 0.0567(7) 0.0381(5) 0.0121(5) 0.0083(4) 0.0099(5) N1A 0.037(3) 0.036(3) 0.0244(19) 0.002(2) -0.0003(18) 0.0085(19) N2A 0.038(2) 0.045(3) 0.030(2) 0.000(2) -0.0042(18) 0.004(2) C7A 0.045(4) 0.046(3) 0.028(2) 0.001(2) -0.007(3) -0.001(3) C8A 0.052(4) 0.055(3) 0.056(4) 0.000(3) -0.019(4) -0.007(4) C9A 0.057(5) 0.071(5) 0.079(5) 0.003(4) -0.021(4) -0.024(4) C10A 0.089(4) 0.059(3) 0.056(4) 0.003(3) -0.023(3) -0.025(3) C11A 0.087(4) 0.046(4) 0.060(3) 0.003(4) -0.020(3) -0.007(4) C12A 0.058(5) 0.042(5) 0.061(3) 0.005(4) -0.015(3) 0.003(3) N1C 0.037(3) 0.036(3) 0.0244(19) 0.002(2) -0.0003(18) 0.0085(19) N2C 0.038(2) 0.045(3) 0.030(2) 0.000(2) -0.0042(18) 0.004(2) C7C 0.045(4) 0.046(3) 0.028(2) 0.001(2) -0.007(3) -0.001(3) C8C 0.052(4) 0.055(3) 0.056(4) 0.000(3) -0.019(4) -0.007(4) C9C 0.057(5) 0.071(5) 0.079(5) 0.003(4) -0.021(4) -0.024(4) C10C 0.089(4) 0.059(3) 0.056(4) 0.003(3) -0.023(3) -0.025(3) C11C 0.087(4) 0.046(4) 0.060(3) 0.003(4) -0.020(3) -0.007(4) C12C 0.058(5) 0.042(5) 0.061(3) 0.005(4) -0.015(3) 0.003(3) N1B 0.0380(18) 0.0385(18) 0.0391(18) -0.0011(15) -0.0041(15) 0.0027(15) N2B 0.0368(18) 0.0348(17) 0.044(2) 0.0017(15) -0.0013(15) 0.0048(14) C1A 0.040(2) 0.0320(19) 0.0305(18) 0.0020(15) 0.0067(16) 0.0072(16) C2A 0.042(2) 0.040(2) 0.050(2) 0.0060(19) 0.007(2) -0.0006(19) C3A 0.067(3) 0.032(2) 0.052(3) 0.006(2) 0.012(2) -0.003(2) C4A 0.074(3) 0.045(3) 0.038(2) 0.013(2) 0.011(2) 0.025(2) C5A 0.046(2) 0.058(3) 0.0286(19) 0.007(2) 0.0043(18) 0.016(2) C6A 0.040(2) 0.046(2) 0.0204(16) -0.0005(16) 0.0046(15) 0.0020(18) C1B 0.046(2) 0.0346(19) 0.0287(19) 0.0020(16) 0.0003(17) 0.0009(17) C2B 0.057(3) 0.036(2) 0.041(2) -0.0063(19) -0.005(2) 0.0049(19) C3B 0.071(3) 0.037(2) 0.042(2) -0.010(2) -0.010(2) -0.001(2) C4B 0.058(3) 0.051(3) 0.044(2) -0.001(2) -0.017(2) -0.004(2) C5B 0.045(2) 0.044(2) 0.042(2) -0.001(2) -0.0085(19) 0.004(2) C6B 0.048(2) 0.0351(19) 0.0265(18) -0.0002(15) -0.0017(16) 0.0036(16) C7B 0.045(2) 0.0271(19) 0.0335(19) 0.0016(15) 0.0033(17) 0.0033(16) C8B 0.040(2) 0.042(2) 0.046(2) -0.0039(19) -0.0001(19) -0.0017(18) C9B 0.049(3) 0.043(2) 0.059(3) -0.005(2) 0.011(2) 0.009(2) C10B 0.059(3) 0.035(2) 0.044(2) -0.0038(19) 0.006(2) -0.002(2) C11B 0.054(3) 0.037(2) 0.061(3) -0.005(2) -0.009(2) -0.004(2) C12B 0.044(2) 0.036(2) 0.066(3) -0.003(2) -0.009(2) 0.0053(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te C1A 2.130(4) . ? Te C1B 2.138(4) . ? Te Cl2 2.4941(11) . ? Te Cl1 2.5279(11) . ? Te N2B 2.770(3) . ? Te N1A 2.822(5) . ? Te N2C 2.892(15) . ? N1A N2A 1.253(7) . ? N1A C6A 1.454(7) . ? N2A C7A 1.424(6) . ? C7A C8A 1.3900 . ? C7A C12A 1.3900 . ? C8A C9A 1.3900 . ? C8A H8AA 0.9500 . ? C9A C10A 1.3900 . ? C9A H9AA 0.9500 . ? C10A C11A 1.3900 . ? C10A H10A 0.9500 . ? C11A C12A 1.3900 . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? N1C N2C 1.26(2) . ? N1C C6A 1.397(17) . ? N2C C7C 1.42(2) . ? C7C C8C 1.3900 . ? C7C C12C 1.3900 . ? C8C C9C 1.3900 . ? C8C H8CA 0.9500 . ? C9C C10C 1.3900 . ? C9C H9CA 0.9500 . ? C10C C11C 1.3900 . ? C10C H10C 0.9500 . ? C11C C12C 1.3900 . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? N1B N2B 1.235(5) . ? N1B C6B 1.434(5) . ? N2B C7B 1.435(5) . ? C1A C2A 1.377(6) . ? C1A C6A 1.398(6) . ? C2A C3A 1.385(6) . ? C2A H2AA 0.9500 . ? C3A C4A 1.389(7) . ? C3A H3AA 0.9500 . ? C4A C5A 1.367(7) . ? C4A H4AA 0.9500 . ? C5A C6A 1.385(6) . ? C5A H5AA 0.9500 . ? C1B C2B 1.382(6) . ? C1B C6B 1.404(6) . ? C2B C3B 1.392(6) . ? C2B H2BA 0.9500 . ? C3B C4B 1.376(7) . ? C3B H3BA 0.9500 . ? C4B C5B 1.381(6) . ? C4B H4BA 0.9500 . ? C5B C6B 1.387(6) . ? C5B H5BA 0.9500 . ? C7B C12B 1.379(6) . ? C7B C8B 1.391(6) . ? C8B C9B 1.388(6) . ? C8B H8BA 0.9500 . ? C9B C10B 1.386(7) . ? C9B H9BA 0.9500 . ? C10B C11B 1.368(6) . ? C10B H10B 0.9500 . ? C11B C12B 1.378(6) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Te C1B 98.64(16) . . ? C1A Te Cl2 91.16(10) . . ? C1B Te Cl2 86.24(11) . . ? C1A Te Cl1 85.89(11) . . ? C1B Te Cl1 86.26(11) . . ? Cl2 Te Cl1 171.44(4) . . ? C1A Te N2B 158.33(13) . . ? C1B Te N2B 66.52(13) . . ? Cl2 Te N2B 102.97(8) . . ? Cl1 Te N2B 77.74(8) . . ? C1A Te N1A 53.94(16) . . ? C1B Te N1A 145.33(15) . . ? Cl2 Te N1A 74.91(9) . . ? Cl1 Te N1A 109.45(10) . . ? N2B Te N1A 145.56(13) . . ? C1A Te N2C 67.4(4) . . ? C1B Te N2C 155.1(3) . . ? Cl2 Te N2C 74.0(3) . . ? Cl1 Te N2C 112.0(3) . . ? N2B Te N2C 132.1(4) . . ? N1A Te N2C 13.5(3) . . ? N2A N1A C6A 113.2(5) . . ? N2A N1A Te 164.2(5) . . ? C6A N1A Te 82.1(3) . . ? N1A N2A C7A 113.6(5) . . ? C8A C7A C12A 120.0 . . ? C8A C7A N2A 115.2(4) . . ? C12A C7A N2A 124.8(4) . . ? C9A C8A C7A 120.0 . . ? C9A C8A H8AA 120.0 . . ? C7A C8A H8AA 120.0 . . ? C8A C9A C10A 120.0 . . ? C8A C9A H9AA 120.0 . . ? C10A C9A H9AA 120.0 . . ? C11A C10A C9A 120.0 . . ? C11A C10A H10A 120.0 . . ? C9A C10A H10A 120.0 . . ? C10A C11A C12A 120.0 . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C11A C12A C7A 120.0 . . ? C11A C12A H12A 120.0 . . ? C7A C12A H12A 120.0 . . ? N2C N1C C6A 106.2(13) . . ? N1C N2C C7C 115.2(15) . . ? N1C N2C Te 110.4(13) . . ? C7C N2C Te 133.8(11) . . ? C8C C7C C12C 120.0 . . ? C8C C7C N2C 122.6(13) . . ? C12C C7C N2C 117.3(13) . . ? C7C C8C C9C 120.0 . . ? C7C C8C H8CA 120.0 . . ? C9C C8C H8CA 120.0 . . ? C10C C9C C8C 120.0 . . ? C10C C9C H9CA 120.0 . . ? C8C C9C H9CA 120.0 . . ? C9C C10C C11C 120.0 . . ? C9C C10C H10C 120.0 . . ? C11C C10C H10C 120.0 . . ? C12C C11C C10C 120.0 . . ? C12C C11C H11C 120.0 . . ? C10C C11C H11C 120.0 . . ? C11C C12C C7C 120.0 . . ? C11C C12C H12C 120.0 . . ? C7C C12C H12C 120.0 . . ? N2B N1B C6B 111.8(3) . . ? N1B N2B C7B 116.3(3) . . ? N1B N2B Te 109.9(3) . . ? C7B N2B Te 128.7(3) . . ? C2A C1A C6A 119.7(4) . . ? C2A C1A Te 125.8(3) . . ? C6A C1A Te 114.4(3) . . ? C1A C2A C3A 119.7(4) . . ? C1A C2A H2AA 120.1 . . ? C3A C2A H2AA 120.1 . . ? C2A C3A C4A 120.2(4) . . ? C2A C3A H3AA 119.9 . . ? C4A C3A H3AA 119.9 . . ? C5A C4A C3A 120.4(4) . . ? C5A C4A H4AA 119.8 . . ? C3A C4A H4AA 119.8 . . ? C4A C5A C6A 119.7(4) . . ? C4A C5A H5AA 120.2 . . ? C6A C5A H5AA 120.2 . . ? C5A C6A N1C 98.6(7) . . ? C5A C6A C1A 120.2(4) . . ? N1C C6A C1A 141.2(7) . . ? C5A C6A N1A 130.3(4) . . ? N1C C6A N1A 31.7(6) . . ? C1A C6A N1A 109.5(4) . . ? C2B C1B C6B 119.1(4) . . ? C2B C1B Te 121.0(3) . . ? C6B C1B Te 119.9(3) . . ? C1B C2B C3B 120.3(4) . . ? C1B C2B H2BA 119.9 . . ? C3B C2B H2BA 119.9 . . ? C4B C3B C2B 120.4(4) . . ? C4B C3B H3BA 119.8 . . ? C2B C3B H3BA 119.8 . . ? C3B C4B C5B 119.8(4) . . ? C3B C4B H4BA 120.1 . . ? C5B C4B H4BA 120.1 . . ? C4B C5B C6B 120.4(4) . . ? C4B C5B H5BA 119.8 . . ? C6B C5B H5BA 119.8 . . ? C5B C6B C1B 119.8(4) . . ? C5B C6B N1B 113.9(4) . . ? C1B C6B N1B 126.3(4) . . ? C12B C7B C8B 120.4(4) . . ? C12B C7B N2B 115.4(4) . . ? C8B C7B N2B 124.3(4) . . ? C9B C8B C7B 118.7(4) . . ? C9B C8B H8BA 120.6 . . ? C7B C8B H8BA 120.6 . . ? C10B C9B C8B 120.5(4) . . ? C10B C9B H9BA 119.7 . . ? C8B C9B H9BA 119.7 . . ? C11B C10B C9B 120.0(4) . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C10B C11B C12B 120.3(5) . . ? C10B C11B H11B 119.9 . . ? C12B C11B H11B 119.9 . . ? C11B C12B C7B 120.1(4) . . ? C11B C12B H12B 119.9 . . ? C7B C12B H12B 119.9 . . ? 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 C1A Te N1A N2A -168.0(14) . . . . ? C1B Te N1A N2A -124.6(13) . . . . ? Cl2 Te N1A N2A -65.2(13) . . . . ? Cl1 Te N1A N2A 122.5(13) . . . . ? N2B Te N1A N2A 25.8(15) . . . . ? N2C Te N1A N2A 19.1(15) . . . . ? C1A Te N1A C6A -0.8(2) . . . . ? C1B Te N1A C6A 42.7(4) . . . . ? Cl2 Te N1A C6A 102.1(2) . . . . ? Cl1 Te N1A C6A -70.2(2) . . . . ? N2B Te N1A C6A -166.9(2) . . . . ? N2C Te N1A C6A -173.6(15) . . . . ? C6A N1A N2A C7A -179.3(4) . . . . ? Te N1A N2A C7A -13.1(16) . . . . ? N1A N2A C7A C8A 178.3(4) . . . . ? N1A N2A C7A C12A -2.0(7) . . . . ? C12A C7A C8A C9A 0.0 . . . . ? N2A C7A C8A C9A 179.7(6) . . . . ? C7A C8A C9A C10A 0.0 . . . . ? C8A C9A C10A C11A 0.0 . . . . ? C9A C10A C11A C12A 0.0 . . . . ? C10A C11A C12A C7A 0.0 . . . . ? C8A C7A C12A C11A 0.0 . . . . ? N2A C7A C12A C11A -179.6(7) . . . . ? C6A N1C N2C C7C 178.8(11) . . . . ? C6A N1C N2C Te 6.3(13) . . . . ? C1A Te N2C N1C -5.9(10) . . . . ? C1B Te N2C N1C 53.4(16) . . . . ? Cl2 Te N2C N1C 92.2(11) . . . . ? Cl1 Te N2C N1C -81.3(11) . . . . ? N2B Te N2C N1C -174.6(9) . . . . ? N1A Te N2C N1C 0.3(9) . . . . ? C1A Te N2C C7C -176.4(15) . . . . ? C1B Te N2C C7C -117.1(14) . . . . ? Cl2 Te N2C C7C -78.2(14) . . . . ? Cl1 Te N2C C7C 108.2(14) . . . . ? N2B Te N2C C7C 15.0(16) . . . . ? N1A Te N2C C7C -170(3) . . . . ? N1C N2C C7C C8C -3(2) . . . . ? Te N2C C7C C8C 167.1(11) . . . . ? N1C N2C C7C C12C -179.4(16) . . . . ? Te N2C C7C C12C -9(2) . . . . ? C12C C7C C8C C9C 0.0 . . . . ? N2C C7C C8C C9C -176(2) . . . . ? C7C C8C C9C C10C 0.0 . . . . ? C8C C9C C10C C11C 0.0 . . . . ? C9C C10C C11C C12C 0.0 . . . . ? C10C C11C C12C C7C 0.0 . . . . ? C8C C7C C12C C11C 0.0 . . . . ? N2C C7C C12C C11C 176.4(19) . . . . ? C6B N1B N2B C7B -179.7(3) . . . . ? C6B N1B N2B Te 23.3(4) . . . . ? C1A Te N2B N1B 28.3(5) . . . . ? C1B Te N2B N1B -21.1(3) . . . . ? Cl2 Te N2B N1B -101.1(3) . . . . ? Cl1 Te N2B N1B 70.1(3) . . . . ? N1A Te N2B N1B 176.7(3) . . . . ? N2C Te N2B N1B 178.8(5) . . . . ? C1A Te N2B C7B -125.0(4) . . . . ? C1B Te N2B C7B -174.5(4) . . . . ? Cl2 Te N2B C7B 105.5(3) . . . . ? Cl1 Te N2B C7B -83.3(3) . . . . ? N1A Te N2B C7B 23.3(4) . . . . ? N2C Te N2B C7B 25.5(5) . . . . ? C1B Te C1A C2A 27.3(4) . . . . ? Cl2 Te C1A C2A 113.6(4) . . . . ? Cl1 Te C1A C2A -58.3(4) . . . . ? N2B Te C1A C2A -17.6(6) . . . . ? N1A Te C1A C2A -176.1(4) . . . . ? N2C Te C1A C2A -174.2(5) . . . . ? C1B Te C1A C6A -155.8(3) . . . . ? Cl2 Te C1A C6A -69.4(3) . . . . ? Cl1 Te C1A C6A 118.6(3) . . . . ? N2B Te C1A C6A 159.4(3) . . . . ? N1A Te C1A C6A 0.9(2) . . . . ? N2C Te C1A C6A 2.7(4) . . . . ? C6A C1A C2A C3A 2.2(6) . . . . ? Te C1A C2A C3A 178.9(3) . . . . ? C1A C2A C3A C4A -0.1(7) . . . . ? C2A C3A C4A C5A -1.8(7) . . . . ? C3A C4A C5A C6A 1.6(7) . . . . ? C4A C5A C6A N1C -179.1(7) . . . . ? C4A C5A C6A C1A 0.5(6) . . . . ? C4A C5A C6A N1A -177.1(4) . . . . ? N2C N1C C6A C5A 173.7(11) . . . . ? N2C N1C C6A C1A -5.8(18) . . . . ? N2C N1C C6A N1A -3.4(9) . . . . ? C2A C1A C6A C5A -2.3(6) . . . . ? Te C1A C6A C5A -179.5(3) . . . . ? C2A C1A C6A N1C 177.0(10) . . . . ? Te C1A C6A N1C -0.1(11) . . . . ? C2A C1A C6A N1A 175.7(4) . . . . ? Te C1A C6A N1A -1.5(4) . . . . ? N2A N1A C6A C5A -5.0(7) . . . . ? Te N1A C6A C5A 178.8(4) . . . . ? N2A N1A C6A N1C -1.1(11) . . . . ? Te N1A C6A N1C -177.4(12) . . . . ? N2A N1A C6A C1A 177.3(4) . . . . ? Te N1A C6A C1A 1.0(3) . . . . ? C1A Te C1B C2B 29.3(4) . . . . ? Cl2 Te C1B C2B -61.3(3) . . . . ? Cl1 Te C1B C2B 114.6(3) . . . . ? N2B Te C1B C2B -167.1(4) . . . . ? N1A Te C1B C2B -4.9(5) . . . . ? N2C Te C1B C2B -24.1(10) . . . . ? C1A Te C1B C6B -151.3(3) . . . . ? Cl2 Te C1B C6B 118.1(3) . . . . ? Cl1 Te C1B C6B -66.0(3) . . . . ? N2B Te C1B C6B 12.3(3) . . . . ? N1A Te C1B C6B 174.5(3) . . . . ? N2C Te C1B C6B 155.3(8) . . . . ? C6B C1B C2B C3B 3.6(7) . . . . ? Te C1B C2B C3B -177.0(3) . . . . ? C1B C2B C3B C4B 0.0(7) . . . . ? C2B C3B C4B C5B -2.2(7) . . . . ? C3B C4B C5B C6B 0.6(7) . . . . ? C4B C5B C6B C1B 3.1(6) . . . . ? C4B C5B C6B N1B -175.7(4) . . . . ? C2B C1B C6B C5B -5.1(6) . . . . ? Te C1B C6B C5B 175.5(3) . . . . ? C2B C1B C6B N1B 173.4(4) . . . . ? Te C1B C6B N1B -6.0(6) . . . . ? N2B N1B C6B C5B 162.8(4) . . . . ? N2B N1B C6B C1B -15.9(6) . . . . ? N1B N2B C7B C12B -176.0(4) . . . . ? Te N2B C7B C12B -24.0(5) . . . . ? N1B N2B C7B C8B 3.9(6) . . . . ? Te N2B C7B C8B 155.8(3) . . . . ? C12B C7B C8B C9B -0.3(7) . . . . ? N2B C7B C8B C9B 179.8(4) . . . . ? C7B C8B C9B C10B 1.5(7) . . . . ? C8B C9B C10B C11B -1.3(7) . . . . ? C9B C10B C11B C12B -0.1(8) . . . . ? C10B C11B C12B C7B 1.3(8) . . . . ? C8B C7B C12B C11B -1.1(7) . . . . ? N2B C7B C12B C11B 178.8(4) . . . . ? 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 C8A H8AA Cl1 0.95 2.81 3.453(5) 125.4 3_655 C3B H3BA Cl1 0.95 2.89 3.768(5) 154.1 7_576 C9B H9BA Cl1 0.95 2.80 3.642(5) 148.4 8_755 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.401 _refine_diff_density_min -1.661 _refine_diff_density_rms 0.097 #===END data_azo-dite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Br2 N4 Te' _chemical_formula_sum 'C24 H18 Br2 N4 Te' _chemical_formula_weight 649.84 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9613(2) _cell_length_b 13.7629(4) _cell_length_c 20.4098(6) _cell_angle_alpha 78.860(2) _cell_angle_beta 88.143(2) _cell_angle_gamma 72.840(2) _cell_volume 2359.03(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10555 _cell_measurement_theta_min 4.6239 _cell_measurement_theta_max 32.4866 _exptl_crystal_description prism _exptl_crystal_colour 'orange-brown' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 4.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51323 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 26878 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 32.55 _reflns_number_total 14411 _reflns_number_gt 8278 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0278P)^2^+6.1393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14411 _refine_ls_number_parameters 554 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.078 _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 Te1 Te 0.22707(4) 0.76970(2) 0.097620(16) 0.02935(8) Uani 1 1 d . . . Br1A Br 0.19878(7) 0.57798(4) 0.10703(3) 0.04151(13) Uani 1 1 d . . . Br2A Br 0.26376(7) 0.95230(4) 0.10455(3) 0.04615(15) Uani 1 1 d . . . N1A N 0.3990(5) 0.6615(3) -0.0348(2) 0.0355(9) Uani 1 1 d . . . N2A N 0.2655(5) 0.7183(3) -0.0326(2) 0.0339(9) Uani 1 1 d . . . N1B N 0.0375(6) 0.8490(4) 0.2334(2) 0.0490(12) Uani 1 1 d . . . N2B N -0.0125(6) 0.8621(3) 0.1756(2) 0.0426(11) Uani 1 1 d . . . C1A C 0.4639(5) 0.7235(4) 0.0656(3) 0.0346(11) Uani 1 1 d . . . C2A C 0.5815(6) 0.7399(4) 0.1013(3) 0.0415(12) Uani 1 1 d . . . H2AA H 0.5562 0.7721 0.1391 0.050 Uiso 1 1 calc R . . C3A C 0.7362(6) 0.7092(4) 0.0815(3) 0.0472(14) Uani 1 1 d . . . H3AA H 0.8154 0.7216 0.1056 0.057 Uiso 1 1 calc R . . C4A C 0.7756(6) 0.6613(4) 0.0277(3) 0.0453(14) Uani 1 1 d . . . H4AA H 0.8817 0.6386 0.0155 0.054 Uiso 1 1 calc R . . C5A C 0.6597(6) 0.6465(4) -0.0087(3) 0.0390(12) Uani 1 1 d . . . H5AA H 0.6864 0.6142 -0.0463 0.047 Uiso 1 1 calc R . . C6A C 0.5041(6) 0.6784(4) 0.0093(2) 0.0319(10) Uani 1 1 d . . . C7A C 0.1550(6) 0.7018(4) -0.0751(2) 0.0379(12) Uani 1 1 d . . . C8A C 0.1746(7) 0.6095(5) -0.0960(3) 0.0483(14) Uani 1 1 d . . . H8AA H 0.2652 0.5528 -0.0826 0.058 Uiso 1 1 calc R . . C9A C 0.0611(9) 0.6001(5) -0.1369(3) 0.0651(19) Uani 1 1 d . . . H9AA H 0.0735 0.5368 -0.1517 0.078 Uiso 1 1 calc R . . C10A C -0.0704(8) 0.6833(6) -0.1560(3) 0.0616(19) Uani 1 1 d . . . H10A H -0.1476 0.6777 -0.1847 0.074 Uiso 1 1 calc R . . C11A C -0.0897(7) 0.7742(6) -0.1338(3) 0.0558(16) Uani 1 1 d . . . H11A H -0.1807 0.8308 -0.1468 0.067 Uiso 1 1 calc R . . C12A C 0.0203(7) 0.7834(5) -0.0934(3) 0.0487(14) Uani 1 1 d . . . H12A H 0.0051 0.8461 -0.0776 0.058 Uiso 1 1 calc R . . C1B C 0.2824(7) 0.7219(4) 0.2028(2) 0.0377(12) Uani 1 1 d . . . C2B C 0.4135(7) 0.6413(4) 0.2251(3) 0.0466(14) Uani 1 1 d . . . H2BA H 0.4793 0.6062 0.1943 0.056 Uiso 1 1 calc R . . C3B C 0.4490(8) 0.6116(5) 0.2935(3) 0.0597(18) Uani 1 1 d . . . H3BA H 0.5391 0.5558 0.3096 0.072 Uiso 1 1 calc R . . C4B C 0.3529(10) 0.6634(6) 0.3374(3) 0.069(2) Uani 1 1 d . . . H4BA H 0.3781 0.6436 0.3839 0.082 Uiso 1 1 calc R . . C5B C 0.2220(9) 0.7427(5) 0.3155(3) 0.0577(17) Uani 1 1 d . . . H5BA H 0.1580 0.7784 0.3466 0.069 Uiso 1 1 calc R . . C6B C 0.1824(7) 0.7713(4) 0.2483(3) 0.0405(13) Uani 1 1 d . . . C7B C -0.1599(6) 0.9385(4) 0.1593(3) 0.0434(13) Uani 1 1 d . . . C8B C -0.2561(8) 0.9865(5) 0.2059(3) 0.0584(17) Uani 1 1 d . . . H8BA H -0.2244 0.9699 0.2517 0.070 Uiso 1 1 calc R . . C9B C -0.3974(8) 1.0580(6) 0.1851(4) 0.069(2) Uani 1 1 d . . . H9BA H -0.4629 1.0909 0.2170 0.082 Uiso 1 1 calc R . . C10B C -0.4454(7) 1.0828(5) 0.1192(4) 0.0583(17) Uani 1 1 d . . . H10B H -0.5428 1.1329 0.1053 0.070 Uiso 1 1 calc R . . C11B C -0.3513(7) 1.0343(5) 0.0739(3) 0.0582(17) Uani 1 1 d . . . H11B H -0.3844 1.0502 0.0283 0.070 Uiso 1 1 calc R . . C12B C -0.2089(7) 0.9629(5) 0.0935(3) 0.0484(14) Uani 1 1 d . . . H12B H -0.1443 0.9303 0.0613 0.058 Uiso 1 1 calc R . . Te2 Te 0.73251(4) 0.76083(2) 0.476809(16) 0.03181(8) Uani 1 1 d . . . Br1B Br 0.67485(6) 0.57980(4) 0.52357(3) 0.04361(14) Uani 1 1 d . A . Br2B Br 0.80669(9) 0.92899(5) 0.41590(3) 0.05925(19) Uani 1 1 d . A . N1C N 0.7777(8) 0.7169(5) 0.6193(3) 0.0273(14) Uani 0.65 1 d PD A 1 N2C N 0.7718(7) 0.6788(5) 0.6779(3) 0.0379(15) Uani 0.65 1 d PD A 1 C1C C 0.9466(11) 0.7126(16) 0.5290(5) 0.0279(16) Uani 0.65 1 d PGD A 1 C2C C 1.0894(14) 0.7022(12) 0.4981(6) 0.035(3) Uani 0.65 1 d PGD A 1 H2CA H 1.0932 0.7166 0.4507 0.042 Uiso 0.65 1 calc PR A 1 C3C C 1.2268(11) 0.6708(9) 0.5364(8) 0.044(3) Uani 0.65 1 d PGD A 1 H3CA H 1.3244 0.6637 0.5152 0.053 Uiso 0.65 1 calc PR A 1 C4C C 1.2214(8) 0.6499(10) 0.6057(7) 0.044(3) Uani 0.65 1 d PGD A 1 H4CA H 1.3153 0.6284 0.6319 0.053 Uiso 0.65 1 calc PR A 1 C5C C 1.0786(9) 0.6603(14) 0.6366(6) 0.042(2) Uani 0.65 1 d PGD A 1 H5CA H 1.0748 0.6459 0.6840 0.050 Uiso 0.65 1 calc PR A 1 C6C C 0.9412(8) 0.6917(17) 0.5983(5) 0.0287(19) Uani 0.65 1 d PGD A 1 C7C C 0.6136(6) 0.7061(5) 0.6962(4) 0.041(2) Uani 0.65 1 d PGD A 1 C8C C 0.5885(8) 0.6413(5) 0.7540(3) 0.041(2) Uani 0.65 1 d PGD A 1 H8CA H 0.6724 0.5846 0.7750 0.049 Uiso 0.65 1 calc PR A 1 C9C C 0.4407(11) 0.6594(9) 0.7811(5) 0.049(2) Uani 0.65 1 d PGD A 1 H9CA H 0.4236 0.6151 0.8206 0.058 Uiso 0.65 1 calc PR A 1 C10C C 0.3181(9) 0.7424(12) 0.7504(7) 0.046(2) Uani 0.65 1 d PGD A 1 H10C H 0.2171 0.7547 0.7689 0.055 Uiso 0.65 1 calc PR A 1 C11C C 0.3432(10) 0.8072(10) 0.6926(7) 0.041(2) Uani 0.65 1 d PGD A 1 H11C H 0.2593 0.8639 0.6716 0.050 Uiso 0.65 1 calc PR A 1 C12C C 0.4909(10) 0.7891(6) 0.6655(5) 0.037(2) Uani 0.65 1 d PGD A 1 H12C H 0.5081 0.8334 0.6260 0.044 Uiso 0.65 1 calc PR A 1 N1E N 0.8496(13) 0.6794(9) 0.6473(5) 0.0273(14) Uani 0.35 1 d PD A 2 N2E N 0.7118(14) 0.7354(12) 0.6251(7) 0.0379(15) Uani 0.35 1 d PD A 2 C1E C 0.966(2) 0.716(3) 0.5309(10) 0.0279(16) Uani 0.35 1 d PGD A 2 C2E C 1.097(3) 0.724(2) 0.4950(11) 0.035(3) Uani 0.35 1 d PGD A 2 H2EA H 1.0888 0.7486 0.4480 0.042 Uiso 0.35 1 calc PR A 2 C3E C 1.242(2) 0.6962(19) 0.5277(15) 0.044(3) Uani 0.35 1 d PGD A 2 H3EA H 1.3319 0.7016 0.5031 0.053 Uiso 0.35 1 calc PR A 2 C4E C 1.255(2) 0.660(2) 0.5964(16) 0.044(3) Uani 0.35 1 d PGD A 2 H4EA H 1.3533 0.6412 0.6188 0.053 Uiso 0.35 1 calc PR A 2 C5E C 1.123(2) 0.652(3) 0.6323(12) 0.042(2) Uani 0.35 1 d PGD A 2 H5EA H 1.1316 0.6278 0.6793 0.050 Uiso 0.35 1 calc PR A 2 C6E C 0.9785(19) 0.680(3) 0.5996(10) 0.0287(19) Uani 0.35 1 d PGD A 2 C7E C 0.5894(14) 0.7365(13) 0.6662(6) 0.041(2) Uani 0.35 1 d PGD A 2 C8E C 0.6027(16) 0.6560(11) 0.7207(6) 0.041(2) Uani 0.35 1 d PGD A 2 H8EA H 0.6959 0.5997 0.7282 0.049 Uiso 0.35 1 calc PR A 2 C9E C 0.480(2) 0.6580(17) 0.7641(9) 0.049(2) Uani 0.35 1 d PGD A 2 H9EA H 0.4887 0.6029 0.8014 0.058 Uiso 0.35 1 calc PR A 2 C10E C 0.343(2) 0.740(2) 0.7531(14) 0.046(2) Uani 0.35 1 d PGD A 2 H10D H 0.2591 0.7417 0.7828 0.055 Uiso 0.35 1 calc PR A 2 C11E C 0.330(2) 0.821(2) 0.6987(14) 0.041(2) Uani 0.35 1 d PGD A 2 H11D H 0.2368 0.8772 0.6912 0.050 Uiso 0.35 1 calc PR A 2 C12E C 0.453(2) 0.8190(15) 0.6552(9) 0.037(2) Uani 0.35 1 d PGD A 2 H12D H 0.4440 0.8740 0.6180 0.044 Uiso 0.35 1 calc PR A 2 N1D N 0.5951(5) 0.8151(3) 0.3168(2) 0.0425(11) Uani 1 1 d . . . N2D N 0.5310(5) 0.8417(3) 0.3676(2) 0.0378(10) Uani 1 1 d . A . C1D C 0.8172(5) 0.6949(4) 0.3913(2) 0.0309(10) Uani 1 1 d . A . C2D C 0.9494(6) 0.6107(4) 0.3970(3) 0.0389(12) Uani 1 1 d . . . H2DA H 0.9989 0.5797 0.4395 0.047 Uiso 1 1 calc R A . C3D C 1.0106(7) 0.5709(4) 0.3408(3) 0.0442(13) Uani 1 1 d . A . H3DA H 1.1038 0.5146 