Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'W. Levason' 'Matthew J. Hesford' 'Melissa L. Matthews' 'Gillian Reid' _publ_contact_author_name 'Prof W Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email WXL@SOTON.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and complexation of the mixed tellurium-oxygen macrocycles 1-tellura-4,7-dioxacyclononane, [9]aneO2Te, and 1,10-ditellura-4,7,13,16-tetraoxacyclooctadecane, [18]aneO4Te2. ; data_03mlm034 _database_code_CSD 207103 _audit_creation_date 2003-03-12 _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 10.5179(3) _cell_length_b 15.9441(5) _cell_length_c 11.0394(3) _cell_angle_alpha 90 _cell_angle_beta 96.440(2) _cell_angle_gamma 90 _cell_volume 1839.61(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.720 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 753.52 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H24 Cl2 O4 Pt Te2 ' _chemical_formula_moiety 'C12 H24 Cl2 O4 Pt Te2 ' _chemical_formula_structural [PtCl2([18]aneTe2O4)] _chemical_compound_source MeOH _exptl_crystal_F_000 1376.00 _exptl_absorpt_coefficient_mu 11.007 _exptl_absorpt_correction_type multiscan _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max. and min. absorption corrections: 0.86633, 0.72414 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Nonius Kappa CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method - _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8075 _reflns_number_total 4369 _reflns_number_gt 3517 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04093 _diffrn_reflns_av_sigmaI/netI 0.109 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Te 0 8 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.02485(3) 0.20218(2) 0.31302(2) 0.01048(9) 1.000 . Uani d ? Te(1) 0.10494(5) 0.07643(3) 0.20318(4) 0.01197(13) 1.000 . Uani d ? Te(2) -0.08954(5) 0.10256(3) 0.44288(4) 0.01163(13) 1.000 . Uani d ? Cl(1) 0.1432(2) 0.29316(12) 0.2021(2) 0.0186(5) 1.000 . Uani d ? Cl(2) -0.0675(2) 0.31668(12) 0.4059(2) 0.0155(5) 1.000 . Uani d ? O(1) 0.3176(5) 0.0361(3) 0.4231(4) 0.018(2) 1.000 . Uani d ? O(2) 0.1674(5) 0.1378(4) 0.5742(4) 0.017(2) 1.000 . Uani d ? O(3) -0.2967(5) 0.0719(3) 0.2308(5) 0.017(1) 1.000 . Uani d ? O(4) -0.1402(5) 0.0884(3) 0.0329(5) 0.018(2) 1.000 . Uani d ? C(1) 0.3107(7) 0.0907(5) 0.2170(7) 0.015(2) 1.000 . Uani d ? C(2) 0.3722(8) 0.0309(5) 0.3090(7) 0.018(2) 1.000 . Uani d ? C(3) 0.3601(8) 0.1092(5) 0.4917(7) 0.018(2) 1.000 . Uani d ? C(4) 0.2990(7) 0.1127(5) 0.6069(7) 0.015(2) 1.000 . Uani d ? C(5) 0.0886(8) 0.1290(5) 0.6711(7) 0.017(2) 1.000 . Uani d ? C(6) -0.0451(7) 0.1574(5) 0.6211(7) 0.018(2) 1.000 . Uani d ? C(7) -0.2821(7) 0.1515(5) 0.4130(7) 0.017(2) 1.000 . Uani d ? C(8) -0.3217(7) 0.1524(5) 0.2768(7) 0.016(2) 1.000 . Uani d ? C(9) -0.3416(7) 0.0604(5) 0.1043(6) 0.017(2) 1.000 . Uani d ? C(10) -0.2714(7) 0.1137(5) 0.0206(7) 0.016(2) 1.000 . Uani d ? C(11) -0.0571(8) 0.1493(5) -0.0108(7) 0.018(2) 1.000 . Uani d ? C(12) 0.0791(7) 0.1179(5) 