# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Alan H. Cowley' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Gregor Reeske' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_email cowley@mail.utexas.edu _publ_contact_author_fax 512-471-6822 _publ_contact_author_phone 512-471-7710 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Alan H. Cowley' _publ_contact_letter ; Please consider this CIF submission for publication in ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Direct reactions of tellurium tetrahalides with chelating nitrogen ligands: Trapping of TeI2 and C-H activation of an a,a'-diiminopyridine (DIMPY) Ligand ; data_squeeze1 _database_code_depnum_ccdc_archive 'CCDC 614916' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 I2 N2 Te' _chemical_formula_sum 'C36 H40 I2 N2 Te' _chemical_formula_weight 882.10 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/n _symmetry_space_group_name_Hall -p2yn 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 11.663(2) _cell_length_b 16.601(3) _cell_length_c 20.231(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.21(3) _cell_angle_gamma 90.00 _cell_volume 3914.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 2.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26108 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8948 _reflns_number_gt 5399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of what appeared to be thf was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8948 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1545 _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 C1 C 0.0750(5) 0.2713(3) -0.0093(3) 0.0281(13) Uani 1 1 d . . . C2 C 0.0749(5) 0.3139(3) -0.0738(3) 0.0300(13) Uani 1 1 d . . . C3 C -0.0076(6) 0.3275(4) -0.1241(3) 0.0396(16) Uani 1 1 d . . . H3 H -0.0823 0.3087 -0.1209 0.048 Uiso 1 1 calc R . . C4 C 0.0252(6) 0.3696(4) -0.1783(3) 0.0423(16) Uani 1 1 d . . . H4 H -0.0301 0.3797 -0.2116 0.051 Uiso 1 1 calc R . . C5 C 0.1343(7) 0.3978(4) -0.1869(3) 0.0476(18) Uani 1 1 d . . . H5 H 0.1511 0.4260 -0.2251 0.057 Uiso 1 1 calc R . . C6 C 0.2223(6) 0.3838(4) -0.1367(3) 0.0380(15) Uani 1 1 d . . . C7 C 0.3373(7) 0.4083(4) -0.1357(3) 0.0476(18) Uani 1 1 d . . . H7 H 0.3646 0.4373 -0.1712 0.057 Uiso 1 1 calc R . . C8 C 0.4107(6) 0.3899(4) -0.0823(4) 0.0448(17) Uani 1 1 d . . . H8 H 0.4873 0.4051 -0.0838 0.054 Uiso 1 1 calc R . . C9 C 0.3753(5) 0.3506(4) -0.0281(3) 0.0371(15) Uani 1 1 d . . . H9 H 0.4260 0.3415 0.0077 0.045 Uiso 1 1 calc R . . C10 C 0.2622(6) 0.3239(3) -0.0265(3) 0.0312(14) Uani 1 1 d . . . C11 C 0.1879(6) 0.3415(4) -0.0810(3) 0.0351(14) Uani 1 1 d . . . C12 C 0.1939(5) 0.2789(3) 0.0210(3) 0.0308(13) Uani 1 1 d . . . C13 C -0.1214(5) 0.2405(4) -0.0025(3) 0.0336(14) Uani 1 1 d . . . C14 C -0.1889(5) 0.3064(4) 0.0162(3) 0.0342(14) Uani 1 1 d . . . C15 C -0.2977(6) 0.3106(4) -0.0143(4) 0.0465(18) Uani 1 1 d . . . H15 H -0.3449 0.3538 -0.0046 0.056 Uiso 1 1 calc R . . C16 C -0.3374(6) 0.2537(4) -0.0579(4) 0.055(2) Uani 1 1 d . . . H16 H -0.4102 0.2592 -0.0779 0.065 Uiso 1 1 calc R . . C17 C -0.2701(6) 0.1875(4) -0.0729(4) 0.0502(19) Uani 1 1 d . . . H17 H -0.2982 0.1486 -0.1024 0.060 Uiso 1 1 calc R . . C18 C -0.1611(6) 0.1794(4) -0.0437(3) 0.0398(16) Uani 1 1 d . . . C19 C -0.1488(7) 0.3688(4) 0.0665(4) 0.0487(18) Uani 1 1 d . . . H19 H -0.0835 0.3456 0.0918 0.058 Uiso 1 1 calc R . . C20 C -0.1081(11) 0.4434(5) 0.0356(5) 0.098(4) Uani 1 1 d . . . H20A H -0.0449 0.4312 0.0083 0.146 Uiso 1 1 calc R . . H20B H -0.0837 0.4809 0.0694 0.146 Uiso 1 1 calc R . . H20C H -0.1694 0.4667 0.0089 0.146 Uiso 1 1 calc R . . C21 C -0.2400(13) 0.3895(7) 0.1155(5) 0.120(5) Uani 1 1 d . . . H21A H -0.2080 0.4252 0.1487 0.180 Uiso 1 1 calc R . . H21B H -0.2658 0.3410 0.1361 0.180 Uiso 1 1 calc R . . H21C H -0.3036 0.4153 0.0927 0.180 Uiso 1 1 calc R . . C22 C -0.0892(7) 0.1049(4) -0.0591(3) 0.0504(19) Uani 1 1 d . . . H22 H -0.0130 0.1124 -0.0379 0.060 Uiso 1 1 calc R . . C23 C -0.0735(9) 0.0922(7) -0.1322(5) 0.092(3) Uani 1 1 d . . . H23A H -0.1466 0.0819 -0.1539 0.138 Uiso 1 1 calc R . . H23B H -0.0236 0.0470 -0.1384 0.138 Uiso 1 1 calc R . . H23C H -0.0402 0.1396 -0.1507 0.138 Uiso 1 1 calc R . . C24 C -0.1439(10) 0.0289(5) -0.0274(5) 0.086(3) Uani 1 1 d . . . H24A H -0.2211 0.0224 -0.0448 0.128 Uiso 1 1 calc R . . H24B H -0.1446 0.0355 0.0197 0.128 Uiso 1 1 calc R . . H24C H -0.0997 -0.0179 -0.0377 0.128 Uiso 1 1 calc R . . C25 C 0.3218(6) 0.2670(4) 0.1151(3) 0.0359(15) Uani 1 1 d . . . C26 C 0.3363(6) 0.3429(4) 0.1461(3) 0.0416(16) Uani 1 1 d . . . C27 C 0.4372(7) 0.3546(5) 0.1830(4) 0.055(2) Uani 1 1 d . . . H27 H 0.4497 0.4038 0.2040 0.067 Uiso 1 1 calc R . . C28 C 0.5174(8) 0.2971(6) 0.1892(4) 0.070(3) Uani 1 1 d . . . H28 H 0.5845 0.3073 0.2141 0.084 Uiso 1 1 calc R . . C29 C 0.5019(6) 0.2218(6) 0.1588(4) 0.059(2) Uani 1 1 d . . . H29 H 0.5590 0.1829 0.1635 0.071 Uiso 1 1 calc R . . C30 C 0.4023(6) 0.2047(4) 0.1217(3) 0.0421(16) Uani 1 1 d . . . C31 C 0.2477(8) 0.4091(4) 0.1402(4) 0.057(2) Uani 1 1 d . . . H31 H 0.1879 0.3913 0.1081 0.068 Uiso 1 1 calc R . . C32 C 0.2954(11) 0.4880(5) 0.1150(4) 0.086(3) Uani 1 1 d . . . H32A H 0.3631 0.5022 0.1409 0.130 Uiso 1 1 calc R . . H32B H 0.2389 0.5296 0.1187 0.130 Uiso 1 1 calc R . . H32C H 0.3143 0.4819 0.0695 0.130 Uiso 1 1 calc R . . C33 C 0.1907(9) 0.4218(5) 0.2063(5) 0.075(3) Uani 1 1 d . . . H33A H 0.1609 0.3715 0.2214 0.112 Uiso 1 1 calc R . . H33B H 0.1291 0.4599 0.2006 0.112 Uiso 1 1 calc R . . H33C H 0.2463 0.4421 0.2383 0.112 Uiso 1 1 calc R . . C34 C 0.3841(7) 0.1238(4) 0.0876(4) 0.0492(18) Uani 1 1 d . . . H34 H 0.3024 0.1184 0.0753 0.059 Uiso 1 1 calc R . . C35 C 0.4526(12) 0.1192(6) 0.0241(5) 0.106(4) Uani 1 1 d . . . H35A H 0.4200 0.1557 -0.0083 0.159 Uiso 1 1 calc R . . H35B H 0.4495 0.0653 0.0069 0.159 Uiso 1 1 calc R . . H35C H 0.5311 0.1338 0.0340 0.159 Uiso 1 1 calc R . . C36 C 0.4188(10) 0.0529(5) 0.1319(5) 0.088(3) Uani 1 1 d . . . H36A H 0.4985 0.0576 0.1451 0.132 Uiso 1 1 calc R . . H36B H 0.4066 0.0035 0.1080 0.132 Uiso 1 1 calc R . . H36C H 0.3733 0.0530 0.1704 0.132 Uiso 1 1 calc R . . N1 N -0.0046(4) 0.2377(3) 0.0238(2) 0.0332(12) Uani 1 1 d . . . N2 N 0.2141(4) 0.2515(3) 0.0793(2) 0.0329(12) Uani 1 1 d . . . Te1 Te 0.05448(4) 0.19344(2) 0.13290(2) 0.03440(14) Uani 1 1 d . . . I1 I -0.17163(5) 0.13956(4) 0.16227(3) 0.0737(2) Uani 1 1 d . . . I2 I 0.17407(5) 0.16669(4) 0.25753(3) 0.0671(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.030(3) 0.034(3) -0.002(2) -0.005(3) 0.009(2) C2 0.023(3) 0.036(3) 0.032(3) -0.003(2) 0.007(2) 0.004(3) C3 0.038(4) 0.045(4) 0.035(4) -0.003(3) -0.011(3) 0.010(3) C4 0.040(4) 0.052(4) 0.035(4) 0.001(3) 0.002(3) 0.006(3) C5 0.057(5) 0.053(4) 0.033(4) 0.004(3) 0.003(3) 0.013(4) C6 0.030(4) 0.047(4) 0.038(4) 0.006(3) 0.008(3) 0.010(3) C7 0.050(5) 0.054(4) 0.040(4) 0.012(3) 0.015(3) -0.003(3) C8 0.027(4) 0.047(4) 0.061(5) 0.006(3) 0.005(3) 0.002(3) C9 0.019(3) 0.047(4) 0.046(4) -0.001(3) 0.005(3) 0.000(3) C10 0.034(4) 0.027(3) 0.033(3) 0.002(2) 0.002(3) 0.002(2) C11 0.034(4) 0.042(3) 0.030(3) -0.006(3) -0.004(3) 0.005(3) C12 0.027(3) 0.028(3) 0.038(4) 0.002(2) 0.001(3) 0.004(2) C13 0.028(4) 0.039(3) 0.034(3) 0.007(3) -0.002(3) -0.001(3) C14 0.022(3) 0.031(3) 0.049(4) 0.005(3) 0.002(3) -0.001(3) C15 0.027(4) 0.028(3) 0.085(5) 0.007(3) 0.001(3) 0.007(3) C16 0.028(4) 0.053(5) 0.081(6) 0.014(4) -0.008(4) 0.000(3) C17 0.037(4) 0.043(4) 0.068(5) -0.003(3) -0.022(4) 0.003(3) C18 0.037(4) 0.039(4) 0.042(4) -0.002(3) -0.007(3) 0.002(3) C19 0.048(5) 0.040(4) 0.057(5) -0.004(3) -0.012(4) 0.008(3) C20 0.141(10) 0.065(6) 0.092(7) -0.037(5) 0.068(7) -0.063(6) C21 0.211(16) 0.077(7) 0.078(7) -0.020(5) 0.077(8) -0.041(8) C22 0.050(5) 0.048(4) 0.053(5) -0.015(3) -0.013(4) 0.006(3) C23 0.089(8) 0.099(8) 0.089(7) -0.023(6) 0.013(6) 0.029(6) C24 0.103(9) 0.055(5) 0.098(7) -0.005(5) -0.013(6) 0.020(5) C25 0.030(4) 0.047(4) 0.031(3) 0.011(3) 0.003(3) -0.005(3) C26 0.050(5) 0.040(4) 0.034(4) 0.002(3) -0.005(3) -0.006(3) C27 0.057(6) 0.062(5) 0.046(4) 0.002(3) -0.017(4) -0.019(4) C28 0.044(5) 0.109(8) 0.054(5) 0.011(5) -0.016(4) -0.026(5) C29 0.025(4) 0.092(6) 0.060(5) 0.021(4) -0.006(3) 0.007(4) C30 0.029(4) 0.056(4) 0.041(4) 0.013(3) 0.004(3) 0.010(3) C31 0.079(6) 0.037(4) 0.052(5) -0.008(3) -0.010(4) -0.002(4) C32 0.146(11) 0.054(5) 0.061(6) 0.000(4) 0.017(6) -0.010(6) C33 0.079(7) 0.056(5) 0.090(7) 0.002(4) 0.006(5) 0.015(5) C34 0.041(4) 0.056(4) 0.052(4) 0.004(3) 0.005(3) 0.018(3) C35 0.167(13) 0.060(6) 0.095(8) 0.003(5) 0.060(8) 0.019(7) C36 0.102(9) 0.052(5) 0.109(8) 0.036(5) -0.012(6) 0.018(5) N1 0.027(3) 0.041(3) 0.031(3) -0.002(2) -0.001(2) -0.001(2) N2 0.026(3) 0.031(3) 0.041(3) 0.000(2) -0.004(2) -0.001(2) Te1 0.0295(2) 0.0355(2) 0.0381(3) 0.00685(17) 0.00067(17) 0.00238(18) I1 0.0362(3) 0.1038(5) 0.0816(4) 0.0350(3) 0.0087(3) -0.0125(3) I2 0.0609(4) 0.0913(4) 0.0480(3) 0.0250(3) -0.0115(3) 0.0062(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 C1 N1 1.291(8) . ? C1 C2 1.484(8) . ? C1 C12 1.501(8) . ? C2 C3 1.391(9) . ? C2 C11 1.408(9) . ? C3 C4 1.368(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(10) . ? C4 H4 0.9300 . ? C5 C6 1.434(10) . ? C5 H5 0.9300 . ? C6 C11 1.399(9) . ? C6 C7 1.402(10) . ? C7 C8 1.386(10) . ? C7 H7 0.9300 . ? C8 C9 1.355(9) . ? C8 H8 0.9300 . ? C9 C10 1.393(9) . ? C9 H9 0.9300 . ? C10 C11 1.407(8) . ? C10 C12 1.476(9) . ? C12 N2 1.277(8) . ? C13 C18 1.382(9) . ? C13 C14 1.409(9) . ? C13 N1 1.443(8) . ? C14 C15 1.391(9) . ? C14 C19 1.514(9) . ? C15 C16 1.361(10) . ? C15 H15 0.9300 . ? C16 C17 1.392(10) . ? C16 H16 0.9300 . ? C17 C18 1.387(9) . ? C17 H17 0.9300 . ? C18 C22 1.533(10) . ? C19 C20 1.474(11) . ? C19 C21 1.522(13) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.512(11) . ? C22 C24 1.561(12) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.400(9) . ? C25 C26 1.414(9) . ? C25 N2 1.448(8) . ? C26 C27 1.383(10) . ? C26 C31 1.511(10) . ? C27 C28 1.339(12) . ? C27 H27 0.9300 . ? C28 C29 1.402(12) . ? C28 H28 0.9300 . ? C29 C30 1.387(10) . ? C29 H29 0.9300 . ? C30 C34 1.522(10) . ? C31 C32 1.519(11) . ? C31 C33 1.530(12) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C36 1.524(10) . ? C34 C35 1.542(12) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? N1 Te1 2.403(5) . ? N2 Te1 2.393(5) . ? Te1 I1 2.8686(9) . ? Te1 I2 2.8687(10) . ? 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 N1 C1 C2 133.3(5) . . ? N1 C1 C12 119.7(5) . . ? C2 C1 C12 106.8(5) . . ? C3 C2 C11 119.7(6) . . ? C3 C2 C1 134.1(6) . . ? C11 C2 C1 106.1(5) . . ? C4 C3 C2 117.5(7) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 124.4(6) . . ? C3 C4 H4 117.8 . . ? C5 C4 H4 117.8 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C11 C6 C7 116.0(6) . . ? C11 C6 C5 115.6(6) . . ? C7 C6 C5 128.4(6) . . ? C8 C7 C6 120.6(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 122.7(7) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 119.3(6) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 118.1(6) . . ? C9 C10 C12 135.4(6) . . ? C11 C10 C12 106.5(6) . . ? C6 C11 C2 123.0(6) . . ? C6 C11 C10 123.2(6) . . ? C2 C11 C10 113.8(6) . . ? N2 C12 C10 134.2(6) . . ? N2 C12 C1 118.9(6) . . ? C10 C12 C1 106.8(5) . . ? C18 C13 C14 123.7(6) . . ? C18 C13 N1 119.3(6) . . ? C14 C13 N1 117.1(5) . . ? C15 C14 C13 115.5(6) . . ? C15 C14 C19 121.1(6) . . ? C13 C14 C19 123.4(6) . . ? C16 C15 C14 122.3(6) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C17 120.5(7) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C13 C18 C17 117.8(6) . . ? C13 C18 C22 122.8(6) . . ? C17 