0.3446 0.053 Uiso 1 1 calc R . . C4D C 0.9350(7) 0.6139(5) 0.2795(3) 0.0509(15) Uani 1 1 d . . . H4DA H 0.9763 0.5873 0.2409 0.061 Uiso 1 1 calc R A . C5D C 0.7993(6) 0.6956(4) 0.2741(3) 0.0446(13) Uani 1 1 d . A . H5DA H 0.7473 0.7242 0.2318 0.054 Uiso 1 1 calc R . . C6D C 0.7380(6) 0.7363(4) 0.3295(3) 0.0345(11) Uani 1 1 d . A . C7D C 0.3836(6) 0.9209(4) 0.3586(3) 0.0395(12) Uani 1 1 d . . . C8D C 0.3129(7) 0.9657(5) 0.2962(3) 0.0546(16) Uani 1 1 d . A . H8DA H 0.3624 0.9461 0.2569 0.065 Uiso 1 1 calc R . . C9D C 0.1700(8) 1.0389(5) 0.2924(4) 0.069(2) Uani 1 1 d . . . H9DA H 0.1185 1.0687 0.2502 0.083 Uiso 1 1 calc R A . C10D C 0.0999(8) 1.0698(5) 0.3490(4) 0.065(2) Uani 1 1 d . A . H10E H 0.0019 1.1219 0.3454 0.078 Uiso 1 1 calc R . . C11D C 0.1698(7) 1.0264(5) 0.4097(4) 0.067(2) Uani 1 1 d . . . H11E H 0.1210 1.0475 0.4487 0.080 Uiso 1 1 calc R A . C12D C 0.3131(7) 0.9511(5) 0.4144(3) 0.0565(17) Uani 1 1 d . A . H12F H 0.3626 0.9203 0.4570 0.068 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 0.03266(17) 0.03110(16) 0.02727(16) -0.00989(12) 0.00177(13) -0.01126(13) Br1A 0.0513(3) 0.0393(3) 0.0438(3) -0.0131(2) 0.0045(2) -0.0255(2) Br2A 0.0614(4) 0.0356(3) 0.0488(3) -0.0145(2) 0.0157(3) -0.0229(3) N1A 0.037(2) 0.034(2) 0.034(2) -0.0026(18) 0.0005(19) -0.0102(19) N2A 0.042(2) 0.036(2) 0.027(2) -0.0060(17) -0.0017(18) -0.0142(19) N1B 0.054(3) 0.067(3) 0.040(3) -0.017(2) 0.010(2) -0.035(3) N2B 0.062(3) 0.048(3) 0.029(2) -0.015(2) 0.012(2) -0.030(2) C1A 0.026(2) 0.036(3) 0.039(3) -0.005(2) 0.002(2) -0.007(2) C2A 0.046(3) 0.048(3) 0.033(3) -0.010(2) -0.003(2) -0.016(3) C3A 0.034(3) 0.048(3) 0.060(4) -0.002(3) -0.011(3) -0.017(2) C4A 0.031(3) 0.043(3) 0.056(4) -0.004(3) 0.002(3) -0.006(2) C5A 0.040(3) 0.035(3) 0.040(3) -0.006(2) 0.008(2) -0.010(2) C6A 0.038(3) 0.029(2) 0.030(3) -0.007(2) 0.001(2) -0.010(2) C7A 0.045(3) 0.051(3) 0.024(2) -0.004(2) 0.000(2) -0.026(3) C8A 0.050(3) 0.054(4) 0.050(4) -0.006(3) -0.009(3) -0.029(3) C9A 0.091(5) 0.059(4) 0.060(4) -0.008(3) -0.007(4) -0.047(4) C10A 0.064(4) 0.097(5) 0.037(3) 0.001(3) -0.015(3) -0.051(4) C11A 0.042(3) 0.079(5) 0.048(4) -0.006(3) -0.008(3) -0.024(3) C12A 0.052(4) 0.056(4) 0.037(3) -0.006(3) 0.003(3) -0.017(3) C1B 0.053(3) 0.041(3) 0.028(3) -0.005(2) 0.001(2) -0.029(3) C2B 0.058(4) 0.042(3) 0.045(3) -0.002(3) -0.006(3) -0.025(3) C3B 0.074(5) 0.056(4) 0.052(4) 0.015(3) -0.027(4) -0.036(3) C4B 0.106(6) 0.092(5) 0.028(3) 0.009(3) -0.002(4) -0.072(5) C5B 0.084(5) 0.075(5) 0.030(3) -0.003(3) 0.007(3) -0.053(4) C6B 0.056(3) 0.051(3) 0.029(3) -0.008(2) 0.005(2) -0.037(3) C7B 0.040(3) 0.042(3) 0.056(4) -0.017(3) 0.020(3) -0.022(2) C8B 0.068(4) 0.070(4) 0.051(4) -0.032(3) 0.015(3) -0.030(4) C9B 0.051(4) 0.071(5) 0.095(6) -0.041(4) 0.027(4) -0.020(3) C10B 0.044(3) 0.055(4) 0.080(5) -0.013(4) 0.011(3) -0.021(3) C11B 0.055(4) 0.059(4) 0.057(4) -0.006(3) 0.017(3) -0.016(3) C12B 0.053(4) 0.054(4) 0.042(3) -0.015(3) 0.018(3) -0.020(3) Te2 0.02684(16) 0.03181(17) 0.03467(18) -0.00402(13) -0.00306(13) -0.00652(12) Br1B 0.0326(3) 0.0412(3) 0.0587(4) -0.0057(3) 0.0046(2) -0.0163(2) Br2B 0.0923(5) 0.0463(3) 0.0465(4) 0.0060(3) -0.0201(3) -0.0387(3) N1C 0.046(4) 0.028(4) 0.013(3) -0.003(2) 0.003(3) -0.020(3) N2C 0.036(3) 0.039(4) 0.035(3) -0.008(3) -0.009(3) -0.003(3) C1C 0.022(3) 0.035(3) 0.030(3) -0.007(2) -0.004(2) -0.012(3) C2C 0.033(3) 0.051(8) 0.031(3) -0.007(4) 0.008(2) -0.028(4) C3C 0.019(3) 0.051(7) 0.078(6) -0.035(6) 0.014(3) -0.022(3) C4C 0.028(5) 0.044(5) 0.067(6) -0.012(4) -0.015(5) -0.018(4) C5C 0.047(7) 0.050(5) 0.035(4) 0.001(3) -0.014(5) -0.027(7) C6C 0.030(5) 0.026(5) 0.034(3) -0.005(2) 0.004(3) -0.014(6) C7C 0.025(4) 0.036(6) 0.068(8) -0.033(6) 0.003(4) -0.004(3) C8C 0.042(4) 0.032(4) 0.044(6) -0.011(5) -0.008(5) -0.002(3) C9C 0.048(7) 0.051(4) 0.048(7) -0.012(5) 0.011(4) -0.016(5) C10C 0.033(4) 0.054(4) 0.053(4) -0.018(3) 0.010(4) -0.015(4) C11C 0.028(3) 0.044(5) 0.052(4) -0.017(4) 0.007(3) -0.007(3) C12C 0.033(6) 0.031(7) 0.049(5) -0.011(4) 0.013(4) -0.012(4) N1E 0.046(4) 0.028(4) 0.013(3) -0.003(2) 0.003(3) -0.020(3) N2E 0.036(3) 0.039(4) 0.035(3) -0.008(3) -0.009(3) -0.003(3) C1E 0.022(3) 0.035(3) 0.030(3) -0.007(2) -0.004(2) -0.012(3) C2E 0.033(3) 0.051(8) 0.031(3) -0.007(4) 0.008(2) -0.028(4) C3E 0.019(3) 0.051(7) 0.078(6) -0.035(6) 0.014(3) -0.022(3) C4E 0.028(5) 0.044(5) 0.067(6) -0.012(4) -0.015(5) -0.018(4) C5E 0.047(7) 0.050(5) 0.035(4) 0.001(3) -0.014(5) -0.027(7) C6E 0.030(5) 0.026(5) 0.034(3) -0.005(2) 0.004(3) -0.014(6) C7E 0.025(4) 0.036(6) 0.068(8) -0.033(6) 0.003(4) -0.004(3) C8E 0.042(4) 0.032(4) 0.044(6) -0.011(5) -0.008(5) -0.002(3) C9E 0.048(7) 0.051(4) 0.048(7) -0.012(5) 0.011(4) -0.016(5) C10E 0.033(4) 0.054(4) 0.053(4) -0.018(3) 0.010(4) -0.015(4) C11E 0.028(3) 0.044(5) 0.052(4) -0.017(4) 0.007(3) -0.007(3) C12E 0.033(6) 0.031(7) 0.049(5) -0.011(4) 0.013(4) -0.012(4) N1D 0.042(3) 0.047(3) 0.039(3) -0.011(2) -0.002(2) -0.012(2) N2D 0.036(2) 0.038(2) 0.040(3) -0.008(2) -0.011(2) -0.0105(19) C1D 0.025(2) 0.039(3) 0.033(3) -0.010(2) -0.0034(19) -0.015(2) C2D 0.037(3) 0.032(3) 0.050(3) -0.009(2) 0.005(2) -0.015(2) C3D 0.041(3) 0.036(3) 0.058(4) -0.020(3) 0.009(3) -0.010(2) C4D 0.055(4) 0.064(4) 0.051(4) -0.026(3) 0.017(3) -0.037(3) C5D 0.039(3) 0.058(4) 0.045(3) -0.018(3) 0.003(3) -0.022(3) C6D 0.026(2) 0.044(3) 0.036(3) -0.014(2) 0.001(2) -0.011(2) C7D 0.035(3) 0.029(3) 0.053(3) -0.005(2) -0.013(2) -0.009(2) C8D 0.043(3) 0.055(4) 0.057(4) 0.003(3) -0.015(3) -0.008(3) C9D 0.065(5) 0.056(4) 0.078(5) 0.004(4) -0.033(4) -0.012(4) C10D 0.045(4) 0.042(4) 0.105(6) -0.021(4) -0.021(4) -0.004(3) C11D 0.044(4) 0.068(5) 0.089(5) -0.042(4) -0.008(4) 0.000(3) C12D 0.051(4) 0.062(4) 0.055(4) -0.023(3) -0.019(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 C1A 2.148(5) . ? Te1 C1B 2.150(5) . ? Te1 Br2A 2.6592(6) . ? Te1 Br1A 2.6944(6) . ? Te1 N2B 2.776(5) . ? Te1 N2A 2.864(4) . ? N1A N2A 1.226(5) . ? N1A C6A 1.420(6) . ? N2A C7A 1.431(6) . ? N1B N2B 1.238(6) . ? N1B C6B 1.416(7) . ? N2B C7B 1.426(7) . ? C1A C2A 1.395(7) . ? C1A C6A 1.397(7) . ? C2A C3A 1.396(8) . ? C2A H2AA 0.9500 . ? C3A C4A 1.372(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.379(8) . ? C4A H4AA 0.9500 . ? C5A C6A 1.393(7) . ? C5A H5AA 0.9500 . ? C7A C8A 1.379(8) . ? C7A C12A 1.388(8) . ? C8A C9A 1.386(8) . ? C8A H8AA 0.9500 . ? C9A C10A 1.383(10) . ? C9A H9AA 0.9500 . ? C10A C11A 1.373(9) . ? C10A H10A 0.9500 . ? C11A C12A 1.354(8) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C2B 1.374(8) . ? C1B C6B 1.399(8) . ? C2B C3B 1.397(8) . ? C2B H2BA 0.9500 . ? C3B C4B 1.374(10) . ? C3B H3BA 0.9500 . ? C4B C5B 1.363(10) . ? C4B H4BA 0.9500 . ? C5B C6B 1.379(8) . ? C5B H5BA 0.9500 . ? C7B C12B 1.374(8) . ? C7B C8B 1.392(8) . ? C8B C9B 1.374(9) . ? C8B H8BA 0.9500 . ? C9B C10B 1.374(10) . ? C9B H9BA 0.9500 . ? C10B C11B 1.367(9) . ? C10B H10B 0.9500 . ? C11B C12B 1.377(8) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? Te2 C1C 2.089(11) . ? Te2 C1D 2.137(5) . ? Te2 C1E 2.26(2) . ? Te2 Br2B 2.6620(7) . ? Te2 Br1B 2.6821(6) . ? Te2 N2D 2.754(4) . ? Te2 N1C 2.871(6) . ? Te2 N2E 2.986(14) . ? N1C N2C 1.215(8) . ? N1C C6C 1.472(8) . ? N2C C7C 1.413(8) . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C2C H2CA 0.9500 . ? C3C C4C 1.3900 . ? C3C H3CA 0.9500 . ? C4C C5C 1.3900 . ? C4C H4CA 0.9500 . ? C5C C6C 1.3900 . ? C5C H5CA 0.9500 . ? C7C C8C 1.3900 . ? C7C C12C 1.3900 . ? C8C C9C 1.3900 . ? C8C H8CA 0.9500 . ? C9C C10C 1.3900 . ? C9C H9CA 0.9500 . ? C10C C11C 1.3900 . ? C10C H10C 0.9500 . ? C11C C12C 1.3900 . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? N1E N2E 1.289(13) . ? N1E C6E 1.488(12) . ? N2E C7E 1.357(13) . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C2E C3E 1.3900 . ? C2E H2EA 0.9500 . ? C3E C4E 1.3900 . ? C3E H3EA 0.9500 . ? C4E C5E 1.3900 . ? C4E H4EA 0.9500 . ? C5E C6E 1.3900 . ? C5E H5EA 0.9500 . ? C7E C8E 1.3900 . ? C7E C12E 1.3900 . ? C8E C9E 1.3900 . ? C8E H8EA 0.9500 . ? C9E C10E 1.3900 . ? C9E H9EA 0.9500 . ? C10E C11E 1.3900 . ? C10E H10D 0.9500 . ? C11E C12E 1.3900 . ? C11E H11D 0.9500 . ? C12E H12D 0.9500 . ? N1D N2D 1.235(6) . ? N1D C6D 1.406(6) . ? N2D C7D 1.434(6) . ? C1D C2D 1.381(7) . ? C1D C6D 1.399(7) . ? C2D C3D 1.393(7) . ? C2D H2DA 0.9500 . ? C3D C4D 1.382(8) . ? C3D H3DA 0.9500 . ? C4D C5D 1.381(8) . ? C4D H4DA 0.9500 . ? C5D C6D 1.384(7) . ? C5D H5DA 0.9500 . ? C7D C12D 1.361(8) . ? C7D C8D 1.386(8) . ? C8D C9D 1.370(9) . ? C8D H8DA 0.9500 . ? C9D C10D 1.377(10) . ? C9D H9DA 0.9500 . ? C10D C11D 1.351(10) . ? C10D H10E 0.9500 . ? C11D C12D 1.385(8) . ? C11D H11E 0.9500 . ? C12D H12F 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Te1 C1B 96.0(2) . . ? C1A Te1 Br2A 88.13(14) . . ? C1B Te1 Br2A 88.32(13) . . ? C1A Te1 Br1A 92.59(13) . . ? C1B Te1 Br1A 84.53(13) . . ? Br2A Te1 Br1A 172.86(2) . . ? C1A Te1 N2B 155.12(17) . . ? C1B Te1 N2B 67.13(18) . . ? Br2A Te1 N2B 73.78(9) . . ? Br1A Te1 N2B 103.31(9) . . ? C1A Te1 N2A 64.61(16) . . ? C1B Te1 N2A 147.89(17) . . ? Br2A Te1 N2A 114.77(8) . . ? Br1A Te1 N2A 71.82(8) . . ? N2B Te1 N2A 138.52(13) . . ? N2A N1A C6A 112.4(4) . . ? N1A N2A C7A 114.2(4) . . ? N1A N2A Te1 107.6(3) . . ? C7A N2A Te1 129.7(3) . . ? N2B N1B C6B 114.4(5) . . ? N1B N2B C7B 115.8(5) . . ? N1B N2B Te1 109.5(4) . . ? C7B N2B Te1 132.6(3) . . ? C2A C1A C6A 118.7(5) . . ? C2A C1A Te1 119.3(4) . . ? C6A C1A Te1 121.9(4) . . ? C1A C2A C3A 119.9(5) . . ? C1A C2A H2AA 120.0 . . ? C3A C2A H2AA 120.0 . . ? C4A C3A C2A 121.0(5) . . ? C4A C3A H3AA 119.5 . . ? C2A C3A H3AA 119.5 . . ? C3A C4A C5A 119.4(5) . . ? C3A C4A H4AA 120.3 . . ? C5A C4A H4AA 120.3 . . ? C4A C5A C6A 120.7(5) . . ? C4A C5A H5AA 119.7 . . ? C6A C5A H5AA 119.7 . . ? C5A C6A C1A 120.2(5) . . ? C5A C6A N1A 113.6(4) . . ? C1A C6A N1A 126.2(4) . . ? C8A C7A C12A 119.9(5) . . ? C8A C7A N2A 123.3(5) . . ? C12A C7A N2A 116.7(5) . . ? C7A C8A C9A 119.5(6) . . ? C7A C8A H8AA 120.2 . . ? C9A C8A H8AA 120.2 . . ? C10A C9A C8A 119.5(6) . . ? C10A C9A H9AA 120.2 . . ? C8A C9A H9AA 120.2 . . ? C11A C10A C9A 120.3(6) . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C12A C11A C10A 120.4(6) . . ? C12A C11A H11A 119.8 . . ? C10A C11A H11A 119.8 . . ? C11A C12A C7A 120.3(6) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C2B C1B C6B 120.4(5) . . ? C2B C1B Te1 119.8(4) . . ? C6B C1B Te1 119.8(4) . . ? C1B C2B C3B 119.3(6) . . ? C1B C2B H2BA 120.3 . . ? C3B C2B H2BA 120.3 . . ? C4B C3B C2B 119.6(6) . . ? C4B C3B H3BA 120.2 . . ? C2B C3B H3BA 120.2 . . ? C5B C4B C3B 121.2(6) . . ? C5B C4B H4BA 119.4 . . ? C3B C4B H4BA 119.4 . . ? C4B C5B C6B 120.1(7) . . ? C4B C5B H5BA 120.0 . . ? C6B C5B H5BA 120.0 . . ? C5B C6B C1B 119.3(6) . . ? C5B C6B N1B 113.9(6) . . ? C1B C6B N1B 126.8(5) . . ? C12B C7B C8B 119.3(6) . . ? C12B C7B N2B 116.7(5) . . ? C8B C7B N2B 124.1(6) . . ? C9B C8B C7B 119.5(7) . . ? C9B C8B H8BA 120.3 . . ? C7B C8B H8BA 120.3 . . ? C10B C9B C8B 121.1(6) . . ? C10B C9B H9BA 119.4 . . ? C8B C9B H9BA 119.4 . . ? C11B C10B C9B 119.1(7) . . ? C11B C10B H10B 120.5 . . ? C9B C10B H10B 120.5 . . ? C10B C11B C12B 120.8(7) . . ? C10B C11B H11B 119.6 . . ? C12B C11B H11B 119.6 . . ? C7B C12B C11B 120.3(6) . . ? C7B C12B H12B 119.9 . . ? C11B C12B H12B 119.9 . . ? C1C Te2 C1D 96.6(4) . . ? C1C Te2 C1E 2.8(15) . . ? C1D Te2 C1E 96.6(8) . . ? C1C Te2 Br2B 88.2(5) . . ? C1D Te2 Br2B 87.15(13) . . ? C1E Te2 Br2B 85.4(9) . . ? C1C Te2 Br1B 92.3(5) . . ? C1D Te2 Br1B 84.90(13) . . ? C1E Te2 Br1B 95.1(10) . . ? Br2B Te2 Br1B 172.03(3) . . ? C1C Te2 N2D 156.6(3) . . ? C1D Te2 N2D 66.92(16) . . ? C1E Te2 N2D 154.7(5) . . ? Br2B Te2 N2D 75.04(9) . . ? Br1B Te2 N2D 102.11(9) . . ? C1C Te2 N1C 53.7(3) . . ? C1D Te2 N1C 140.33(19) . . ? C1E Te2 N1C 55.0(5) . . ? Br2B Te2 N1C 113.90(13) . . ? Br1B Te2 N1C 72.46(13) . . ? N2D Te2 N1C 148.57(17) . . ? C1C Te2 N2E 64.7(4) . . ? C1D Te2 N2E 148.9(3) . . ? C1E Te2 N2E 65.9(5) . . ? Br2B Te2 N2E 115.2(3) . . ? Br1B Te2 N2E 72.0(3) . . ? N2D Te2 N2E 137.3(2) . . ? N1C Te2 N2E 11.3(2) . . ? N2C N1C C6C 109.9(7) . . ? N2C N1C Te2 160.9(6) . . ? C6C N1C Te2 79.6(5) . . ? N1C N2C C7C 108.1(6) . . ? C2C C1C C6C 120.0 . . ? C2C C1C Te2 123.5(5) . . ? C6C C1C Te2 116.5(5) . . ? C3C C2C C1C 120.0 . . ? C3C C2C H2CA 120.0 . . ? C1C C2C H2CA 120.0 . . ? C4C C3C C2C 120.0 . . ? C4C C3C H3CA 120.0 . . ? C2C C3C H3CA 120.0 . . ? C3C C4C C5C 120.0 . . ? C3C C4C H4CA 120.0 . . ? C5C C4C H4CA 120.0 . . ? C6C C5C C4C 120.0 . . ? C6C C5C H5CA 120.0 . . ? C4C C5C H5CA 120.0 . . ? C5C C6C C1C 120.0 . . ? C5C C6C N1C 129.7(6) . . ? C1C C6C N1C 110.0(6) . . ? C8C C7C C12C 120.0 . . ? C8C C7C N2C 112.0(5) . . ? C12C C7C N2C 127.9(5) . . ? C9C C8C C7C 120.0 . . ? C9C C8C H8CA 120.0 . . ? C7C C8C H8CA 120.0 . . ? C10C C9C C8C 120.0 . . ? C10C C9C H9CA 120.0 . . ? C8C C9C H9CA 120.0 . . ? C11C C10C C9C 120.0 . . ? C11C C10C H10C 120.0 . . ? C9C C10C H10C 120.0 . . ? C10C C11C C12C 120.0 . . ? C10C C11C H11C 120.0 . . ? C12C C11C H11C 120.0 . . ? C11C C12C C7C 120.0 . . ? C11C C12C H12C 120.0 . . ? C7C C12C H12C 120.0 . . ? N2E N1E C6E 116.1(13) . . ? N1E N2E C7E 118.6(12) . . ? N1E N2E Te2 104.5(8) . . ? C7E N2E Te2 131.6(10) . . ? C2E C1E C6E 120.0 . . ? C2E C1E Te2 119.5(9) . . ? C6E C1E Te2 120.5(9) . . ? C1E C2E C3E 120.0 . . ? C1E C2E H2EA 120.0 . . ? C3E C2E H2EA 120.0 . . ? C4E C3E C2E 120.0 . . ? C4E C3E H3EA 120.0 . . ? C2E C3E H3EA 120.0 . . ? C5E C4E C3E 120.0 . . ? C5E C4E H4EA 120.0 . . ? C3E C4E H4EA 120.0 . . ? C4E C5E C6E 120.0 . . ? C4E C5E H5EA 120.0 . . ? C6E C5E H5EA 120.0 . . ? C5E C6E C1E 120.0 . . ? C5E C6E N1E 111.9(12) . . ? C1E C6E N1E 127.6(12) . . ? N2E C7E C8E 119.6(11) . . ? N2E C7E C12E 120.4(11) . . ? C8E C7E C12E 120.0 . . ? C9E C8E C7E 120.0 . . ? C9E C8E H8EA 120.0 . . ? C7E C8E H8EA 120.0 . . ? C10E C9E C8E 120.0 . . ? C10E C9E H9EA 120.0 . . ? C8E C9E H9EA 120.0 . . ? C9E C10E C11E 120.0 . . ? C9E C10E H10D 120.0 . . ? C11E C10E H10D 120.0 . . ? C12E C11E C10E 120.0 . . ? C12E C11E H11D 120.0 . . ? C10E C11E H11D 120.0 . . ? C11E C12E C7E 120.0 . . ? C11E C12E H12D 120.0 . . ? C7E C12E H12D 120.0 . . ? N2D N1D C6D 113.9(4) . . ? N1D N2D C7D 117.0(4) . . ? N1D N2D Te2 110.8(3) . . ? C7D N2D Te2 131.0(3) . . ? C2D C1D C6D 119.9(5) . . ? C2D C1D Te2 120.0(4) . . ? C6D C1D Te2 120.1(4) . . ? C1D C2D C3D 120.4(5) . . ? C1D C2D H2DA 119.8 . . ? C3D C2D H2DA 119.8 . . ? C4D C3D C2D 119.6(5) . . ? C4D C3D H3DA 120.2 . . ? C2D C3D H3DA 120.2 . . ? C5D C4D C3D 120.1(6) . . ? C5D C4D H4DA 120.0 . . ? C3D C4D H4DA 120.0 . . ? C4D C5D C6D 120.9(6) . . ? C4D C5D H5DA 119.6 . . ? C6D C5D H5DA 119.6 . . ? C5D C6D C1D 119.1(5) . . ? C5D C6D N1D 114.1(5) . . ? C1D C6D N1D 126.7(5) . . ? C12D C7D C8D 120.3(5) . . ? C12D C7D N2D 117.2(5) . . ? C8D C7D N2D 122.5(5) . . ? C9D C8D C7D 118.6(7) . . ? C9D C8D H8DA 120.7 . . ? C7D C8D H8DA 120.7 . . ? C8D C9D C10D 120.9(7) . . ? C8D C9D H9DA 119.6 . . ? C10D C9D H9DA 119.6 . . ? C11D C10D C9D 120.3(6) . . ? C11D C10D H10E 119.8 . . ? C9D C10D H10E 119.8 . . ? C10D C11D C12D 119.5(7) . . ? C10D C11D H11E 120.3 . . ? C12D C11D H11E 120.3 . . ? C7D C12D C11D 120.5(6) . . ? C7D C12D H12F 119.8 . . ? C11D C12D H12F 119.8 . . ? 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 C6A N1A N2A C7A -178.5(4) . . . . ? C6A N1A N2A Te1 -27.1(4) . . . . ? C1A Te1 N2A N1A 23.0(3) . . . . ? C1B Te1 N2A N1A -34.5(5) . . . . ? Br2A Te1 N2A N1A 98.0(3) . . . . ? Br1A Te1 N2A N1A -79.1(3) . . . . ? N2B Te1 N2A N1A -168.7(3) . . . . ? C1A Te1 N2A C7A 168.3(4) . . . . ? C1B Te1 N2A C7A 110.9(5) . . . . ? Br2A Te1 N2A C7A -116.7(4) . . . . ? Br1A Te1 N2A C7A 66.3(4) . . . . ? N2B Te1 N2A C7A -23.4(5) . . . . ? C6B N1B N2B C7B 178.8(4) . . . . ? C6B N1B N2B Te1 -15.7(5) . . . . ? C1A Te1 N2B N1B -36.4(6) . . . . ? C1B Te1 N2B N1B 13.8(3) . . . . ? Br2A Te1 N2B N1B -81.3(3) . . . . ? Br1A Te1 N2B N1B 92.0(3) . . . . ? N2A Te1 N2B N1B 169.4(3) . . . . ? C1A Te1 N2B C7B 125.8(5) . . . . ? C1B Te1 N2B C7B 176.0(5) . . . . ? Br2A Te1 N2B C7B 80.9(4) . . . . ? Br1A Te1 N2B C7B -105.9(4) . . . . ? N2A Te1 N2B C7B -28.4(5) . . . . ? C1B Te1 C1A C2A -39.5(4) . . . . ? Br2A Te1 C1A C2A 48.7(4) . . . . ? Br1A Te1 C1A C2A -124.2(4) . . . . ? N2B Te1 C1A C2A 5.9(7) . . . . ? N2A Te1 C1A C2A 167.3(5) . . . . ? C1B Te1 C1A C6A 141.4(4) . . . . ? Br2A Te1 C1A C6A -130.5(4) . . . . ? Br1A Te1 C1A C6A 56.6(4) . . . . ? N2B Te1 C1A C6A -173.2(3) . . . . ? N2A Te1 C1A C6A -11.9(3) . . . . ? C6A C1A C2A C3A -1.5(8) . . . . ? Te1 C1A C2A C3A 179.3(4) . . . . ? C1A C2A C3A C4A -1.0(8) . . . . ? C2A C3A C4A C5A 2.2(8) . . . . ? C3A C4A C5A C6A -0.9(8) . . . . ? C4A C5A C6A C1A -1.6(7) . . . . ? C4A C5A C6A N1A 177.5(5) . . . . ? C2A C1A C6A C5A 2.8(7) . . . . ? Te1 C1A C6A C5A -178.0(4) . . . . ? C2A C1A C6A N1A -176.2(5) . . . . ? Te1 C1A C6A N1A 3.0(7) . . . . ? N2A N1A C6A C5A -157.3(4) . . . . ? N2A N1A C6A C1A 21.8(7) . . . . ? N1A N2A C7A C8A 24.5(7) . . . . ? Te1 N2A C7A C8A -119.1(5) . . . . ? N1A N2A C7A C12A -157.7(5) . . . . ? Te1 N2A C7A C12A 58.7(6) . . . . ? C12A C7A C8A C9A 1.8(8) . . . . ? N2A C7A C8A C9A 179.6(5) . . . . ? C7A C8A C9A C10A -0.1(9) . . . . ? C8A C9A C10A C11A -1.1(10) . . . . ? C9A C10A C11A C12A 0.6(10) . . . . ? C10A C11A C12A C7A 1.2(9) . . . . ? C8A C7A C12A C11A -2.4(8) . . . . ? N2A C7A C12A C11A 179.7(5) . . . . ? C1A Te1 C1B C2B -28.8(4) . . . . ? Br2A Te1 C1B C2B -116.7(4) . . . . ? Br1A Te1 C1B C2B 63.2(4) . . . . ? N2B Te1 C1B C2B 170.2(5) . . . . ? N2A Te1 C1B C2B 21.2(6) . . . . ? C1A Te1 C1B C6B 152.9(4) . . . . ? Br2A Te1 C1B C6B 64.9(4) . . . . ? Br1A Te1 C1B C6B -115.1(4) . . . . ? N2B Te1 C1B C6B -8.1(3) . . . . ? N2A Te1 C1B C6B -157.2(3) . . . . ? C6B C1B C2B C3B -2.3(8) . . . . ? Te1 C1B C2B C3B 179.4(4) . . . . ? C1B C2B C3B C4B -0.2(8) . . . . ? C2B C3B C4B C5B 0.8(9) . . . . ? C3B C4B C5B C6B 1.1(9) . . . . ? C4B C5B C6B C1B -3.6(8) . . . . ? C4B C5B C6B N1B 175.2(5) . . . . ? C2B C1B C6B C5B 4.2(7) . . . . ? Te1 C1B C6B C5B -177.5(4) . . . . ? C2B C1B C6B N1B -174.4(5) . . . . ? Te1 C1B C6B N1B 3.9(7) . . . . ? N2B N1B C6B C5B -167.8(5) . . . . ? N2B N1B C6B C1B 10.9(7) . . . . ? N1B N2B C7B C12B 172.7(5) . . . . ? Te1 N2B C7B C12B 11.4(7) . . . . ? N1B N2B C7B C8B -9.1(8) . . . . ? Te1 N2B C7B C8B -170.4(4) . . . . ? C12B C7B C8B C9B -0.7(9) . . . . ? N2B C7B C8B C9B -178.9(6) . . . . ? C7B C8B C9B C10B 0.2(10) . . . . ? C8B C9B C10B C11B 0.7(10) . . . . ? C9B C10B C11B C12B -1.1(10) . . . . ? C8B C7B C12B C11B 0.3(9) . . . . ? N2B C7B C12B C11B 178.7(5) . . . . ? C10B C11B C12B C7B 0.5(9) . . . . ? C1C Te2 N1C N2C -124.2(19) . . . . ? C1D Te2 N1C N2C -75.9(17) . . . . ? C1E Te2 N1C N2C -127(2) . . . . ? Br2B Te2 N1C N2C 167.4(16) . . . . ? Br1B Te2 N1C N2C -17.7(16) . . . . ? N2D Te2 N1C N2C 66.9(17) . . . . ? N2E Te2 N1C N2C 68(2) . . . . ? C1C Te2 N1C C6C -2.2(5) . . . . ? C1D Te2 N1C C6C 46.1(10) . . . . ? C1E Te2 N1C C6C -5(2) . . . . ? Br2B Te2 N1C C6C -70.5(10) . . . . ? Br1B Te2 N1C C6C 104.3(10) . . . . ? N2D Te2 N1C C6C -171.1(9) . . . . ? N2E Te2 N1C C6C -170(2) . . . . ? C6C N1C N2C C7C 179.2(11) . . . . ? Te2 N1C N2C C7C -63.4(18) . . . . ? C1D Te2 C1C C2C 32.0(11) . . . . ? C1E Te2 C1C C2C -60(22) . . . . ? Br2B Te2 C1C C2C -54.9(10) . . . . ? Br1B Te2 C1C C2C 117.1(10) . . . . ? N2D Te2 C1C C2C -11(2) . . . . ? N1C Te2 C1C C2C -176.7(14) . . . . ? N2E Te2 C1C C2C -174.0(13) . . . . ? C1D Te2 C1C C6C -148.7(6) . . . . ? C1E Te2 C1C C6C 120(23) . . . . ? Br2B Te2 C1C C6C 124.3(7) . . . . ? Br1B Te2 C1C C6C -63.6(7) . . . . ? N2D Te2 C1C C6C 168.0(11) . . . . ? N1C Te2 C1C C6C 2.6(6) . . . . ? N2E Te2 C1C C6C 5.3(6) . . . . ? C6C C1C C2C C3C 0.0 . . . . ? Te2 C1C C2C C3C 179.3(14) . . . . ? C1C C2C C3C C4C 0.0 . . . . ? C2C C3C C4C C5C 0.0 . . . . ? C3C C4C C5C C6C 0.0 . . . . ? C4C C5C C6C C1C 0.0 . . . . ? C4C C5C C6C N1C -173.9(19) . . . . ? C2C C1C C6C C5C 0.0 . . . . ? Te2 C1C C6C C5C -179.3(13) . . . . ? C2C C1C C6C N1C 175.0(16) . . . . ? Te2 C1C C6C N1C -4.3(9) . . . . ? N2C N1C C6C C5C -20.0(18) . . . . ? Te2 N1C C6C C5C 177.2(15) . . . . ? N2C N1C C6C C1C 165.7(7) . . . . ? Te2 N1C C6C C1C 2.8(6) . . . . ? N1C N2C C7C C8C 160.7(6) . . . . ? N1C N2C C7C C12C -22.3(11) . . . . ? C12C C7C C8C C9C 0.0 . . . . ? N2C C7C C8C C9C 177.2(9) . . . . ? C7C C8C C9C C10C 0.0 . . . . ? C8C C9C C10C C11C 0.0 . . . . ? C9C C10C C11C C12C 0.0 . . . . ? C10C C11C C12C C7C 0.0 . . . . ? C8C C7C C12C C11C 0.0 . . . . ? N2C C7C C12C C11C -176.7(11) . . . . ? C6E N1E N2E C7E 179(2) . . . . ? C6E N1E N2E Te2 22(2) . . . . ? C1C Te2 N2E N1E -17.4(12) . . . . ? C1D Te2 N2E N1E 40.1(15) . . . . ? C1E Te2 N2E N1E -20.1(16) . . . . ? Br2B Te2 N2E N1E -92.3(11) . . . . ? Br1B Te2 N2E N1E 84.1(11) . . . . ? N2D Te2 N2E N1E 172.7(8) . . . . ? N1C Te2 N2E N1E -6.2(13) . . . . ? C1C Te2 N2E C7E -170.3(18) . . . . ? C1D Te2 N2E C7E -112.8(14) . . . . ? C1E Te2 N2E C7E -173(2) . . . . ? Br2B Te2 N2E C7E 114.8(15) . . . . ? Br1B Te2 N2E C7E -68.8(15) . . . . ? N2D Te2 N2E C7E 19.7(18) . . . . ? N1C Te2 N2E C7E -159(3) . . . . ? C1C Te2 C1E C2E 129(24) . . . . ? C1D Te2 C1E C2E 40.2(19) . . . . ? Br2B Te2 C1E C2E -46.4(18) . . . . ? Br1B Te2 C1E C2E 125.6(18) . . . . ? N2D Te2 C1E C2E -7(4) . . . . ? N1C Te2 C1E C2E -170(3) . . . . ? N2E Te2 C1E C2E -167(2) . . . . ? C1C Te2 C1E C6E -51(22) . . . . ? C1D Te2 C1E C6E -139.4(14) . . . . ? Br2B Te2 C1E C6E 134.0(15) . . . . ? Br1B Te2 C1E C6E -54.0(15) . . . . ? N2D Te2 C1E C6E 173.2(19) . . . . ? N1C Te2 C1E C6E 10.4(12) . . . . ? N2E Te2 C1E C6E 13.7(13) . . . . ? C6E C1E C2E C3E 0.0 . . . . ? Te2 C1E C2E C3E -180(3) . . . . ? C1E C2E C3E C4E 0.0 . . . . ? C2E C3E C4E C5E 0.0 . . . . ? C3E C4E C5E C6E 0.0 . . . . ? C4E C5E C6E C1E 0.0 . . . . ? C4E C5E C6E N1E -173(3) . . . . ? C2E C1E C6E C5E 0.0 . . . . ? Te2 C1E C6E C5E 180(3) . . . . ? C2E C1E C6E N1E 171(4) . . . . ? Te2 C1E C6E N1E -9(3) . . . . ? N2E N1E C6E C5E 157.6(17) . . . . ? N2E N1E C6E C1E -14(3) . . . . ? N1E N2E C7E C8E -21(2) . . . . ? Te2 N2E C7E C8E 129.1(12) . . . . ? N1E N2E C7E C12E 157.4(16) . . . . ? Te2 N2E C7E C12E -53(2) . . . . ? N2E C7E C8E C9E 178(2) . . . . ? C12E C7E C8E C9E 0.0 . . . . ? C7E C8E C9E C10E 0.0 . . . . ? C8E C9E C10E C11E 0.0 . . . . ? C9E C10E C11E C12E 0.0 . . . . ? C10E C11E C12E C7E 0.0 . . . . ? N2E C7E C12E C11E -178(2) . . . . ? C8E C7E C12E C11E 0.0 . . . . ? C6D N1D N2D C7D -179.2(4) . . . . ? C6D N1D N2D Te2 11.9(5) . . . . ? C1C Te2 N2D N1D 36.3(16) . . . . ? C1D Te2 N2D N1D -11.5(3) . . . . ? C1E Te2 N2D N1D 41(3) . . . . ? Br2B Te2 N2D N1D 81.8(3) . . . . ? Br1B Te2 N2D N1D -90.5(3) . . . . ? N1C Te2 N2D N1D -166.6(4) . . . . ? N2E Te2 N2D N1D -167.1(6) . . . . ? C1C Te2 N2D C7D -130.5(16) . . . . ? C1D Te2 N2D C7D -178.3(5) . . . . ? C1E Te2 N2D C7D -126(3) . . . . ? Br2B Te2 N2D C7D -85.0(4) . . . . ? Br1B Te2 N2D C7D 102.7(4) . . . . ? N1C Te2 N2D C7D 26.5(6) . . . . ? N2E Te2 N2D C7D 26.1(7) . . . . ? C1C Te2 C1D C2D 25.6(7) . . . . ? C1E Te2 C1D C2D 28.4(10) . . . . ? Br2B Te2 C1D C2D 113.4(4) . . . . ? Br1B Te2 C1D C2D -66.1(4) . . . . ? N2D Te2 C1D C2D -171.6(4) . . . . ? N1C Te2 C1D C2D -11.7(5) . . . . ? N2E Te2 C1D C2D -24.5(8) . . . . ? C1C Te2 C1D C6D -155.0(6) . . . . ? C1E Te2 C1D C6D -152.2(10) . . . . ? Br2B Te2 C1D C6D -67.2(4) . . . . ? Br1B Te2 C1D C6D 113.3(4) . . . . ? N2D Te2 C1D C6D 7.8(3) . . . . ? N1C Te2 C1D C6D 167.7(3) . . . . ? N2E Te2 C1D C6D 154.9(6) . . . . ? C6D C1D C2D C3D 4.3(7) . . . . ? Te2 C1D C2D C3D -176.3(4) . . . . ? C1D C2D C3D C4D -2.3(8) . . . . ? C2D C3D C4D C5D -0.2(8) . . . . ? C3D C4D C5D C6D 0.7(8) . . . . ? C4D C5D C6D C1D 1.2(8) . . . . ? C4D C5D C6D N1D -176.6(5) . . . . ? C2D C1D C6D C5D -3.7(7) . . . . ? Te2 C1D C6D C5D 176.8(4) . . . . ? C2D C1D C6D N1D 173.8(5) . . . . ? Te2 C1D C6D N1D -5.6(7) . . . . ? N2D N1D C6D C5D 171.1(5) . . . . ? N2D N1D C6D C1D -6.6(8) . . . . ? N1D N2D C7D C12D -179.5(5) . . . . ? Te2 N2D C7D C12D -13.3(7) . . . . ? N1D N2D C7D C8D 0.8(8) . . . . ? Te2 N2D C7D C8D 167.0(4) . . . . ? C12D C7D C8D C9D -1.4(9) . . . . ? N2D C7D C8D C9D 178.3(6) . . . . ? C7D C8D C9D C10D 2.0(10) . . . . ? C8D C9D C10D C11D -1.5(11) . . . . ? C9D C10D C11D C12D 0.5(11) . . . . ? C8D C7D C12D C11D 0.3(9) . . . . ? N2D C7D C12D C11D -179.4(6) . . . . ? C10D C11D C12D C7D 0.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.168 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.157 #===END data_azotei4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 I N4 Te, I3' _chemical_formula_sum 'C24 H18 I4 N4 Te' _chemical_formula_weight 997.62 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' 'I' 'I' -0.4742 1.8119 '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' _cell_length_a 8.468 _cell_length_b 8.927 _cell_length_c 19.089 _cell_angle_alpha 102.77 _cell_angle_beta 96.82 _cell_angle_gamma 95.65 _cell_volume 1385.7 _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 15944 _cell_measurement_theta_min 4.7113 _cell_measurement_theta_max 32.5950 _exptl_crystal_description 'thick needle' _exptl_crystal_colour red-purple _exptl_crystal_size_max 0.5767 _exptl_crystal_size_mid 0.2399 _exptl_crystal_size_min 0.1453 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 5.549 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.040 _exptl_absorpt_correction_T_max 0.244 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby (Gemini Mo) ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 18483 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.72 _diffrn_reflns_theta_max 32.67 _reflns_number_total 13236 _reflns_number_gt 12610 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0480P)^2^+55.9445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(6) _refine_ls_number_reflns 13236 _refine_ls_number_parameters 596 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.006 _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 I11 I 1.38865(15) 1.57430(15) 1.05704(6) 0.0367(3) Uani 1 1 d . . . I12 I 1.31176(11) 1.43280(10) 0.89985(5) 0.01959(16) Uani 1 1 d . . . I13 I 1.23312(13) 1.29638(13) 0.74679(5) 0.0300(2) Uani 1 1 d . . . I21 I 0.81795(11) 0.86284(11) 0.27935(5) 0.02379(19) Uani 1 1 d . . . I22 I 0.94015(10) 0.87757(10) 0.43131(5) 0.01665(15) Uani 1 1 d . . . I23 I 1.08165(13) 0.88343(13) 0.57833(5) 0.0300(2) Uani 1 1 d . . . Te1 Te 0.80387(9) 0.49870(9) 0.49367(4) 0.01249(14) Uani 1 1 d . . . I1 I 0.96645(11) 0.41754(11) 0.61241(5) 0.02052(17) Uani 1 1 d . . . N1A N 0.7494(13) 0.4413(14) 0.3184(7) 0.019(2) Uani 1 1 d . . . N2A N 0.6722(14) 0.4889(13) 0.3692(6) 0.016(2) Uani 1 1 d . . . N3A N 0.4889(14) 0.4477(14) 0.5851(6) 0.018(2) Uani 1 1 d . . . N4A N 0.5723(16) 0.5681(14) 0.5814(6) 0.020(2) Uani 1 1 d . . . C1A C 0.9430(16) 0.3868(13) 0.4156(7) 0.013(2) Uani 1 1 d . . . C2A C 1.0797(17) 0.3241(18) 0.4353(7) 0.020(3) Uani 1 1 d . . . H2AA H 1.1099 0.3199 0.4843 0.024 Uiso 1 1 calc R . . C3A C 1.1734(17) 0.2666(18) 0.3820(8) 0.021(3) Uani 1 1 d . . . H3AA H 1.2717 0.2301 0.3951 0.025 Uiso 1 1 calc R . . C4A C 1.1195(19) 0.263(2) 0.3074(8) 0.025(3) Uani 1 1 d . . . H4AA H 1.1796 0.2202 0.2707 0.030 Uiso 1 1 calc R . . C5A C 0.9836(19) 0.3220(17) 0.2895(7) 0.020(3) Uani 1 1 d . . . H5AA H 0.9478 0.3190 0.2400 0.024 Uiso 1 1 calc R . . C6A C 0.8939(17) 0.3877(14) 0.3435(7) 0.016(2) Uani 1 1 d . . . C7A C 0.5298(17) 0.5526(15) 0.3518(7) 0.016(2) Uani 1 1 d . . . C8A C 0.4734(14) 0.5612(15) 0.2803(7) 0.014(2) Uani 1 1 d . . . H8AA H 0.5363 0.5311 0.2428 0.017 Uiso 1 1 calc R . . C9A C 0.3264(17) 0.613(2) 0.2641(8) 0.025(3) Uani 1 1 d . . . H9AA H 0.2868 0.6171 0.2159 0.029 Uiso 1 1 calc R . . C10A C 0.2390(19) 0.6599(18) 0.3214(8) 0.025(3) Uani 1 1 d . . . H10A H 0.1396 0.6976 0.3116 0.029 Uiso 1 1 calc R . . C11A C 0.2935(16) 0.6526(15) 0.3919(8) 0.017(2) Uani 1 1 d . . . H11A H 0.2311 0.6839 0.4295 0.021 Uiso 1 1 calc R . . C12A C 0.4389(18) 0.5994(16) 0.4073(7) 0.019(3) Uani 1 1 d . . . H12A H 0.4767 0.5948 0.4556 0.023 Uiso 1 1 calc R . . C13A C 0.6277(16) 0.3067(15) 0.4850(7) 0.0153(14) Uani 1 1 d U . . C14A C 0.6329(17) 0.1706(16) 0.4350(7) 0.017(2) Uani 1 1 d . . . H14A H 0.7063 0.1668 0.4008 0.020 Uiso 1 1 calc R . . C15A C 0.5283(18) 0.0364(15) 0.4347(8) 0.020(3) Uani 1 1 d . . . H15A H 0.5321 -0.0574 0.4002 0.024 Uiso 1 1 calc R . . C16A C 0.420(2) 0.040(2) 0.4844(10) 0.030(4) Uani 1 1 d . . . H16A H 0.3508 -0.0502 0.4849 0.036 Uiso 1 1 calc R . . C17A C 0.4150(17) 0.1793(19) 0.5329(8) 0.022(3) Uani 1 1 d . . . H17A H 0.3412 0.1832 0.5669 0.026 Uiso 1 1 calc R . . C18A C 0.5126(16) 0.3122(14) 0.5340(6) 0.014(2) Uani 1 1 d . . . C19A C 0.5509(18) 0.7065(19) 0.6300(8) 0.023(3) Uani 1 1 d . . . C20A C 0.452(2) 0.721(2) 0.6837(9) 0.029(3) Uani 1 1 d . . . H20A H 0.3893 0.6309 0.6892 0.034 Uiso 1 1 calc R . . C21A C 0.444(2) 0.861(2) 0.7286(9) 0.035(4) Uani 1 1 d . . . H21A H 0.3779 0.8664 0.7657 0.042 Uiso 1 1 calc R . . C22A C 0.529(2) 0.992(2) 0.7213(10) 0.037(4) Uani 1 1 d . . . H22A H 0.5252 1.0889 0.7536 0.045 Uiso 1 1 calc R . . C23A C 0.622(2) 0.982(2) 0.6654(11) 0.034(4) Uani 1 1 d . . . H23A H 0.6783 1.0742 0.6585 0.041 Uiso 1 1 calc R . . C24A C 0.635(2) 0.842(2) 0.6198(9) 0.031(4) Uani 1 1 d . . . H24A H 0.6989 0.8370 0.5821 0.037 Uiso 1 1 calc R . . Te2 Te 0.96502(10) 1.34560(11) 1.00296(5) 0.01918(18) Uani 1 1 d . . . I2 I 0.90318(12) 1.54545(13) 1.12756(5) 0.0267(2) Uani 1 1 d . . . N1B N 0.8724(18) 1.2301(15) 0.8288(7) 0.023(3) Uani 1 1 d . . . N2B N 0.9354(15) 1.1762(14) 0.8793(6) 0.017(2) Uani 1 1 d . . . C1B C 0.8392(17) 1.4574(19) 0.9278(8) 0.024(3) Uani 1 1 d . . . C2B C 0.792(2) 1.598(2) 0.9482(10) 0.029(3) Uani 1 1 d . . . H2BA H 0.8054 1.6508 0.9979 0.034 Uiso 1 1 calc R . . C3B C 0.721(2) 1.6644(18) 0.8924(10) 0.027(3) Uani 1 1 d . . . H3BA H 0.6852 1.7633 0.9051 0.032 Uiso 1 1 calc R . . C4B C 0.703(2) 1.588(2) 0.8221(9) 0.028(3) Uani 1 1 d . . . H4BA H 0.6546 1.6349 0.7862 0.034 Uiso 1 1 calc R . . C5B C 0.7533(18) 1.445(2) 0.8003(8) 0.025(3) Uani 1 1 d . . . H5BA H 0.7377 1.3928 0.7505 0.030 Uiso 1 1 calc R . . C6B C 0.8285(18) 1.3793(18) 0.8540(7) 0.020(3) Uani 1 1 d . . . C7B C 0.9892(17) 1.0295(18) 0.8565(7) 0.019(3) Uani 1 1 d . . . C8B C 0.973(2) 0.946(2) 0.7832(11) 0.035(4) Uani 1 1 d . . . H8BA H 0.9256 0.9885 0.7456 0.042 Uiso 1 1 calc R . . C9B C 1.024(3) 0.807(2) 0.7669(11) 0.038(4) Uani 1 1 d . . . H9BA H 1.0123 0.7508 0.7176 0.045 Uiso 1 1 calc R . . C10B C 1.095(2) 0.7421(19) 0.8225(10) 0.027(3) Uani 1 1 d . . . H10B H 1.1328 0.6441 0.8102 0.033 Uiso 1 1 calc R . . C11B C 1.1107(17) 0.8191(19) 0.8929(8) 0.023(3) Uani 1 1 d . . . H11B H 1.1551 0.7731 0.9298 0.027 Uiso 1 1 calc R . . C12B C 1.0619(18) 0.9648(19) 0.9116(8) 0.024(3) Uani 1 1 d . . . H12B H 1.0773 1.0206 0.9609 0.029 Uiso 1 1 calc R . . C13B C 0.7641(17) 1.1813(18) 1.0046(8) 0.020(3) Uani 1 1 d . A . C14B C 0.618(2) 1.1803(18) 0.9669(9) 0.027(3) Uani 1 1 d . . . H14B H 0.6022 1.2548 0.9390 0.033 Uiso 1 1 calc R . . C15B C 0.492(2) 1.074(2) 0.9687(11) 0.033(4) Uani 1 1 d . . . H15B H 0.3907 1.0739 0.9417 0.040 Uiso 1 1 calc R . . C16B C 0.513(2) 0.963(2) 1.0101(11) 0.039(4) Uani 1 1 d . . . H16B H 0.4253 0.8895 1.0123 0.047 Uiso 1 1 calc R . . C17B C 0.669(3) 0.965(2) 1.0490(10) 0.040(4) Uani 1 1 d . A . H17B H 0.6867 0.8899 1.0765 0.048 Uiso 1 1 calc R . . C18B C 0.791(2) 1.074(2) 1.0464(9) 0.032(4) Uani 1 1 d . . . N3B N 0.917(3) 1.028(2) 1.0893(11) 0.0132(12) Uani 0.525(15) 1 d PU A 1 N4B N 1.040(3) 1.133(3) 1.0908(13) 0.0180(12) Uani 0.525(15) 1 d PU A 1 C19B C 1.1857(19) 1.108(2) 1.1314(10) 0.021(4) Uani 0.525(15) 1 d PGU A 1 C20B C 1.208(2) 0.984(2) 1.1625(13) 0.037(6) Uani 0.525(15) 1 d PGU A 1 H20B H 1.1207 0.9053 1.1588 0.044 Uiso 0.525(15) 1 calc PR A 1 C21B C 1.357(3) 0.974(3) 1.1989(14) 0.034(5) Uani 0.525(15) 1 d PGU A 1 H21B H 1.3722 0.8886 1.2202 0.040 Uiso 0.525(15) 1 calc PR A 1 C22B C 1.484(2) 1.089(3) 1.2043(14) 0.025(3) Uani 0.525(15) 1 d PGU A 1 H22B H 1.5865 1.0818 1.2292 0.031 Uiso 0.525(15) 1 calc PR A 1 C23B C 1.462(2) 1.213(3) 1.1732(13) 0.025(4) Uani 0.525(15) 1 d PGU A 1 H23B H 1.5494 1.2917 1.1769 0.030 Uiso 0.525(15) 1 calc PR A 1 C24B C 1.313(2) 1.223(2) 1.1368(11) 0.018(4) Uani 0.525(15) 1 d PGU A 1 H24B H 1.2979 1.3083 1.1155 0.022 Uiso 0.525(15) 1 calc PR A 1 N3C N 0.962(3) 1.113(3) 1.0799(12) 0.0132(12) Uani 0.475(15) 1 d PU A 2 N4C N 1.012(3) 1.014(3) 1.1089(13) 0.0180(12) Uani 0.475(15) 1 d PU A 2 C19C C 1.179(2) 1.047(3) 1.1373(11) 0.021(4) Uani 0.475(15) 1 d PGU A 2 C20C C 1.230(3) 0.953(3) 1.1824(14) 0.037(6) Uani 0.475(15) 1 d PGU A 2 H20C H 1.1583 0.8716 1.1896 0.044 Uiso 0.475(15) 1 calc PR A 2 C21C C 1.388(3) 0.980(3) 1.2171(15) 0.034(5) Uani 0.475(15) 1 d PGU A 2 H21C H 1.4235 0.9157 1.2479 0.040 Uiso 0.475(15) 1 calc PR A 2 C22C C 1.494(2) 1.099(3) 1.2065(16) 0.025(3) Uani 0.475(15) 1 d PGU A 2 H22C H 1.6014 1.1173 1.2302 0.031 Uiso 0.475(15) 1 calc PR A 2 C23C C 1.442(3) 1.193(3) 1.1614(15) 0.025(4) Uani 0.475(15) 1 d PGU A 2 H23C H 1.5141 1.2746 1.1542 0.030 Uiso 0.475(15) 1 calc PR A 2 C24C C 1.284(3) 1.167(3) 1.1268(12) 0.018(4) Uani 0.475(15) 1 d PGU A 2 H24C H 1.2488 1.2305 1.0959 0.022 Uiso 0.475(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I11 0.0402(6) 0.0418(6) 0.0220(4) 0.0035(4) 0.0046(4) -0.0154(5) I12 0.0180(4) 0.0229(4) 0.0214(4) 0.0113(3) 0.0048(3) 0.0038(3) I13 0.0360(5) 0.0392(6) 0.0183(4) 0.0090(4) 0.0040(4) 0.0166(4) I21 0.0239(4) 0.0304(5) 0.0191(4) 0.0089(3) 0.0010(3) 0.0089(4) I22 0.0156(3) 0.0163(3) 0.0194(3) 0.0060(3) 0.0034(3) 0.0034(3) I23 0.0286(5) 0.0419(6) 0.0177(4) 0.0118(4) -0.0008(3) -0.0098(4) Te1 0.0137(3) 0.0126(3) 0.0112(3) 0.0032(3) 0.0019(2) 0.0015(3) I1 0.0245(4) 0.0245(4) 0.0124(3) 0.0054(3) -0.0016(3) 0.0046(3) N1A 0.011(4) 0.022(6) 0.027(5) 0.005(4) 0.014(4) 0.004(4) N2A 0.018(5) 0.019(5) 0.009(4) 0.008(4) -0.003(4) -0.009(4) N3A 0.019(5) 0.019(5) 0.017(5) 0.006(4) 0.007(4) -0.005(4) N4A 0.027(6) 0.019(5) 0.014(5) 0.004(4) 0.003(4) 0.006(5) C1A 0.019(5) 0.006(4) 0.017(5) 0.009(4) 0.005(4) 0.001(4) C2A 0.019(6) 0.031(7) 0.017(5) 0.015(5) 0.011(4) 0.011(5) C3A 0.012(5) 0.025(7) 0.022(6) -0.001(5) -0.001(5) 0.006(5) C4A 0.024(7) 0.036(8) 0.019(6) 0.005(6) 0.009(5) 0.013(6) C5A 0.030(7) 0.018(6) 0.015(5) -0.001(5) 0.013(5) 0.011(5) C6A 0.025(6) 0.009(5) 0.015(5) 0.002(4) 0.010(5) 0.006(5) C7A 0.022(6) 0.011(5) 0.015(5) 0.002(4) -0.001(4) 0.007(5) C8A 0.009(5) 0.022(6) 0.013(5) 0.010(4) 0.000(4) -0.003(4) C9A 0.013(6) 0.039(8) 0.018(6) 0.003(6) -0.007(5) 0.007(6) C10A 0.021(6) 0.022(7) 0.026(7) 0.006(5) -0.013(5) 0.005(6) C11A 0.015(5) 0.011(5) 0.022(6) -0.001(5) -0.001(4) 0.004(5) C12A 0.030(7) 0.019(6) 0.011(5) 0.006(4) 0.008(5) 0.008(5) C13A 0.0153(16) 0.0150(16) 0.0154(16) 0.0036(9) 0.0019(9) 0.0016(9) C14A 0.021(6) 0.019(6) 0.008(5) -0.003(4) 0.005(4) 0.002(5) C15A 0.024(6) 0.010(5) 0.026(6) 0.005(5) 0.002(5) 0.005(5) C16A 0.022(7) 0.029(8) 0.036(8) -0.003(6) 0.016(6) -0.002(6) C17A 0.016(6) 0.032(7) 0.019(6) 0.010(5) 0.005(5) -0.002(6) C18A 0.019(5) 0.010(5) 0.011(5) 0.004(4) 0.002(4) -0.004(4) C19A 0.021(6) 0.029(7) 0.019(6) 0.003(5) 0.000(5) 0.010(6) C20A 0.027(7) 0.034(8) 0.022(7) 0.005(6) 0.000(6) 0.001(7) C21A 0.039(9) 0.040(10) 0.023(7) 0.000(7) -0.002(7) 0.013(8) C22A 0.030(8) 0.036(9) 0.034(8) -0.014(7) -0.011(7) 0.017(7) C23A 0.024(8) 0.025(8) 0.049(10) -0.001(7) 0.004(7) 0.007(6) C24A 0.034(8) 0.029(8) 0.024(7) -0.004(6) 0.005(6) -0.001(7) Te2 0.0151(4) 0.0247(4) 0.0152(3) 0.0016(3) 0.0015(3) -0.0017(3) I2 0.0254(4) 0.0332(5) 0.0163(4) -0.0030(3) 0.0025(3) -0.0007(4) N1B 0.035(7) 0.017(5) 0.014(5) 0.001(4) -0.004(5) 0.002(5) N2B 0.019(5) 0.015(5) 0.014(4) 0.001(4) 0.001(4) 0.001(4) C1B 0.014(5) 0.037(8) 0.029(7) 0.023(6) 0.000(5) -0.001(6) C2B 0.029(7) 0.029(8) 0.033(8) 0.008(6) 0.016(6) 0.009(6) C3B 0.027(7) 0.013(6) 0.043(8) 0.008(6) 0.015(6) -0.003(5) C4B 0.022(7) 0.028(7) 0.035(8) 0.014(6) -0.006(6) 0.002(6) C5B 0.019(6) 0.036(8) 0.023(6) 0.004(6) 0.007(5) 0.012(6) C6B 0.024(6) 0.023(7) 0.016(5) 0.003(5) 0.011(5) 0.004(5) C7B 0.017(6) 0.025(7) 0.016(5) 0.004(5) 0.003(5) 0.001(5) C8B 0.044(10) 0.020(7) 0.038(9) 0.001(6) -0.010(7) 0.015(7) C9B 0.045(10) 0.024(8) 0.037(9) -0.012(7) 0.004(8) 0.018(7) C10B 0.021(7) 0.018(7) 0.041(9) 0.005(6) -0.001(6) 0.001(6) C11B 0.018(6) 0.030(7) 0.022(6) 0.009(6) 0.000(5) 0.008(6) C12B 0.019(6) 0.030(7) 0.021(6) 0.001(6) -0.006(5) 0.011(6) C13B 0.017(6) 0.025(7) 0.021(6) 0.005(5) 0.010(5) 0.005(5) C14B 0.031(8) 0.019(7) 0.031(7) 0.007(6) -0.001(6) 0.006(6) C15B 0.019(7) 0.030(8) 0.046(10) 0.007(7) -0.002(7) -0.008(6) C16B 0.039(9) 0.038(10) 0.041(9) 0.005(8) 0.025(8) -0.006(8) C17B 0.062(13) 0.036(9) 0.032(8) 0.022(7) 0.010(8) 0.017(9) C18B 0.035(8) 0.041(9) 0.020(7) 0.003(6) 0.002(6) 0.021(7) N3B 0.0132(12) 0.0132(13) 0.0133(13) 0.0032(7) 0.0020(7) 0.0016(7) N4B 0.0180(13) 0.0179(13) 0.0179(14) 0.0042(7) 0.0026(7) 0.0024(7) C19B 0.023(6) 0.023(7) 0.017(5) 0.002(5) 0.005(5) 0.005(6) C20B 0.039(7) 0.033(8) 0.037(8) 0.008(6) 0.005(6) 0.006(6) C21B 0.032(7) 0.030(6) 0.034(8) 0.000(5) -0.003(6) 0.010(5) C22B 0.031(5) 0.023(5) 0.023(5) 0.009(4) -0.001(4) 0.006(4) C23B 0.022(6) 0.023(6) 0.026(6) 0.001(5) -0.003(5) 0.003(5) C24B 0.020(6) 0.016(7) 0.019(5) 0.008(5) -0.001(4) 0.002(5) N3C 0.0132(12) 0.0132(13) 0.0133(13) 0.0032(7) 0.0020(7) 0.0016(7) N4C 0.0180(13) 0.0179(13) 0.0179(14) 0.0042(7) 0.0026(7) 0.0024(7) C19C 0.023(6) 0.023(7) 0.017(5) 0.002(5) 0.005(5) 0.005(6) C20C 0.039(7) 0.033(8) 0.037(8) 0.008(6) 0.005(6) 0.006(6) C21C 0.032(7) 0.030(6) 0.034(8) 0.000(5) -0.003(6) 0.010(5) C22C 0.031(5) 0.023(5) 0.023(5) 0.009(4) -0.001(4) 0.006(4) C23C 0.022(6) 0.023(6) 0.026(6) 0.001(5) -0.003(5) 0.003(5) C24C 0.020(6) 0.016(7) 0.019(5) 0.008(5) -0.001(4) 0.002(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 I11 I12 2.9533(14) . ? I12 I13 2.8753(14) . ? I21 I22 2.9316(12) . ? I22 I23 2.9049(13) . ? Te1 C13A 2.122(13) . ? Te1 C1A 2.145(13) . ? Te1 N2A 2.481(10) . ? Te1 I1 2.7820(11) . ? N1A N2A 1.254(16) . ? N1A C6A 1.426(18) . ? N2A C7A 1.418(18) . ? N3A N4A 1.247(17) . ? N3A C18A 1.424(18) . ? N4A C19A 1.41(2) . ? C1A C2A 1.383(18) . ? C1A C6A 1.390(17) . ? C2A C3A 1.403(19) . ? C2A H2AA 0.9500 . ? C3A C4A 1.44(2) . ? C3A H3AA 0.9500 . ? C4A C5A 1.35(2) . ? C4A H4AA 0.9500 . ? C5A C6A 1.411(18) . ? C5A H5AA 0.9500 . ? C7A C12A 1.398(19) . ? C7A C8A 1.412(17) . ? C8A C9A 1.396(19) . ? C8A H8AA 0.9500 . ? C9A C10A 1.40(2) . ? C9A H9AA 0.9500 . ? C10A C11A 1.39(2) . ? C10A H10A 0.9500 . ? C11A C12A 1.38(2) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C14A 1.377(18) . ? C13A C18A 1.426(18) . ? C14A C15A 1.417(19) . ? C14A H14A 0.9500 . ? C15A C16A 1.40(2) . ? C15A H15A 0.9500 . ? C16A C17A 1.38(2) . ? C16A H16A 0.9500 . ? C17A C18A 1.372(18) . ? C17A H17A 0.9500 . ? C19A C20A 1.39(2) . ? C19A C24A 1.40(2) . ? C20A C21A 1.36(3) . ? C20A H20A 0.9500 . ? C21A C22A 1.36(3) . ? C21A H21A 0.9500 . ? C22A C23A 1.39(3) . ? C22A H22A 0.9500 . ? C23A C24A 1.38(2) . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? Te2 C13B 2.143(14) . ? Te2 C1B 2.160(14) . ? Te2 N2B 2.476(11) . ? Te2 I2 2.7781(13) . ? N1B N2B 1.256(17) . ? N1B C6B 1.41(2) . ? N2B C7B 1.422(19) . ? C1B C2B 1.34(2) . ? C1B C6B 1.42(2) . ? C2B C3B 1.43(3) . ? C2B H2BA 0.9500 . ? C3B C4B 1.35(2) . ? C3B H3BA 0.9500 . ? C4B C5B 1.38(2) . ? C4B H4BA 0.9500 . ? C5B C6B 1.41(2) . ? C5B H5BA 0.9500 . ? C7B C8B 1.42(2) . ? C7B C12B 1.42(2) . ? C8B C9B 1.34(2) . ? C8B H8BA 0.9500 . ? C9B C10B 1.42(3) . ? C9B H9BA 0.9500 . ? C10B C11B 1.35(2) . ? C10B H10B 0.9500 . ? C11B C12B 1.39(2) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.36(2) . ? C13B C18B 1.40(2) . ? C14B C15B 1.36(2) . ? C14B H14B 0.9500 . ? C15B C16B 1.40(3) . ? C15B H15B 0.9500 . ? C16B C17B 1.43(3) . ? C16B H16B 0.9500 . ? C17B C18B 1.37(3) . ? C17B H17B 0.9500 . ? C18B N3B 1.42(3) . ? C18B N3C 1.48(3) . ? N3B N4B 1.32(3) . ? N4B C19B 1.44(3) . ? C19B C20B 1.3900 . ? C19B C24B 1.3900 . ? C20B C21B 1.3900 . ? C20B H20B 0.9500 . ? C21B C22B 1.3900 . ? C21B H21B 0.9500 . ? C22B C23B 1.3900 . ? C22B H22B 0.9500 . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? N3C N4C 1.23(3) . ? N4C C19C 1.43(3) . ? C19C C20C 1.3900 . ? C19C C24C 1.3900 . ? C20C C21C 1.3900 . ? C20C H20C 0.9500 . ? C21C C22C 1.3900 . ? C21C H21C 0.9500 . ? C22C C23C 1.3900 . ? C22C H22C 0.9500 . ? C23C C24C 1.3900 . ? C23C H23C 0.9500 . ? C24C H24C 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I13 I12 I11 179.30(5) . . ? I23 I22 I21 175.88(5) . . ? C13A Te1 C1A 97.4(5) . . ? C13A Te1 N2A 82.8(4) . . ? C1A Te1 N2A 70.3(4) . . ? C13A Te1 I1 88.1(3) . . ? C1A Te1 I1 96.0(3) . . ? N2A Te1 I1 162.2(3) . . ? N2A N1A C6A 111.9(12) . . ? N1A N2A C7A 117.3(11) . . ? N1A N2A Te1 116.4(10) . . ? C7A N2A Te1 125.6(8) . . ? N4A N3A C18A 114.3(11) . . ? N3A N4A C19A 116.5(13) . . ? C2A C1A C6A 121.0(12) . . ? C2A C1A Te1 122.5(9) . . ? C6A C1A Te1 116.4(9) . . ? C1A C2A C3A 119.1(12) . . ? C1A C2A H2AA 120.4 . . ? C3A C2A H2AA 120.4 . . ? C2A C3A C4A 119.5(13) . . ? C2A C3A H3AA 120.2 . . ? C4A C3A H3AA 120.2 . . ? C5A C4A C3A 119.9(14) . . ? C5A C4A H4AA 120.0 . . ? C3A C4A H4AA 120.0 . . ? C4A C5A C6A 120.6(13) . . ? C4A C5A H5AA 119.7 . . ? C6A C5A H5AA 119.7 . . ? C1A C6A C5A 119.6(13) . . ? C1A C6A N1A 124.3(12) . . ? C5A C6A N1A 116.0(12) . . ? C12A C7A C8A 119.7(13) . . ? C12A C7A N2A 117.8(12) . . ? C8A C7A N2A 122.4(12) . . ? C9A C8A C7A 120.8(12) . . ? C9A C8A H8AA 119.6 . . ? C7A C8A H8AA 119.6 . . ? C8A C9A C10A 117.7(13) . . ? C8A C9A H9AA 121.1 . . ? C10A C9A H9AA 121.1 . . ? C11A C10A C9A 122.0(14) . . ? C11A C10A H10A 119.0 . . ? C9A C10A H10A 119.0 . . ? C12A C11A C10A 119.8(13) . . ? C12A C11A H11A 120.1 . . ? C10A C11A H11A 120.1 . . ? C11A C12A C7A 119.9(12) . . ? C11A C12A H12A 120.0 . . ? C7A C12A H12A 120.0 . . ? C14A C13A C18A 119.5(12) . . ? C14A C13A Te1 119.3(10) . . ? C18A C13A Te1 121.0(9) . . ? C13A C14A C15A 119.7(12) . . ? C13A C14A H14A 120.2 . . ? C15A C14A H14A 120.2 . . ? C16A C15A C14A 120.9(14) . . ? C16A C15A H15A 119.5 . . ? C14A C15A H15A 119.5 . . ? C17A C16A C15A 118.0(14) . . ? C17A C16A H16A 121.0 . . ? C15A C16A H16A 121.0 . . ? C18A C17A C16A 122.7(13) . . ? C18A C17A H17A 118.7 . . ? C16A C17A H17A 118.7 . . ? C17A C18A N3A 116.0(12) . . ? C17A C18A C13A 119.2(12) . . ? N3A C18A C13A 124.8(11) . . ? C20A C19A C24A 118.2(15) . . ? C20A C19A N4A 126.6(15) . . ? C24A C19A N4A 115.2(14) . . ? C21A C20A C19A 121.2(17) . . ? C21A C20A H20A 119.4 . . ? C19A C20A H20A 119.4 . . ? C22A C21A C20A 121.2(18) . . ? C22A C21A H21A 119.4 . . ? C20A C21A H21A 119.4 . . ? C21A C22A C23A 118.6(17) . . ? C21A C22A H22A 120.7 . . ? C23A C22A H22A 120.7 . . ? C24A C23A C22A 121.5(18) . . ? C24A C23A H23A 119.3 . . ? C22A C23A H23A 119.3 . . ? C23A C24A C19A 119.1(16) . . ? C23A C24A H24A 120.4 . . ? C19A C24A H24A 120.4 . . ? C13B Te2 C1B 95.5(6) . . ? C13B Te2 N2B 78.6(5) . . ? C1B Te2 N2B 71.4(5) . . ? C13B Te2 I2 91.8(4) . . ? C1B Te2 I2 95.6(5) . . ? N2B Te2 I2 162.7(3) . . ? N2B N1B C6B 112.7(12) . . ? N1B N2B C7B 114.9(11) . . ? N1B N2B Te2 116.0(9) . . ? C7B N2B Te2 128.9(9) . . ? C2B C1B C6B 122.3(14) . . ? C2B C1B Te2 123.1(12) . . ? C6B C1B Te2 114.2(12) . . ? C1B C2B C3B 117.7(16) . . ? C1B C2B H2BA 121.2 . . ? C3B C2B H2BA 121.2 . . ? C4B C3B C2B 120.6(15) . . ? C4B C3B H3BA 119.7 . . ? C2B C3B H3BA 119.7 . . ? C3B C4B C5B 122.4(15) . . ? C3B C4B H4BA 118.8 . . ? C5B C4B H4BA 118.8 . . ? C4B C5B C6B 118.2(14) . . ? C4B C5B H5BA 120.9 . . ? C6B C5B H5BA 120.9 . . ? C5B C6B N1B 115.7(13) . . ? C5B C6B C1B 118.8(14) . . ? N1B C6B C1B 125.2(13) . . ? C8B C7B C12B 119.0(14) . . ? C8B C7B N2B 124.1(13) . . ? C12B C7B N2B 116.8(12) . . ? C9B C8B C7B 120.1(17) . . ? C9B C8B H8BA 120.0 . . ? C7B C8B H8BA 120.0 . . ? C8B C9B C10B 120.5(17) . . ? C8B C9B H9BA 119.7 . . ? C10B C9B H9BA 119.7 . . ? C11B C10B C9B 120.5(15) . . ? C11B C10B H10B 119.8 . . ? C9B C10B H10B 119.8 . . ? C10B C11B C12B 120.5(14) . . ? C10B C11B H11B 119.8 . . ? C12B C11B H11B 119.8 . . ? C11B C12B C7B 119.4(14) . . ? C11B C12B H12B 120.3 . . ? C7B C12B H12B 120.3 . . ? C14B C13B C18B 121.3(15) . . ? C14B C13B Te2 122.1(12) . . ? C18B C13B Te2 116.5(12) . . ? C13B C14B C15B 120.7(16) . . ? C13B C14B H14B 119.6 . . ? C15B C14B H14B 119.6 . . ? C14B C15B C16B 120.5(17) . . ? C14B C15B H15B 119.7 . . ? C16B C15B H15B 119.7 . . ? C15B C16B C17B 118.0(16) . . ? C15B C16B H16B 121.0 . . ? C17B C16B H16B 121.0 . . ? C18B C17B C16B 120.0(16) . . ? C18B C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? C17B C18B C13B 119.4(16) . . ? C17B C18B N3B 99.9(17) . . ? C13B C18B N3B 140.6(19) . . ? C17B C18B N3C 135.0(18) . . ? C13B C18B N3C 105.6(17) . . ? N3B C18B N3C 35.3(13) . . ? N4B N3B C18B 103.0(19) . . ? N3B N4B C19B 113(2) . . ? C20B C19B C24B 120.0 . . ? C20B C19B N4B 126.4(16) . . ? C24B C19B N4B 113.6(16) . . ? C21B C20B C19B 120.0 . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C22B 120.0 . . ? C20B C21B H21B 120.0 . . ? C22B C21B H21B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B H22B 120.0 . . ? C23B C22B H22B 120.0 . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C23B C24B C19B 120.0 . . ? C23B C24B H24B 120.0 . . ? C19B C24B H24B 120.0 . . ? N4C N3C C18B 113(2) . . ? N3C N4C C19C 113(2) . . ? C20C C19C C24C 120.0 . . ? C20C C19C N4C 114.2(18) . . ? C24C C19C N4C 125.7(18) . . ? C19C C20C C21C 120.00(6) . . ? C19C C20C H20C 120.0 . . ? C21C C20C H20C 120.0 . . ? C22C C21C C20C 120.0 . . ? C22C C21C H21C 120.0 . . ? C20C C21C H21C 120.0 . . ? C23C C22C C21C 120.0 . . ? C23C C22C H22C 120.0 . . ? C21C C22C H22C 120.0 . . ? C22C C23C C24C 120.00(5) . . ? C22C C23C H23C 120.0 . . ? C24C C23C H23C 120.0 . . ? C23C C24C C19C 120.0 . . ? C23C C24C H24C 120.0 . . ? C19C C24C H24C 120.0 . . ? 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 C6A N1A N2A C7A 176.9(11) . . . . ? C6A N1A N2A Te1 5.7(14) . . . . ? C13A Te1 N2A N1A -107.9(10) . . . . ? C1A Te1 N2A N1A -7.3(9) . . . . ? I1 Te1 N2A N1A -48.3(15) . . . . ? C13A Te1 N2A C7A 81.7(10) . . . . ? C1A Te1 N2A C7A -177.7(11) . . . . ? I1 Te1 N2A C7A 141.3(9) . . . . ? C18A N3A N4A C19A 178.8(12) . . . . ? C13A Te1 C1A C2A -97.1(11) . . . . ? N2A Te1 C1A C2A -176.6(11) . . . . ? I1 Te1 C1A C2A -8.2(11) . . . . ? C13A Te1 C1A C6A 86.4(10) . . . . ? N2A Te1 C1A C6A 6.9(9) . . . . ? I1 Te1 C1A C6A 175.3(9) . . . . ? C6A C1A C2A C3A 3(2) . . . . ? Te1 C1A C2A C3A -173.6(11) . . . . ? C1A C2A C3A C4A -5(2) . . . . ? C2A C3A C4A C5A 3(2) . . . . ? C3A C4A C5A C6A 1(2) . . . . ? C2A C1A C6A C5A 0.8(19) . . . . ? Te1 C1A C6A C5A 177.4(10) . . . . ? C2A C1A C6A N1A 175.9(12) . . . . ? Te1 C1A C6A N1A -7.6(16) . . . . ? C4A C5A C6A C1A -2(2) . . . . ? C4A C5A C6A N1A -177.9(14) . . . . ? N2A N1A C6A C1A 0.6(18) . . . . ? N2A N1A C6A C5A 175.8(12) . . . . ? N1A N2A C7A C12A 177.1(12) . . . . ? Te1 N2A C7A C12A -12.6(17) . . . . ? N1A N2A C7A C8A 0.9(18) . . . . ? Te1 N2A C7A C8A 171.3(9) . . . . ? C12A C7A C8A C9A -1(2) . . . . ? N2A C7A C8A C9A 174.9(13) . . . . ? C7A C8A C9A C10A 1(2) . . . . ? C8A C9A C10A C11A -1(2) . . . . ? C9A C10A C11A C12A 1(2) . . . . ? C10A C11A C12A C7A 0(2) . . . . ? C8A C7A C12A C11A 1(2) . . . . ? N2A C7A C12A C11A -175.7(12) . . . . ? C1A Te1 C13A C14A -3.1(11) . . . . ? N2A Te1 C13A C14A 65.8(11) . . . . ? I1 Te1 C13A C14A -98.9(11) . . . . ? C1A Te1 C13A C18A 171.6(11) . . . . ? N2A Te1 C13A C18A -119.5(11) . . . . ? I1 Te1 C13A C18A 75.8(10) . . . . ? C18A C13A C14A C15A -2(2) . . . . ? Te1 C13A C14A C15A 172.4(10) . . . . ? C13A C14A C15A C16A 0(2) . . . . ? C14A C15A C16A C17A 1(3) . . . . ? C15A C16A C17A C18A 0(3) . . . . ? C16A C17A C18A N3A 177.4(15) . . . . ? C16A C17A C18A C13A -2(2) . . . . ? N4A N3A C18A C17A -175.6(13) . . . . ? N4A N3A C18A C13A 4(2) . . . . ? C14A C13A C18A C17A 3(2) . . . . ? Te1 C13A C18A C17A -171.2(10) . . . . ? C14A C13A C18A N3A -176.1(13) . . . . ? Te1 C13A C18A N3A 9.2(18) . . . . ? N3A N4A C19A C20A 3(2) . . . . ? N3A N4A C19A C24A -174.1(14) . . . . ? C24A C19A C20A C21A -4(2) . . . . ? N4A C19A C20A C21A 178.6(15) . . . . ? C19A C20A C21A C22A 2(3) . . . . ? C20A C21A C22A C23A 2(3) . . . . ? C21A C22A C23A C24A -3(3) . . . . ? C22A C23A C24A C19A 0(3) . . . . ? C20A C19A C24A C23A 3(3) . . . . ? N4A C19A C24A C23A -179.3(16) . . . . ? C6B N1B N2B C7B -177.0(12) . . . . ? C6B N1B N2B Te2 -0.8(16) . . . . ? C13B Te2 N2B N1B 103.8(12) . . . . ? C1B Te2 N2B N1B 4.0(11) . . . . ? I2 Te2 N2B N1B 46.5(17) . . . . ? C13B Te2 N2B C7B -80.6(12) . . . . ? C1B Te2 N2B C7B 179.5(12) . . . . ? I2 Te2 N2B C7B -138.0(10) . . . . ? C13B Te2 C1B C2B 105.6(13) . . . . ? N2B Te2 C1B C2B -178.4(14) . . . . ? I2 Te2 C1B C2B 13.2(13) . . . . ? C13B Te2 C1B C6B -82.0(11) . . . . ? N2B Te2 C1B C6B -6.0(10) . . . . ? I2 Te2 C1B C6B -174.3(10) . . . . ? C6B C1B C2B C3B 3(2) . . . . ? Te2 C1B C2B C3B 175.3(11) . . . . ? C1B C2B C3B C4B 0(2) . . . . ? C2B C3B C4B C5B -1(3) . . . . ? C3B C4B C5B C6B -1(3) . . . . ? C4B C5B C6B N1B 177.8(14) . . . . ? C4B C5B C6B C1B 4(2) . . . . ? N2B N1B C6B C5B -178.5(14) . . . . ? N2B N1B C6B C1B -5(2) . . . . ? C2B C1B C6B C5B -5(2) . . . . ? Te2 C1B C6B C5B -177.9(11) . . . . ? C2B C1B C6B N1B -178.4(15) . . . . ? Te2 C1B C6B N1B 9.1(19) . . . . ? N1B N2B C7B C8B -1(2) . . . . ? Te2 N2B C7B C8B -176.5(13) . . . . ? N1B N2B C7B C12B 179.6(14) . . . . ? Te2 N2B C7B C12B 4.0(19) . . . . ? C12B C7B C8B C9B 1(3) . . . . ? N2B C7B C8B C9B -178.5(18) . . . . ? C7B C8B C9B C10B 0(3) . . . . ? C8B C9B C10B C11B 1(3) . . . . ? C9B C10B C11B C12B -2(3) . . . . ? C10B C11B C12B C7B 3(2) . . . . ? C8B C7B C12B C11B -2(2) . . . . ? N2B C7B C12B C11B 177.3(13) . . . . ? C1B Te2 C13B C14B -2.1(14) . . . . ? N2B Te2 C13B C14B -71.8(13) . . . . ? I2 Te2 C13B C14B 93.7(13) . . . . ? C1B Te2 C13B C18B 177.7(12) . . . . ? N2B Te2 C13B C18B 107.9(12) . . . . ? I2 Te2 C13B C18B -86.6(11) . . . . ? C18B C13B C14B C15B 0(3) . . . . ? Te2 C13B C14B C15B 179.6(14) . . . . ? C13B C14B C15B C16B 0(3) . . . . ? C14B C15B C16B C17B -1(3) . . . . ? C15B C16B C17B C18B 2(3) . . . . ? C16B C17B C18B C13B -1(3) . . . . ? C16B C17B C18B N3B -178.3(18) . . . . ? C16B C17B C18B N3C 178(2) . . . . ? C14B C13B C18B C17B 1(3) . . . . ? Te2 C13B C18B C17B -179.1(14) . . . . ? C14B C13B C18B N3B 176(2) . . . . ? Te2 C13B C18B N3B -4(3) . . . . ? C14B C13B C18B N3C -178.9(16) . . . . ? Te2 C13B C18B N3C 1.3(18) . . . . ? C17B C18B N3B N4B -178.3(18) . . . . ? C13B C18B N3B N4B 6(3) . . . . ? N3C C18B N3B N4B -2.8(19) . . . . ? C18B N3B N4B C19B -179.3(18) . . . . ? N3B N4B C19B C20B 5(3) . . . . ? N3B N4B C19B C24B -176.4(17) . . . . ? C24B C19B C20B C21B 0.0 . . . . ? N4B C19B C20B C21B 178(2) . . . . ? C19B C20B C21B C22B 0.0 . . . . ? C20B C21B C22B C23B 0.0 . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C22B C23B C24B C19B 0.0 . . . . ? C20B C19B C24B C23B 0.0 . . . . ? N4B C19B C24B C23B -178.7(17) . . . . ? C17B C18B N3C N4C 12(4) . . . . ? C13B C18B N3C N4C -169(2) . . . . ? N3B C18B N3C N4C 6(2) . . . . ? C18B N3C N4C C19C 176.4(19) . . . . ? N3C N4C C19C C20C 168(2) . . . . ? N3C N4C C19C C24C -8(3) . . . . ? C24C C19C C20C C21C 0.0 . . . . ? N4C C19C C20C C21C -176(2) . . . . ? C19C C20C C21C C22C 0.0 . . . . ? C20C C21C C22C C23C 0.0 . . . . ? C21C C22C C23C C24C 0.0 . . . . ? C22C C23C C24C C19C 0.0 . . . . ? C20C C19C C24C C23C 0.0 . . . . ? N4C C19C C24C C23C 176(2) . . . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 5.116 _refine_diff_density_min -2.379 _refine_diff_density_rms 0.399 #===END data_ups494 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 Cl N2 Te' _chemical_formula_sum 'C12 H9 Cl N2 Te' _chemical_formula_weight 344.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'C 2/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 31.3486(10) _cell_length_b 4.09590(10) _cell_length_c 20.1937(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.074(2) _cell_angle_gamma 90.00 _cell_volume 2329.00(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8636 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 28.82 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 2.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24344 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 30.14 _reflns_number_total 3428 _reflns_number_gt 2841 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker 2000)' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0311P)^2^+2.0107P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3428 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Te Te 0.177431(5) 0.05802(4) 0.438750(8) 0.03569(6) Uani 1 1 d . . . Cl Cl 0.21934(2) -0.1637(2) 0.56907(4) 0.05144(17) Uani 1 1 d . . . N1 N 0.08077(7) 0.2232(6) 0.31437(10) 0.0404(5) Uani 1 1 d . . . N2 N 0.12498(7) 0.2347(5) 0.32929(10) 0.0338(4) Uani 1 1 d . . . C1 C 0.11181(9) -0.0172(6) 0.43660(13) 0.0361(5) Uani 1 1 d . . . C2 C 0.10242(10) -0.1619(7) 0.49162(15) 0.0450(6) Uani 1 1 d . . . H2A H 0.1278 -0.2370 0.5360 0.054 Uiso 1 1 calc R . . C3 C 0.05624(11) -0.1943(9) 0.48096(17) 0.0569(8) Uani 1 1 d . . . H3A H 0.0500 -0.2929 0.5184 0.068 Uiso 1 1 calc R . . C4 C 0.01823(11) -0.0862(10) 0.41657(19) 0.0630(9) Uani 1 1 d . . . H4A H -0.0134 -0.1092 0.4109 0.076 Uiso 1 1 calc R . . C5 C 0.02645(10) 0.0539(9) 0.36117(17) 0.0555(8) Uani 1 1 d . . . H5A H 0.0007 0.1265 0.3170 0.067 Uiso 1 1 calc R . . C6 C 0.07343(9) 0.0877(7) 0.37110(14) 0.0401(6) Uani 1 1 d . . . C7 C 0.13683(9) 0.3698(6) 0.27412(13) 0.0354(5) Uani 1 1 d . . . C8 C 0.10403(10) 0.5508(7) 0.21611(15) 0.0448(6) Uani 1 1 d . . . H8A H 0.0731 0.5889 0.2120 0.054 Uiso 1 1 calc R . . C9 C 0.11746(11) 0.6748(8) 0.16429(15) 0.0524(7) Uani 1 1 d . . . H9A H 0.0956 0.8030 0.1248 0.063 Uiso 1 1 calc R . . C10 C 0.16175(11) 0.6160(7) 0.16895(16) 0.0484(7) Uani 1 1 d . . . H10A H 0.1701 0.6990 0.1323 0.058 Uiso 1 1 calc R . . C11 C 0.19395(11) 0.4367(7) 0.22670(17) 0.0492(6) Uani 1 1 d . . . H11A H 0.2247 0.3975 0.2302 0.059 Uiso 1 1 calc R . . C12 C 0.18181(9) 0.3131(7) 0.27983(15) 0.0441(6) Uani 1 1 d . . . H12A H 0.2042 0.1901 0.3199 0.053 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 Te 0.03096(9) 0.04359(10) 0.02974(9) -0.00010(6) 0.01078(6) 0.00182(6) Cl 0.0447(3) 0.0719(5) 0.0321(3) 0.0062(3) 0.0117(3) 0.0090(3) N1 0.0334(10) 0.0545(14) 0.0294(10) -0.0010(9) 0.0104(8) 0.0030(10) N2 0.0331(10) 0.0387(11) 0.0283(9) -0.0040(8) 0.0125(8) 0.0012(8) C1 0.0359(12) 0.0409(14) 0.0313(12) -0.0053(9) 0.0145(10) -0.0007(9) C2 0.0461(14) 0.0554(16) 0.0351(13) -0.0013(11) 0.0194(11) -0.0008(13) C3 0.0569(18) 0.075(2) 0.0462(16) -0.0048(15) 0.0298(15) -0.0126(16) C4 0.0421(16) 0.098(3) 0.0552(19) -0.0115(17) 0.0269(15) -0.0147(16) C5 0.0350(14) 0.088(2) 0.0415(15) -0.0022(15) 0.0150(12) 0.0001(14) C6 0.0350(12) 0.0528(16) 0.0323(12) -0.0039(11) 0.0146(10) 0.0015(11) C7 0.0394(12) 0.0385(13) 0.0269(11) -0.0051(9) 0.0132(10) -0.0026(10) C8 0.0420(14) 0.0544(15) 0.0352(13) 0.0036(11) 0.0144(11) 0.0055(12) C9 0.0566(17) 0.0601(18) 0.0364(14) 0.0092(13) 0.0168(13) 0.0050(15) C10 0.0586(17) 0.0519(17) 0.0409(15) -0.0018(12) 0.0275(13) -0.0072(13) C11 0.0452(15) 0.0561(17) 0.0522(17) -0.0027(13) 0.0269(14) -0.0042(13) C12 0.0396(13) 0.0520(15) 0.0388(14) 0.0006(12) 0.0155(11) 0.0012(12) _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 Te C1 2.062(2) . ? Te N2 2.2178(19) . ? Te Cl 2.5371(7) . ? N1 N2 1.283(3) . ? N1 C6 1.380(3) . ? N2 C7 1.432(3) . ? C1 C2 1.400(4) . ? C1 C6 1.408(4) . ? C2 C3 1.373(4) . ? C2 H2A 0.9500 . ? C3 C4 1.394(5) . ? C3 H3A 0.9500 . ? C4 C5 1.379(5) . ? C4 H4A 0.9500 . ? C5 C6 1.403(4) . ? C5 H5A 0.9500 . ? C7 C12 1.383(4) . ? C7 C8 1.386(4) . ? C8 C9 1.385(4) . ? C8 H8A 0.9500 . ? C9 C10 1.371(4) . ? C9 H9A 0.9500 . ? C10 C11 1.372(5) . ? C10 H10A 0.9500 . ? C11 C12 1.382(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te N2 74.45(9) . . ? C1 Te Cl 91.45(7) . . ? N2 Te Cl 165.86(5) . . ? N2 N1 C6 112.1(2) . . ? N1 N2 C7 117.04(19) . . ? N1 N2 Te 118.23(15) . . ? C7 N2 Te 124.71(15) . . ? C2 C1 C6 118.9(2) . . ? C2 C1 Te 127.0(2) . . ? C6 C1 Te 114.01(18) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? N1 C6 C5 117.9(2) . . ? N1 C6 C1 121.1(2) . . ? C5 C6 C1 120.9(2) . . ? C12 C7 C8 120.7(2) . . ? C12 C7 N2 118.3(2) . . ? C8 C7 N2 121.0(2) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C10 C9 C8 121.3(3) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 119.5(3) . . ? C11 C12 H12A 120.3 . . ? C7 C12 H12A 120.3 . . ? 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 C6 N1 N2 C7 179.8(2) . . . . ? C6 N1 N2 Te -1.8(3) . . . . ? C1 Te N2 N1 1.80(17) . . . . ? Cl Te N2 N1 -2.9(4) . . . . ? C1 Te N2 C7 -179.9(2) . . . . ? Cl Te N2 C7 175.39(16) . . . . ? N2 Te C1 C2 177.6(2) . . . . ? Cl Te C1 C2 -3.5(2) . . . . ? N2 Te C1 C6 -1.28(18) . . . . ? Cl Te C1 C6 177.58(18) . . . . ? C6 C1 C2 C3 -0.8(4) . . . . ? Te C1 C2 C3 -179.7(2) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 0.8(6) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? N2 N1 C6 C5 -178.6(2) . . . . ? N2 N1 C6 C1 0.6(4) . . . . ? C4 C5 C6 N1 178.8(3) . . . . ? C4 C5 C6 C1 -0.4(5) . . . . ? C2 C1 C6 N1 -178.1(2) . . . . ? Te C1 C6 N1 0.9(3) . . . . ? C2 C1 C6 C5 1.1(4) . . . . ? Te C1 C6 C5 -179.9(2) . . . . ? N1 N2 C7 C12 -164.1(2) . . . . ? Te N2 C7 C12 17.6(3) . . . . ? N1 N2 C7 C8 15.4(3) . . . . ? Te N2 C7 C8 -162.9(2) . . . . ? C12 C7 C8 C9 -0.4(4) . . . . ? N2 C7 C8 C9 -179.8(3) . . . . ? C7 C8 C9 C10 1.3(5) . . . . ? C8 C9 C10 C11 -1.4(5) . . . . ? C9 C10 C11 C12 0.5(5) . . . . ? C10 C11 C12 C7 0.4(5) . . . . ? C8 C7 C12 C11 -0.4(4) . . . . ? N2 C7 C12 C11 179.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.030 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.086 #===END data_teocl _vrf_PLAT417_teocl ; PROBLEM: Short Inter D-H..H-D H3W5 .. H9W1 .. 1.38 Ang. RESPONSE: This is a co-crystal of acid and its sodium salt with disordered water molecules. Therefore there are reported close contacts between hydrogen atoms which are not contiguous as there are in separate unit cells. ; _vrf_PLAT432_teocl ; PROBLEM: Short Inter X...Y Contact Te1 .. O2WB .. 2.99 Ang. RESPONSE: While this is within the sum of van der Waals radii for the respective atoms it only involves in minor component (0.36 occupancy). However, this water molecule is trans to a Te-C bond and can thus be considered as a weak interaction. ; _vrf_PLAT772_teocl ; PROBLEM: Suspect O-H Bond in CIF: O3WC -- H3W1 .. 1.31 Ang. RESPONSE: This is a co-crystal of acid and its sodium salt with disordered water molecules. Therefore there are reported close contacts between hydrogen atoms which are not contiguous as there are in separate unit cells. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H87 N8 Na3 O33 Te4' _chemical_formula_weight 1883.63 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' 'Na' 'Na' 0.0362 0.0249 '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 c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.0833(6) _cell_length_b 5.0482(3) _cell_length_c 38.0518(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3473.