data_added_by_encifer _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Jens Beckmann' _publ_contact_author_address ;Institut f\"ur Chemie und Biochemie, Freie Universit\"at Berlin, Fabeckstr. 34-36, 14195 Berlin, Germany ; _publ_contact_author_email beckmann@chemie.fu-berlin.de _publ_contact_author_phone '+49 (0)30-838-54697' _publ_contact_author_fax '+49 (0)30-838-52440' loop_ _publ_author_name _publ_author_address 'Beckmann, Jens' ;Institut f\"ur Chemie und Biochemie, Freie Universit\"at Berlin, Fabeckstr. 34-36, 14195 Berlin, Germany ; 'Heitz, Stephan' ;Institut f\"ur Chemie und Biochemie, Freie Universit\"at Berlin, Fabeckstr. 34-36, 14195 Berlin, Germany ; 'Hesse, Malte' ;Institut f\"ur Chemie und Biochemie, Freie Universit\"at Berlin, Fabeckstr. 34-36, 14195 Berlin, Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H29 Cl3 Te1' _chemical_formula_weight 479.36 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' 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1127(19) _cell_length_b 10.224(2) _cell_length_c 11.903(2) _cell_angle_alpha 105.140(5) _cell_angle_beta 108.065(4) _cell_angle_gamma 107.293(4) _cell_volume 1029.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .26 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type 'empiric' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans with .3 deg in omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12766 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.56 _reflns_number_total 6130 _reflns_number_gt 5511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0658P)^2^+2.2689P] 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_number_reflns 6130 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.07634(2) 0.19492(2) 0.707387(18) 0.01913(7) Uani 1 1 d . . . Cl1 Cl 0.02404(10) 0.18223(9) 0.48405(8) 0.02849(17) Uani 1 1 d . . . Cl3 Cl -0.17761(9) 0.15956(10) 0.65073(10) 0.03262(19) Uani 1 1 d . . . Cl2 Cl 0.08286(12) 0.21597(12) 0.92190(9) 0.03502(19) Uani 1 1 d . . . C20 C 0.0725(3) 0.5763(3) 0.7739(3) 0.0185(5) Uani 1 1 d . . . C12 C 0.3168(3) 0.6587(4) 0.7493(3) 0.0212(6) Uani 1 1 d . . . H12 H 0.2981 0.7420 0.7470 0.025 Uiso 1 1 calc R . . C30 C 0.3691(4) 0.1558(4) 0.6551(4) 0.0305(7) Uani 1 1 d . . . H30A H 0.3848 0.1874 0.5893 0.046 Uiso 1 1 calc R . . H30B H 0.2616 0.1066 0.6306 0.046 Uiso 1 1 calc R . . H30C H 0.4160 0.0884 0.6662 0.046 Uiso 1 1 calc R . . C23 C -0.0623(3) 0.5063(4) 0.6403(3) 0.0249(6) Uani 1 1 d . . . H23A H -0.0296 0.5432 0.5828 0.037 Uiso 1 1 calc R . . H23B H -0.1442 0.5319 0.6471 0.037 Uiso 1 1 calc R . . H23C H -0.0968 0.4001 0.6080 0.037 Uiso 1 1 calc R . . C10 C 0.2414(3) 