C18 C22 119.4(6) . . ? C20 C19 C14 112.7(6) . . ? C20 C19 C21 109.4(7) . . ? C14 C19 C21 112.8(7) . . ? C20 C19 H19 107.2 . . ? C14 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C18 113.5(6) . . ? C23 C22 C24 110.8(7) . . ? C18 C22 C24 109.5(7) . . ? C23 C22 H22 107.6 . . ? C18 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 123.1(6) . . ? C30 C25 N2 118.9(6) . . ? C26 C25 N2 117.8(6) . . ? C27 C26 C25 116.7(7) . . ? C27 C26 C31 120.3(6) . . ? C25 C26 C31 122.9(6) . . ? C28 C27 C26 121.8(7) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 121.2(7) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 120.6(8) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 116.5(7) . . ? C29 C30 C34 121.6(7) . . ? C25 C30 C34 121.8(6) . . ? C26 C31 C32 113.3(8) . . ? C26 C31 C33 110.6(6) . . ? C32 C31 C33 110.6(6) . . ? C26 C31 H31 107.4 . . ? C32 C31 H31 107.4 . . ? C33 C31 H31 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C30 112.7(7) . . ? C36 C34 C35 108.5(7) . . ? C30 C34 C35 110.8(7) . . ? C36 C34 H34 108.3 . . ? C30 C34 H34 108.3 . . ? C35 C34 H34 108.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C13 118.9(5) . . ? C1 N1 Te1 115.0(4) . . ? C13 N1 Te1 125.5(4) . . ? C12 N2 C25 121.5(5) . . ? C12 N2 Te1 116.3(4) . . ? C25 N2 Te1 121.4(4) . . ? N2 Te1 N1 70.17(17) . . ? N2 Te1 I1 163.13(12) . . ? N1 Te1 I1 93.01(13) . . ? N2 Te1 I2 95.75(12) . . ? N1 Te1 I2 165.36(12) . . ? I1 Te1 I2 100.92(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 N1 C1 C2 C3 -6.2(12) . . . . ? C12 C1 C2 C3 179.6(6) . . . . ? N1 C1 C2 C11 176.2(6) . . . . ? C12 C1 C2 C11 2.0(6) . . . . ? C11 C2 C3 C4 -1.6(9) . . . . ? C1 C2 C3 C4 -178.9(6) . . . . ? C2 C3 C4 C5 1.3(10) . . . . ? C3 C4 C5 C6 -0.2(11) . . . . ? C4 C5 C6 C11 -0.6(10) . . . . ? C4 C5 C6 C7 -179.0(7) . . . . ? C11 C6 C7 C8 0.9(10) . . . . ? C5 C6 C7 C8 179.4(7) . . . . ? C6 C7 C8 C9 -2.6(11) . . . . ? C7 C8 C9 C10 3.2(10) . . . . ? C8 C9 C10 C11 -2.1(9) . . . . ? C8 C9 C10 C12 178.3(7) . . . . ? C7 C6 C11 C2 178.9(6) . . . . ? C5 C6 C11 C2 0.2(9) . . . . ? C7 C6 C11 C10 0.0(9) . . . . ? C5 C6 C11 C10 -178.6(6) . . . . ? C3 C2 C11 C6 0.9(9) . . . . ? C1 C2 C11 C6 178.9(6) . . . . ? C3 C2 C11 C10 179.8(5) . . . . ? C1 C2 C11 C10 -2.2(7) . . . . ? C9 C10 C11 C6 0.6(9) . . . . ? C12 C10 C11 C6 -179.7(6) . . . . ? C9 C10 C11 C2 -178.4(5) . . . . ? C12 C10 C11 C2 1.4(7) . . . . ? C9 C10 C12 N2 3.9(12) . . . . ? C11 C10 C12 N2 -175.8(7) . . . . ? C9 C10 C12 C1 179.7(7) . . . . ? C11 C10 C12 C1 0.0(6) . . . . ? N1 C1 C12 N2 0.2(8) . . . . ? C2 C1 C12 N2 175.3(5) . . . . ? N1 C1 C12 C10 -176.4(5) . . . . ? C2 C1 C12 C10 -1.3(6) . . . . ? C18 C13 C14 C15 -5.3(10) . . . . ? N1 C13 C14 C15 174.9(6) . . . . ? C18 C13 C14 C19 173.8(6) . . . . ? N1 C13 C14 C19 -6.0(9) . . . . ? C13 C14 C15 C16 1.6(10) . . . . ? C19 C14 C15 C16 -177.6(7) . . . . ? C14 C15 C16 C17 1.2(12) . . . . ? C15 C16 C17 C18 -0.6(12) . . . . ? C14 C13 C18 C17 6.0(10) . . . . ? N1 C13 C18 C17 -174.2(6) . . . . ? C14 C13 C18 C22 -175.1(6) . . . . ? N1 C13 C18 C22 4.7(10) . . . . ? C16 C17 C18 C13 -2.9(11) . . . . ? C16 C17 C18 C22 178.2(7) . . . . ? C15 C14 C19 C20 -80.8(10) . . . . ? C13 C14 C19 C20 100.1(9) . . . . ? C15 C14 C19 C21 43.7(10) . . . . ? C13 C14 C19 C21 -135.5(8) . . . . ? C13 C18 C22 C23 -123.5(8) . . . . ? C17 C18 C22 C23 55.3(10) . . . . ? C13 C18 C22 C24 112.1(8) . . . . ? C17 C18 C22 C24 -69.1(9) . . . . ? C30 C25 C26 C27 1.7(10) . . . . ? N2 C25 C26 C27 176.5(6) . . . . ? C30 C25 C26 C31 -178.2(7) . . . . ? N2 C25 C26 C31 -3.5(10) . . . . ? C25 C26 C27 C28 -0.1(12) . . . . ? C31 C26 C27 C28 179.9(8) . . . . ? C26 C27 C28 C29 -0.5(13) . . . . ? C27 C28 C29 C30 -0.5(13) . . . . ? C28 C29 C30 C25 2.0(11) . . . . ? C28 C29 C30 C34 179.3(7) . . . . ? C26 C25 C30 C29 -2.7(10) . . . . ? N2 C25 C30 C29 -177.4(6) . . . . ? C26 C25 C30 C34 -179.9(6) . . . . ? N2 C25 C30 C34 5.4(9) . . . . ? C27 C26 C31 C32 55.0(9) . . . . ? C25 C26 C31 C32 -125.1(7) . . . . ? C27 C26 C31 C33 -69.8(9) . . . . ? C25 C26 C31 C33 110.2(8) . . . . ? C29 C30 C34 C36 44.5(10) . . . . ? C25 C30 C34 C36 -138.4(8) . . . . ? C29 C30 C34 C35 -77.2(10) . . . . ? C25 C30 C34 C35 99.9(9) . . . . ? C2 C1 N1 C13 -1.6(10) . . . . ? C12 C1 N1 C13 171.9(5) . . . . ? C2 C1 N1 Te1 -172.7(5) . . . . ? C12 C1 N1 Te1 0.9(7) . . . . ? C18 C13 N1 C1 89.9(7) . . . . ? C14 C13 N1 C1 -90.3(7) . . . . ? C18 C13 N1 Te1 -100.0(6) . . . . ? C14 C13 N1 Te1 79.8(6) . . . . ? C10 C12 N2 C25 4.4(10) . . . . ? C1 C12 N2 C25 -171.0(5) . . . . ? C10 C12 N2 Te1 174.3(5) . . . . ? C1 C12 N2 Te1 -1.1(7) . . . . ? C30 C25 N2 C12 -105.4(7) . . . . ? C26 C25 N2 C12 79.6(8) . . . . ? C30 C25 N2 Te1 85.2(6) . . . . ? C26 C25 N2 Te1 -89.8(6) . . . . ? C12 N2 Te1 N1 1.1(4) . . . . ? C25 N2 Te1 N1 171.0(5) . . . . ? C12 N2 Te1 I1 -3.7(7) . . . . ? C25 N2 Te1 I1 166.2(3) . . . . ? C12 N2 Te1 I2 -174.8(4) . . . . ? C25 N2 Te1 I2 -4.9(4) . . . . ? C1 N1 Te1 N2 -1.0(4) . . . . ? C13 N1 Te1 N2 -171.4(5) . . . . ? C1 N1 Te1 I1 177.6(4) . . . . ? C13 N1 Te1 I1 7.2(5) . . . . ? C1 N1 Te1 I2 15.5(8) . . . . ? C13 N1 Te1 I2 -154.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.086 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.181 # Attachment 'CCDC614917.cif' data_squeeze2 _database_code_depnum_ccdc_archive 'CCDC 614917' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 I2 N2 Te ' _chemical_formula_sum 'C30 H28 I2 N2 Te' _chemical_formula_weight 797.94 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/n _symmetry_space_group_name_Hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.841(5) _cell_length_b 14.198(5) _cell_length_c 18.808(5) _cell_angle_alpha 90.000 _cell_angle_beta 91.621(5) _cell_angle_gamma 90.000 _cell_volume 2893.