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 4.9383 _cell_measurement_theta_max 34.8638 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.6276 _exptl_crystal_size_mid 0.0664 _exptl_crystal_size_min 0.0330 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.775 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 42132 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 4.98 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10541 _reflns_number_gt 7360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material SHELXTL _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^)+(0.0340P)^2^] 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 mixed _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 0.012(17) _refine_ls_number_reflns 10541 _refine_ls_number_parameters 557 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.004 _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 0.297619(10) 0.84393(4) 0.890878(6) 0.02491(5) Uani 1 1 d D . . Te2 Te 0.347624(11) 0.67772(5) 1.109791(4) 0.03368(6) Uani 1 1 d D . . Na1 Na 0.01332(13) 0.8048(6) 0.98650(6) 0.0233(6) Uani 0.50 1 d PD . . Na2 Na 0.13303(8) 0.3143(3) 1.01393(4) 0.0373(4) Uani 1 1 d D . . O1A O 0.22795(13) 0.7781(6) 0.92636(6) 0.0335(7) Uani 1 1 d . A . O2AA O 0.37995(9) 0.7149(8) 0.91362(8) 0.0263(8) Uani 0.50 1 d PDU A 1 H2C H 0.3867 0.5561 0.9079 0.032 Uiso 0.50 1 calc PR A 1 O2AB O 0.37254(10) 0.6192(5) 0.90486(11) 0.0263(8) Uani 0.476(6) 1 d PDU A 2 O1BA O 0.42708(9) 0.6982(10) 1.07783(6) 0.0311(11) Uani 0.572(4) 1 d PD B 1 O2BA O 0.27229(10) 0.9062(5) 1.09513(10) 0.0355(8) Uani 0.572(4) 1 d PDU B 1 O1BB O 0.41474(13) 0.7888(11) 1.07487(7) 0.0311(11) Uani 0.428(4) 1 d PD B 2 O2BB O 0.26950(11) 0.8064(9) 1.08274(9) 0.0355(8) Uani 0.428(4) 1 d PDU B 2 O1W O 0.07774(13) 0.8105(5) 0.92839(7) 0.0343(7) Uani 1 1 d D C . H1W1 H 0.1199(7) 0.830(6) 0.9292(5) 0.051 Uiso 1 1 d D . . H1W2 H 0.0651(13) 0.688(4) 0.9164(4) 0.051 Uiso 1 1 d D . . O2WA O -0.0993(3) 0.7943(10) 0.95167(12) 0.0412(12) Uani 0.640(6) 1 d PD C 1 H2W1 H -0.1229(10) 0.655(4) 0.9529(7) 0.062 Uiso 0.640(6) 1 d PD C 1 H2W2 H -0.0930(13) 0.811(8) 0.9302(4) 0.062 Uiso 0.640(6) 1 d PD C 1 O2WB O -0.1206(5) 0.7814(18) 0.9376(2) 0.0412(12) Uani 0.360(6) 1 d PD C 2 H2W3 H -0.1619(11) 0.747(9) 0.9448(12) 0.062 Uiso 0.360(6) 1 d PD C 2 H2W4 H -0.107(3) 0.651(7) 0.9266(15) 0.062 Uiso 0.360(6) 1 d PD C 2 O3WA O -0.0709(2) 0.7686(10) 1.03514(12) 0.0257(12) Uani 0.50 1 d PD C 1 H3W1 H -0.1126(8) 0.827(5) 1.0326(7) 0.039 Uiso 0.50 1 d PD D 1 H3W2 H -0.0754(15) 0.624(4) 1.0443(7) 0.039 Uiso 0.50 1 d PD E 1 O3WB O -0.1067(3) 0.5074(11) 1.01911(12) 0.0339(13) Uani 0.50 1 d PD C 2 H3W3 H -0.1325 0.4907 1.0368 0.051 Uiso 0.50 1 d PRD C 2 H3W4 H -0.0789 0.6313 1.0244 0.051 Uiso 0.50 1 d PRD C 2 O3WC O -0.0776(3) 1.0324(13) 1.01988(14) 0.0461(15) Uani 0.50 1 d PD C 3 H3W5 H -0.1121 1.1135 1.0109 0.069 Uiso 0.50 1 d PRD C 3 H3W6 H -0.0799 0.8839 1.0115 0.069 Uiso 0.50 1 d PRD C 3 O4W O 0.07139(15) 0.3029(6) 1.07130(7) 0.0379(7) Uani 1 1 d D . . H4W1 H 0.0268(7) 0.316(6) 1.0706(5) 0.057 Uiso 1 1 d D . . H4W2 H 0.0789(14) 0.159(4) 1.0814(5) 0.057 Uiso 1 1 d D . . O5WA O 0.24060(19) 0.3039(9) 1.04926(9) 0.0442(11) Uani 0.808(6) 1 d PD . 1 H5W1 H 0.2818(7) 0.347(6) 1.0406(7) 0.066 Uiso 0.808(6) 1 d PD . 1 H5W2 H 0.2530(12) 0.168(4) 1.0601(7) 0.066 Uiso 0.808(6) 1 d PD . 1 O5WB O 0.2513(8) 0.185(3) 1.0398(4) 0.0442(11) Uani 0.192(6) 1 d PD . 2 H5W3 H 0.259(3) 0.114(7) 1.0590(7) 0.066 Uiso 0.192(6) 1 d PD . 2 H5W4 H 0.2883(18) 0.280(10) 1.0374(18) 0.066 Uiso 0.192(6) 1 d PD . 2 O6W O 0.20086(14) 0.2915(5) 0.96171(7) 0.0358(7) Uani 1 1 d D . . H6W1 H 0.2124 0.1493 0.9529 0.054 Uiso 1 1 d RD C . H6W2 H 0.2294 0.3997 0.9554 0.054 Uiso 1 1 d RD . . O7W O 0.01911(16) 0.3087(7) 0.98462(7) 0.0491(9) Uani 1 1 d D . . H7W1 H 0.0154(10) 0.264(3) 0.9638(3) 0.074 Uiso 1 1 d D . . H7W2 H -0.0193(7) 0.254(3) 0.9938(5) 0.074 Uiso 1 1 d D . . O8WA O 0.1328(2) 0.8154(9) 1.01532(11) 0.0369(11) Uani 0.651(5) 1 d PD . 1 H8W1 H 0.1325(11) 0.858(3) 1.0358(3) 0.055 Uiso 0.651(5) 1 d PD . 1 H8W2 H 0.1674(7) 0.867(3) 1.0053(5) 0.055 Uiso 0.651(5) 1 d PD . 1 O8WB O 0.0991(5) 0.8054(17) 1.0027(2) 0.0369(11) Uani 0.349(5) 1 d PD . 2 H8W3 H 0.1179(14) 0.940(6) 1.0111(16) 0.055 Uiso 0.349(5) 1 d PD . 2 H8W4 H 0.0586(12) 0.798(10) 1.0128(13) 0.055 Uiso 0.349(5) 1 d PD . 2 O9W O -0.21401(16) 1.2086(7) 0.99331(7) 0.0529(9) Uani 1 1 d D . . H9W1 H -0.1699(8) 1.239(11) 0.9939(9) 0.079 Uiso 1 1 d D . . H9W2 H -0.2282(15) 1.216(11) 0.9734(5) 0.079 Uiso 1 1 d D . . O10W O 0.12450(13) 0.8045(6) 1.09193(7) 0.0339(7) Uani 1 1 d D . . H101 H 0.1694(9) 0.807(9) 1.0937(11) 0.051 Uiso 1 1 d D . . H102 H 0.109(2) 0.666(4) 1.0844(10) 0.051 Uiso 1 1 d D . . O11W O -0.18267(16) 0.7281(6) 0.99945(7) 0.0364(7) Uani 1 1 d D . . H111 H -0.1741 0.5784 0.9917 0.055 Uiso 1 1 d RD . . H112 H -0.1532 0.8228 0.9886 0.055 Uiso 1 1 d RD . . O12W O 0.02271(12) 1.3065(5) 0.90889(7) 0.0300(6) Uani 1 1 d D . . H121 H -0.0207(7) 1.297(6) 0.9066(10) 0.045 Uiso 1 1 d D . . H122 H 0.0382(13) 1.154(4) 0.9095(11) 0.045 Uiso 1 1 d D . . N1A N 0.35079(15) 0.6413(6) 0.80931(8) 0.0259(7) Uani 1 1 d . . . N2A N 0.37527(15) 0.8130(6) 0.83062(7) 0.0208(6) Uani 1 1 d . A . N1B N 0.29091(15) 0.8703(6) 1.19110(8) 0.0253(7) Uani 1 1 d . . . N2B N 0.26664(15) 0.7034(6) 1.16956(7) 0.0227(7) Uani 1 1 d . B . C1A C 0.25520(18) 0.5506(7) 0.85553(8) 0.0194(7) Uani 1 1 d . A . C2A C 0.19327(17) 0.4064(7) 0.86440(9) 0.0264(9) Uani 1 1 d . . . H2AA H 0.1686 0.4437 0.8859 0.032 Uiso 1 1 calc R A . C3A C 0.16639(18) 0.2098(8) 0.84288(10) 0.0289(10) Uani 1 1 d . A . H3AA H 0.1235 0.1135 0.8496 0.035 Uiso 1 1 calc R . . C4A C 0.20174(19) 0.1513(8) 0.81135(9) 0.0279(8) Uani 1 1 d . . . H4AA H 0.1842 0.0123 0.7967 0.034 Uiso 1 1 calc R A . C5A C 0.2624(2) 0.2982(8) 0.80173(9) 0.0267(9) Uani 1 1 d . A . H5AA H 0.2863 0.2619 0.7800 0.032 Uiso 1 1 calc R . . C6A C 0.28916(17) 0.4988(7) 0.82320(9) 0.0235(8) Uani 1 1 d . A . C7A C 0.43543(16) 0.9692(7) 0.81849(8) 0.0221(8) Uani 1 1 d . . . C8A C 0.46884(18) 0.9388(7) 0.78565(9) 0.0249(8) Uani 1 1 d . A . H8AA H 0.4524 0.8062 0.7698 0.030 Uiso 1 1 calc R . . C9A C 0.52666(18) 1.1071(8) 0.77678(9) 0.0276(9) Uani 1 1 d . . . H9AA H 0.5503 1.0880 0.7546 0.033 Uiso 1 1 calc R A . C10A C 0.55022(19) 1.3016(8) 0.79963(9) 0.0268(9) Uani 1 1 d . A . H10A H 0.5895 1.4163 0.7931 0.032 Uiso 1 1 calc R . . C11A C 0.51677(18) 1.3296(8) 0.83203(9) 0.0271(8) Uani 1 1 d . . . H11A H 0.5331 1.4631 0.8478 0.033 Uiso 1 1 calc R A . C12A C 0.45958(17) 1.1630(8) 0.84139(8) 0.0252(8) Uani 1 1 d . A . H12A H 0.4367 1.1817 0.8637 0.030 Uiso 1 1 calc R . . C1B C 0.38756(17) 0.9677(7) 1.14633(9) 0.0237(8) Uani 1 1 d . B . C2B C 0.45015(18) 1.1117(7) 1.13724(10) 0.0304(9) Uani 1 1 d . . . H2BA H 0.4753 1.0753 1.1159 0.037 Uiso 1 1 calc R B . C3B C 0.4757(2) 1.3091(8) 1.15952(12) 0.0392(12) Uani 1 1 d . B . H3BA H 0.5182 1.4084 1.1531 0.047 Uiso 1 1 calc R . . C4B C 0.4404(2) 1.3634(8) 1.19079(11) 0.0370(11) Uani 1 1 d . . . H4BA H 0.4585 1.5001 1.2056 0.044 Uiso 1 1 calc R B . C5B C 0.3787(2) 1.2192(8) 1.20062(11) 0.0324(10) Uani 1 1 d . B . H5BA H 0.3543 1.2558 1.2222 0.039 Uiso 1 1 calc R . . C6B C 0.35235(16) 1.0165(7) 1.17815(9) 0.0207(8) Uani 1 1 d . B . C7B C 0.20794(17) 0.5389(7) 1.18118(8) 0.0202(7) Uani 1 1 d . . . C8B C 0.17502(19) 0.5577(8) 1.21436(9) 0.0268(9) Uani 1 1 d . B . H8BA H 0.1911 0.6877 1.2307 0.032 Uiso 1 1 calc R . . C9B C 0.11949(19) 0.3862(7) 1.22285(9) 0.0270(9) Uani 1 1 d . . . H9BA H 0.0965 0.3993 1.2452 0.032 Uiso 1 1 calc R B . C10B C 0.09572(19) 0.1918(8) 1.19930(10) 0.0256(9) Uani 1 1 d . B . H10B H 0.0577 0.0714 1.2058 0.031 Uiso 1 1 calc R . . C11B C 0.12789(18) 0.1758(8) 1.16641(9) 0.0269(8) Uani 1 1 d . . . H11B H 0.1115 0.0457 1.1501 0.032 Uiso 1 1 calc R B . C12B C 0.18483(19) 0.3516(8) 1.15697(9) 0.0259(9) Uani 1 1 d . B . H12B H 0.2071 0.3420 1.1344 0.031 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 0.02337(8) 0.03228(10) 0.01909(8) -0.00251(13) 0.00113(9) -0.00944(10) Te2 0.02820(10) 0.05060(15) 0.02224(9) -0.00543(15) 0.00299(9) -0.01981(11) Na1 0.0197(11) 0.0256(16) 0.0246(12) 0.0039(12) 0.0011(10) 0.0022(12) Na2 0.0446(8) 0.0405(10) 0.0268(7) 0.0006(7) 0.0057(6) -0.0050(8) O1A 0.0297(12) 0.0479(18) 0.0229(12) -0.0008(12) 0.0062(10) -0.0140(12) O2AA 0.0227(10) 0.0320(13) 0.0241(12) 0.0005(9) -0.0123(9) -0.0068(10) O2AB 0.0227(10) 0.0320(13) 0.0241(12) 0.0005(9) -0.0123(9) -0.0068(10) O1BA 0.0322(16) 0.037(3) 0.0238(14) 0.0020(15) 0.0008(12) -0.0138(17) O2BA 0.0320(11) 0.0420(13) 0.0324(12) 0.0015(10) -0.0081(9) -0.0088(10) O1BB 0.0322(16) 0.037(3) 0.0238(14) 0.0020(15) 0.0008(12) -0.0138(17) O2BB 0.0320(11) 0.0420(13) 0.0324(12) 0.0015(10) -0.0081(9) -0.0088(10) O1W 0.0285(12) 0.0243(15) 0.0500(15) 0.0012(13) 0.0063(11) -0.0011(12) O2WA 0.041(2) 0.046(2) 0.037(3) -0.003(2) -0.0099(18) 0.002(2) O2WB 0.041(2) 0.046(2) 0.037(3) -0.003(2) -0.0099(18) 0.002(2) O3WA 0.024(2) 0.031(3) 0.022(2) 0.006(2) 0.0055(19) -0.002(2) O3WB 0.038(3) 0.029(3) 0.035(3) -0.001(2) -0.002(2) 0.008(3) O3WC 0.056(3) 0.038(4) 0.045(3) 0.002(3) 0.004(3) -0.007(3) O4W 0.0419(15) 0.0365(18) 0.0353(14) 0.0051(13) 0.0027(12) -0.0042(13) O5WA 0.0387(17) 0.064(3) 0.0296(18) -0.0043(18) 0.0050(14) -0.0231(19) O5WB 0.0387(17) 0.064(3) 0.0296(18) -0.0043(18) 0.0050(14) -0.0231(19) O6W 0.0413(14) 0.0311(16) 0.0350(14) 0.0006(12) 0.0083(12) 0.0018(13) O7W 0.0525(16) 0.064(2) 0.0309(14) 0.0071(14) -0.0004(12) 0.0288(16) O8WA 0.042(2) 0.033(2) 0.035(2) 0.0022(19) 0.0083(16) -0.002(2) O8WB 0.042(2) 0.033(2) 0.035(2) 0.0022(19) 0.0083(16) -0.002(2) O9W 0.0565(17) 0.073(2) 0.0288(14) -0.0054(15) -0.0094(13) 0.0264(17) O10W 0.0222(11) 0.0296(16) 0.0499(15) -0.0009(13) -0.0004(11) -0.0040(12) O11W 0.0298(12) 0.0439(18) 0.0354(13) 0.0018(11) 0.0041(10) 0.0010(11) O12W 0.0186(11) 0.0260(15) 0.0453(14) 0.0023(12) -0.0047(10) -0.0012(11) N1A 0.0280(14) 0.0239(17) 0.0257(14) 0.0005(13) -0.0001(11) -0.0013(14) N2A 0.0230(13) 0.0233(16) 0.0159(12) 0.0013(12) -0.0030(10) 0.0014(13) N1B 0.0189(13) 0.0269(18) 0.0300(15) 0.0020(13) -0.0018(11) -0.0012(13) N2B 0.0220(13) 0.0188(16) 0.0274(14) 0.0016(13) -0.0010(12) -0.0038(12) C1A 0.0173(14) 0.0184(17) 0.0226(16) -0.0018(14) -0.0015(12) 0.0031(15) C2A 0.0178(16) 0.026(2) 0.0350(18) 0.0019(15) 0.0012(14) 0.0024(14) C3A 0.0166(15) 0.027(2) 0.043(2) -0.0007(17) -0.0007(15) -0.0018(15) C4A 0.0297(16) 0.0220(18) 0.0321(17) -0.0067(16) -0.0061(15) -0.0063(17) C5A 0.0280(17) 0.029(2) 0.0234(16) -0.0072(16) 0.0004(14) -0.0005(16) C6A 0.0168(15) 0.0198(18) 0.0338(18) 0.0000(16) 0.0004(13) 0.0002(14) C7A 0.0158(15) 0.025(2) 0.0255(16) 0.0055(15) -0.0010(13) 0.0025(15) C8A 0.0270(17) 0.022(2) 0.0253(17) -0.0015(14) 0.0001(14) 0.0019(15) C9A 0.0252(16) 0.037(2) 0.0203(16) 0.0054(15) 0.0035(13) 0.0041(16) C10A 0.0171(15) 0.026(2) 0.0370(19) 0.0091(17) 0.0000(14) -0.0009(15) C11A 0.0245(16) 0.0209(19) 0.0361(18) -0.0057(17) -0.0038(14) -0.0020(16) C12A 0.0220(15) 0.031(2) 0.0226(15) 0.0010(16) 0.0031(13) -0.0003(16) C1B 0.0192(15) 0.0202(19) 0.0316(18) -0.0013(16) -0.0065(13) 0.0019(15) C2B 0.0174(15) 0.024(2) 0.050(2) 0.0035(17) 0.0048(15) 0.0038(15) C3B 0.0238(18) 0.020(2) 0.074(3) -0.004(2) 0.0009(19) -0.0006(17) C4B 0.0243(17) 0.020(2) 0.067(3) -0.008(2) -0.0086(19) 0.0015(17) C5B 0.0249(17) 0.028(2) 0.044(2) -0.0054(18) -0.0061(16) 0.0045(16) C6B 0.0158(15) 0.0203(19) 0.0259(17) -0.0033(15) -0.0065(13) 0.0044(14) C7B 0.0190(15) 0.0137(16) 0.0280(16) 0.0026(14) -0.0028(13) -0.0020(14) C8B 0.0274(17) 0.026(2) 0.0265(17) -0.0020(16) -0.0031(14) -0.0042(16) C9B 0.0260(16) 0.031(2) 0.0243(17) 0.0023(15) 0.0020(14) -0.0004(16) C10B 0.0194(15) 0.022(2) 0.0351(19) 0.0021(17) -0.0019(15) -0.0011(16) C11B 0.0241(16) 0.030(2) 0.0267(17) 0.0009(17) -0.0023(13) -0.0024(17) C12B 0.0248(16) 0.033(2) 0.0201(16) -0.0010(16) 0.0024(13) 0.0011(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 Te1 O2AA 1.8411(12) . ? Te1 O2AB 1.8454(12) . ? Te1 O1A 1.876(2) . ? Te1 C1A 2.143(3) . ? Te1 N2A 2.693(3) . ? Te2 O2BB 1.8648(13) . ? Te2 O2BA 1.8702(12) . ? Te2 O1BB 1.8850(13) . ? Te2 O1BA 1.8851(12) . ? Te2 C1B 2.144(4) . ? Te2 N2B 2.708(3) . ? Na1 O8WB 1.669(9) . ? Na1 O3WC 2.373(6) . ? Na1 O3WA 2.404(5) . ? Na1 O8WA 2.424(5) . ? Na1 O2WA 2.431(5) . ? Na1 O1W 2.499(3) . ? Na1 O7W 2.508(5) . ? Na1 O7W 2.547(5) 1_565 ? Na1 O3WB 2.917(6) . ? Na1 Na2 3.451(3) . ? Na1 Na2 3.520(3) 1_565 ? Na1 H3W4 2.3728 . ? Na1 H3W6 1.9762 . ? Na1 H8W3 2.22(3) . ? Na1 H8W4 1.29(5) . ? Na2 O6W 2.338(3) . ? Na2 O7W 2.343(3) . ? Na2 O5WA 2.365(4) . ? Na2 O5WB 2.443(15) . ? Na2 O4W 2.452(3) . ? Na2 O8WA 2.519(5) 1_545 ? Na2 O8WA 2.530(5) . ? Na2 O8WB 2.589(9) . ? Na2 O8WB 2.676(9) 1_545 ? Na2 Na1 3.520(3) 1_545 ? O2AA H2C 0.8400 . ? O1W H1W1 0.770(12) . ? O1W H1W2 0.801(15) . ? O2WA H2W1 0.824(16) . ? O2WA H2W2 0.828(14) . ? O2WA H2W3 1.18(3) . ? O2WA H2W4 1.21(4) . ? O2WB H2W1 0.86(2) . ? O2WB H2W2 0.59(2) . ? O2WB H2W3 0.815(18) . ? O2WB H2W4 0.817(19) . ? O3WA H3W1 0.815(14) . ? O3WA H3W2 0.812(14) . ? O3WA H3W4 0.8169 . ? O3WA H3W6 1.0839 . ? O3WB H3W2 1.26(3) . ? O3WB H3W3 0.8228 . ? O3WB H3W4 0.8284 . ? O3WC H3W1 1.31(2) . ? O3WC H3W5 0.8219 . ? O3WC H3W6 0.8156 . ? O4W H4W1 0.809(12) . ? O4W H4W2 0.832(14) . ? O5WA H5W1 0.844(14) . ? O5WA H5W2 0.830(14) . ? O5WA H5W3 1.08(3) . ? O5WA H5W4 0.98(5) . ? O5WB H5W1 0.99(3) . ? O5WB H5W2 0.78(3) . ? O5WB H5W3 0.828(19) . ? O5WB H5W4 0.828(19) . ? O6W H6W1 0.8189 . ? O6W H6W2 0.7890 . ? O7W Na1 2.547(5) 1_545 ? O7W H7W1 0.827(12) . ? O7W H7W2 0.824(12) . ? O8WA Na2 2.519(5) 1_565 ? O8WA H8W1 0.809(12) . ? O8WA H8W2 0.779(13) . ? O8WA H8W3 0.71(4) . ? O8WA H8W4 1.35(2) . ? O8WB Na2 2.676(9) 1_565 ? O8WB H8W1 1.422(15) . ? O8WB H8W2 1.278(15) . ? O8WB H8W3 0.826(19) . ? O8WB H8W4 0.827(18) . ? O9W H9W1 0.813(16) . ? O9W H9W2 0.800(16) . ? O10W H101 0.815(16) . ? O10W H102 0.808(18) . ? O11W H111 0.8260 . ? O11W H112 0.8260 . ? O12W H121 0.792(14) . ? O12W H122 0.821(15) . ? N1A N2A 1.267(4) . ? N1A C6A 1.428(4) . ? N2A C7A 1.420(4) . ? N1B N2B 1.255(4) . ? N1B C6B 1.422(4) . ? N2B C7B 1.418(4) . ? C1A C2A 1.377(5) . ? C1A C6A 1.400(5) . ? C2A C3A 1.376(5) . ? C2A H2AA 0.9500 . ? C3A C4A 1.391(5) . ? C3A H3AA 0.9500 . ? C4A C5A 1.373(5) . ? C4A H4AA 0.9500 . ? C5A C6A 1.389(5) . ? C5A H5AA 0.9500 . ? C7A C12A 1.381(5) . ? C7A C8A 1.397(5) . ? C8A C9A 1.389(5) . ? C8A H8AA 0.9500 . ? C9A C10A 1.379(5) . ? C9A H9AA 0.9500 . ? C10A C11A 1.380(5) . ? C10A H10A 0.9500 . ? C11A C12A 1.380(5) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C2B 1.389(5) . ? C1B C6B 1.390(5) . ? C2B C3B 1.387(6) . ? C2B H2BA 0.9500 . ? C3B C4B 1.378(6) . ? C3B H3BA 0.9500 . ? C4B C5B 1.383(6) . ? C4B H4BA 0.9500 . ? C5B C6B 1.416(5) . ? C5B H5BA 0.9500 . ? C7B C12B 1.385(5) . ? C7B C8B 1.399(5) . ? C8B C9B 1.365(5) . ? C8B H8BA 0.9500 . ? C9B C10B 1.397(5) . ? C9B H9BA 0.9500 . ? C10B C11B 1.383(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.406(5) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2AA Te1 O2AB 18.80(17) . . ? O2AA Te1 O1A 98.17(12) . . ? O2AB Te1 O1A 100.18(14) . . ? O2AA Te1 C1A 109.88(16) . . ? O2AB Te1 C1A 91.08(15) . . ? O1A Te1 C1A 95.10(12) . . ? O2AA Te1 N2A 87.60(11) . . ? O2AB Te1 N2A 80.04(14) . . ? O1A Te1 N2A 162.26(10) . . ? C1A Te1 N2A 67.18(11) . . ? O2BB Te2 O2BA 21.35(18) . . ? O2BB Te2 O1BB 89.71(14) . . ? O2BA Te2 O1BB 94.32(16) . . ? O2BB Te2 O1BA 101.66(14) . . ? O2BA Te2 O1BA 109.21(16) . . ? O1BB Te2 O1BA 15.9(2) . . ? O2BB Te2 C1B 112.04(19) . . ? O2BA Te2 C1B 91.01(14) . . ? O1BB Te2 C1B 92.14(18) . . ? O1BA Te2 C1B 97.13(16) . . ? O2BB Te2 N2B 92.14(13) . . ? O2BA Te2 N2B 80.04(13) . . ? O1BB Te2 N2B 157.82(18) . . ? O1BA Te2 N2B 162.04(11) . . ? C1B Te2 N2B 66.73(11) . . ? O8WB Na1 O3WC 116.4(3) . . ? O8WB Na1 O3WA 107.7(3) . . ? O3WC Na1 O3WA 35.52(19) . . ? O8WB Na1 O8WA 5.3(3) . . ? O3WC Na1 O8WA 111.4(2) . . ? O3WA Na1 O8WA 102.60(17) . . ? O8WB Na1 O2WA 168.6(3) . . ? O3WC Na1 O2WA 73.87(19) . . ? O3WA Na1 O2WA 83.51(17) . . ? O8WA Na1 O2WA 173.87(18) . . ? O8WB Na1 O1W 83.9(3) . . ? O3WC Na1 O1W 142.3(2) . . ? O3WA Na1 O1W 167.76(17) . . ? O8WA Na1 O1W 89.11(13) . . ? O2WA Na1 O1W 84.76(14) . . ? O8WB Na1 O7W 88.5(3) . . ? O3WC Na1 O7W 121.8(2) . . ? O3WA Na1 O7W 88.42(16) . . ? O8WA Na1 O7W 89.85(15) . . ? O2WA Na1 O7W 89.86(16) . . ? O1W Na1 O7W 88.09(12) . . ? O8WB Na1 O7W 88.3(3) . 1_565 ? O3WC Na1 O7W 63.91(18) . 1_565 ? O3WA Na1 O7W 97.10(16) . 1_565 ? O8WA Na1 O7W 87.37(15) . 1_565 ? O2WA Na1 O7W 92.36(16) . 1_565 ? O1W Na1 O7W 86.83(12) . 1_565 ? O7W Na1 O7W 174.25(17) . 1_565 ? O8WB Na1 O3WB 122.3(3) . . ? O3WC Na1 O3WB 60.40(19) . . ? O3WA Na1 O3WB 33.04(16) . . ? O8WA Na1 O3WB 118.84(16) . . ? O2WA Na1 O3WB 66.23(16) . . ? O1W Na1 O3WB 136.81(16) . . ? O7W Na1 O3WB 61.90(14) . . ? O7W Na1 O3WB 123.83(15) 1_565 . ? O8WB Na1 Na2 46.1(3) . . ? O3WC Na1 Na2 128.29(16) . . ? O3WA Na1 Na2 96.32(14) . . ? O8WA Na1 Na2 47.12(12) . . ? O2WA Na1 Na2 132.44(16) . . ? O1W Na1 Na2 89.04(9) . . ? O7W Na1 Na2 42.75(8) . . ? O7W Na1 Na2 134.38(11) 1_565 . ? O3WB Na1 Na2 88.21(12) . . ? O8WB Na1 Na2 47.0(3) . 1_565 ? O3WC Na1 Na2 85.04(17) . 1_565 ? O3WA Na1 Na2 102.53(14) . 1_565 ? O8WA Na1 Na2 45.70(12) . 1_565 ? O2WA Na1 Na2 133.88(16) . 1_565 ? O1W Na1 Na2 88.13(9) . 1_565 ? O7W Na1 Na2 135.43(11) . 1_565 ? O7W Na1 Na2 41.69(8) 1_565 1_565 ? O3WB Na1 Na2 135.05(13) . 1_565 ? Na2 Na1 Na2 92.80(6) . 1_565 ? O8WB Na1 H3W4 115.4 . . ? O3WC Na1 H3W4 50.7 . . ? O3WA Na1 H3W4 19.7 . . ? O8WA Na1 H3W4 111.0 . . ? O2WA Na1 H3W4 74.6 . . ? O1W Na1 H3W4 150.4 . . ? O7W Na1 H3W4 71.2 . . ? O7W Na1 H3W4 114.5 1_565 . ? O3WB Na1 H3W4 13.6 . . ? Na2 Na1 H3W4 89.5 . . ? Na2 Na1 H3W4 121.4 1_565 . ? O8WB Na1 H3W6 127.9 . . ? O3WC Na1 H3W6 18.9 . . ? O3WA Na1 H3W6 26.4 . . ? O8WA Na1 H3W6 122.6 . . ? O2WA Na1 H3W6 63.4 . . ? O1W Na1 H3W6 145.2 . . ? O7W Na1 H3W6 104.5 . . ? O7W Na1 H3W6 81.2 1_565 . ? O3WB Na1 H3W6 42.6 . . ? Na2 Na1 H3W6 122.3 . . ? Na2 Na1 H3W6 103.5 1_565 . ? H3W4 Na1 H3W6 35.2 . . ? O8WB Na1 H8W3 18.4(8) . . ? O3WC Na1 H8W3 102.4(10) . . ? O3WA Na1 H8W3 103.9(15) . . ? O8WA Na1 H8W3 16.7(9) . . ? O2WA Na1 H8W3 162.0(13) . . ? O1W Na1 H8W3 88.4(15) . . ? O7W Na1 H8W3 106.5(9) . . ? O7W Na1 H8W3 70.6(10) 1_565 . ? O3WB Na1 H8W3 127.9(16) . . ? Na2 Na1 H8W3 63.8(9) . . ? Na2 Na1 H8W3 29.0(9) 1_565 . ? H3W4 Na1 H8W3 117.2 . . ? H3W6 Na1 H8W3 117.5 . . ? O8WB Na1 H8W4 29.0(11) . . ? O3WC Na1 H8W4 92.2(16) . . ? O3WA Na1 H8W4 78.7(12) . . ? O8WA Na1 H8W4 23.9(12) . . ? O2WA Na1 H8W4 162.1(12) . . ? O1W Na1 H8W4 112.9(12) . . ? O7W Na1 H8W4 88(2) . . ? O7W Na1 H8W4 91(2) 1_565 . ? O3WB Na1 H8W4 97.3(15) . . ? Na2 Na1 H8W4 49(2) . . ? Na2 Na1 H8W4 53(2) 1_565 . ? H3W4 Na1 H8W4 87.9 . . ? H3W6 Na1 H8W4 100.0 . . ? H8W3 Na1 H8W4 31.0(19) . . ? O6W Na2 O7W 93.23(10) . . ? O6W Na2 O5WA 92.90(12) . . ? O7W Na2 O5WA 173.47(13) . . ? O6W Na2 O5WB 82.6(3) . . ? O7W Na2 O5WB 163.5(4) . . ? O5WA Na2 O5WB 17.2(4) . . ? O6W Na2 O4W 173.76(12) . . ? O7W Na2 O4W 91.36(10) . . ? O5WA Na2 O4W 82.37(11) . . ? O5WB Na2 O4W 91.8(3) . . ? O6W Na2 O8WA 88.26(13) . 1_545 ? O7W Na2 O8WA 89.80(14) . 1_545 ? O5WA Na2 O8WA 88.11(16) . 1_545 ? O5WB Na2 O8WA 74.1(4) . 1_545 ? O4W Na2 O8WA 87.53(13) . 1_545 ? O6W Na2 O8WA 93.89(13) . . ? O7W Na2 O8WA 91.19(14) . . ? O5WA Na2 O8WA 90.66(16) . . ? O5WB Na2 O8WA 105.0(4) . . ? O4W Na2 O8WA 90.24(13) . . ? O8WA Na2 O8WA 177.6(2) 1_545 . ? O6W Na2 O8WB 91.81(19) . . ? O7W Na2 O8WB 74.0(2) . . ? O5WA Na2 O8WB 108.1(2) . . ? O5WB Na2 O8WB 121.9(5) . . ? O4W Na2 O8WB 93.52(19) . . ? O8WA Na2 O8WB 163.8(3) 1_545 . ? O8WA Na2 O8WB 17.42(18) . . ? O6W Na2 O8WB 86.43(19) . 1_545 ? O7W Na2 O8WB 73.2(2) . 1_545 ? O5WA Na2 O8WB 104.9(2) . 1_545 ? O5WB Na2 O8WB 90.5(5) . 1_545 ? O4W Na2 O8WB 90.86(19) . 1_545 ? O8WA Na2 O8WB 16.87(18) 1_545 1_545 ? O8WA Na2 O8WB 164.4(2) . 1_545 ? O8WB Na2 O8WB 147.0(4) . 1_545 ? O6W Na2 Na1 96.17(9) . . ? O7W Na2 Na1 46.61(10) . . ? O5WA Na2 Na1 134.73(13) . . ? O5WB Na2 Na1 149.6(4) . . ? O4W Na2 Na1 90.06(9) . . ? O8WA Na2 Na1 136.29(12) 1_545 . ? O8WA Na2 Na1 44.60(12) . . ? O8WB Na2 Na1 27.7(2) . . ? O8WB Na2 Na1 119.80(19) 1_545 . ? O6W Na2 Na1 91.99(9) . 1_545 ? O7W Na2 Na1 46.30(10) . 1_545 ? O5WA Na2 Na1 131.15(13) . 1_545 ? O5WB Na2 Na1 117.6(4) . 1_545 ? O4W Na2 Na1 88.12(9) . 1_545 ? O8WA Na2 Na1 43.52(12) 1_545 1_545 ? O8WA Na2 Na1 137.37(12) . 1_545 ? O8WB Na2 Na1 120.3(2) . 1_545 ? O8WB Na2 Na1 27.14(19) 1_545 1_545 ? Na1 Na2 Na1 92.80(6) . 