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 Cl Te' _chemical_formula_weight 408.46 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 'Orthorhombic' _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 5.9188(12) _cell_length_b 15.599(3) _cell_length_c 20.123(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1857.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'blue' _exptl_crystal_size_max .23 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.736 _exptl_absorpt_correction_type 'empiric' _exptl_absorpt_correction_T_min 0.87 _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 23197 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.53 _reflns_number_total 5691 _reflns_number_gt 4718 _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^)+(0.0368P)^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 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 -0.03(2) _refine_ls_number_reflns 5691 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 -0.01939(4) 0.302855(11) 0.834832(11) 0.02870(7) Uani 1 1 d . . . C28 C -0.0079(6) 0.41718(18) 0.98270(14) 0.0256(6) Uani 1 1 d . . . C20 C 0.0323(6) 0.47584(17) 0.72667(15) 0.0225(6) Uani 1 1 d . . . C24 C 0.4579(6) 0.66215(17) 0.88935(16) 0.0248(7) Uani 1 1 d . . . C10 C 0.0563(5) 0.43443(17) 0.85357(15) 0.0216(7) Uani 1 1 d . . . C15 C 0.0921(5) 0.46122(18) 0.91998(16) 0.0207(6) Uani 1 1 d . . . C12 C 0.2419(6) 0.56141(18) 0.81410(16) 0.0209(6) Uani 1 1 d . . . H12 H 0.2854 0.5968 0.7792 0.025 Uiso 1 1 calc R . . C11 C 0.1139(5) 0.48833(18) 0.79937(16) 0.0201(6) Uani 1 1 d . . . C13 C 0.3068(5) 0.58364(18) 0.87755(16) 0.0203(6) Uani 1 1 d . . . C14 C 0.2194(6) 0.53593(17) 0.92965(17) 0.0220(6) Uani 1 1 d . . . H14 H 0.2464 0.5543 0.9729 0.026 Uiso 1 1 calc R . . Cl1 Cl 0.36875(16) 0.26230(6) 0.83043(6) 0.0422(2) Uani 1 1 d . . . C31 C 0.0036(8) 0.4774(2) 1.04397(16) 0.0382(8) Uani 1 1 d . . . H31A H -0.0758 0.5297 1.0344 0.057 Uiso 1 1 calc R . . H31B H 0.1586 0.4902 1.0539 0.057 Uiso 1 1 calc R . . H31C H -0.0649 0.4497 1.0815 0.057 Uiso 1 1 calc R . . C21 C 0.0589(7) 0.5597(2) 0.68653(17) 0.0352(9) Uani 1 1 d . . . H21A H -0.0233 0.6048 0.7081 0.053 Uiso 1 1 calc R . . H21B H 0.0005 0.5515 0.6425 0.053 Uiso 1 1 calc R . . H21C H 0.2159 0.5748 0.6841 0.053 Uiso 1 1 calc R . . C27 C 0.5262(8) 0.6716(2) 0.96216(18) 0.0398(9) Uani 1 1 d . . . H27A H 0.6201 0.7214 0.9672 0.060 Uiso 1 1 calc R . . H27B H 0.6083 0.6216 0.9760 0.060 Uiso 1 1 calc R . . H27C H 0.3932 0.6778 0.9890 0.060 Uiso 1 1 calc R . . C23 C 0.1669(6) 0.4067(2) 0.68890(18) 0.0297(8) Uani 1 1 d . . . H23A H 0.1098 0.4018 0.6444 0.045 Uiso 1 1 calc R . . H23B H 0.1511 0.3526 0.7112 0.045 Uiso 1 1 calc R . . H23C H 0.3235 0.4225 0.6875 0.045 Uiso 1 1 calc R . . C29 C -0.2584(6) 0.3974(2) 0.97318(19) 0.0325(8) Uani 1 1 d . . . H29A H -0.3369 0.4488 0.9609 0.049 Uiso 1 1 calc R . . H29B H -0.3200 0.3755 1.0139 0.049 Uiso 1 1 calc R . . H29C H -0.2759 0.3553 0.9387 0.049 Uiso 1 1 calc R . . C30 C 0.1251(7) 0.3362(2) 1.0026(2) 0.0361(9) Uani 1 1 d . . . H30A H 0.2819 0.3504 1.0080 0.054 Uiso 1 1 calc R . . H30B H 0.1097 0.2936 0.9685 0.054 Uiso 1 1 calc R . . H30C H 0.0667 0.3142 1.0437 0.054 Uiso 1 1 calc R . . C26 C 0.3277(7) 0.7438(2) 0.8689(2) 0.0365(9) Uani 1 1 d . . . H26A H 0.4212 0.7932 0.8762 0.055 Uiso 1 1 calc R . . H26B H 0.1927 0.7486 0.8951 0.055 Uiso 1 1 calc R . . H26C H 0.2882 0.7403 0.8227 0.055 