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6209 _exptl_absorpt_correction_T_max 0.6209 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10912 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6564 _reflns_number_gt 4164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6564 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4446(4) 0.2589(3) 0.5763(2) 0.0224(11) Uani 1 1 d . . . C2 C 0.4444(4) 0.3150(3) 0.5104(2) 0.0220(11) Uani 1 1 d . . . C3 C 0.3609(4) 0.3316(3) 0.4560(2) 0.0273(12) Uani 1 1 d . . . H3 H 0.2810 0.3040 0.4560 0.033 Uiso 1 1 calc R . . C4 C 0.3968(5) 0.3909(4) 0.3998(2) 0.0305(12) Uani 1 1 d . . . H4 H 0.3384 0.4045 0.3627 0.037 Uiso 1 1 calc R . . C5 C 0.5116(5) 0.4291(4) 0.3969(2) 0.0322(13) Uani 1 1 d . . . H5 H 0.5324 0.4666 0.3572 0.039 Uiso 1 1 calc R . . C6 C 0.6014(4) 0.4137(3) 0.4527(2) 0.0259(11) Uani 1 1 d . . . C7 C 0.7228(4) 0.4481(3) 0.4577(3) 0.0304(12) Uani 1 1 d . . . H7 H 0.7542 0.4846 0.4199 0.036 Uiso 1 1 calc R . . C8 C 0.7970(5) 0.4296(3) 0.5168(2) 0.0303(12) Uani 1 1 d . . . H8 H 0.8790 0.4533 0.5183 0.036 Uiso 1 1 calc R . . C9 C 0.7558(4) 0.3767(3) 0.5750(2) 0.0249(11) Uani 1 1 d . . . H9 H 0.8068 0.3680 0.6164 0.030 Uiso 1 1 calc R . . C10 C 0.6395(4) 0.3382(3) 0.5700(2) 0.0204(11) Uani 1 1 d . . . C11 C 0.5631(4) 0.3579(3) 0.5094(2) 0.0218(11) Uani 1 1 d . . . C12 C 0.5667(4) 0.2756(3) 0.6146(2) 0.0208(11) Uani 1 1 d . . . C13 C 0.2503(4) 0.1875(3) 0.5669(2) 0.0233(11) Uani 1 1 d . . . C14 C 0.1534(4) 0.2488(3) 0.5816(2) 0.0252(11) Uani 1 1 d . . . C15 C 0.0429(4) 0.2358(4) 0.5432(2) 0.0296(12) Uani 1 1 d . . . H15 H -0.0237 0.2773 0.5517 0.036 Uiso 1 1 calc R . . C16 C 0.0257(4) 0.1645(4) 0.4930(3) 0.0327(13) Uani 1 1 d . . . C17 C 0.1234(5) 0.1028(4) 0.4837(2) 0.0309(12) Uani 1 1 d . . . H17 H 0.1121 0.0517 0.4516 0.037 Uiso 1 1 calc R . . C18 C 0.2370(4) 0.1123(3) 0.5193(2) 0.0275(12) Uani 1 1 d . . . C19 C 0.1684(5) 0.3243(4) 0.6373(3) 0.0377(13) Uani 1 1 d . . . H19A H 0.1799 0.2950 0.6842 0.057 Uiso 1 1 calc R . . H19B H 0.0944 0.3640 0.6370 0.057 Uiso 1 1 calc R . . H19C H 0.2405 0.3630 0.6270 0.057 Uiso 1 1 calc R . . C20 C -0.0938(5) 0.1570(4) 0.4502(3) 0.0461(15) Uani 1 1 d . . . H20A H -0.1623 0.1776 0.4794 0.069 Uiso 1 1 calc R . . H20B H -0.1071 0.0914 0.4357 0.069 Uiso 1 1 calc R . . H20C H -0.0897 0.1970 0.4079 0.069 Uiso 1 1 calc R . . C21 C 0.3423(5) 0.0460(4) 0.5076(3) 0.0392(14) Uani 1 1 d . . . H21A H 0.3168 -0.0020 0.4727 0.059 Uiso 1 1 calc R . . H21B H 0.3659 0.0154 0.5527 0.059 Uiso 1 1 calc R . . H21C H 0.4128 0.0812 0.4898 0.059 Uiso 1 1 calc R . . C22 C 0.7019(4) 0.2547(3) 0.7140(2) 0.0232(11) Uani 1 1 d . . . C23 C 0.7042(4) 0.3274(4) 0.7639(2) 0.0276(12) Uani 1 1 d . . . C24 C 0.8161(4) 0.3453(4) 0.8006(2) 0.0330(13) Uani 1 1 d . . . H24 H 0.8193 0.3938 0.8354 0.040 Uiso 1 1 calc R . . C25 C 0.9210(4) 0.2947(3) 0.7879(2) 0.0257(11) Uani 1 1 d . . . C26 C 0.9136(4) 0.2226(4) 0.7382(2) 0.0300(12) Uani 1 1 d . . . H26 H 0.9856 0.1871 0.7291 0.036 Uiso 1 1 calc R . . C27 C 0.8058(4) 0.2008(3) 0.7017(2) 0.0247(11) Uani 1 1 d . . . C28 C 0.5915(5) 0.3857(4) 0.7767(3) 0.0442(15) Uani 1 1 d . . . H28A H 0.5784 0.4300 0.7373 0.066 Uiso 1 1 calc R . . H28B H 0.6030 0.4207 0.8213 0.066 Uiso 1 1 calc R . . H28C H 0.5195 0.3443 0.7800 0.066 Uiso 1 1 calc R . . C29 C 1.0410(4) 0.3157(4) 0.8280(3) 0.0409(14) Uani 1 1 d . . . H29A H 1.0789 0.3721 0.8079 0.061 Uiso 1 1 calc R . . H29B H 1.0972 0.2621 0.8236 0.061 Uiso 1 1 calc R . . H29C H 1.0245 0.3265 0.8783 0.061 Uiso 1 1 calc R . . C30 C 0.7987(5) 0.1218(4) 0.6477(3) 0.0393(14) Uani 1 1 d . . . H30A H 0.8789 0.0901 0.6461 0.059 Uiso 1 1 calc R . . H30B H 0.7774 0.1478 0.6007 0.059 Uiso 1 1 calc R . . H30C H 0.7354 0.0765 0.6613 0.059 Uiso 1 1 calc R . . N1 N 0.3670(3) 0.2012(3) 0.60321(18) 0.0234(9) Uani 1 1 d . . . N2 N 0.5870(3) 0.2365(3) 0.67574(18) 0.0230(9) Uani 1 1 d . . . Te1 Te 0.42628(3) 0.13585(2) 0.714540(16) 0.02550(10) Uani 1 1 d . . . I1 I 0.20259(3) 0.02639(2) 0.719119(17) 0.03397(11) Uani 1 1 d . . . I2 I 0.54664(3) 0.08936(3) 0.849035(19) 0.04876(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(3) 0.025(3) 0.021(2) 0.000(2) 0.000(2) 0.004(2) C2 0.022(3) 0.027(3) 0.017(2) 0.004(2) 0.002(2) 0.006(2) C3 0.025(3) 0.030(3) 0.027(3) 0.000(2) 0.006(2) 0.002(2) C4 0.030(3) 0.039(3) 0.022(3) -0.001(2) -0.001(2) 0.006(3) C5 0.035(3) 0.035(3) 0.027(3) 0.006(2) 0.004(2) 0.006(3) C6 0.032(3) 0.022(3) 0.024(3) 0.001(2) 0.005(2) 0.002(2) C7 0.029(3) 0.028(3) 0.035(3) 0.008(2) 0.006(2) 0.000(2) C8 0.029(3) 0.027(3) 0.035(3) 0.004(2) 0.006(2) -0.002(2) C9 0.021(3) 0.027(3) 0.027(3) -0.002(2) -0.002(2) 0.003(2) C10 0.023(3) 0.016(3) 0.023(2) 0.001(2) 0.000(2) -0.002(2) C11 0.022(3) 0.024(3) 0.019(2) -0.005(2) 0.006(2) 0.000(2) C12 0.022(3) 0.021(3) 0.020(2) 0.001(2) 0.003(2) 0.001(2) C13 0.023(3) 0.025(3) 0.022(2) 0.004(2) -0.002(2) -0.001(2) C14 0.024(3) 0.026(3) 0.026(3) 0.001(2) 0.004(2) 0.000(2) C15 0.020(3) 0.031(3) 0.037(3) 0.004(3) -0.001(2) 0.008(2) C16 0.021(3) 0.047(4) 0.030(3) 0.007(3) 0.000(2) -0.005(3) C17 0.034(3) 0.034(3) 0.024(3) -0.006(2) -0.004(2) -0.004(3) C18 0.028(3) 0.031(3) 0.023(3) -0.002(2) -0.001(2) 0.000(2) C19 0.033(3) 0.028(3) 0.052(3) -0.005(3) 0.005(3) 0.004(3) C20 0.031(3) 0.062(4) 0.045(3) -0.006(3) -0.008(3) -0.001(3) C21 0.040(3) 0.036(3) 0.042(3) -0.017(3) -0.002(3) 0.008(3) C22 0.025(3) 0.025(3) 0.019(2) 0.003(2) -0.002(2) -0.001(2) C23 0.025(3) 0.034(3) 0.024(3) 0.000(2) 0.003(2) 0.006(2) C24 0.032(3) 0.035(3) 0.032(3) -0.003(2) -0.008(2) -0.004(3) C25 0.019(3) 0.029(3) 0.028(3) 0.006(2) -0.009(2) -0.009(2) C26 0.019(3) 0.034(3) 0.036(3) 0.007(3) -0.002(2) 0.004(2) C27 0.028(3) 0.019(3) 0.028(3) 0.006(2) 0.004(2) 0.004(2) C28 0.039(4) 0.044(4) 0.049(4) -0.017(3) -0.002(3) 0.012(3) C29 0.030(3) 0.046(4) 