0.4195(3) 0.7626(3) 0.0178(5) Uani 1 1 d . . . C22 C 0.1122(4) 0.7453(4) 0.8267(4) 0.0275(7) Uani 1 1 d . . . H22A H 0.1417 0.7875 0.7705 0.041 Uiso 1 1 calc R . . H22B H 0.1950 0.7927 0.9107 0.041 Uiso 1 1 calc R . . H22C H 0.0245 0.7603 0.8317 0.041 Uiso 1 1 calc R . . C13 C 0.4493(3) 0.6534(3) 0.7398(3) 0.0202(5) Uani 1 1 d . . . C15 C 0.3824(3) 0.4147(3) 0.7653(3) 0.0183(5) Uani 1 1 d . . . C14 C 0.4807(3) 0.5335(4) 0.7525(3) 0.0213(6) Uani 1 1 d . . . H14 H 0.5721 0.5319 0.7525 0.026 Uiso 1 1 calc R . . C24 C 0.5563(3) 0.7801(4) 0.7222(3) 0.0244(6) Uani 1 1 d . . . C21 C 0.0276(4) 0.5219(4) 0.8703(3) 0.0241(6) Uani 1 1 d . . . H21A H 0.1142 0.5679 0.9520 0.036 Uiso 1 1 calc R . . H21B H -0.0061 0.4158 0.8403 0.036 Uiso 1 1 calc R . . H21C H -0.0536 0.5476 0.8791 0.036 Uiso 1 1 calc R . . C11 C 0.2104(3) 0.5467(3) 0.7620(3) 0.0181(5) Uani 1 1 d . . . C29 C 0.6149(4) 0.3510(5) 0.8197(5) 0.0390(10) Uani 1 1 d . . . H29A H 0.6673 0.4370 0.8988 0.059 Uiso 1 1 calc R . . H29B H 0.6361 0.3776 0.7536 0.059 Uiso 1 1 calc R . . H29C H 0.6492 0.2752 0.8304 0.059 Uiso 1 1 calc R . . C28 C 0.4407(3) 0.2918(3) 0.7815(3) 0.0216(6) Uani 1 1 d . . . C27 C 0.4652(4) 0.8001(5) 0.6030(4) 0.0331(8) Uani 1 1 d . . . H27A H 0.5315 0.8796 0.5914 0.050 Uiso 1 1 calc R . . H27B H 0.3839 0.8237 0.6143 0.050 Uiso 1 1 calc R . . H27C H 0.4233 0.7097 0.5289 0.050 Uiso 1 1 calc R . . C31 C 0.4191(5) 0.2468(5) 0.8901(4) 0.0359(8) Uani 1 1 d . . . H31A H 0.4651 0.3340 0.9677 0.054 Uiso 1 1 calc R . . H31B H 0.4666 0.1801 0.9028 0.054 Uiso 1 1 calc R . . H31C H 0.3121 0.1982 0.8676 0.054 Uiso 1 1 calc R . . C25 C 0.6899(5) 0.7503(5) 0.7047(5) 0.0419(10) Uani 1 1 d . . . H25A H 0.7536 0.8327 0.6942 0.063 Uiso 1 1 calc R . . H25B H 0.6512 0.6613 0.6300 0.063 Uiso 1 1 calc R . . H25C H 0.7487 0.7384 0.7789 0.063 Uiso 1 1 calc R . . C26 C 0.6221(5) 0.9241(4) 0.8415(4) 0.0383(9) Uani 1 1 d . . . H26A H 0.6894 1.0041 0.8311 0.057 Uiso 1 1 calc R . . H26B H 0.6778 0.9107 0.9160 0.057 Uiso 1 1 calc R . . H26C H 0.5403 0.9473 0.8518 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.02077(10) 0.01831(11) 0.01944(11) 0.00918(8) 0.00871(7) 0.00764(7) Cl1 0.0365(4) 0.0242(4) 0.0197(3) 0.0095(3) 0.0082(3) 0.0089(3) Cl3 0.0201(3) 0.0332(4) 0.0415(5) 0.0162(4) 0.0113(3) 0.0074(3) Cl2 0.0492(5) 0.0444(5) 0.0299(4) 0.0236(4) 0.0248(4) 0.0263(4) C20 0.0179(11) 0.0215(14) 0.0213(13) 0.0100(11) 0.0100(10) 0.0116(10) C12 0.0209(12) 0.0220(14) 0.0274(15) 0.0127(12) 0.0127(11) 0.0122(11) C30 0.0300(15) 0.0255(16) 0.0355(18) 0.0054(14) 0.0151(14) 0.0149(13) C23 0.0207(12) 0.0315(17) 0.0235(14) 0.0120(13) 0.0072(11) 0.0131(12) C10 