1_545 ? Te1 O2AA H2C 109.5 . . ? Na1 O1W H1W1 115.4(15) . . ? Na1 O1W H1W2 111.3(14) . . ? H1W1 O1W H1W2 114(2) . . ? Na1 O2WA H2W1 115.0(15) . . ? Na1 O2WA H2W2 114.7(16) . . ? H2W1 O2WA H2W2 102(2) . . ? Na1 O2WA H2W3 158(2) . . ? H2W1 O2WA H2W3 49(3) . . ? H2W2 O2WA H2W3 86(3) . . ? Na1 O2WA H2W4 123(2) . . ? H2W1 O2WA H2W4 58(3) . . ? H2W2 O2WA H2W4 46(4) . . ? H2W3 O2WA H2W4 65.7(19) . . ? H2W1 O2WB H2W2 123(4) . . ? H2W1 O2WB H2W3 64(4) . . ? H2W2 O2WB H2W3 171(4) . . ? H2W1 O2WB H2W4 76(5) . . ? H2W2 O2WB H2W4 74(5) . . ? H2W3 O2WB H2W4 105(3) . . ? Na1 O3WA H3W1 117.9(17) . . ? Na1 O3WA H3W2 117.4(16) . . ? H3W1 O3WA H3W2 106(2) . . ? Na1 O3WA H3W4 78.0 . . ? H3W1 O3WA H3W4 95.0 . . ? H3W2 O3WA H3W4 55.4 . . ? Na1 O3WA H3W6 54.2 . . ? H3W1 O3WA H3W6 64.5 . . ? H3W2 O3WA H3W6 145.3 . . ? H3W4 O3WA H3W6 90.9 . . ? Na1 O3WB H3W2 75.4(8) . . ? Na1 O3WB H3W3 145.3 . . ? H3W2 O3WB H3W3 71.4 . . ? Na1 O3WB H3W4 42.5 . . ? H3W2 O3WB H3W4 35.6 . . ? H3W3 O3WB H3W4 102.9 . . ? Na1 O3WC H3W1 98.7(10) . . ? Na1 O3WC H3W5 123.1 . . ? H3W1 O3WC H3W5 100.4 . . ? Na1 O3WC H3W6 51.8 . . ? H3W1 O3WC H3W6 52.6 . . ? H3W5 O3WC H3W6 104.8 . . ? Na2 O4W H4W1 114.8(14) . . ? Na2 O4W H4W2 110.9(14) . . ? H4W1 O4W H4W2 104(2) . . ? Na2 O5WA H5W1 119.9(16) . . ? Na2 O5WA H5W2 121.6(15) . . ? H5W1 O5WA H5W2 99.8(18) . . ? Na2 O5WA H5W3 118(3) . . ? H5W1 O5WA H5W3 95(3) . . ? H5W2 O5WA H5W3 10(3) . . ? Na2 O5WA H5W4 118(4) . . ? H5W1 O5WA H5W4 22(4) . . ? H5W2 O5WA H5W4 84(3) . . ? H5W3 O5WA H5W4 77(3) . . ? Na2 O5WB H5W1 106.3(16) . . ? Na2 O5WB H5W2 118(2) . . ? H5W1 O5WB H5W2 92(2) . . ? Na2 O5WB H5W3 129(4) . . ? H5W1 O5WB H5W3 104(4) . . ? H5W2 O5WB H5W3 21(4) . . ? Na2 O5WB H5W4 120(3) . . ? H5W1 O5WB H5W4 22(5) . . ? H5W2 O5WB H5W4 98(5) . . ? H5W3 O5WB H5W4 102(3) . . ? Na2 O6W H6W1 121.6 . . ? Na2 O6W H6W2 124.6 . . ? H6W1 O6W H6W2 108.4 . . ? Na2 O7W Na1 90.64(13) . . ? Na2 O7W Na1 92.01(12) . 1_545 ? Na1 O7W Na1 174.25(17) . 1_545 ? Na2 O7W H7W1 122.1(13) . . ? Na1 O7W H7W1 107.2(12) . . ? Na1 O7W H7W1 75.6(13) 1_545 . ? Na2 O7W H7W2 122.9(13) . . ? Na1 O7W H7W2 106.6(13) . . ? Na1 O7W H7W2 67.7(13) 1_545 . ? H7W1 O7W H7W2 104.3(17) . . ? Na1 O8WA Na2 90.79(17) . 1_565 ? Na1 O8WA Na2 88.28(16) . . ? Na2 O8WA Na2 177.6(2) 1_565 . ? Na1 O8WA H8W1 115.8(14) . . ? Na2 O8WA H8W1 75.6(13) 1_565 . ? Na2 O8WA H8W1 106.8(13) . . ? Na1 O8WA H8W2 120.1(14) . . ? Na2 O8WA H8W2 69.6(14) 1_565 . ? Na2 O8WA H8W2 109.0(14) . . ? H8W1 O8WA H8W2 112.8(18) . . ? Na1 O8WA H8W3 65(2) . . ? Na2 O8WA H8W3 26(2) 1_565 . ? Na2 O8WA H8W3 153(2) . . ? H8W1 O8WA H8W3 89(5) . . ? H8W2 O8WA H8W3 84(4) . . ? Na1 O8WA H8W4 23(2) . . ? Na2 O8WA H8W4 94(2) 1_565 . ? Na2 O8WA H8W4 86(2) . . ? H8W1 O8WA H8W4 95(2) . . ? H8W2 O8WA H8W4 142(3) . . ? H8W3 O8WA H8W4 70(2) . . ? Na1 O8WB Na2 106.2(4) . . ? Na1 O8WB Na2 105.9(4) . 1_565 ? Na2 O8WB Na2 147.0(4) . 1_565 ? Na1 O8WB H8W1 136.3(9) . . ? Na2 O8WB H8W1 86.2(8) . . ? Na2 O8WB H8W1 65.2(8) 1_565 . ? Na1 O8WB H8W2 157.9(10) . . ? Na2 O8WB H8W2 89.6(9) . . ? Na2 O8WB H8W2 62.0(9) 1_565 . ? H8W1 O8WB H8W2 58.4(10) . . ? Na1 O8WB H8W3 122(3) . . ? Na2 O8WB H8W3 129(3) . . ? Na2 O8WB H8W3 18(4) 1_565 . ? H8W1 O8WB H8W3 48(4) . . ? H8W2 O8WB H8W3 51(2) . . ? Na1 O8WB H8W4 49(4) . . ? Na2 O8WB H8W4 95(4) . . ? Na2 O8WB H8W4 100(4) 1_565 . ? H8W1 O8WB H8W4 89(4) . . ? H8W2 O8WB H8W4 146(4) . . ? H8W3 O8WB H8W4 103(3) . . ? H9W1 O9W H9W2 109(3) . . ? H101 O10W H102 113(4) . . ? H111 O11W H112 103.3 . . ? H121 O12W H122 106(2) . . ? N2A N1A C6A 112.4(3) . . ? N1A N2A C7A 116.1(3) . . ? N1A N2A Te1 113.7(2) . . ? C7A N2A Te1 130.1(2) . . ? N2B N1B C6B 113.3(3) . . ? N1B N2B C7B 116.8(3) . . ? N1B N2B Te2 113.0(2) . . ? C7B N2B Te2 129.7(2) . . ? C2A C1A C6A 118.3(3) . . ? C2A C1A Te1 120.2(2) . . ? C6A C1A Te1 121.6(2) . . ? C3A C2A C1A 121.5(3) . . ? C3A C2A H2AA 119.2 . . ? C1A C2A H2AA 119.2 . . ? C2A C3A C4A 120.3(3) . . ? C2A C3A H3AA 119.9 . . ? C4A C3A H3AA 119.9 . . ? C5A C4A C3A 118.8(3) . . ? C5A C4A H4AA 120.6 . . ? C3A C4A H4AA 120.6 . . ? C4A C5A C6A 121.0(3) . . ? C4A C5A H5AA 119.5 . . ? C6A C5A H5AA 119.5 . . ? C5A C6A C1A 120.0(3) . . ? C5A C6A N1A 115.0(3) . . ? C1A C6A N1A 125.0(3) . . ? C12A C7A C8A 120.4(3) . . ? C12A C7A N2A 115.5(3) . . ? C8A C7A N2A 124.1(3) . . ? C9A C8A C7A 118.4(3) . . ? C9A C8A H8AA 120.8 . . ? C7A C8A H8AA 120.8 . . ? C10A C9A C8A 121.0(3) . . ? C10A C9A H9AA 119.5 . . ? C8A C9A H9AA 119.5 . . ? C9A C10A C11A 120.1(3) . . ? C9A C10A H10A 120.0 . . ? C11A C10A H10A 120.0 . . ? C12A C11A C10A 119.8(3) . . ? C12A C11A H11A 120.1 . . ? C10A C11A H11A 120.1 . . ? C11A C12A C7A 120.4(3) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C2B C1B C6B 119.8(3) . . ? C2B C1B Te2 118.0(3) . . ? C6B C1B Te2 122.1(2) . . ? C3B C2B C1B 119.7(4) . . ? C3B C2B H2BA 120.2 . . ? C1B C2B H2BA 120.2 . . ? C4B C3B C2B 121.1(4) . . ? C4B C3B H3BA 119.5 . . ? C2B C3B H3BA 119.5 . . ? C3B C4B C5B 120.2(4) . . ? C3B C4B H4BA 119.9 . . ? C5B C4B H4BA 119.9 . . ? C4B C5B C6B 119.2(4) . . ? C4B C5B H5BA 120.4 . . ? C6B C5B H5BA 120.4 . . ? C1B C6B C5B 120.0(3) . . ? C1B C6B N1B 124.6(3) . . ? C5B C6B N1B 115.4(3) . . ? C12B C7B C8B 121.2(3) . . ? C12B C7B N2B 114.7(3) . . ? C8B C7B N2B 124.1(3) . . ? C9B C8B C7B 118.9(3) . . ? C9B C8B H8BA 120.5 . . ? C7B C8B H8BA 120.5 . . ? C8B C9B C10B 121.4(3) . . ? C8B C9B H9BA 119.3 . . ? C10B C9B H9BA 119.3 . . ? C11B C10B C9B 119.5(3) . . ? C11B C10B H10B 120.3 . . ? C9B C10B H10B 120.3 . . ? C10B C11B C12B 120.2(3) . . ? C10B C11B H11B 119.9 . . ? C12B C11B H11B 119.9 . . ? C7B C12B C11B 118.8(3) . . ? C7B C12B H12B 120.6 . . ? C11B C12B H12B 120.6 . . ? 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 O8WB Na1 Na2 O6W -82.1(4) . . . . ? O3WC Na1 Na2 O6W -173.6(2) . . . . ? O3WA Na1 Na2 O6W 169.36(15) . . . . ? O8WA Na1 Na2 O6W -89.29(16) . . . . ? O2WA Na1 Na2 O6W 82.4(2) . . . . ? O1W Na1 Na2 O6W 0.39(12) . . . . ? O7W Na1 Na2 O6W 88.61(13) . . . . ? O7W Na1 Na2 O6W -84.23(17) 1_565 . . . ? O3WB Na1 Na2 O6W 137.28(13) . . . . ? Na2 Na1 Na2 O6W -87.69(9) 1_565 . . . ? O8WB Na1 Na2 O7W -170.7(4) . . . . ? O3WC Na1 Na2 O7W 97.8(2) . . . . ? O3WA Na1 Na2 O7W 80.75(17) . . . . ? O8WA Na1 Na2 O7W -177.9(2) . . . . ? O2WA Na1 Na2 O7W -6.22(19) . . . . ? O1W Na1 Na2 O7W -88.22(13) . . . . ? O7W Na1 Na2 O7W -172.8(2) 1_565 . . . ? O3WB Na1 Na2 O7W 48.67(14) . . . . ? Na2 Na1 Na2 O7W -176.30(12) 1_565 . . . ? O8WB Na1 Na2 O5WA 18.2(4) . . . . ? O3WC Na1 Na2 O5WA -73.3(3) . . . . ? O3WA Na1 Na2 O5WA -90.35(19) . . . . ? O8WA Na1 Na2 O5WA 11.00(19) . . . . ? O2WA Na1 Na2 O5WA -177.3(2) . . . . ? O1W Na1 Na2 O5WA 100.68(16) . . . . ? O7W Na1 Na2 O5WA -171.10(17) . . . . ? O7W Na1 Na2 O5WA 16.1(2) 1_565 . . . ? O3WB Na1 Na2 O5WA -122.43(17) . . . . ? Na2 Na1 Na2 O5WA 12.60(16) 1_565 . . . ? O8WB Na1 Na2 O5WB 3.7(7) . . . . ? O3WC Na1 Na2 O5WB -87.7(7) . . . . ? O3WA Na1 Na2 O5WB -104.8(7) . . . . ? O8WA Na1 Na2 O5WB -3.5(7) . . . . ? O2WA Na1 Na2 O5WB 168.2(7) . . . . ? O1W Na1 Na2 O5WB 86.2(7) . . . . ? O7W Na1 Na2 O5WB 174.4(7) . . . . ? O7W Na1 Na2 O5WB 1.6(7) 1_565 . . . ? O3WB Na1 Na2 O5WB -136.9(7) . . . . ? Na2 Na1 Na2 O5WB -1.9(7) 1_565 . . . ? O8WB Na1 Na2 O4W 97.5(4) . . . . ? O3WC Na1 Na2 O4W 6.0(2) . . . . ? O3WA Na1 Na2 O4W -11.07(15) . . . . ? O8WA Na1 Na2 O4W 90.28(16) . . . . ? O2WA Na1 Na2 O4W -98.0(2) . . . . ? O1W Na1 Na2 O4W 179.96(12) . . . . ? O7W Na1 Na2 O4W -91.82(13) . . . . ? O7W Na1 Na2 O4W 95.33(16) 1_565 . . . ? O3WB Na1 Na2 O4W -43.15(13) . . . . ? Na2 Na1 Na2 O4W 91.88(9) 1_565 . . . ? O8WB Na1 Na2 O8WA -176.0(4) . . . 1_545 ? O3WC Na1 Na2 O8WA 92.5(3) . . . 1_545 ? O3WA Na1 Na2 O8WA 75.4(2) . . . 1_545 ? O8WA Na1 Na2 O8WA 176.8(3) . . . 1_545 ? O2WA Na1 Na2 O8WA -11.6(3) . . . 1_545 ? O1W Na1 Na2 O8WA -93.55(18) . . . 1_545 ? O7W Na1 Na2 O8WA -5.33(17) . . . 1_545 ? O7W Na1 Na2 O8WA -178.18(19) 1_565 . . 1_545 ? O3WB Na1 Na2 O8WA 43.34(19) . . . 1_545 ? Na2 Na1 Na2 O8WA 178.37(14) 1_565 . . 1_545 ? O8WB Na1 Na2 O8WA 7.2(4) . . . . ? O3WC Na1 Na2 O8WA -84.3(3) . . . . ? O3WA Na1 Na2 O8WA -101.3(2) . . . . ? O2WA Na1 Na2 O8WA 171.7(2) . . . . ? O1W Na1 Na2 O8WA 89.68(16) . . . . ? O7W Na1 Na2 O8WA 177.9(2) . . . . ? O7W Na1 Na2 O8WA 5.05(17) 1_565 . . . ? O3WB Na1 Na2 O8WA -133.43(18) . . . . ? Na2 Na1 Na2 O8WA 1.60(14) 1_565 . . . ? O3WC Na1 Na2 O8WB -91.5(4) . . . . ? O3WA Na1 Na2 O8WB -108.5(4) . . . . ? O8WA Na1 Na2 O8WB -7.2(4) . . . . ? O2WA Na1 Na2 O8WB 164.5(4) . . . . ? O1W Na1 Na2 O8WB 82.5(4) . . . . ? O7W Na1 Na2 O8WB 170.7(4) . . . . ? O7W Na1 Na2 O8WB -2.1(4) 1_565 . . . ? O3WB Na1 Na2 O8WB -140.6(4) . . . . ? Na2 Na1 Na2 O8WB -5.6(4) 1_565 . . . ? O8WB Na1 Na2 O8WB -171.5(6) . . . 1_545 ? O3WC Na1 Na2 O8WB 97.0(3) . . . 1_545 ? O3WA Na1 Na2 O8WB 80.0(2) . . . 1_545 ? O8WA Na1 Na2 O8WB -178.7(2) . . . 1_545 ? O2WA Na1 Na2 O8WB -7.0(3) . . . 1_545 ? O1W Na1 Na2 O8WB -89.0(2) . . . 1_545 ? O7W Na1 Na2 O8WB -0.8(2) . . . 1_545 ? O7W Na1 Na2 O8WB -173.6(2) 1_565 . . 1_545 ? O3WB Na1 Na2 O8WB 47.9(2) . . . 1_545 ? Na2 Na1 Na2 O8WB -177.10(19) 1_565 . . 1_545 ? O8WB Na1 Na2 Na1 -174.4(4) . . . 1_545 ? O3WC Na1 Na2 Na1 94.1(2) . . . 1_545 ? O3WA Na1 Na2 Na1 77.05(14) . . . 1_545 ? O8WA Na1 Na2 Na1 178.40(14) . . . 1_545 ? O2WA Na1 Na2 Na1 -9.9(2) . . . 1_545 ? O1W Na1 Na2 Na1 -91.92(9) . . . 1_545 ? O7W Na1 Na2 Na1 -3.70(12) . . . 1_545 ? O7W Na1 Na2 Na1 -176.55(11) 1_565 . . 1_545 ? O3WB Na1 Na2 Na1 44.97(13) . . . 1_545 ? Na2 Na1 Na2 Na1 180.0 1_565 . . 1_545 ? O6W Na2 O7W Na1 -95.44(12) . . . . ? O5WA Na2 O7W Na1 105.0(14) . . . . ? O5WB Na2 O7W Na1 -170.1(12) . . . . ? O4W Na2 O7W Na1 88.79(12) . . . . ? O8WA Na2 O7W Na1 176.32(12) 1_545 . . . ? O8WA Na2 O7W Na1 -1.47(14) . . . . ? O8WB Na2 O7W Na1 -4.48(19) . . . . ? O8WB Na2 O7W Na1 179.3(2) 1_545 . . . ? Na1 Na2 O7W Na1 174.89(17) 1_545 . . . ? O6W Na2 O7W Na1 89.67(12) . . . 1_545 ? O5WA Na2 O7W Na1 -69.9(14) . . . 1_545 ? O5WB Na2 O7W Na1 15.0(12) . . . 1_545 ? O4W Na2 O7W Na1 -86.10(12) . . . 1_545 ? O8WA Na2 O7W Na1 1.43(14) 1_545 . . 1_545 ? O8WA Na2 O7W Na1 -176.36(12) . . . 1_545 ? O8WB Na2 O7W Na1 -179.4(2) . . . 1_545 ? O8WB Na2 O7W Na1 4.39(19) 1_545 . . 1_545 ? Na1 Na2 O7W Na1 -174.89(17) . . . 1_545 ? O8WB Na1 O7W Na2 6.7(3) . . . . ? O3WC Na1 O7W Na2 -113.8(2) . . . . ? O3WA Na1 O7W Na2 -101.07(14) . . . . ? O8WA Na1 O7W Na2 1.54(14) . . . . ? O2WA Na1 O7W Na2 175.41(14) . . . . ? O1W Na1 O7W Na2 90.66(11) . . . . ? O7W Na1 O7W Na2 62.6(17) 1_565 . . . ? O3WB Na1 O7W Na2 -121.70(14) . . . . ? Na2 Na1 O7W Na2 5.26(17) 1_565 . . . ? O8WB Na1 O7W Na1 124.0(17) . . . 1_545 ? O3WC Na1 O7W Na1 3.6(18) . . . 1_545 ? O3WA Na1 O7W Na1 16.3(17) . . . 1_545 ? O8WA Na1 O7W Na1 118.9(17) . . . 1_545 ? O2WA Na1 O7W Na1 -67.2(17) . . . 1_545 ? O1W Na1 O7W Na1 -152.0(17) . . . 1_545 ? O7W Na1 O7W Na1 179.98(6) 1_565 . . 1_545 ? O3WB Na1 O7W Na1 -4.4(17) . . . 1_545 ? Na2 Na1 O7W Na1 117.3(17) . . . 1_545 ? Na2 Na1 O7W Na1 122.6(16) 1_565 . . 1_545 ? O8WB Na1 O8WA Na2 101(4) . . . 1_565 ? O3WC Na1 O8WA Na2 -59.2(2) . . . 1_565 ? O3WA Na1 O8WA Na2 -95.31(18) . . . 1_565 ? O2WA Na1 O8WA Na2 89.0(19) . . . 1_565 ? O1W Na1 O8WA Na2 88.25(13) . . . 1_565 ? O7W Na1 O8WA Na2 176.35(12) . . . 1_565 ? O7W Na1 O8WA Na2 1.39(13) 1_565 . . 1_565 ? O3WB Na1 O8WA Na2 -126.27(17) . . . 1_565 ? Na2 Na1 O8WA Na2 177.77(19) . . . 1_565 ? O8WB Na1 O8WA Na2 -76(4) . . . . ? O3WC Na1 O8WA Na2 123.0(2) . . . . ? O3WA Na1 O8WA Na2 86.92(18) . . . . ? O2WA Na1 O8WA Na2 -88.8(19) . . . . ? O1W Na1 O8WA Na2 -89.52(13) . . . . ? O7W Na1 O8WA Na2 -1.42(13) . . . . ? O7W Na1 O8WA Na2 -176.39(12) 1_565 . . . ? O3WB Na1 O8WA Na2 56.0(2) . . . . ? Na2 Na1 O8WA Na2 -177.77(19) 1_565 . . . ? O6W Na2 O8WA Na1 94.84(13) . . . . ? O7W Na2 O8WA Na1 1.53(14) . . . . ? O5WA Na2 O8WA Na1 -172.21(13) . . . . ? O5WB Na2 O8WA Na1 178.2(3) . . . . ? O4W Na2 O8WA Na1 -89.84(13) . . . . ? O8WA Na2 O8WA Na1 -113(5) 1_545 . . . ? O8WB Na2 O8WA Na1 11.2(6) . . . . ? O8WB Na2 O8WA Na1 4.2(7) 1_545 . . . ? Na1 Na2 O8WA Na1 -2.4(2) 1_545 . . . ? O6W Na2 O8WA Na2 27(5) . . . 1_565 ? O7W Na2 O8WA Na2 -66(5) . . . 1_565 ? O5WA Na2 O8WA Na2 120(5) . . . 1_565 ? O5WB Na2 O8WA Na2 111(5) . . . 1_565 ? O4W Na2 O8WA Na2 -157(5) . . . 1_565 ? O8WA Na2 O8WA Na2 -179.99(5) 1_545 . . 1_565 ? O8WB Na2 O8WA Na2 -56(5) . . . 1_565 ? O8WB Na2 O8WA Na2 -63(5) 1_545 . . 1_565 ? Na1 Na2 O8WA Na2 -67(5) . . . 1_565 ? Na1 Na2 O8WA Na2 -70(5) 1_545 . . 1_565 ? O3WC Na1 O8WB Na2 118.9(3) . . . . ? O3WA Na1 O8WB Na2 81.5(3) . . . . ? O8WA Na1 O8WB Na2 99(4) . . . . ? O2WA Na1 O8WB Na2 -88.0(18) . . . . ? O1W Na1 O8WB Na2 -94.5(3) . . . . ? O7W Na1 O8WB Na2 -6.3(3) . . . . ? O7W Na1 O8WB Na2 178.5(3) 1_565 . . . ? O3WB Na1 O8WB Na2 48.6(4) . . . . ? Na2 Na1 O8WB Na2 172.3(5) 1_565 . . . ? O3WC Na1 O8WB Na2 -53.5(4) . . . 1_565 ? O3WA Na1 O8WB Na2 -90.8(3) . . . 1_565 ? O8WA Na1 O8WB Na2 -74(4) . . . 1_565 ? O2WA Na1 O8WB Na2 99.7(18) . . . 1_565 ? O1W Na1 O8WB Na2 93.1(3) . . . 1_565 ? O7W Na1 O8WB Na2 -178.6(3) . . . 1_565 ? O7W Na1 O8WB Na2 6.1(3) 1_565 . . 1_565 ? O3WB Na1 O8WB Na2 -123.7(3) . . . 1_565 ? Na2 Na1 O8WB Na2 -172.3(5) . . . 1_565 ? O6W Na2 O8WB Na1 99.9(3) . . . . ? O7W Na2 O8WB Na1 7.0(3) . . . . ? O5WA Na2 O8WB Na1 -166.5(3) . . . . ? O5WB Na2 O8WB Na1 -177.8(4) . . . . ? O4W Na2 O8WB Na1 -83.4(3) . . . . ? O8WA Na2 O8WB Na1 9.9(10) 1_545 . . . ? O8WA Na2 O8WB Na1 -162.9(10) . . . . ? O8WB Na2 O8WB Na1 13.6(9) 1_545 . . . ? Na1 Na2 O8WB Na1 6.5(4) 1_545 . . . ? O6W Na2 O8WB Na2 -93.8(6) . . . 1_565 ? O7W Na2 O8WB Na2 173.4(6) . . . 1_565 ? O5WA Na2 O8WB Na2 -0.1(6) . . . 1_565 ? O5WB Na2 O8WB Na2 -11.4(8) . . . 1_565 ? O4W Na2 O8WB Na2 83.0(6) . . . 1_565 ? O8WA Na2 O8WB Na2 176.2(4) 1_545 . . 1_565 ? O8WA Na2 O8WB Na2 3.5(3) . . . 1_565 ? O8WB Na2 O8WB Na2 179.999(2) 1_545 . . 1_565 ? Na1 Na2 O8WB Na2 166.4(9) . . . 1_565 ? Na1 Na2 O8WB Na2 172.9(5) 1_545 . . 1_565 ? C6A N1A N2A C7A -178.3(3) . . . . ? C6A N1A N2A Te1 -2.1(3) . . . . ? O2AA Te1 N2A N1A 113.0(3) . . . . ? O2AB Te1 N2A N1A 95.7(2) . . . . ? O1A Te1 N2A N1A 3.4(5) . . . . ? C1A Te1 N2A N1A 0.3(2) . . . . ? O2AA Te1 N2A C7A -71.4(3) . . . . ? O2AB Te1 N2A C7A -88.8(3) . . . . ? O1A Te1 N2A C7A 178.9(3) . . . . ? C1A Te1 N2A C7A 175.8(3) . . . . ? C6B N1B N2B C7B 176.6(3) . . . . ? C6B N1B N2B Te2 3.5(3) . . . . ? O2BB Te2 N2B N1B -114.2(3) . . . . ? O2BA Te2 N2B N1B -96.5(2) . . . . ? O1BB Te2 N2B N1B -19.7(4) . . . . ? O1BA Te2 N2B N1B 26.3(6) . . . . ? C1B Te2 N2B N1B -1.1(2) . . . . ? O2BB Te2 N2B C7B 73.8(3) . . . . ? O2BA Te2 N2B C7B 91.5(3) . . . . ? O1BB Te2 N2B C7B 168.3(3) . . . . ? O1BA Te2 N2B C7B -145.8(5) . . . . ? C1B Te2 N2B C7B -173.1(3) . . . . ? O2AA Te1 C1A C2A 103.1(3) . . . . ? O2AB Te1 C1A C2A 102.8(3) . . . . ? O1A Te1 C1A C2A 2.5(3) . . . . ? N2A Te1 C1A C2A -178.5(3) . . . . ? O2AA Te1 C1A C6A -76.6(3) . . . . ? O2AB Te1 C1A C6A -76.9(3) . . . . ? O1A Te1 C1A C6A -177.2(3) . . . . ? N2A Te1 C1A C6A 1.8(3) . . . . ? C6A C1A C2A C3A 2.3(5) . . . . ? Te1 C1A C2A C3A -177.5(3) . . . . ? C1A C2A C3A C4A 0.1(5) . . . . ? C2A C3A C4A C5A -1.8(6) . . . . ? C3A C4A C5A C6A 1.1(6) . . . . ? C4A C5A C6A C1A 1.3(6) . . . . ? C4A C5A C6A N1A -177.8(3) . . . . ? C2A C1A C6A C5A -2.9(5) . . . . ? Te1 C1A C6A C5A 176.8(3) . . . . ? C2A C1A C6A N1A 176.1(3) . . . . ? Te1 C1A C6A N1A -4.2(5) . . . . ? N2A N1A C6A C5A -176.8(3) . . . . ? N2A N1A C6A C1A 4.2(5) . . . . ? N1A N2A C7A C12A 177.4(3) . . . . ? Te1 N2A C7A C12A 2.0(4) . . . . ? N1A N2A C7A C8A -1.6(5) . . . . ? Te1 N2A C7A C8A -177.0(2) . . . . ? C12A C7A C8A C9A 0.2(5) . . . . ? N2A C7A C8A C9A 179.1(3) . . . . ? C7A C8A C9A C10A -0.6(5) . . . . ? C8A C9A C10A C11A 0.7(5) . . . . ? C9A C10A C11A C12A -0.2(5) . . . . ? C10A C11A C12A C7A -0.3(5) . . . . ? C8A C7A C12A C11A 0.3(5) . . . . ? N2A C7A C12A C11A -178.7(3) . . . . ? O2BB Te2 C1B C2B -98.5(3) . . . . ? O2BA Te2 C1B C2B -102.3(3) . . . . ? O1BB Te2 C1B C2B -7.9(3) . . . . ? O1BA Te2 C1B C2B 7.2(3) . . . . ? N2B Te2 C1B C2B 179.0(3) . . . . ? O2BB Te2 C1B C6B 80.7(3) . . . . ? O2BA Te2 C1B C6B 76.9(3) . . . . ? O1BB Te2 C1B C6B 171.2(3) . . . . ? O1BA Te2 C1B C6B -173.6(3) . . . . ? N2B Te2 C1B C6B -1.8(3) . . . . ? C6B C1B C2B C3B -2.0(5) . . . . ? Te2 C1B C2B C3B 177.2(3) . . . . ? C1B C2B C3B C4B 0.6(6) . . . . ? C2B C3B C4B C5B 0.5(6) . . . . ? C3B C4B C5B C6B -0.2(6) . . . . ? C2B C1B C6B C5B 2.3(5) . . . . ? Te2 C1B C6B C5B -176.8(3) . . . . ? C2B C1B C6B N1B -175.9(3) . . . . ? Te2 C1B C6B N1B 5.0(5) . . . . ? C4B C5B C6B C1B -1.2(5) . . . . ? C4B C5B C6B N1B 177.1(3) . . . . ? N2B N1B C6B C1B -5.7(5) . . . . ? N2B N1B C6B C5B 176.1(3) . . . . ? N1B N2B C7B C12B -177.8(3) . . . . ? Te2 N2B C7B C12B -6.0(4) . . . . ? N1B N2B C7B C8B 1.8(5) . . . . ? Te2 N2B C7B C8B 173.6(2) . . . . ? C12B C7B C8B C9B 0.4(5) . . . . ? N2B C7B C8B C9B -179.1(3) . . . . ? C7B C8B C9B C10B 0.7(5) . . . . ? C8B C9B C10B C11B -1.4(6) . . . . ? C9B C10B C11B C12B 0.9(5) . . . . ? C8B C7B C12B C11B -0.9(5) . . . . ? N2B C7B C12B C11B 178.7(3) . . . . ? C10B C11B C12B C7B 0.2(5) . . . . ? 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 O2AA H2C O2WA 0.84 2.44 2.974(6) 121.9 3_565 O1W H1W1 O1A 0.770(12) 1.974(14) 2.722(3) 164(3) . O1W H1W2 O12W 0.801(15) 2.093(18) 2.831(4) 153(2) 1_545 O2WA H2W1 O2AA 0.824(16) 2.39(3) 2.974(6) 128(2) 3_465 O2WB H2W3 O11W 0.815(18) 2.11(4) 2.622(9) 120(4) . O2WB H2W3 O6W 0.815(18) 2.571(16) 3.377(9) 170(5) 3_465 O2WB H2W4 O2AB 0.817(19) 1.63(3) 2.379(9) 150(5) 3_465 O3WA H3W1 O11W 0.815(14) 1.86(3) 2.443(5) 128(3) . O3WA H3W2 O1BA 0.812(14) 2.069(16) 2.862(7) 165(3) 3_465 O3WB H3W3 O1BB 0.82 2.20 2.624(7) 112.6 3_465 O3WC H3W5 O9W 0.82 2.02 2.811(6) 162.0 . O3WC H3W6 O11W 0.82 2.07 2.565(7) 118.8 . O4W H4W1 O1BA 0.809(12) 1.827(13) 2.621(3) 167(2) 3_465 O4W H4W1 O1BB 0.809(12) 2.101(16) 2.873(4) 160(3) 3_465 O4W H4W2 O10W 0.832(14) 2.011(16) 2.805(4) 159.2(19) 1_545 O5WA H5W1 O11W 0.844(14) 1.73(3) 2.355(4) 129(3) 3_565 O5WA H5W2 O2BA 0.830(14) 1.909(16) 2.721(5) 165(3) 1_545 O5WB H5W3 O2BB 0.828(19) 1.80(3) 2.536(16) 147(4) 1_545 O5WB H5W4 O11W 0.828(19) 1.54(7) 1.995(14) 112(6) 3_565 O5WB H5W4 O3WB 0.828(19) 2.29(2) 3.102(15) 167(7) 3_565 O6W H6W1 O1A 0.82 2.15 2.961(4) 172.0 1_545 O6W H6W2 O1A 0.79 2.21 2.843(4) 138.1 . O6W H6W2 O9W 0.79 2.65 3.191(4) 127.1 3_575 O7W H7W1 O12W 0.827(12) 2.104(13) 2.883(4) 156.8(17) 1_545 O7W H7W2 O3WC 0.824(12) 1.830(15) 2.608(6) 156.7(17) 1_545 O7W H7W2 O3WB 0.824(12) 2.249(17) 2.812(5) 125.8(15) . O8WA H8W1 O10W 0.809(12) 2.158(14) 2.920(5) 156.9(17) . O8WA H8W2 O9W 0.779(13) 2.226(14) 2.896(5) 144.7(17) 3_575 O9W H9W1 O3WB 0.813(16) 2.01(4) 2.646(6) 134(4) 1_565 O9W H9W1 O3WC 0.813(16) 2.20(3) 2.811(6) 132(4) . O9W H9W2 O1A 0.800(16) 1.959(16) 2.756(4) 174(3) 3_475 O10W H101 O2BB 0.815(16) 1.857(19) 2.645(3) 162(4) . O10W H101 O2BA 0.815(16) 1.927(19) 2.724(3) 166(5) . O10W H102 O4W 0.808(18) 2.016(18) 2.820(4) 173(4) . O11W H111 O9W 0.83 2.00 2.693(5) 140.8 1_545 O11W H112 O2WA 0.83 1.72 2.385(5) 136.6 . O11W H112 O2WB 0.83 2.04 2.622(9) 127.1 . O11W H112 O3WC 0.83 2.10 2.565(7) 115.4 . O12W H121 O2AA 0.792(14) 1.817(16) 2.590(3) 165(4) 3_475 O12W H121 O2AB 0.792(14) 1.977(14) 2.746(3) 163(3) 3_475 O12W H122 O1W 0.821(15) 2.01(2) 2.795(4) 161(4) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.077 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.105 #===END data_azote2o _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N4 O Te2' _chemical_formula_sum 'C24 H18 N4 O Te2' _chemical_formula_weight 633.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.1759 6.3531 '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 1 21/c 1' 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 13.3187(7) _cell_length_b 7.7901(4) _cell_length_c 21.9666(14) _cell_angle_alpha 90.00 _cell_angle_beta 104.597(6) _cell_angle_gamma 90.00 _cell_volume 2205.