0.046(3) -0.001(3) -0.014(3) -0.008(3) C30 0.036(3) 0.033(3) 0.050(3) -0.008(3) 0.003(3) 0.011(3) N1 0.024(2) 0.026(2) 0.020(2) -0.0017(18) 0.0003(17) -0.0022(19) N2 0.021(2) 0.025(2) 0.023(2) 0.0005(19) 0.0000(17) 0.0005(18) Te1 0.02261(18) 0.0275(2) 0.02625(17) 0.00281(15) -0.00130(13) -0.00139(15) I1 0.02453(19) 0.0360(2) 0.0415(2) 0.00232(17) 0.00288(15) -0.00475(16) I2 0.0399(2) 0.0652(3) 0.0404(2) 0.0184(2) -0.01461(17) -0.0064(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 C1 N1 1.287(5) . ? C1 C2 1.474(6) . ? C1 C12 1.507(6) . ? C2 C3 1.367(6) . ? C2 C11 1.424(6) . ? C3 C4 1.415(6) . ? C3 H3 0.9500 . ? C4 C5 1.360(7) . ? C4 H4 0.9500 . ? C5 C6 1.427(6) . ? C5 H5 0.9500 . ? C6 C11 1.401(6) . ? C6 C7 1.405(7) . ? C7 C8 1.378(6) . ? C7 H7 0.9500 . ? C8 C9 1.411(6) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.418(6) . ? C10 C12 1.468(6) . ? C12 N2 1.290(5) . ? C13 C14 1.398(6) . ? C13 C18 1.399(6) . ? C13 N1 1.434(5) . ? C14 C15 1.393(6) . ? C14 C19 1.504(6) . ? C15 C16 1.393(7) . ? C15 H15 0.9500 . ? C16 C17 1.389(7) . ? C16 C20 1.510(6) . ? C17 C18 1.391(6) . ? C17 H17 0.9500 . ? C18 C21 1.500(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.386(6) . ? C22 C23 1.394(6) . ? C22 N2 1.444(5) . ? C23 C24 1.403(6) . ? C23 C28 1.501(7) . ? C24 C25 1.371(6) . ? C24 H24 0.9500 . ? C25 C26 1.387(7) . ? C25 C29 1.514(6) . ? C26 C27 1.374(6) . ? C26 H26 0.9500 . ? C27 C30 1.514(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N1 Te1 2.363(3) . ? N2 Te1 2.384(4) . ? Te1 I1 2.8836(11) . ? Te1 I2 2.8897(8) . ? 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 N1 C1 C2 133.5(4) . . ? N1 C1 C12 119.2(4) . . ? C2 C1 C12 107.3(4) . . ? C3 C2 C11 119.7(4) . . ? C3 C2 C1 135.0(4) . . ? C11 C2 C1 105.2(4) . . ? C2 C3 C4 118.1(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 122.6(4) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C11 C6 C7 116.3(4) . . ? C11 C6 C5 115.8(4) . . ? C7 C6 C5 127.9(4) . . ? C8 C7 C6 120.8(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 122.4(5) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 118.0(4) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 119.3(4) . . ? C9 C10 C12 135.2(4) . . ? C11 C10 C12 105.5(4) . . ? C6 C11 C10 123.0(4) . . ? C6 C11 C2 122.6(4) . . ? C10 C11 C2 114.3(4) . . ? N2 C12 C10 133.5(4) . . ? N2 C12 C1 118.9(4) . . ? C10 C12 C1 107.6(4) . . ? C14 C13 C18 122.5(4) . . ? C14 C13 N1 118.7(4) . . ? C18 C13 N1 118.8(4) . . ? C15 C14 C13 117.1(4) . . ? C15 C14 C19 122.0(4) . . ? C13 C14 C19 120.9(4) . . ? C16 C15 C14 123.0(4) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C17 C16 C15 117.1(4) . . ? C17 C16 C20 122.3(5) . . ? C15 C16 C20 120.6(5) . . ? C16 C17 C18 123.1(5) . . ? C16 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C13 117.1(4) . . ? C17 C18 C21 122.4(4) . . ? C13 C18 C21 120.5(4) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 121.4(4) . . ? C27 C22 N2 120.8(4) . . ? C23 C22 N2 117.8(4) . . ? C22 C23 C24 117.7(4) . . ? C22 C23 C28 121.2(4) . . ? C24 C23 C28 121.2(4) . . ? C25 C24 C23 122.0(4) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 118.1(4) . . ? C24 C25 C29 121.0(4) . . ? C26 C25 C29 120.8(5) . . ? C27 C26 C25 122.4(4) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C26 C27 C22 118.4(4) . . ? C26 C27 C30 121.9(4) . . ? C22 C27 C30 119.7(4) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C1 N1 C13 118.5(4) . . ? C1 N1 Te1 115.7(3) . . ? C13 N1 Te1 125.6(3) . . ? C12 N2 C22 119.3(4) . . ? C12 N2 Te1 115.0(3) . . ? C22 N2 Te1 125.6(3) . . ? N1 Te1 N2 71.09(13) . . ? N1 Te1 I1 91.75(9) . . ? N2 Te1 I1 162.71(8) . . ? N1 Te1 I2 165.98(9) . . ? N2 Te1 I2 95.11(8) . . ? I1 Te1 I2 102.12(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 4.7(10) . . . . ? C12 C1 C2 C3 -177.5(5) . . . . ? N1 C1 C2 C11 -175.0(5) . . . . ? C12 C1 C2 C11 2.8(5) . . . . ? C11 C2 C3 C4 0.5(7) . . . . ? C1 C2 C3 C4 -179.2(5) . . . . ? C2 C3 C4 C5 2.2(7) . . . . ? C3 C4 C5 C6 -2.3(8) . . . . ? C4 C5 C6 C11 -0.2(7) . . . . ? C4 C5 C6 C7 -179.8(5) . . . . ? C11 C6 C7 C8 -2.1(7) . . . . ? C5 C6 C7 C8 177.5(5) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C7 C8 C9 C10 3.8(7) . . . . ? C8 C9 C10 C11 -4.1(6) . . . . ? C8 C9 C10 C12 175.2(5) . . . . ? C7 C6 C11 C10 1.7(7) . . . . ? C5 C6 C11 C10 -178.0(4) . . . . ? C7 C6 C11 C2 -177.4(4) . . . . ? C5 C6 C11 C2 2.9(7) . . . . ? C9 C10 C11 C6 1.5(7) . . . . ? C12 C10 C11 C6 -178.0(4) . . . . ? C9 C10 C11 C2 -179.4(4) . . . . ? C12 C10 C11 C2 1.2(5) . . . . ? C3 C2 C11 C6 -3.1(7) . . . . ? C1 C2 C11 C6 176.7(4) . . . . ? C3 C2 C11 C10 177.7(4) . . . . ? C1 C2 C11 C10 -2.5(5) . . . . ? C9 C10 C12 N2 2.0(9) . . . . ? C11 C10 C12 N2 -178.6(5) . . . . ? C9 C10 C12 C1 -178.7(5) . . . . ? C11 C10 C12 C1 0.7(5) . . . . ? N1 C1 C12 N2 -4.6(6) . . . . ? C2 C1 C12 N2 177.3(4) . . . . ? N1 C1 C12 C10 176.0(4) . . . . ? C2 C1 C12 C10 -2.2(5) . . . . ? C18 C13 C14 C15 -3.7(7) . . . . ? N1 C13 C14 C15 177.4(4) . . . . ? C18 C13 C14 C19 175.2(4) . . . . ? N1 C13 C14 C19 -3.6(7) . . . . ? C13 C14 C15 C16 1.1(7) . . . . ? C19 C14 C15 C16 -177.9(5) . . . . ? C14 C15 C16 C17 2.3(7) . . . . ? C14 C15 C16 C20 -176.7(5) . . . . ? C15 C16 C17 C18 -3.3(7) . . . . ? C20 C16 C17 C18 175.6(5) . . . . ? C16 C17 C18 C13 0.9(7) . . . . ? C16 C17 C18 C21 -178.9(5) . . . . ? C14 C13 C18 C17 2.8(7) . . . . ? N1 C13 C18 C17 -178.4(4) . . . . ? C14 C13 C18 C21 -177.4(4) . . . . ? N1 C13 C18 C21 1.4(7) . . . . ? C27 C22 C23 C24 1.0(7) . . . . ? N2 C22 C23 C24 -179.7(4) . . . . ? C27 C22 C23 C28 179.9(5) . . . . ? N2 C22 C23 C28 -0.8(7) . . . . ? C22 C23 C24 C25 1.0(7) . . . . ? C28 C23 C24 C25 -177.9(5) . . . . ? C23 C24 C25 C26 -1.5(7) . . . . ? C23 C24 C25 C29 179.6(4) . . . . ? C24 C25 C26 C27 0.1(7) . . . . ? C29 C25 C26 C27 