Uiso 1 1 calc R . . C22 C -0.2217(6) 0.4553(2) 0.72434(19) 0.0299(8) Uani 1 1 d . . . H22A H -0.3038 0.4986 0.7481 0.045 Uiso 1 1 calc R . . H22B H -0.2484 0.4005 0.7445 0.045 Uiso 1 1 calc R . . H22C H -0.2715 0.4541 0.6789 0.045 Uiso 1 1 calc R . . C25 C 0.6713(6) 0.6543(2) 0.8478(2) 0.0377(9) Uani 1 1 d . . . H25A H 0.7656 0.7035 0.8553 0.057 Uiso 1 1 calc R . . H25B H 0.6316 0.6513 0.8016 0.057 Uiso 1 1 calc R . . H25C H 0.7515 0.6034 0.8603 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 0.03306(12) 0.01687(7) 0.03616(12) -0.00146(8) -0.00162(12) -0.00416(9) C28 0.0244(17) 0.0280(12) 0.0243(15) 0.0040(11) 0.0032(16) 0.0007(15) C20 0.0253(18) 0.0217(11) 0.0204(14) -0.0025(10) -0.0020(15) 0.0000(13) C24 0.0241(18) 0.0178(11) 0.0325(17) -0.0004(11) -0.0030(15) -0.0034(12) C10 0.0209(16) 0.0169(11) 0.0269(16) -0.0014(10) -0.0001(12) -0.0017(11) C15 0.0183(16) 0.0207(12) 0.0232(17) 0.0024(11) -0.0013(13) 0.0014(11) C12 0.0214(16) 0.0192(12) 0.0222(16) 0.0018(11) 0.0015(13) -0.0011(11) C11 0.0180(15) 0.0185(12) 0.0239(17) -0.0016(11) -0.0005(13) 0.0017(11) C13 0.0180(16) 0.0179(12) 0.0250(17) 0.0000(11) -0.0002(13) 0.0005(11) C14 0.0248(17) 0.0204(13) 0.0206(17) 0.0003(11) -0.0013(13) -0.0001(12) Cl1 0.0385(5) 0.0360(4) 0.0519(6) -0.0055(5) -0.0069(5) 0.0111(3) C31 0.045(2) 0.0467(18) 0.0227(16) -0.0006(13) 0.006(2) -0.009(2) C21 0.046(3) 0.0361(16) 0.0238(16) 0.0021(13) -0.0057(16) -0.0057(16) C27 0.048(3) 0.0322(14) 0.039(2) -0.0030(13) -0.009(2) -0.0150(17) C23 0.032(2) 0.0322(16) 0.0247(18) -0.0064(14) -0.0001(15) 0.0013(14) C29 0.0261(19) 0.0347(17) 0.037(2) 0.0037(15) 0.0046(16) -0.0020(15) C30 0.032(2) 0.0400(18) 0.036(2) 0.0183(17) 0.0007(18) 0.0015(15) C26 0.041(2) 0.0170(14) 0.052(2) -0.0004(15) -0.0080(19) 0.0001(14) C22 0.029(2) 0.0331(17) 0.0281(19) -0.0025(14) -0.0050(16) 0.0022(14) C25 0.032(2) 0.0317(17) 0.049(3) -0.0036(17) 0.0043(18) -0.0097(14) _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 2.134(3) . ? Te1 Cl1 2.3845(11) . ? C28 C29 1.527(5) . ? C28 C30 1.541(4) . ? C28 C31 1.552(4) . ? C28 C15 1.554(4) . ? C20 C22 1.538(5) . ? C20 C23 1.541(4) . ? C20 C21 1.545(4) . ? C20 C11 1.553(4) . ? C24 C25 1.519(5) . ? C24 C27 1.527(5) . ? C24 C13 1.535(4) . ? C24 C26 1.544(4) . ? C10 C15 1.416(4) . ? C10 C11 1.419(4) . ? C15 C14 1.401(4) . ? C12 C13 1.378(5) . ? C12 C11 1.401(4) . ? C13 C14 1.386(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Te1 Cl1 93.40(9) . . ? C29 C28 C30 111.3(3) . . ? C29 C28 C31 105.4(3) . . ? C30 C28 C31 105.5(3) . . ? C29 C28 C15 110.9(3) . . ? C30 C28 C15 112.2(3) . . ? C31 C28 C15 111.1(3) . . ? C22 C20 C23 110.2(3) . . ? C22 C20 C21 105.1(3) . . ? C23 C20 C21 106.4(3) . . ? C22 C20 C11 111.0(3) . . ? C23 C20 C11 113.1(3) . . ? C21 C20 C11 110.8(2) . . ? C25 C24 C27 108.4(3) . . ? C25 C24 C13 109.6(3) . . ? C27 C24 C13 112.3(3) . . ? C25 C24 C26 109.5(3) . . ? C27 C24 C26 107.9(3) . . ? C13 C24 C26 109.0(3) . . ? C15 C10 C11 121.0(3) . . ? C15 C10 Te1 118.8(2) . . ? C11 C10 Te1 119.0(2) . . ? C14 C15 C10 117.2(3) . . ? C14 C15 C28 117.4(3) . . ? C10 C15 C28 125.4(3) . . ? C13 C12 C11 123.5(3) . . ? C12 C11 C10 116.7(3) . . ? C12 C11 C20 118.0(3) . . ? C10 C11 C20 125.1(3) . . ? C12 C13 C14 117.5(3) . . ? C12 C13 C24 120.4(3) . . ? C14 C13 C24 121.9(3) . . ? C13 C14 C15 122.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.105 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.123