0.0172(11) 0.0197(13) 0.0180(12) 0.0076(11) 0.0077(10) 0.0093(10) C22 0.0282(14) 0.0253(16) 0.0353(18) 0.0103(14) 0.0175(13) 0.0161(13) C13 0.0186(11) 0.0221(14) 0.0233(14) 0.0111(12) 0.0103(11) 0.0095(10) C15 0.0174(11) 0.0204(13) 0.0187(13) 0.0077(11) 0.0067(10) 0.0106(10) C14 0.0175(11) 0.0229(14) 0.0260(14) 0.0094(12) 0.0100(11) 0.0108(11) C24 0.0202(12) 0.0248(15) 0.0337(17) 0.0157(13) 0.0145(12) 0.0093(11) C21 0.0245(13) 0.0334(17) 0.0228(14) 0.0130(13) 0.0148(12) 0.0157(12) C11 0.0183(11) 0.0214(13) 0.0193(13) 0.0091(11) 0.0095(10) 0.0115(10) C29 0.0227(15) 0.0322(19) 0.062(3) 0.0202(19) 0.0106(16) 0.0172(14) C28 0.0216(12) 0.0209(14) 0.0264(15) 0.0104(12) 0.0095(11) 0.0136(11) C27 0.0314(16) 0.038(2) 0.0364(19) 0.0231(17) 0.0165(15) 0.0127(15) C31 0.046(2) 0.044(2) 0.0331(19) 0.0245(17) 0.0164(16) 0.0311(18) C25 0.0319(17) 0.047(2) 0.074(3) 0.039(2) 0.036(2) 0.0229(17) C26 0.0357(18) 0.0286(18) 0.042(2) 0.0125(16) 0.0163(16) 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 C10 2.178(3) . ? Te1 Cl3 2.3296(9) . ? Te1 Cl2 2.4841(10) . ? Te1 Cl1 2.5041(10) . ? C20 C21 1.530(4) . ? C20 C23 1.542(4) . ? C20 C22 1.551(4) . ? C20 C11 1.552(4) . ? C12 C13 1.395(4) . ? C12 C11 1.397(4) . ? C30 C28 1.534(5) . ? C10 C11 1.426(4) . ? C10 C15 1.431(4) . ? C13 C14 1.387(4) . ? C13 C24 1.530(4) . ? C15 C14 1.400(4) . ? C15 C28 1.569(4) . ? C24 C25 1.533(5) . ? C24 C27 1.535(5) . ? C24 C26 1.539(5) . ? C29 C28 1.549(5) . ? C28 C31 1.534(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Te1 Cl3 116.82(7) . . ? C10 Te1 Cl2 98.20(8) . . ? Cl3 Te1 Cl2 84.76(3) . . ? C10 Te1 Cl1 83.71(8) . . ? Cl3 Te1 Cl1 84.68(3) . . ? Cl2 Te1 Cl1 168.96(3) . . ? C21 C20 C23 112.0(3) . . ? C21 C20 C22 104.7(3) . . ? C23 C20 C22 107.0(2) . . ? C21 C20 C11 111.8(2) . . ? C23 C20 C11 109.8(2) . . ? C22 C20 C11 111.3(2) . . ? C13 C12 C11 124.0(3) . . ? C11 C10 C15 121.6(3) . . ? C11 C10 Te1 127.1(2) . . ? C15 C10 Te1 109.1(2) . . ? C14 C13 C12 117.1(3) . . ? C14 C13 C24 122.9(3) . . ? C12 C13 C24 119.9(3) . . ? C14 C15 C10 116.6(3) . . ? C14 C15 C28 115.7(2) . . ? C10 C15 C28 127.7(3) . . ? C13 C14 C15 123.7(3) . . ? C13 C24 C25 112.6(3) . . ? C13 C24 C27 109.0(3) . . ? C25 C24 C27 108.5(3) . . ? C13 C24 C26 109.0(3) . . ? C25 C24 C26 108.1(3) . . ? C27 C24 C26 109.7(3) . . ? C12 C11 C10 116.4(3) . . ? C12 C11 C20 115.7(2) . . ? C10 C11 C20 127.9(3) . . ? C30 C28 C31 111.4(3) . . ? C30 C28 C29 105.0(3) . . ? C31 C28 C29 105.1(3) . . ? C30 C28 C15 111.9(3) . . ? C31 C28 C15 112.5(3) . . ? C29 C28 C15 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 3.011 _refine_diff_density_min -3.266 _refine_diff_density_rms 0.148