179.0(4) . . . . ? C25 C26 C27 C22 1.7(7) . . . . ? C25 C26 C27 C30 -179.9(5) . . . . ? C23 C22 C27 C26 -2.3(7) . . . . ? N2 C22 C27 C26 178.4(4) . . . . ? C23 C22 C27 C30 179.3(4) . . . . ? N2 C22 C27 C30 0.0(7) . . . . ? C2 C1 N1 C13 -3.7(8) . . . . ? C12 C1 N1 C13 178.8(4) . . . . ? C2 C1 N1 Te1 -179.1(4) . . . . ? C12 C1 N1 Te1 3.4(5) . . . . ? C14 C13 N1 C1 -86.7(5) . . . . ? C18 C13 N1 C1 94.5(5) . . . . ? C14 C13 N1 Te1 88.2(5) . . . . ? C18 C13 N1 Te1 -90.6(5) . . . . ? C10 C12 N2 C22 1.4(7) . . . . ? C1 C12 N2 C22 -177.8(4) . . . . ? C10 C12 N2 Te1 -177.6(4) . . . . ? C1 C12 N2 Te1 3.2(5) . . . . ? C27 C22 N2 C12 -86.8(6) . . . . ? C23 C22 N2 C12 93.9(5) . . . . ? C27 C22 N2 Te1 92.1(4) . . . . ? C23 C22 N2 Te1 -87.2(5) . . . . ? C1 N1 Te1 N2 -1.3(3) . . . . ? C13 N1 Te1 N2 -176.3(4) . . . . ? C1 N1 Te1 I1 -179.2(3) . . . . ? C13 N1 Te1 I1 5.8(3) . . . . ? C1 N1 Te1 I2 9.1(6) . . . . ? C13 N1 Te1 I2 -165.9(3) . . . . ? C12 N2 Te1 N1 -1.1(3) . . . . ? C22 N2 Te1 N1 180.0(4) . . . . ? C12 N2 Te1 I1 6.0(6) . . . . ? C22 N2 Te1 I1 -172.9(2) . . . . ? C12 N2 Te1 I2 -178.6(3) . . . . ? C22 N2 Te1 I2 2.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.973 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.152 # Attachment 'CCDC614918.cif' data_squeeze3 _database_code_depnum_ccdc_archive 'CCDC 614918' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H42 Cl3 N3 Te' _chemical_formula_sum 'C33 H42 Cl3 N3 Te' _chemical_formula_weight 714.65 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 p21/c _symmetry_space_group_name_Hall -p2ybc 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 14.910(3) _cell_length_b 14.050(3) _cell_length_c 21.163(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.93(3) _cell_angle_gamma 90.00 _cell_volume 4352.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \f-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18001 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.1175 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9933 _reflns_number_gt 5918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of what appeared to be thf was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9933 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _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 C1 C 0.1172(3) 0.8933(3) 0.52231(19) 0.0391(11) Uani 1 1 d . . . H1A H 0.0777 0.9456 0.5032 0.059 Uiso 1 1 calc R . . H1B H 0.1662 0.9185 0.5557 0.059 Uiso 1 1 calc R . . H1C H 0.0811 0.8471 0.5415 0.059 Uiso 1 1 calc R . . C2 C 0.1579(3) 0.8455(3) 0.47128(18) 0.0251(9) Uani 1 1 d . . . C3 C 0.2286(3) 0.7693(3) 0.49202(18) 0.0284(9) Uani 1 1 d . . . C4 C 0.2481(3) 0.7366(3) 0.55476(19) 0.0362(10) Uani 1 1 d . . . H4 H 0.2182 0.7632 0.5865 0.043 Uiso 1 1 calc R . . C5 C 0.3119(3) 0.6643(3) 0.57083(19) 0.0378(11) Uani 1 1 d . . . H5 H 0.3253 0.6405 0.6136 0.045 Uiso 1 1 calc R . . C6 C 0.3555(3) 0.6275(3) 0.52500(19) 0.0324(10) Uani 1 1 d . . . H6 H 0.4004 0.5792 0.5355 0.039 Uiso 1 1 calc R . . C7 C 0.3323(3) 0.6627(2) 0.46247(18) 0.0252(9) Uani 1 1 d . . . C8 C 0.3766(3) 0.6261(3) 0.41027(18) 0.0273(9) Uani 1 1 d . . . C9 C 0.3356(3) 0.6541(3) 0.34263(18) 0.0312(10) Uani 1 1 d . . . H9A H 0.3010 0.5995 0.3207 0.037 Uiso 1 1 calc R . . H9B H 0.3853 0.6694 0.3192 0.037 Uiso 1 1 calc R . . C10 C 0.0722(3) 0.9308(3) 0.38372(18) 0.0279(9) Uani 1 1 d . . . C11 C -0.0202(3) 0.9056(3) 0.37386(19) 0.0342(10) Uani 1 1 d . . . C12 C -0.0835(3) 0.9721(4) 0.3449(2) 0.0458(12) Uani 1 1 d . . . H12 H -0.1467 0.9569 0.3380 0.055 Uiso 1 1 calc R . . C13 C -0.0570(4) 1.0593(4) 0.3258(2) 0.0560(15) Uani 1 1 d . . . H13 H -0.1019 1.1041 0.3070 0.067 Uiso 1 1 calc R . . C14 C 0.0348(4) 1.0825(3) 0.3337(2) 0.0501(13) Uani 1 1 d . . . H14 H 0.0524 1.1427 0.3197 0.060 Uiso 1 1 calc R . . C15 C 0.1014(3) 1.0179(3) 0.3621(2) 0.0365(10) Uani 1 1 d . . . C16 C -0.0529(3) 0.8089(3) 0.3930(2) 0.0458(12) Uani 1 1 d . . . H16 H 0.0022 0.7705 0.4117 0.055 Uiso 1 1 calc R . . C17 C -0.1044(4) 0.7557(4) 0.3344(3) 0.0625(15) Uani 1 1 d . . . H17A H -0.1571 0.7935 0.3138 0.094 Uiso 1 1 calc R . . H17B H -0.1255 0.6943 0.3480 0.094 Uiso 1 1 calc R . . H17C H -0.0637 0.7451 0.3038 0.094 Uiso 1 1 calc R . . C18 C -0.1117(4) 0.8194(4) 0.4449(2) 0.0600(14) Uani 1 1 d . . . H18A H -0.0765 0.8522 0.4824 0.090 Uiso 1 1 calc R . . H18B H -0.1295 0.7561 0.4578 0.090 Uiso 1 1 calc R . . H18C H -0.1666 0.8563 0.4276 0.090 Uiso 1 1 calc R . . C19 C 0.2018(3) 1.0439(3) 0.3709(2) 0.0434(12) Uani 1 1 d . . . H19 H 0.2374 0.9845 0.3840 0.052 Uiso 1 1 calc R . . C20 C 0.2289(4) 1.0786(5) 0.3090(3) 0.0765(17) Uani 1 1 d . . . H20A H 0.2182 1.0278 0.2766 0.115 Uiso 1 1 calc R . . H20B H 0.2938 1.0958 0.3175 0.115 Uiso 1 1 calc R . . H20C H 0.1922 1.1344 0.2929 0.115 Uiso 1 1 calc R . . C21 C 0.2298(4) 1.1164(4) 0.4252(3) 0.0670(16) Uani 1 1 d . . . H21A H 0.1941 1.1748 0.4151 0.101 Uiso 1 1 calc R . . H21B H 0.2950 1.1310 0.4295 0.101 Uiso 1 1 calc R . . H21C H 0.2183 1.0896 0.4657 0.101 Uiso 1 1 calc R . . C22 C 0.4911(3) 0.5382(3) 0.37613(19) 0.0295(9) Uani 1 1 d . . . C23 C 0.4562(3) 0.4589(3) 0.3408(2) 0.0371(11) Uani 1 1 d . . . C24 C 0.5061(3) 0.4254(3) 0.2943(2) 0.0483(13) Uani 1 1 d . . . H24 H 0.4852 0.3707 0.2694 0.058 Uiso 1 1 calc R . . C25 C 0.5846(3) 0.4711(4) 0.2845(2) 0.0490(13) Uani 1 1 d . . . H25 H 0.6164 0.4485 0.2527 0.059 Uiso 1 1 calc R . . C26 C 0.6164(3) 0.5490(3) 0.3209(2) 0.0464(12) Uani 1 1 d . . . H26 H 0.6705 0.5796 0.3139 0.056 Uiso 1 1 calc R . . C27 C 0.5720(3) 0.5838(3) 0.3671(2) 0.0354(10) Uani 1 1 d . . . C28 C 0.3728(3) 0.4066(3) 0.3540(2) 0.0474(12) Uani 1 1 d . . . H28 H 0.3391 0.4519 0.3775 0.057 Uiso 1 1 calc R . . C29 C 0.3066(5) 0.3767(6) 0.2931(3) 0.116(3) Uani 1 1 d . . . H29A H 0.2967 0.4302 0.2629 0.174 Uiso 1 1 calc