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5829 _cell_measurement_theta_min 4.1536 _cell_measurement_theta_max 74.1188 _exptl_crystal_description needle _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.9611 _exptl_crystal_size_mid 0.1081 _exptl_crystal_size_min 0.0510 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 21.068 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.031 _exptl_absorpt_correction_T_max 0.418 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby (Gemini Cu) ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 9197 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 74.20 _reflns_number_total 4375 _reflns_number_gt 3953 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4375 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.302572(18) 0.42018(3) 0.289260(10) 0.01971(10) Uani 1 1 d . . . Te2 Te 0.165063(17) 0.46663(3) 0.129545(10) 0.01949(10) Uani 1 1 d . . . O1 O 0.1761(2) 0.3802(4) 0.21706(12) 0.0224(6) Uani 1 1 d . . . N1A N 0.5063(2) 0.2437(5) 0.36923(15) 0.0215(7) Uani 1 1 d . . . N2A N 0.4593(3) 0.3855(5) 0.36769(14) 0.0206(7) Uani 1 1 d . . . N1B N 0.1043(2) 0.7935(5) 0.04162(15) 0.0220(7) Uani 1 1 d . . . N2B N 0.1329(2) 0.6396(5) 0.03705(14) 0.0208(7) Uani 1 1 d . . . C1A C 0.3586(3) 0.1762(6) 0.28128(16) 0.0190(7) Uani 1 1 d . . . C2A C 0.3095(3) 0.0553(6) 0.23607(18) 0.0219(8) Uani 1 1 d . . . H2AA H 0.2469 0.0839 0.2061 0.026 Uiso 1 1 calc R . . C3A C 0.3532(3) -0.1062(6) 0.23552(19) 0.0248(9) Uani 1 1 d . . . H3AA H 0.3202 -0.1870 0.2045 0.030 Uiso 1 1 calc R . . C4A C 0.4451(3) -0.1531(6) 0.27975(18) 0.0241(8) Uani 1 1 d . . . H4AA H 0.4730 -0.2651 0.2791 0.029 Uiso 1 1 calc R . . C5A C 0.4941(3) -0.0355(6) 0.32387(19) 0.0234(8) Uani 1 1 d . . . H5AA H 0.5566 -0.0655 0.3537 0.028 Uiso 1 1 calc R . . C6A C 0.4519(3) 0.1280(6) 0.32470(17) 0.0196(8) Uani 1 1 d . . . C7A C 0.5120(3) 0.5148(6) 0.40971(18) 0.0231(8) Uani 1 1 d . . . C8A C 0.6207(3) 0.5208(7) 0.4278(2) 0.0298(10) Uani 1 1 d . . . H8AA H 0.6611 0.4391 0.4123 0.036 Uiso 1 1 calc R . . C9A C 0.6677(4) 0.6492(7) 0.4689(2) 0.0331(10) Uani 1 1 d . . . H9AA H 0.7412 0.6562 0.4813 0.040 Uiso 1 1 calc R . . C10A C 0.6090(4) 0.7681(7) 0.4923(2) 0.0327(10) Uani 1 1 d . . . H10A H 0.6424 0.8545 0.5208 0.039 Uiso 1 1 calc R . . C11A C 0.5018(3) 0.7599(6) 0.47394(18) 0.0289(9) Uani 1 1 d . . . H11A H 0.4615 0.8403 0.4901 0.035 Uiso 1 1 calc R . . C12A C 0.4532(3) 0.6342(6) 0.43188(18) 0.0255(9) Uani 1 1 d . . . H12A H 0.3797 0.6303 0.4184 0.031 Uiso 1 1 calc R . . C1B C 0.1070(3) 0.7019(5) 0.14870(17) 0.0184(7) Uani 1 1 d . . . C2B C 0.0830(3) 0.7408(6) 0.20574(17) 0.0218(8) Uani 1 1 d . . . H2BA H 0.0960 0.6589 0.2389 0.026 Uiso 1 1 calc R . . C3B C 0.0406(3) 0.8983(6) 0.21369(19) 0.0241(9) Uani 1 1 d . . . H3BA H 0.0236 0.9225 0.2523 0.029 Uiso 1 1 calc R . . C4B C 0.0219(3) 1.0233(6) 0.1665(2) 0.0258(9) Uani 1 1 d . . . H4BA H -0.0070 1.1310 0.1732 0.031 Uiso 1 1 calc R . . C5B C 0.0458(3) 0.9889(6) 0.10990(19) 0.0253(9) Uani 1 1 d . . . H5BA H 0.0344 1.0731 0.0776 0.030 Uiso 1 1 calc R . . C6B C 0.0872(3) 0.8271(6) 0.10086(17) 0.0204(8) Uani 1 1 d . . . C7B C 0.1500(3) 0.5901(6) -0.02178(17) 0.0226(9) Uani 1 1 d . . . C8B C 0.1845(3) 0.7065(6) -0.06038(19) 0.0267(9) Uani 1 1 d . . . H8BA H 0.1982 0.8226 -0.0477 0.032 Uiso 1 1 calc R . . C9B C 0.1986(3) 0.6495(7) -0.11768(19) 0.0291(9) Uani 1 1 d . . . H9BA H 0.2207 0.7277 -0.1448 0.035 Uiso 1 1 calc R . . C10B C 0.1804(3) 0.4785(7) -0.13543(19) 0.0279(9) Uani 1 1 d . . . H10B H 0.1913 0.4400 -0.1743 0.034 Uiso 1 1 calc R . . C11B C 0.1464(3) 0.3642(6) -0.09658(18) 0.0257(9) Uani 1 1 d . . . H11B H 0.1333 0.2478 -0.1090 0.031 Uiso 1 1 calc R . . C12B C 0.1314(3) 0.4201(6) -0.03963(18) 0.0217(8) Uani 1 1 d . . . H12B H 0.1084 0.3419 -0.0128 0.026 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 0.01888(16) 0.02072(17) 0.01854(14) 0.00037(8) 0.00287(9) -0.00011(9) Te2 0.01694(15) 0.02200(18) 0.01841(14) -0.00054(8) 0.00236(9) 0.00212(9) O1 0.0217(13) 0.0250(16) 0.0200(12) 0.0051(11) 0.0040(10) 0.0035(12) N1A 0.0175(14) 0.025(2) 0.0209(14) 0.0001(13) 0.0035(11) -0.0015(14) N2A 0.0182(15) 0.0253(19) 0.0167(13) -0.0001(13) 0.0015(11) -0.0023(14) N1B 0.0184(15) 0.028(2) 0.0189(14) 0.0009(13) 0.0043(11) 0.0003(14) N2B 0.0151(14) 0.028(2) 0.0184(14) -0.0018(13) 0.0027(11) -0.0011(14) C1A 0.0152(16) 0.024(2) 0.0191(16) 0.0026(14) 0.0061(13) -0.0005(15) C2A 0.0183(18) 0.026(2) 0.0220(17) -0.0016(15) 0.0050(14) -0.0032(16) C3A 0.0228(19) 0.026(2) 0.0260(18) -0.0041(16) 0.0079(15) -0.0045(17) C4A 0.0212(18) 0.025(2) 0.0284(18) 0.0013(16) 0.0107(15) 0.0026(16) C5A 0.0177(18) 0.027(2) 0.0260(18) 0.0020(16) 0.0074(14) 0.0029(16) C6A 0.0163(16) 0.024(2) 0.0198(16) -0.0001(15) 0.0060(13) -0.0024(15) C7A 0.0221(19) 0.026(2) 0.0204(17) 0.0025(15) 0.0040(14) 0.0002(17) C8A 0.023(2) 0.038(3) 0.027(2) -0.0054(18) 0.0049(16) -0.0039(19) C9A 0.027(2) 0.036(3) 0.032(2) -0.0044(19) -0.0005(16) -0.008(2) C10A 0.037(2) 0.028(3) 0.0298(19) -0.0052(18) 0.0023(17) -0.009(2) C11A 0.034(2) 0.029(3) 0.0217(17) -0.0026(16) 0.0020(15) 0.0021(19) C12A 0.025(2) 0.026(2) 0.0243(18) 0.0002(16) 0.0044(15) 0.0020(17) C1B 0.0146(16) 0.019(2) 0.0192(15) 0.0001(14) 0.0001(12) 0.0007(14) C2B 0.0172(16) 0.027(2) 0.0202(16) 0.0014(15) 0.0039(13) -0.0011(16) C3B 0.0209(18) 0.030(2) 0.0208(17) -0.0044(16) 0.0041(14) 0.0010(17) C4B 0.024(2) 0.023(2) 0.030(2) -0.0038(16) 0.0051(16) 0.0021(17) C5B 0.026(2) 0.024(2) 0.0257(19) 0.0020(16) 0.0042(15) 0.0024(17) C6B 0.0179(17) 0.023(2) 0.0208(17) -0.0011(14) 0.0049(13) -0.0016(15) C7B 0.0140(17) 0.034(3) 0.0177(17) 0.0005(15) -0.0003(13) 0.0030(16) C8B 0.0249(19) 0.031(3) 0.0248(18) -0.0007(17) 0.0071(15) 0.0003(18) C9B 0.025(2) 0.040(3) 0.0238(18) 0.0024(17) 0.0090(15) -0.0011(19) C10B 0.0197(19) 0.043(3) 0.0203(18) -0.0041(17) 0.0042(14) 0.0081(19) C11B 0.0200(18) 0.033(3) 0.0224(17) -0.0048(16) 0.0018(14) 0.0041(17) C12B 0.0110(16) 0.031(2) 0.0218(17) 0.0011(15) 0.0014(13) 0.0029(15) _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 O1 2.026(3) . ? Te1 C1A 2.065(4) . ? Te1 N2A 2.363(3) . ? Te2 O1 2.007(3) . ? Te2 C1B 2.073(4) . ? Te2 N2B 2.385(3) . ? N1A N2A 1.266(5) . ? N1A C6A 1.392(5) . ? N2A C7A 1.426(5) . ? N1B N2B 1.270(5) . ? N1B C6B 1.401(5) . ? N2B C7B 1.421(5) . ? C1A C2A 1.405(5) . ? C1A C6A 1.414(5) . ? C2A C3A 1.387(6) . ? C2A H2AA 0.9500 . ? C3A C4A 1.406(6) . ? C3A H3AA 0.9500 . ? C4A C5A 1.373(6) . ? C4A H4AA 0.9500 . ? C5A C6A 1.394(6) . ? C5A H5AA 0.9500 . ? C7A C12A 1.380(6) . ? C7A C8A 1.403(6) . ? C8A C9A 1.386(6) . ? C8A H8AA 0.9500 . ? C9A C10A 1.390(7) . ? C9A H9AA 0.9500 . ? C10A C11A 1.384(6) . ? C10A H10A 0.9500 . ? C11A C12A 1.390(6) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C2B 1.402(5) . ? C1B C6B 1.409(5) . ? C2B C3B 1.381(6) . ? C2B H2BA 0.9500 . ? C3B C4B 1.397(6) . ? C3B H3BA 0.9500 . ? C4B C5B 1.386(6) . ? C4B H4BA 0.9500 . ? C5B C6B 1.410(6) . ? C5B H5BA 0.9500 . ? C7B C12B 1.385(6) . ? C7B C8B 1.397(6) . ? C8B C9B 1.391(6) . ? C8B H8BA 0.9500 . ? C9B C10B 1.392(7) . ? C9B H9BA 0.9500 . ? C10B C11B 1.386(7) . ? C10B H10B 0.9500 . ? C11B C12B 1.386(6) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Te1 C1A 92.22(14) . . ? O1 Te1 N2A 163.85(13) . . ? C1A Te1 N2A 71.66(14) . . ? O1 Te2 C1B 92.48(14) . . ? O1 Te2 N2B 163.66(12) . . ? C1B Te2 N2B 71.18(13) . . ? Te2 O1 Te1 122.95(15) . . ? N2A N1A C6A 112.4(3) . . ? N1A N2A C7A 116.1(3) . . ? N1A N2A Te1 117.3(2) . . ? C7A N2A Te1 126.3(3) . . ? N2B N1B C6B 111.8(3) . . ? N1B N2B C7B 116.6(3) . . ? N1B N2B Te2 117.3(2) . . ? C7B N2B Te2 125.9(3) . . ? C2A C1A C6A 118.1(4) . . ? C2A C1A Te1 124.3(3) . . ? C6A C1A Te1 117.5(3) . . ? C3A C2A C1A 119.5(4) . . ? C3A C2A H2AA 120.2 . . ? C1A C2A H2AA 120.2 . . ? C2A C3A C4A 121.6(4) . . ? C2A C3A H3AA 119.2 . . ? C4A C3A H3AA 119.2 . . ? C5A C4A C3A 119.4(4) . . ? C5A C4A H4AA 120.3 . . ? C3A C4A H4AA 120.3 . . ? C4A C5A C6A 119.8(4) . . ? C4A C5A H5AA 120.1 . . ? C6A C5A H5AA 120.1 . . ? N1A C6A C5A 117.4(3) . . ? N1A C6A C1A 121.0(4) . . ? C5A C6A C1A 121.5(4) . . ? C12A C7A C8A 120.9(4) . . ? C12A C7A N2A 118.3(4) . . ? C8A C7A N2A 120.8(4) . . ? C9A C8A C7A 118.2(4) . . ? C9A C8A H8AA 120.9 . . ? C7A C8A H8AA 120.9 . . ? C8A C9A C10A 121.2(4) . . ? C8A C9A H9AA 119.4 . . ? C10A C9A H9AA 119.4 . . ? C11A C10A C9A 119.8(4) . . ? C11A C10A H10A 120.1 . . ? C9A C10A H10A 120.1 . . ? C10A C11A C12A 120.0(4) . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C7A C12A C11A 119.9(4) . . ? C7A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C2B C1B C6B 118.4(4) . . ? C2B C1B Te2 123.6(3) . . ? C6B C1B Te2 118.0(3) . . ? C3B C2B C1B 119.9(4) . . ? C3B C2B H2BA 120.1 . . ? C1B C2B H2BA 120.1 . . ? C2B C3B C4B 121.8(4) . . ? C2B C3B H3BA 119.1 . . ? C4B C3B H3BA 119.1 . . ? C5B C4B C3B 119.5(4) . . ? C5B C4B H4BA 120.2 . . ? C3B C4B H4BA 120.2 . . ? C4B C5B C6B 119.1(4) . . ? C4B C5B H5BA 120.5 . . ? C6B C5B H5BA 120.5 . . ? N1B C6B C1B 121.3(4) . . ? N1B C6B C5B 117.3(4) . . ? C1B C6B C5B 121.3(4) . . ? C12B C7B C8B 120.8(4) . . ? C12B C7B N2B 117.3(4) . . ? C8B C7B N2B 121.9(4) . . ? C9B C8B C7B 118.8(5) . . ? C9B C8B H8BA 120.6 . . ? C7B C8B H8BA 120.6 . . ? C8B C9B C10B 120.4(4) . . ? C8B C9B H9BA 119.8 . . ? C10B C9B H9BA 119.8 . . ? C11B C10B C9B 120.2(4) . . ? C11B C10B H10B 119.9 . . ? C9B C10B H10B 119.9 . . ? C12B C11B C10B 119.9(4) . . ? C12B C11B H11B 120.1 . . ? C10B C11B H11B 120.1 . . ? C7B C12B C11B 120.0(4) . . ? C7B C12B H12B 120.0 . . ? C11B C12B H12B 120.0 . . ? 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 C1B Te2 O1 Te1 -87.30(19) . . . . ? N2B Te2 O1 Te1 -88.4(4) . . . . ? C1A Te1 O1 Te2 -100.12(19) . . . . ? N2A Te1 O1 Te2 -102.9(4) . . . . ? C6A N1A N2A C7A -177.0(3) . . . . ? C6A N1A N2A Te1 -3.1(4) . . . . ? O1 Te1 N2A N1A 4.3(6) . . . . ? C1A Te1 N2A N1A 1.3(3) . . . . ? O1 Te1 N2A C7A 177.5(4) . . . . ? C1A Te1 N2A C7A 174.6(3) . . . . ? C6B N1B N2B C7B 178.5(3) . . . . ? C6B N1B N2B Te2 -5.9(4) . . . . ? O1 Te2 N2B N1B 6.3(6) . . . . ? C1B Te2 N2B N1B 5.1(3) . . . . ? O1 Te2 N2B C7B -178.5(4) . . . . ? C1B Te2 N2B C7B -179.7(3) . . . . ? O1 Te1 C1A C2A 1.0(3) . . . . ? N2A Te1 C1A C2A -179.8(3) . . . . ? O1 Te1 C1A C6A -178.4(3) . . . . ? N2A Te1 C1A C6A 0.8(3) . . . . ? C6A C1A C2A C3A 0.3(6) . . . . ? Te1 C1A C2A C3A -179.0(3) . . . . ? C1A C2A C3A C4A 0.8(6) . . . . ? C2A C3A C4A C5A -1.3(6) . . . . ? C3A C4A C5A C6A 0.6(6) . . . . ? N2A N1A C6A C5A -177.3(3) . . . . ? N2A N1A C6A C1A 4.0(5) . . . . ? C4A C5A C6A N1A -178.2(4) . . . . ? C4A C5A C6A C1A 0.5(6) . . . . ? C2A C1A C6A N1A 177.7(3) . . . . ? Te1 C1A C6A N1A -2.9(5) . . . . ? C2A C1A C6A C5A -1.0(6) . . . . ? Te1 C1A C6A C5A 178.4(3) . . . . ? N1A N2A C7A C12A -150.8(4) . . . . ? Te1 N2A C7A C12A 35.9(5) . . . . ? N1A N2A C7A C8A 29.5(6) . . . . ? Te1 N2A C7A C8A -143.8(3) . . . . ? C12A C7A C8A C9A 0.4(7) . . . . ? N2A C7A C8A C9A -179.8(4) . . . . ? C7A C8A C9A C10A 0.7(7) . . . . ? C8A C9A C10A C11A -0.7(7) . . . . ? C9A C10A C11A C12A -0.5(7) . . . . ? C8A C7A C12A C11A -1.6(6) . . . . ? N2A C7A C12A C11A 178.7(4) . . . . ? C10A C11A C12A C7A 1.7(7) . . . . ? O1 Te2 C1B C2B -4.9(3) . . . . ? N2B Te2 C1B C2B 174.7(3) . . . . ? O1 Te2 C1B C6B 177.4(3) . . . . ? N2B Te2 C1B C6B -2.9(3) . . . . ? C6B C1B C2B C3B 0.3(5) . . . . ? Te2 C1B C2B C3B -177.3(3) . . . . ? C1B C2B C3B C4B -1.0(6) . . . . ? C2B C3B C4B C5B 0.4(6) . . . . ? C3B C4B C5B C6B 0.9(6) . . . . ? N2B N1B C6B C1B 3.4(5) . . . . ? N2B N1B C6B C5B -174.2(3) . . . . ? C2B C1B C6B N1B -176.6(3) . . . . ? Te2 C1B C6B N1B 1.2(5) . . . . ? C2B C1B C6B C5B 0.9(5) . . . . ? Te2 C1B C6B C5B 178.7(3) . . . . ? C4B C5B C6B N1B 176.1(4) . . . . ? C4B C5B C6B C1B -1.5(6) . . . . ? N1B N2B C7B C12B -149.4(4) . . . . ? Te2 N2B C7B C12B 35.4(4) . . . . ? N1B N2B C7B C8B 30.9(5) . . . . ? Te2 N2B C7B C8B -144.3(3) . . . . ? C12B C7B C8B C9B 1.0(6) . . . . ? N2B C7B C8B C9B -179.4(4) . . . . ? C7B C8B C9B C10B -1.3(6) . . . . ? C8B C9B C10B C11B 1.1(6) . . . . ? C9B C10B C11B C12B -0.6(6) . . . . ? C8B C7B C12B C11B -0.5(6) . . . . ? N2B C7B C12B C11B 179.8(3) . . . . ? C10B C11B C12B C7B 0.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.330 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.174 #===END data_azo-teo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N4 O Te, C2 H4 O' _chemical_formula_sum 'C26 H22 N4 O2 Te' _chemical_formula_weight 550.08 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' '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 1 21/n 1' 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 11.3755(2) _cell_length_b 17.8221(3) _cell_length_c 12.1544(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.4164(17) _cell_angle_gamma 90.00 _cell_volume 2430.92(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 18003 _cell_measurement_theta_min 4.8176 _cell_measurement_theta_max 32.4243 _exptl_crystal_description 'irregular chunk' _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75481 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 30734 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.83 _diffrn_reflns_theta_max 32.53 _reflns_number_total 8199 _reflns_number_gt 6613 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0301P)^2^+1.0451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8199 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _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 Te Te 0.616897(9) 0.564187(6) 0.545455(8) 0.02073(4) Uani 1 1 d . . . O O 0.60966(11) 0.47083(6) 0.47549(10) 0.0259(2) Uani 1 1 d . . . O1SA O 0.6102(10) 0.4083(5) 0.2663(8) 0.0655(12) Uani 0.319(7) 1 d P A 1 H1SA H 0.6501 0.4341 0.3170 0.079 Uiso 0.319(7) 1 calc PR A 1 O1SB O 0.6760(5) 0.4163(2) 0.2906(4) 0.0655(12) Uani 0.681(7) 1 d P A 2 H1SB H 0.6630 0.4288 0.3542 0.079 Uiso 0.681(7) 1 calc PR A 2 N1A N 0.59934(15) 0.75313(9) 0.50337(14) 0.0313(3) Uani 1 1 d . . . N2A N 0.63316(13) 0.71364(8) 0.58802(14) 0.0275(3) Uani 1 1 d . . . N1B N 0.83158(13) 0.55715(8) 0.73364(12) 0.0254(3) Uani 1 1 d . . . N2B N 0.89936(15) 0.57032(9) 0.82386(13) 0.0295(3) Uani 1 1 d . . . C1A C 0.56670(15) 0.63129(9) 0.40025(14) 0.0232(3) Uani 1 1 d . . . C2A C 0.53712(16) 0.59591(10) 0.29835(15) 0.0285(4) Uani 1 1 d . . . H2AA H 0.5368 0.5427 0.2945 0.034 Uiso 1 1 calc R . . C3A C 0.50764(19) 0.63813(12) 0.20090(17) 0.0364(4) Uani 1 1 d . . . H3AA H 0.4890 0.6135 0.1309 0.044 Uiso 1 1 calc R . . C4A C 0.5055(2) 0.71557(12) 0.20596(18) 0.0403(5) Uani 1 1 d . . . H4AA H 0.4843 0.7440 0.1396 0.048 Uiso 1 1 calc R . . C5A C 0.53423(19) 0.75163(11) 0.30715(18) 0.0364(4) Uani 1 1 d . . . H5AA H 0.5319 0.8048 0.3105 0.044 Uiso 1 1 calc R . . C6A C 0.56677(16) 0.70998(10) 0.40462(15) 0.0269(3) Uani 1 1 d . . . C7A C 0.67008(16) 0.75333(10) 0.68941(16) 0.0297(4) Uani 1 1 d . . . C8A C 0.69617(18) 0.82990(11) 0.6943(2) 0.0375(4) Uani 1 1 d . . . H8AA H 0.6852 0.8595 0.6284 0.045 Uiso 1 1 calc R . . C9A C 0.73833(19) 0.86189(13) 0.7968(2) 0.0441(5) Uani 1 1 d . . . H9AA H 0.7562 0.9140 0.8011 0.053 Uiso 1 1 calc R . . C10A C 0.75473(18) 0.81959(13) 0.8923(2) 0.0440(5) Uani 1 1 d . . . H10A H 0.7855 0.8423 0.9618 0.053 Uiso 1 1 calc R . . C11A C 0.7267(2) 0.74384(14) 0.88818(19) 0.0453(5) Uani 1 1 d . . . H11A H 0.7362 0.7149 0.9547 0.054 Uiso 1 1 calc R . . C12A C 0.68446(19) 0.71044(12) 0.78570(18) 0.0378(4) Uani 1 1 d . . . H12A H 0.6656 0.6585 0.7819 0.045 Uiso 1 1 calc R . . C1B C 0.80304(15) 0.58269(9) 0.53815(14) 0.0231(3) Uani 1 1 d . . . C2B C 0.84654(17) 0.60072(11) 0.44146(15) 0.0302(4) Uani 1 1 d . . . H2BA H 0.7930 0.6086 0.3738 0.036 Uiso 1 1 calc R . . C3B C 0.96867(18) 0.60733(13) 0.44352(17) 0.0362(4) Uani 1 1 d . . . H3BA H 0.9981 0.6206 0.3774 0.043 Uiso 1 1 calc R . . C4B C 1.04785(17) 0.59471(12) 0.54101(17) 0.0347(4) Uani 1 1 d . . . H4BA H 1.1312 0.5975 0.5407 0.042 Uiso 1 1 calc R . . C5B C 1.00613(16) 0.57814(10) 0.63852(16) 0.0294(4) Uani 1 1 d . . . H5BA H 1.0602 0.5704 0.7058 0.035 Uiso 1 1 calc R . . C6B C 0.88309(15) 0.57287(9) 0.63716(14) 0.0231(3) Uani 1 1 d . . . C7B C 0.84871(18) 0.55572(10) 0.92131(16) 0.0306(4) Uani 1 1 d . . . C8B C 0.7410(2) 0.52015(13) 0.92307(18) 0.0416(5) Uani 1 1 d . . . H8BA H 0.6935 0.5040 0.8556 0.050 Uiso 1 1 calc R . . C9B C 0.7032(2) 0.50843(16) 1.0244(2) 0.0542(6) Uani 1 1 d . . . H9BA H 0.6292 0.4841 1.0262 0.065 Uiso 1 1 calc R . . C10B C 0.7720(3) 0.53181(16) 1.12316(19) 0.0541(6) Uani 1 1 d . . . H10B H 0.7462 0.5226 1.1924 0.065 Uiso 1 1 calc R . . C11B C 0.8776(3) 0.56831(16) 1.12027(19) 0.0560(7) Uani 1 1 d . . . H11B H 0.9239 0.5856 1.1877 0.067 Uiso 1 1 calc R . . C12B C 0.9173(2) 0.58016(14) 1.01987(18) 0.0440(5) Uani 1 1 d . . . H12B H 0.9910 0.6049 1.0185 0.053 Uiso 1 1 calc R . . C1S C 0.6491(3) 0.3395(2) 0.2727(3) 0.0801(10) Uani 1 1 d . . . C2S C 0.6382(4) 0.3146(2) 0.1560(4) 0.1016(14) Uani 1 1 d . A . H2SA H 0.6478 0.2600 0.1538 0.152 Uiso 1 1 calc R . . H2SB H 0.7001 0.3388 0.1209 0.152 Uiso 1 1 calc R . . H2SC H 0.5595 0.3284 0.1155 0.152 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 Te 0.02322(5) 0.01862(5) 0.01953(5) -0.00069(4) 0.00101(4) -0.00296(4) O 0.0306(6) 0.0177(6) 0.0283(6) -0.0029(4) 0.0011(5) -0.0018(5) O1SA 0.096(3) 0.0483(14) 0.065(2) -0.0156(13) 0.054(3) -0.017(2) O1SB 0.096(3) 0.0483(14) 0.065(2) -0.0156(13) 0.054(3) -0.017(2) N1A 0.0336(8) 0.0219(7) 0.0375(8) -0.0018(6) 0.0036(7) 0.0005(6) N2A 0.0272(7) 0.0214(7) 0.0333(8) -0.0044(6) 0.0033(6) -0.0019(5) N1B 0.0275(7) 0.0255(7) 0.0224(7) 0.0007(5) 0.0014(5) -0.0021(6) N2B 0.0317(8) 0.0334(8) 0.0223(7) 0.0000(6) 0.0015(6) -0.0042(6) C1A 0.0227(8) 0.0221(8) 0.0242(8) 0.0021(6) 0.0019(6) -0.0003(6) C2A 0.0312(9) 0.0264(9) 0.0262(8) 0.0015(7) -0.0004(7) -0.0005(7) C3A 0.0400(11) 0.0416(11) 0.0260(9) 0.0035(8) 0.0005(8) -0.0010(9) C4A 0.0438(12) 0.0414(12) 0.0339(10) 0.0152(8) 0.0014(9) 0.0035(9) C5A 0.0417(11) 0.0260(9) 0.0411(11) 0.0090(8) 0.0053(9) 0.0024(8) C6A 0.0270(8) 0.0233(8) 0.0302(9) 0.0027(6) 0.0043(7) 0.0004(6) C7A 0.0239(8) 0.0256(9) 0.0383(10) -0.0107(7) 0.0015(7) -0.0001(6) C8A 0.0320(10) 0.0273(9) 0.0522(12) -0.0106(8) 0.0040(9) -0.0035(7) C9A 0.0347(10) 0.0331(11) 0.0639(15) -0.0244(10) 0.0057(10) -0.0030(8) C10A 0.0308(10) 0.0512(13) 0.0487(13) -0.0282(11) 0.0025(9) 0.0040(9) C11A 0.0469(13) 0.0514(13) 0.0357(11) -0.0138(10) 0.0015(9) 0.0057(10) C12A 0.0428(11) 0.0313(10) 0.0379(11) -0.0099(8) 0.0023(9) 0.0010(8) C1B 0.0232(7) 0.0224(7) 0.0233(8) -0.0018(6) 0.0028(6) -0.0014(6) C2B 0.0289(9) 0.0392(10) 0.0221(8) -0.0013(7) 0.0029(7) -0.0024(8) C3B 0.0342(10) 0.0504(12) 0.0261(9) -0.0012(8) 0.0108(8) -0.0071(9) C4B 0.0255(9) 0.0435(11) 0.0357(10) -0.0047(8) 0.0068(8) -0.0063(8) C5B 0.0257(8) 0.0330(10) 0.0280(9) -0.0039(7) 0.0004(7) -0.0025(7) C6B 0.0245(8) 0.0227(8) 0.0217(7) -0.0020(6) 0.0020(6) -0.0028(6) C7B 0.0368(9) 0.0301(9) 0.0245(8) 0.0002(7) 0.0035(7) -0.0001(7) C8B 0.0446(12) 0.0491(13) 0.0321(10) -0.0023(9) 0.0090(9) -0.0110(10) C9B 0.0547(15) 0.0685(17) 0.0444(13) 0.0017(12) 0.0223(11) -0.0133(13) C10B 0.0692(17) 0.0679(17) 0.0287(11) 0.0055(11) 0.0185(11) 0.0055(14) C11B 0.0651(17) 0.0763(19) 0.0244(10) -0.0023(11) 0.0008(10) 0.0011(14) C12B 0.0445(12) 0.0589(14) 0.0265(10) 0.0003(9) -0.0007(9) -0.0070(10) C1S 0.095(3) 0.070(2) 0.077(2) -0.0305(17) 0.0210(19) -0.0239(18) C2S 0.098(3) 0.095(3) 0.114(3) -0.050(3) 0.027(2) -0.009(2) _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 Te O 1.8642(12) . ? Te C1A 2.1311(16) . ? Te C1B 2.1591(17) . ? Te O 2.6233(12) 3_666 ? O1SA C1S 1.302(10) . ? O1SA H1SA 0.8400 . ? O1SB C1S 1.412(5) . ? O1SB H1SB 0.8400 . ? N1A N2A 1.254(2) . ? N1A C6A 1.423(2) . ? N2A C7A 1.423(2) . ? N1B N2B 1.255(2) . ? N1B C6B 1.422(2) . ? N2B C7B 1.423(2) . ? C1A C2A 1.381(2) . ? C1A C6A 1.403(2) . ? C2A C3A 1.397(3) . ? C2A H2AA 0.9500 . ? C3A C4A 1.382(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.379(3) . ? C4A H4AA 0.9500 . ? C5A C6A 1.396(3) . ? C5A H5AA 0.9500 . ? C7A C12A 1.385(3) . ? C7A C8A 1.396(3) . ? C8A C9A 1.383(3) . ? C8A H8AA 0.9500 . ? C9A C10A 1.371(4) . ? C9A H9AA 0.9500 . ? C10A C11A 1.386(3) . ? C10A H10A 0.9500 . ? C11A C12A 1.393(3) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C2B 1.385(2) . ? C1B C6B 1.396(2) . ? C2B C3B 1.390(3) . ? C2B H2BA 0.9500 . ? C3B C4B 1.384(3) . ? C3B H3BA 0.9500 . ? C4B C5B 1.379(3) . ? C4B H4BA 0.9500 . ? C5B C6B 1.400(2) . ? C5B H5BA 0.9500 . ? C7B C8B 1.383(3) . ? C7B C12B 1.388(3) . ? C8B C9B 1.385(3) . ? C8B H8BA 0.9500 . ? C9B C10B 1.386(4) . ? C9B H9BA 0.9500 . ? C10B C11B 1.371(4) . ? C10B H10B 0.9500 . ? C11B C12B 1.385(3) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C1S C2S 1.472(5) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Te C1A 97.89(6) . . ? O Te C1B 95.05(6) . . ? C1A Te C1B 90.69(6) . . ? O Te O 76.94(5) . 