R . . H29B H 0.2483 0.3578 0.3043 0.174 Uiso 1 1 calc R . . H29C H 0.3324 0.3228 0.2732 0.174 Uiso 1 1 calc R . . C30 C 0.4004(5) 0.3225(4) 0.3984(3) 0.099(2) Uani 1 1 d . . . H30A H 0.4355 0.2771 0.3776 0.148 Uiso 1 1 calc R . . H30B H 0.3456 0.2912 0.4076 0.148 Uiso 1 1 calc R . . H30C H 0.4381 0.3449 0.4387 0.148 Uiso 1 1 calc R . . C31 C 0.6112(3) 0.6684(3) 0.4076(2) 0.0502(13) Uani 1 1 d . . . H31 H 0.5654 0.6886 0.4339 0.060 Uiso 1 1 calc R . . C32 C 0.6310(4) 0.7538(3) 0.3681(3) 0.0633(16) Uani 1 1 d . . . H32A H 0.6786 0.7370 0.3439 0.095 Uiso 1 1 calc R . . H32B H 0.6519 0.8072 0.3970 0.095 Uiso 1 1 calc R . . H32C H 0.5752 0.7721 0.3381 0.095 Uiso 1 1 calc R . . C33 C 0.6987(4) 0.6395(4) 0.4540(3) 0.0760(18) Uani 1 1 d . . . H33A H 0.6839 0.5937 0.4854 0.114 Uiso 1 1 calc R . . H33B H 0.7270 0.6961 0.4766 0.114 Uiso 1 1 calc R . . H33C H 0.7413 0.6103 0.4297 0.114 Uiso 1 1 calc R . . N1 N 0.1409(2) 0.8651(2) 0.41153(15) 0.0252(7) Uani 1 1 d . . . N2 N 0.2698(2) 0.7319(2) 0.44673(15) 0.0265(7) Uani 1 1 d . . . N3 N 0.4469(2) 0.5733(2) 0.42571(15) 0.0289(8) Uani 1 1 d . . . Cl1 Cl 0.25021(8) 0.76718(8) 0.21987(5) 0.0390(3) Uani 1 1 d . . . Cl2 Cl 0.39510(8) 0.86404(8) 0.37644(5) 0.0435(3) Uani 1 1 d . . . Cl3 Cl 0.12042(8) 0.65970(8) 0.33001(6) 0.0475(3) Uani 1 1 d . . . Te1 Te 0.246973(17) 0.773320(17) 0.338680(11) 0.02447(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.050(3) 0.029(2) -0.005(2) 0.007(2) 0.013(2) C2 0.018(2) 0.029(2) 0.028(2) -0.0024(17) 0.0030(17) -0.0010(16) C3 0.029(2) 0.031(2) 0.025(2) 0.0007(18) 0.0066(18) -0.0042(19) C4 0.042(3) 0.044(2) 0.023(2) -0.0013(19) 0.0063(19) 0.006(2) C5 0.037(3) 0.051(3) 0.024(2) 0.014(2) 0.004(2) 0.012(2) C6 0.028(2) 0.037(2) 0.030(2) 0.0042(19) 0.0015(19) 0.0037(19) C7 0.023(2) 0.025(2) 0.026(2) -0.0013(16) 0.0031(17) -0.0026(17) C8 0.032(2) 0.024(2) 0.025(2) 0.0056(17) 0.0047(18) -0.0041(18) C9 0.037(3) 0.034(2) 0.022(2) 0.0024(17) 0.0049(18) 0.0146(19) C10 0.028(2) 0.031(2) 0.024(2) 0.0002(17) 0.0043(17) 0.0120(18) C11 0.028(2) 0.045(3) 0.029(2) -0.0013(19) 0.0045(19) 0.008(2) C12 0.036(3) 0.064(3) 0.036(3) 0.000(2) 0.004(2) 0.014(2) C13 0.057(4) 0.077(4) 0.035(3) 0.013(3) 0.011(2) 0.040(3) C14 0.064(4) 0.046(3) 0.044(3) 0.017(2) 0.018(3) 0.024(3) C15 0.039(3) 0.042(2) 0.031(2) 0.0035(19) 0.012(2) 0.012(2) C16 0.025(2) 0.059(3) 0.052(3) -0.003(2) 0.003(2) 0.002(2) C17 0.040(3) 0.071(4) 0.072(4) -0.017(3) 0.001(3) -0.011(3) C18 0.048(3) 0.077(4) 0.058(3) 0.001(3) 0.019(3) -0.014(3) C19 0.053(3) 0.034(2) 0.047(3) 0.009(2) 0.019(2) 0.010(2) C20 0.071(4) 0.109(5) 0.057(4) 0.014(3) 0.032(3) -0.001(4) C21 0.060(4) 0.064(3) 0.079(4) -0.008(3) 0.018(3) 0.001(3) C22 0.029(2) 0.032(2) 0.028(2) 0.0037(18) 0.0063(19) 0.0116(18) C23 0.035(3) 0.037(2) 0.036(3) -0.002(2) -0.002(2) 0.012(2) C24 0.052(3) 0.050(3) 0.038(3) -0.003(2) -0.004(2) 0.018(3) C25 0.045(3) 0.066(3) 0.038(3) 0.013(2) 0.011(2) 0.028(3) C26 0.043(3) 0.051(3) 0.047(3) 0.006(2) 0.014(2) 0.006(2) C27 0.032(3) 0.042(2) 0.033(2) 0.007(2) 0.007(2) 0.009(2) C28 0.049(3) 0.036(2) 0.053(3) -0.011(2) 0.000(2) -0.005(2) C29 0.078(5) 0.181(8) 0.077(5) -0.017(5) -0.016(4) -0.072(5) C30 0.079(5) 0.084(4) 0.129(6) 0.058(4) 0.008(4) -0.010(4) C31 0.039(3) 0.049(3) 0.067(3) 0.001(3) 0.019(3) -0.005(2) C32 0.043(3) 0.053(3) 0.098(5) 0.015(3) 0.020(3) 0.001(2) C33 0.073(4) 0.066(4) 0.079(4) 0.007(3) -0.011(3) -0.027(3) N1 0.0213(18) 0.0293(17) 0.0248(18) 0.0016(14) 0.0036(14) 0.0043(14) N2 0.0261(18) 0.0296(17) 0.0229(18) 0.0004(15) 0.0023(14) -0.0016(15) N3 0.028(2) 0.0251(17) 0.034(2) 0.0006(15) 0.0067(16) 0.0011(15) Cl1 0.0463(7) 0.0498(6) 0.0219(5) 0.0020(5) 0.0087(5) 0.0045(5) Cl2 0.0369(7) 0.0509(7) 0.0423(7) 0.0009(5) 0.0062(5) -0.0126(5) Cl3 0.0448(7) 0.0531(7) 0.0460(7) -0.0162(5) 0.0121(6) -0.0199(6) Te1 0.02537(15) 0.02658(15) 0.02114(14) 0.00116(11) 0.00361(10) 0.00254(11) _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 C1 C2 1.495(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.272(5) . ? C2 C3 1.508(5) . ? C3 N2 1.340(5) . ? C3 C4 1.383(5) . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.367(6) . ? C5 H5 0.9500 . ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 N2 1.344(5) . ? C7 C8 1.482(5) . ? C8 N3 1.276(5) . ? C8 C9 1.498(5) . ? C9 Te1 2.126(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.399(6) . ? C10 C15 1.405(6) . ? C10 N1 1.421(5) . ? C11 C12 1.386(6) . ? C11 C16 1.523(6) . ? C12 C13 1.371(7) . ? C12 H12 0.9500 . ? C13 C14 1.386(7) . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C14 H14 0.9500 . ? C15 C19 1.518(6) . ? C16 C17 1.526(6) . ? C16 C18 1.536(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.522(7) . ? C19 C21 1.533(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.388(6) . ? C22 C27 1.411(6) . ? C22 N3 1.428(5) . ? C23 C24 1.422(6) . ? C23 C28 1.514(6) . ? C24 C25 1.385(7) . ? C24 H24 0.9500 . ? C25 C26 1.369(7) . ? C25 H25 0.9500 . ? C26 C27 1.371(6) . ? C26 H26 0.9500 . ? C27 C31 1.517(6) . ? C28 C30 1.518(7) . ? C28 C29 1.525(7) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.522(6) . ? C31 C33 1.532(7) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Te1 2.732(3) . ? N2 Te1 2.321(3) . ? Cl1 Te1 2.5255(11) . ? Cl2 Te1 2.5440(12) . ? Cl3 Te1 2.4518(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 126.1(3) . . ? N1 C2 C3 116.1(3) . . ? C1 C2 C3 117.7(3) . . ? N2 C3 C4 121.0(4) . . ? N2 C3 C2 117.4(3) . . ? C4 C3 C2 121.6(4) . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 118.3(4) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? N2 C7 C6 121.8(4) . . ? N2 C7 C8 116.9(3) . . ? C6 C7 C8 121.3(3) . . ? N3 C8 C7 118.1(3) . . ? N3 C8 C9 124.3(4) . . ? C7 C8 C9 117.6(3) . . ? C8 C9 Te1 112.4(3) . . ? C8 C9 H9A 109.1 . . ? Te1 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? Te1 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C15 122.0(4) . . ? C11 C10 N1 120.7(4) . . ? C15 C10 N1 117.1(4) . . ? C12 C11 C10 117.6(4) . . ? C12 C11 C16 119.6(4) . . ? C10 C11 C16 122.8(4) . . ? C13 C12 C11 121.5(5) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 117.8(4) . . ? C14 C15 C19 120.1(4) . . ? C10 C15 C19 122.0(4) . . ? C11 C16 C17 110.9(4) . . ? C11 C16 C18 111.1(4) . . ? C17 C16 C18 111.1(4) . . ? C11 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 112.8(4) . . ? C15 C19 C21 112.0(4) . . ? C20 C19 C21 110.7(4) . . ? C15 C19 H19 107.0 . . ? C20 C19 H19 107.0 . . ? C21 C19 H19 107.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 122.3(4) . . ? C23 C22 N3 119.7(4) . . ? C27 C22 N3 117.9(4) . . ? C22 C23 C24 116.5(4) . . ? C22 C23 C28 121.9(4) . . ? C24 C23 C28 121.5(4) . . ? C25 C24 C23 121.2(4) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C26 C25 C24 120.0(5) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 121.5(5) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C22 118.4(4) . . ? C26 C27 C31 119.8(4) . . ? C22 C27 C31 121.8(4) . . ? C23 C28 C30 110.8(4) . . ? C23 C28 C29 113.6(5) . . ? C30 C28 C29 111.4(5) . . ? C23 C28 H28 106.9 . . ? C30 C28 H28 106.9 . . ? C29 C28 H28 106.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 C32 113.6(4) . . ? C27 C31 C33 110.2(4) . . ? C32 C31 C33 109.3(4) . . ? C27 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C33 C31 H31 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C2 N1 C10 123.0(3) . . ? C2 N1 Te1 115.6(2) . . ? C10 N1 Te1 121.5(2) . . ? C3 N2 C7 119.8(3) . . ? C3 N2 Te1 127.2(3) . . ? C7 N2 Te1 113.0(2) . . ? C8 N3 C22 118.9(3) . . ? C9 Te1 N2 77.87(13) . . ? C9 Te1 Cl3 87.34(12) . . ? N2 Te1 Cl3 82.96(8) . . ? C9 Te1 Cl1 83.29(11) . . ? N2 Te1 Cl1 160.97(8) . . ? Cl3 Te1 Cl1 93.61(4) . . ? C9 Te1 Cl2 83.48(12) . . ? N2 Te1 Cl2 81.94(9) . . ? Cl3 Te1 Cl2 163.68(4) . . ? Cl1 Te1 Cl2 98.65(5) . . ? C9 Te1 N1 140.52(12) . . ? N2 Te1 N1 63.56(10) . . ? Cl3 Te1 N1 80.22(7) . . ? Cl1 Te1 N1 134.45(7) . . ? Cl2 Te1 N1 98.46(7) . . ? 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 N1 C2 C3 N2 2.7(5) . . . . ? C1 C2 C3 N2 -175.1(3) . . . . ? N1 C2 C3 C4 -175.1(4) . . . . ? C1 C2 C3 C4 7.1(6) . . . . ? N2 C3 C4 C5 0.5(6) . . . . ? C2 C3 C4 C5 178.2(4) . . . . ? C3 C4 C5 C6 1.0(7) . . . . ? C4 C5 C6 C7 -1.6(6) . . . . ? C5 C6 C7 N2 0.8(6) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? N2 C7 C8 N3 167.7(3) . . . . ? C6 C7 C8 N3 -11.6(5) . . . . ? N2 C7 C8 C9 -12.1(5) . . . . ? C6 C7 C8 C9 168.7(3) . . . . ? N3 C8 C9 Te1 -162.5(3) . . . . ? C7 C8 C9 Te1 17.3(4) . . . . ? C15 C10 C11 C12 -3.5(6) . . . . ? N1 C10 C11 C12 -178.2(4) . . . . ? C15 C10 C11 C16 175.9(4) . . . . ? N1 C10 C11 C16 1.2(6) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C16 C11 C12 C13 -178.8(4) . . . . ? C11 C12 C13 C14 1.6(7) . . . . ? C12 C13 C14 C15 -1.0(7) . . . . ? C13 C14 C15 C10 -1.8(7) . . . . ? C13 C14 C15 C19 -179.7(4) . . . . ? C11 C10 C15 C14 4.1(6) . . . . ? N1 C10 C15 C14 179.0(4) . . . . ? C11 C10 C15 C19 -178.0(4) . . . . ? N1 C10 C15 C19 -3.1(6) . . . . ? C12 C11 C16 C17 60.4(5) . . . . ? C10 C11 C16 C17 -119.0(5) . . . . ? C12 C11 C16 C18 -63.8(5) . . . . ? C10 C11 C16 C18 116.8(5) . . . . ? C14 C15 C19 C20 -52.1(6) . . . . ? C10 C15 C19 C20 130.1(5) . . . . ? C14 C15 C19 C21 73.6(5) . . . . ? C10 C15 C19 C21 -104.2(5) . . . . ? C27 C22 C23 C24 -0.2(6) . . . . ? N3 C22 C23 C24 -177.2(3) . . . . ? C27 C22 C23 C28 175.9(4) . . . . ? N3 C22 C23 C28 -1.1(6) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C28 C23 C24 C25 -177.1(4) . . . . ? C23 C24 C25 C26 1.2(7) . . . . ? C24 C25 C26 C27 -0.3(7) . . . . ? C25 C26 C27 C22 -0.9(6) . . . . ? C25 C26 C27 C31 178.1(4) . . . . ? C23 C22 C27 C26 1.1(6) . . . . ? N3 C22 C27 C26 178.1(4) . . . . ? C23 C22 C27 C31 -177.9(4) . . . . ? N3 C22 C27 C31 -0.8(6) . . . . ? C22 C23 C28 C30 -95.3(6) . . . . ? C24 C23 C28 C30 80.6(6) . . . . ? C22 C23 C28 C29 138.3(5) . . . . ? C24 C23 C28 C29 -45.7(6) . . . . ? C26 C27 C31 C32 52.8(6) . . . . ? C22 C27 C31 C32 -128.2(4) . . . . ? C26 C27 C31 C33 -70.1(6) . . . . ? C22 C27 C31 C33 108.8(5) . . . . ? C1 C2 N1 C10 -6.5(6) . . . . ? C3 C2 N1 C10 175.9(3) . . . . ? C1 C2 N1 Te1 173.0(3) . . . . ? C3 C2 N1 Te1 -4.6(4) . . . . ? C11 C10 N1 C2 -75.6(5) . . . . ? C15 C10 N1 C2 109.4(4) . . . . ? C11 C10 N1 Te1 104.9(4) . . . . ? C15 C10 N1 Te1 -70.0(4) . . . . ? C4 C3 N2 C7 -1.2(6) . . . . ? C2 C3 N2 C7 -179.0(3) . . . . ? C4 C3 N2 Te1 179.1(3) . . . . ? C2 C3 N2 Te1 1.3(5) . . . . ? C6 C7 N2 C3 0.6(6) . . . . ? C8 C7 N2 C3 -178.7(3) . . . . ? C6 C7 N2 Te1 -179.7(3) . . . . ? C8 C7 N2 Te1 1.0(4) . . . . ? C7 C8 N3 C22 -179.4(3) . . . . ? C9 C8 N3 C22 0.4(5) . . . . ? C23 C22 N3 C8 -81.1(5) . . . . ? C27 C22 N3 C8 101.8(4) . . . . ? C8 C9 Te1 N2 -12.0(3) . . . . ? C8 C9 Te1 Cl3 -95.4(3) . . . . ? C8 C9 Te1 Cl1 170.6(3) . . . . ? C8 C9 Te1 Cl2 71.1(3) . . . . ? C8 C9 Te1 N1 -24.3(4) . . . . ? C3 N2 Te1 C9 -173.9(3) . . . . ? C7 N2 Te1 C9 6.5(3) . . . . ? C3 N2 Te1 Cl3 -85.1(3) . . . . ? C7 N2 Te1 Cl3 95.2(2) . . . . ? C3 N2 Te1 Cl1 -165.7(2) . . . . ? C7 N2 Te1 Cl1 14.6(4) . . . . ? C3 N2 Te1 Cl2 101.1(3) . . . . ? C7 N2 Te1 Cl2 -78.6(2) . . . . ? C3 N2 Te1 N1 -2.5(3) . . . . ? C7 N2 Te1 N1 177.8(3) . . . . ? C2 N1 Te1 C9 17.3(4) . . . . ? C10 N1 Te1 C9 -163.2(3) . . . . ? C2 N1 Te1 N2 3.8(2) . . . . ? C10 N1 Te1 N2 -176.7(3) . . . . ? C2 N1 Te1 Cl3 90.8(3) . . . . ? C10 N1 Te1 Cl3 -89.7(3) . . . . ? C2 N1 Te1 Cl1 176.2(2) . . . . ? C10 N1 Te1 Cl1 -4.3(3) . . . . ? C2 N1 Te1 Cl2 -72.7(3) . . . . ? C10 N1 Te1 Cl2 106.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.392 _refine_diff_density_min -1.470 _refine_diff_density_rms 0.115