3_666 ? C1A Te O 85.83(5) . 3_666 ? C1B Te O 170.70(5) . 3_666 ? C1S O1SA H1SA 109.5 . . ? C1S O1SB H1SB 109.5 . . ? N2A N1A C6A 113.05(15) . . ? N1A N2A C7A 116.04(15) . . ? N2B N1B C6B 113.99(15) . . ? N1B N2B C7B 114.73(16) . . ? C2A C1A C6A 119.25(16) . . ? C2A C1A Te 118.64(12) . . ? C6A C1A Te 122.08(13) . . ? C1A C2A C3A 120.25(18) . . ? C1A C2A H2AA 119.9 . . ? C3A C2A H2AA 119.9 . . ? C4A C3A C2A 120.25(19) . . ? C4A C3A H3AA 119.9 . . ? C2A C3A H3AA 119.9 . . ? C5A C4A C3A 120.13(18) . . ? C5A C4A H4AA 119.9 . . ? C3A C4A H4AA 119.9 . . ? C4A C5A C6A 120.04(18) . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C1A 120.05(17) . . ? C5A C6A N1A 115.15(16) . . ? C1A C6A N1A 124.79(16) . . ? C12A C7A C8A 120.59(18) . . ? C12A C7A N2A 115.76(16) . . ? C8A C7A N2A 123.58(19) . . ? C9A C8A C7A 118.8(2) . . ? C9A C8A H8AA 120.6 . . ? C7A C8A H8AA 120.6 . . ? C10A C9A C8A 121.0(2) . . ? C10A C9A H9AA 119.5 . . ? C8A C9A H9AA 119.5 . . ? C9A C10A C11A 120.4(2) . . ? C9A C10A H10A 119.8 . . ? C11A C10A H10A 119.8 . . ? C10A C11A C12A 119.5(2) . . ? C10A C11A H11A 120.3 . . ? C12A C11A H11A 120.3 . . ? C7A C12A C11A 119.7(2) . . ? C7A C12A H12A 120.1 . . ? C11A C12A H12A 120.1 . . ? C2B C1B C6B 119.15(16) . . ? C2B C1B Te 123.99(13) . . ? C6B C1B Te 116.82(12) . . ? C1B C2B C3B 119.92(18) . . ? C1B C2B H2BA 120.0 . . ? C3B C2B H2BA 120.0 . . ? C4B C3B C2B 120.66(18) . . ? C4B C3B H3BA 119.7 . . ? C2B C3B H3BA 119.7 . . ? C5B C4B C3B 120.22(18) . . ? C5B C4B H4BA 119.9 . . ? C3B C4B H4BA 119.9 . . ? C4B C5B C6B 119.22(17) . . ? C4B C5B H5BA 120.4 . . ? C6B C5B H5BA 120.4 . . ? C1B C6B C5B 120.76(16) . . ? C1B C6B N1B 115.90(15) . . ? C5B C6B N1B 123.34(15) . . ? C8B C7B C12B 120.3(2) . . ? C8B C7B N2B 125.25(18) . . ? C12B C7B N2B 114.46(19) . . ? C7B C8B C9B 119.2(2) . . ? C7B C8B H8BA 120.4 . . ? C9B C8B H8BA 120.4 . . ? C8B C9B C10B 120.7(2) . . ? C8B C9B H9BA 119.6 . . ? C10B C9B H9BA 119.6 . . ? C11B C10B C9B 119.6(2) . . ? C11B C10B H10B 120.2 . . ? C9B C10B H10B 120.2 . . ? C10B C11B C12B 120.5(2) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C11B C12B C7B 119.6(2) . . ? C11B C12B H12B 120.2 . . ? C7B C12B H12B 120.2 . . ? O1SA C1S O1SB 32.7(4) . . ? O1SA C1S C2S 104.6(5) . . ? O1SB C1S C2S 115.0(4) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? 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 C6A N1A N2A C7A 178.43(15) . . . . ? C6B N1B N2B C7B 179.30(14) . . . . ? O Te C1A C2A 2.92(15) . . . . ? C1B Te C1A C2A 98.11(15) . . . . ? O Te C1A C2A -73.26(14) 3_666 . . . ? O Te C1A C6A -174.86(14) . . . . ? C1B Te C1A C6A -79.67(15) . . . . ? O Te C1A C6A 108.96(14) 3_666 . . . ? C6A C1A C2A C3A 0.0(3) . . . . ? Te C1A C2A C3A -177.85(15) . . . . ? C1A C2A C3A C4A -1.3(3) . . . . ? C2A C3A C4A C5A 0.9(3) . . . . ? C3A C4A C5A C6A 0.7(3) . . . . ? C4A C5A C6A C1A -2.0(3) . . . . ? C4A C5A C6A N1A 177.46(19) . . . . ? C2A C1A C6A C5A 1.7(3) . . . . ? Te C1A C6A C5A 179.42(14) . . . . ? C2A C1A C6A N1A -177.76(17) . . . . ? Te C1A C6A N1A 0.0(3) . . . . ? N2A N1A C6A C5A -176.90(17) . . . . ? N2A N1A C6A C1A 2.5(3) . . . . ? N1A N2A C7A C12A 167.59(18) . . . . ? N1A N2A C7A C8A -15.2(3) . . . . ? C12A C7A C8A C9A 1.0(3) . . . . ? N2A C7A C8A C9A -176.06(18) . . . . ? C7A C8A C9A C10A 0.1(3) . . . . ? C8A C9A C10A C11A -1.4(3) . . . . ? C9A C10A C11A C12A 1.6(3) . . . . ? C8A C7A C12A C11A -0.8(3) . . . . ? N2A C7A C12A C11A 176.48(19) . . . . ? C10A C11A C12A C7A -0.5(3) . . . . ? O Te C1B C2B 73.55(16) . . . . ? C1A Te C1B C2B -24.43(16) . . . . ? O Te C1B C2B 43.4(4) 3_666 . . . ? O Te C1B C6B -104.03(13) . . . . ? C1A Te C1B C6B 157.99(13) . . . . ? O Te C1B C6B -134.2(3) 3_666 . . . ? C6B C1B C2B C3B 1.3(3) . . . . ? Te C1B C2B C3B -176.26(15) . . . . ? C1B C2B C3B C4B 1.2(3) . . . . ? C2B C3B C4B C5B -2.4(3) . . . . ? C3B C4B C5B C6B 1.2(3) . . . . ? C2B C1B C6B C5B -2.5(3) . . . . ? Te C1B C6B C5B 175.19(13) . . . . ? C2B C1B C6B N1B 177.80(16) . . . . ? Te C1B C6B N1B -4.50(19) . . . . ? C4B C5B C6B C1B 1.3(3) . . . . ? C4B C5B C6B N1B -179.05(17) . . . . ? N2B N1B C6B C1B -160.09(15) . . . . ? N2B N1B C6B C5B 20.2(2) . . . . ? N1B N2B C7B C8B 8.9(3) . . . . ? N1B N2B C7B C12B -171.37(18) . . . . ? C12B C7B C8B C9B -0.8(3) . . . . ? N2B C7B C8B C9B 178.9(2) . . . . ? C7B C8B C9B C10B -0.1(4) . . . . ? C8B C9B C10B C11B 1.3(4) . . . . ? C9B C10B C11B C12B -1.7(4) . . . . ? C10B C11B C12B C7B 0.9(4) . . . . ? C8B C7B C12B C11B 0.4(4) . . . . ? N2B C7B C12B C11B -179.3(2) . . . . ? 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 O1SA H1SA O 0.84 2.16 2.778(9) 130.8 . O1SB H1SB O 0.84 1.84 2.668(3) 167.0 . _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.985 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.073 #===END data_azo-te2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H42 N8 O2 Te2' _chemical_formula_sum 'C54 H42 N8 O2 Te2' _chemical_formula_weight 1090.16 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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7072(11) _cell_length_b 11.0754(12) _cell_length_c 11.2912(9) _cell_angle_alpha 74.141(8) _cell_angle_beta 71.057(8) _cell_angle_gamma 68.848(10) _cell_volume 1162.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5171 _cell_measurement_theta_min 4.9933 _cell_measurement_theta_max 32.7771 _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89723 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby (Gemini Mo) ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14310 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.01 _diffrn_reflns_theta_max 32.84 _reflns_number_total 7678 _reflns_number_gt 5086 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _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^)+(0.0677P)^2^+17.7659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7678 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.2331 _refine_ls_wR_factor_gt 0.2095 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Te Te 0.55270(6) 0.86061(6) 0.60494(5) 0.01531(15) Uani 1 1 d . . . O1 O 0.6128(6) 1.0035(6) 0.4032(5) 0.0222(12) Uani 1 1 d . . . N1A N 0.5710(7) 0.8048(7) 0.8829(6) 0.0187(13) Uani 1 1 d . . . N2A N 0.5836(8) 0.8072(8) 0.9895(7) 0.0248(15) Uani 1 1 d . . . N1B N 0.7440(7) 0.5523(7) 0.5268(6) 0.0206(14) Uani 1 1 d . . . N2B N 0.7476(7) 0.6092(7) 0.6069(6) 0.0185(13) Uani 1 1 d . . . C1A C 0.4499(8) 0.7490(8) 0.7726(7) 0.0177(15) Uani 1 1 d . . . C2A C 0.3492(9) 0.6980(9) 0.7724(8) 0.0212(17) Uani 1 1 d . . . H2AA H 0.3267 0.7074 0.6950 0.025 Uiso 1 1 calc R . . C3A C 0.2812(10) 0.6335(9) 0.8839(9) 0.0275(19) Uani 1 1 d . . . H3AA H 0.2128 0.5987 0.8822 0.033 Uiso 1 1 calc R . . C4A C 0.3122(10) 0.6190(9) 0.9989(8) 0.0255(18) Uani 1 1 d . . . H4AA H 0.2670 0.5724 1.0747 0.031 Uiso 1 1 calc R . . C5A C 0.4086(10) 0.6727(9) 1.0015(8) 0.0263(19) Uani 1 1 d . . . H5AA H 0.4286 0.6652 1.0797 0.032 Uiso 1 1 calc R . . C6A C 0.4772(8) 0.7385(8) 0.8889(7) 0.0168(15) Uani 1 1 d . . . C7A C 0.6718(9) 0.8823(9) 0.9807(8) 0.0227(17) Uani 1 1 d . . . C8A C 0.6800(10) 0.8929(9) 1.0989(8) 0.0254(18) Uani 1 1 d . . . H8AA H 0.6316 0.8502 1.1755 0.031 Uiso 1 1 calc R . . C9A C 0.7600(10) 0.9669(10) 1.1028(9) 0.030(2) Uani 1 1 d . . . H9AA H 0.7664 0.9748 1.1821 0.036 Uiso 1 1 calc R . . C10A C 0.8299(10) 1.0285(10) 0.9898(10) 0.032(2) Uani 1 1 d . . . H10A H 0.8825 1.0805 0.9922 0.038 Uiso 1 1 calc R . . C11A C 0.8237(10) 1.0149(11) 0.8732(10) 0.031(2) Uani 1 1 d . . . H11A H 0.8744 1.0551 0.7964 0.038 Uiso 1 1 calc R . . C12A C 0.7433(10) 0.9425(10) 0.8691(9) 0.029(2) Uani 1 1 d . . . H12A H 0.7376 0.9344 0.7896 0.034 Uiso 1 1 calc R . . C1B C 0.5418(9) 0.7454(8) 0.4868(7) 0.0180(15) Uani 1 1 d . . . C2B C 0.4348(8) 0.7994(8) 0.4244(7) 0.0175(15) Uani 1 1 d . . . H2BA H 0.3707 0.8832 0.4375 0.021 Uiso 1 1 calc R . . C3B C 0.4210(9) 0.7333(9) 0.3444(8) 0.0218(17) Uani 1 1 d . . . H3BA H 0.3468 0.7709 0.3043 0.026 Uiso 1 1 calc R . . C4B C 0.5164(10) 0.6106(9) 0.3219(8) 0.0259(19) Uani 1 1 d . . . H4BA H 0.5077 0.5649 0.2665 0.031 Uiso 1 1 calc R . . C5B C 0.6234(10) 0.5573(9) 0.3821(8) 0.0257(18) Uani 1 1 d . . . H5BA H 0.6897 0.4752 0.3665 0.031 Uiso 1 1 calc R . . C6B C 0.6345(8) 0.6233(8) 0.4653(7) 0.0179(15) Uani 1 1 d . . . C7B C 0.8541(9) 0.5375(9) 0.6727(8) 0.0209(16) Uani 1 1 d . . . C8B C 0.9312(10) 0.4050(10) 0.6662(9) 0.029(2) Uani 1 1 d . . . H8BA H 0.9173 0.3584 0.6147 0.035 Uiso 1 1 calc R . . C9B C 1.0287(11) 0.3448(10) 0.7379(10) 0.034(2) Uani 1 1 d . . . H9BA H 1.0830 0.2560 0.7341 0.041 Uiso 1 1 calc R . . C10B C 1.0479(9) 0.4108(11) 0.8139(9) 0.032(2) Uani 1 1 d . . . H10B H 1.1143 0.3670 0.8626 0.039 Uiso 1 1 calc R . . C11B C 0.9713(10) 0.5407(11) 0.8201(9) 0.031(2) Uani 1 1 d . . . H11B H 0.9858 0.5862 0.8724 0.037 Uiso 1 1 calc R . . C12B C 0.8732(9) 0.6048(9) 0.7497(8) 0.0249(18) Uani 1 1 d . . . H12B H 0.8196 0.6937 0.7542 0.030 Uiso 1 1 calc R . . C1S C 0.9597(12) 1.1222(11) 0.4260(12) 0.043(3) Uani 1 1 d . . . H1SA H 0.9315 1.2066 0.3760 0.051 Uiso 1 1 calc R . . C2S C 1.0526(11) 1.0975(12) 0.4970(11) 0.039(3) Uani 1 1 d . . . H2SA H 1.0897 1.1646 0.4942 0.046 Uiso 1 1 calc R . . C3S C 0.9079(11) 1.0244(13) 0.4279(11) 0.043(3) Uani 1 1 d . . . H3SA H 0.8454 1.0404 0.3779 0.051 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 Te 0.0196(3) 0.0119(2) 0.0154(2) 0.00073(16) -0.00995(17) -0.00324(18) O1 0.030(3) 0.018(3) 0.016(3) 0.001(2) -0.006(2) -0.006(3) N1A 0.022(3) 0.018(3) 0.015(3) 0.002(2) -0.009(3) -0.004(3) N2A 0.030(4) 0.021(4) 0.022(3) -0.001(3) -0.012(3) -0.005(3) N1B 0.018(3) 0.019(4) 0.020(3) -0.001(3) -0.008(3) 0.001(3) N2B 0.019(3) 0.019(4) 0.015(3) -0.002(3) -0.007(3) -0.002(3) C1A 0.017(4) 0.014(4) 0.018(3) -0.002(3) -0.003(3) -0.001(3) C2A 0.028(4) 0.022(4) 0.018(4) -0.003(3) -0.005(3) -0.013(4) C3A 0.025(5) 0.023(5) 0.034(5) 0.002(4) -0.008(4) -0.011(4) C4A 0.030(5) 0.017(4) 0.024(4) 0.006(3) -0.007(4) -0.006(4) C5A 0.027(5) 0.026(5) 0.020(4) 0.001(3) -0.007(3) -0.003(4) C6A 0.015(4) 0.014(4) 0.018(3) 0.000(3) -0.008(3) 0.001(3) C7A 0.020(4) 0.023(4) 0.024(4) -0.007(3) -0.013(3) 0.003(3) C8A 0.027(5) 0.027(5) 0.022(4) -0.004(3) -0.011(3) -0.003(4) C9A 0.031(5) 0.029(5) 0.033(5) -0.011(4) -0.020(4) 0.003(4) C10A 0.027(5) 0.028(5) 0.045(6) -0.011(4) -0.017(4) -0.004(4) C11A 0.027(5) 0.036(6) 0.033(5) -0.006(4) -0.008(4) -0.012(4) C12A 0.035(5) 0.031(5) 0.024(4) -0.002(4) -0.012(4) -0.012(4) C1B 0.028(4) 0.019(4) 0.012(3) -0.001(3) -0.005(3) -0.015(3) C2B 0.016(4) 0.008(3) 0.021(4) 0.002(3) -0.008(3) 0.004(3) C3B 0.029(4) 0.019(4) 0.021(4) 0.007(3) -0.017(3) -0.011(4) C4B 0.042(5) 0.022(4) 0.019(4) 0.001(3) -0.015(4) -0.012(4) C5B 0.033(5) 0.023(5) 0.023(4) -0.005(3) -0.013(4) -0.005(4) C6B 0.020(4) 0.013(4) 0.017(3) 0.003(3) -0.011(3) 0.000(3) C7B 0.021(4) 0.025(4) 0.018(3) 0.003(3) -0.010(3) -0.009(4) C8B 0.034(5) 0.029(5) 0.023(4) -0.001(4) -0.014(4) -0.004(4) C9B 0.031(5) 0.023(5) 0.034(5) 0.001(4) -0.013(4) 0.009(4) C10B 0.017(4) 0.038(6) 0.032(5) -0.002(4) -0.014(4) 0.009(4) C11B 0.026(5) 0.042(6) 0.030(5) -0.003(4) -0.013(4) -0.012(4) C12B 0.022(4) 0.023(4) 0.027(4) -0.002(3) -0.010(3) -0.001(4) C1S 0.039(6) 0.029(6) 0.053(7) -0.001(5) -0.010(5) -0.008(5) C2S 0.028(5) 0.040(6) 0.051(6) -0.016(5) 0.000(5) -0.016(5) C3S 0.026(5) 0.059(8) 0.043(6) -0.010(6) -0.007(5) -0.013(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 Te O1 1.876(6) 2_676 ? Te C1B 2.136(7) . ? Te C1A 2.162(8) . ? Te O1 2.434(6) . ? Te N2B 2.813(7) . ? Te N1A 3.086(6) . ? O1 Te 1.876(6) 2_676 ? N1A N2A 1.262(9) . ? N1A C6A 1.420(10) . ? N2A C7A 1.434(12) . ? N1B N2B 1.252(10) . ? N1B C6B 1.428(10) . ? N2B C7B 1.434(10) . ? C1A C2A 1.386(11) . ? C1A C6A 1.402(11) . ? C2A C3A 1.383(12) . ? C2A H2AA 0.9500 . ? C3A C4A 1.396(13) . ? C3A H3AA 0.9500 . ? C4A C5A 1.376(13) . ? C4A H4AA 0.9500 . ? C5A C6A 1.400(12) . ? C5A H5AA 0.9500 . ? C7A C12A 1.378(13) . ? C7A C8A 1.403(11) . ? C8A C9A 1.399(14) . ? C8A H8AA 0.9500 . ? C9A C10A 1.388(15) . ? C9A H9AA 0.9500 . ? C10A C11A 1.390(14) . ? C10A H10A 0.9500 . ? C11A C12A 1.389(13) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C6B 1.388(12) . ? C1B C2B 1.401(11) . ? C2B C3B 1.379(12) . ? C2B H2BA 0.9500 . ? C3B C4B 1.404(13) . ? C3B H3BA 0.9500 . ? C4B C5B 1.386(13) . ? C4B H4BA 0.9500 . ? C5B C6B 1.394(12) . ? C5B H5BA 0.9500 . ? C7B C12B 1.391(12) . ? C7B C8B 1.409(13) . ? C8B C9B 1.393(13) . ? C8B H8BA 0.9500 . ? C9B C10B 1.371(15) . ? C9B H9BA 0.9500 . ? C10B C11B 1.384(15) . ? C10B H10B 0.9500 . ? C11B C12B 1.392(13) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C1S C3S 1.377(16) . ? C1S C2S 1.382(17) . ? C1S H1SA 0.9500 . ? C2S C3S 1.384(17) 2_776 ? C2S H2SA 0.9500 . ? C3S C2S 1.384(17) 2_776 ? C3S H3SA 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Te C1B 98.4(3) 2_676 . ? O1 Te C1A 91.9(3) 2_676 . ? C1B Te C1A 90.8(3) . . ? O1 Te O1 76.0(3) 2_676 . ? C1B Te O1 83.3(2) . . ? C1A Te O1 165.6(3) . . ? O1 Te N2B 160.5(2) 2_676 . ? C1B Te N2B 65.0(3) . . ? C1A Te N2B 78.7(3) . . ? O1 Te N2B 110.2(2) . . ? O1 Te N1A 105.7(2) 2_676 . ? C1B Te N1A 133.8(2) . . ? C1A Te N1A 50.3(3) . . ? O1 Te N1A 140.33(19) . . ? N2B Te N1A 81.57(19) . . ? Te O1 Te 104.0(3) 2_676 . ? N2A N1A C6A 114.7(7) . . ? N2A N1A Te 166.9(6) . . ? C6A N1A Te 76.5(4) . . ? N1A N2A C7A 113.3(7) . . ? N2B N1B C6B 113.4(7) . . ? N1B N2B C7B 114.3(7) . . ? N1B N2B Te 111.5(5) . . ? C7B N2B Te 134.1(5) . . ? C2A C1A C6A 118.5(7) . . ? C2A C1A Te 123.0(6) . . ? C6A C1A Te 118.1(6) . . ? C3A C2A C1A 120.7(8) . . ? C3A C2A H2AA 119.7 . . ? C1A C2A H2AA 119.7 . . ? C2A C3A C4A 120.7(8) . . ? C2A C3A H3AA 119.7 . . ? C4A C3A H3AA 119.7 . . ? C5A C4A C3A 119.4(8) . . ? C5A C4A H4AA 120.3 . . ? C3A C4A H4AA 120.3 . . ? C4A C5A C6A 120.0(8) . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C1A 120.6(8) . . ? C5A C6A N1A 124.2(7) . . ? C1A C6A N1A 115.1(7) . . ? C12A C7A C8A 120.6(8) . . ? C12A C7A N2A 125.3(8) . . ? C8A C7A N2A 114.1(8) . . ? C9A C8A C7A 119.4(9) . . ? C9A C8A H8AA 120.3 . . ? C7A C8A H8AA 120.3 . . ? C10A C9A C8A 119.4(8) . . ? C10A C9A H9AA 120.3 . . ? C8A C9A H9AA 120.3 . . ? C9A C10A C11A 120.7(9) . . ? C9A C10A H10A 119.7 . . ? C11A C10A H10A 119.7 . . ? C12A C11A C10A 119.9(9) . . ? C12A C11A H11A 120.0 . . ? C10A C11A H11A 120.0 . . ? C7A C12A C11A 119.9(9) . . ? C7A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C6B C1B C2B 118.2(7) . . ? C6B C1B Te 124.7(6) . . ? C2B C1B Te 117.1(6) . . ? C3B C2B C1B 121.2(8) . . ? C3B C2B H2BA 119.4 . . ? C1B C2B H2BA 119.4 . . ? C2B C3B C4B 120.3(8) . . ? C2B C3B H3BA 119.9 . . ? C4B C3B H3BA 119.9 . . ? C5B C4B C3B 118.8(8) . . ? C5B C4B H4BA 120.6 . . ? C3B C4B H4BA 120.6 . . ? C4B C5B C6B 120.5(9) . . ? C4B C5B H5BA 119.7 . . ? C6B C5B H5BA 119.7 . . ? C1B C6B C5B 121.0(8) . . ? C1B C6B N1B 124.8(7) . . ? C5B C6B N1B 114.1(7) . . ? C12B C7B C8B 121.0(8) . . ? C12B C7B N2B 115.8(8) . . ? C8B C7B N2B 123.0(8) . . ? C9B C8B C7B 117.6(9) . . ? C9B C8B H8BA 121.2 . . ? C7B C8B H8BA 121.2 . . ? C10B C9B C8B 121.6(9) . . ? C10B C9B H9BA 119.2 . . ? C8B C9B H9BA 119.2 . . ? C9B C10B C11B 120.4(9) . . ? C9B C10B H10B 119.8 . . ? C11B C10B H10B 119.8 . . ? C10B C11B C12B 119.9(9) . . ? C10B C11B H11B 120.1 . . ? C12B C11B H11B 120.1 . . ? C7B C12B C11B 119.4(9) . . ? C7B C12B H12B 120.3 . . ? C11B C12B H12B 120.3 . . ? C3S C1S C2S 119.9(11) . . ? C3S C1S H1SA 120.0 . . ? C2S C1S H1SA 120.0 . . ? C1S C2S C3S 120.5(10) . 2_776 ? C1S C2S H2SA 119.8 . . ? C3S C2S H2SA 119.8 2_776 . ? C1S C3S C2S 119.6(11) . 2_776 ? C1S C3S H3SA 120.2 . . ? C2S C3S H3SA 120.2 2_776 . ? 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 Te O1 Te 0.0 2_676 . . 2_676 ? C1B Te O1 Te 100.4(3) . . . 2_676 ? C1A Te O1 Te 34.1(11) . . . 2_676 ? N2B Te O1 Te 160.6(2) . . . 2_676 ? N1A Te O1 Te -97.9(3) . . . 2_676 ? O1 Te N1A N2A -71(3) 2_676 . . . ? C1B Te N1A N2A 170(2) . . . . ? C1A Te N1A N2A -150(3) . . . . ? O1 Te N1A N2A 16(3) . . . . ? N2B Te N1A N2A 128(3) . . . . ? O1 Te N1A C6A 79.3(5) 2_676 . . . ? C1B Te N1A C6A -39.3(6) . . . . ? C1A Te N1A C6A 0.2(5) . . . . ? O1 Te N1A C6A 166.3(4) . . . . ? N2B Te N1A C6A -82.1(4) . . . . ? C6A N1A N2A C7A -176.1(7) . . . . ? Te N1A N2A C7A -28(3) . . . . ? C6B N1B N2B C7B 178.1(7) . . . . ? C6B N1B N2B Te -5.7(8) . . . . ? O1 Te N2B N1B 39.8(9) 2_676 . . . ? C1B Te N2B N1B 6.3(5) . . . . ? C1A Te N2B N1B 102.5(6) . . . . ? O1 Te N2B N1B -65.7(6) . . . . ? N1A Te N2B N1B 153.5(6) . . . . ? O1 Te N2B C7B -145.0(7) 2_676 . . . ? C1B Te N2B C7B -178.5(8) . . . . ? C1A Te N2B C7B -82.3(7) . . . . ? O1 Te N2B C7B 109.4(7) . . . . ? N1A Te N2B C7B -31.3(7) . . . . ? O1 Te C1A C2A 64.7(7) 2_676 . . . ? C1B Te C1A C2A -33.7(7) . . . . ? O1 Te C1A C2A 31.8(15) . . . . ? N2B Te C1A C2A -98.0(7) . . . . ? N1A Te C1A C2A 173.7(8) . . . . ? O1 Te C1A C6A -109.1(6) 2_676 . . . ? C1B Te C1A C6A 152.4(7) . . . . ? O1 Te C1A C6A -142.1(9) . . . . ? N2B Te C1A C6A 88.1(6) . . . . ? N1A Te C1A C6A -0.2(5) . . . . ? C6A C1A C2A C3A -2.6(13) . . . . ? Te C1A C2A C3A -176.4(7) . . . . ? C1A C2A C3A C4A 0.3(14) . . . . ? C2A C3A C4A C5A 1.8(14) . . . . ? C3A C4A C5A C6A -1.6(14) . . . . ? C4A C5A C6A C1A -0.7(13) . . . . ? C4A C5A C6A N1A 175.5(8) . . . . ? C2A C1A C6A C5A 2.8(12) . . . . ? Te C1A C6A C5A 176.9(6) . . . . ? C2A C1A C6A N1A -173.8(7) . . . . ? Te C1A C6A N1A 0.4(9) . . . . ? N2A N1A C6A C5A -3.8(12) . . . . ? Te N1A C6A C5A -176.7(8) . . . . ? N2A N1A C6A C1A 172.6(7) . . . . ? Te N1A C6A C1A -0.2(6) . . . . ? N1A N2A C7A C12A -3.0(13) . . . . ? N1A N2A C7A C8A 176.2(8) . . . . ? C12A C7A C8A C9A 0.9(14) . . . . ? N2A C7A C8A C9A -178.3(8) . . . . ? C7A C8A C9A C10A 0.0(14) . . . . ? C8A C9A C10A C11A -1.5(15) . . . . ? C9A C10A C11A C12A 2.1(15) . . . . ? C8A C7A C12A C11A -0.3(14) . . . . ? N2A C7A C12A C11A 178.8(9) . . . . ? C10A C11A C12A C7A -1.2(15) . . . . ? O1 Te C1B C6B -174.7(7) 2_676 . . . ? C1A Te C1B C6B -82.6(7) . . . . ? O1 Te C1B C6B 110.6(7) . . . . ? N2B Te C1B C6B -5.4(6) . . . . ? N1A Te C1B C6B -53.3(8) . . . . ? O1 Te C1B C2B 7.0(6) 2_676 . . . ? C1A Te C1B C2B 99.1(6) . . . . ? O1 Te C1B C2B -67.8(6) . . . . ? N2B Te C1B C2B 176.2(7) . . . . ? N1A Te C1B C2B 128.3(5) . . . . ? C6B C1B C2B C3B 0.4(12) . . . . ? Te C1B C2B C3B 178.8(6) . . . . ? C1B C2B C3B C4B -1.2(12) . . . . ? C2B C3B C4B C5B 0.4(13) . . . . ? C3B C4B C5B C6B 1.2(13) . . . . ? C2B C1B C6B C5B 1.3(12) . . . . ? Te C1B C6B C5B -177.0(6) . . . . ? C2B C1B C6B N1B -176.4(7) . . . . ? Te C1B C6B N1B 5.3(11) . . . . ? C4B C5B C6B C1B -2.1(13) . . . . ? C4B C5B C6B N1B 175.8(8) . . . . ? N2B N1B C6B C1B 1.8(11) . . . . ? N2B N1B C6B C5B -176.0(7) . . . . ? N1B N2B C7B C12B 171.8(7) . . . . ? Te N2B C7B C12B -3.3(11) . . . . ? N1B N2B C7B C8B -11.3(11) . . . . ? Te N2B C7B C8B 173.7(6) . . . . ? C12B C7B C8B C9B -1.1(13) . . . . ? N2B C7B C8B C9B -177.9(8) . . . . ? C7B C8B C9B C10B 1.0(15) . . . . ? C8B C9B C10B C11B -0.8(16) . . . . ? C9B C10B C11B C12B 0.6(15) . . . . ? C8B C7B C12B C11B 0.9(13) . . . . ? N2B C7B C12B C11B 177.9(8) . . . . ? C10B C11B C12B C7B -0.6(14) . . . . ? C3S C1S C2S C3S -1.3(19) . . . 2_776 ? C2S C1S C3S C2S 1.3(19) . . . 2_776 ? 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 C2B H2BA O1 0.95 2.54 3.112(10) 119.0 2_676 C9A H9AA O1 0.95 2.53 3.312(11) 139.2 1_556 C3S H3SA O1 0.95 2.58 3.354(13) 138.8 . _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.568 _refine_diff_density_min -2.493 _refine_diff_density_rms 0.287 END