0.0158(6) 0.013(2) 1.000 . Uani d ? H(1) 0.3411 0.0815 0.1401 0.018 1.000 . Uiso c ? H(2) 0.3342 0.1473 0.2427 0.018 1.000 . Uiso c ? H(3) 0.4623 0.0417 0.3238 0.021 1.000 . Uiso c ? H(4) 0.3609 -0.0250 0.2776 0.021 1.000 . Uiso c ? H(5) 0.4517 0.1084 0.5088 0.024 1.000 . Uiso c ? H(6) 0.3374 0.1586 0.4439 0.024 1.000 . Uiso c ? H(7) 0.3418 0.1516 0.6641 0.018 1.000 . Uiso c ? H(8) 0.3021 0.0583 0.6458 0.018 1.000 . Uiso c ? H(9) 0.0858 0.0710 0.6956 0.021 1.000 . Uiso c ? H(10) 0.1212 0.1612 0.7402 0.021 1.000 . Uiso c ? H(11) -0.0454 0.2180 0.6148 0.027 1.000 . Uiso c ? H(12) -0.1057 0.1415 0.6738 0.027 1.000 . Uiso c ? H(13) -0.3391 0.1176 0.4531 0.021 1.000 . Uiso c ? H(14) -0.2846 0.2076 0.4454 0.021 1.000 . Uiso c ? H(15) -0.2750 0.1942 0.2385 0.019 1.000 . Uiso c ? H(16) -0.4114 0.1652 0.2602 0.019 1.000 . Uiso c ? H(17) -0.3315 0.0024 0.0826 0.023 1.000 . Uiso c ? H(18) -0.4314 0.0732 0.0904 0.023 1.000 . Uiso c ? H(19) -0.2774 0.1714 0.0431 0.018 1.000 . Uiso c ? H(20) -0.3078 0.1075 -0.0621 0.018 1.000 . Uiso c ? H(21) -0.0785 0.1578 -0.0967 0.022 1.000 . Uiso c ? H(22) -0.0657 0.2019 0.0294 0.022 1.000 . Uiso c ? H(23) 0.1379 0.1610 0.0023 0.016 1.000 . Uiso c ? H(24) 0.0917 0.0718 -0.0380 0.016 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0102(2) 0.0112(2) 0.0100(2) -0.00044(12) 0.00089(13) -0.00038(11) Te(1) 0.0123(3) 0.0118(3) 0.0120(3) -0.0005(2) 0.0028(2) -0.0004(2) Te(2) 0.0114(3) 0.0127(3) 0.0109(3) -0.0001(2) 0.0018(2) 0.0005(2) Cl(1) 0.0221(10) 0.0142(10) 0.0207(10) -0.0053(8) 0.0077(9) 0.0014(8) Cl(2) 0.0182(10) 0.0123(10) 0.0157(9) 0.0021(8) 0.0006(8) -0.0029(8) O(1) 0.022(3) 0.019(3) 0.012(3) -0.003(2) -0.000(2) 0.003(2) O(2) 0.011(3) 0.032(4) 0.008(3) 0.000(3) 0.000(2) 0.008(2) O(3) 0.024(3) 0.008(3) 0.017(3) 0.005(2) 0.001(3) -0.000(2) O(4) 0.015(3) 0.018(3) 0.018(3) 0.002(2) -0.003(2) 0.003(2) C(1) 0.015(4) 0.020(5) 0.012(4) 0.003(3) 0.010(3) 0.001(3) C(2) 0.018(4) 0.017(5) 0.018(4) 0.004(4) 0.002(4) -0.000(3) C(3) 0.021(4) 0.021(5) 0.013(4) -0.008(4) 0.001(4) -0.001(3) C(4) 0.012(4) 0.019(4) 0.014(4) 0.002(3) 0.001(3) 0.001(3) C(5) 0.020(4) 0.011(4) 0.019(4) -0.007(3) -0.000(4) -0.003(3) C(6) 0.017(4) 0.026(5) 0.012(4) 0.009(4) 0.006(4) -0.007(3) C(7) 0.012(4) 0.024(5) 0.016(4) 0.003(4) 0.009(3) 0.004(4) C(8) 0.014(4) 0.008(4) 0.026(4) 0.000(3) -0.002(4) 0.005(3) C(9) 0.020(4) 0.022(5) 0.007(4) -0.001(4) -0.007(3) -0.003(3) C(10) 0.006(4) 0.023(5) 0.018(4) 0.006(3) -0.002(3) 0.003(3) C(11) 0.021(4) 0.013(4) 0.021(4) 0.003(3) 0.009(4) 0.007(4) C(12) 0.016(4) 0.013(4) 0.009(4) -0.000(3) 0.001(3) -0.001(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3517 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_all 0.0500 _refine_ls_wR_factor_ref 0.0500 _refine_ls_goodness_of_fit_all 1.314 _refine_ls_goodness_of_fit_ref 1.310 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0008 _refine_diff_density_min -1.85 _refine_diff_density_max 1.69 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) Te(1) 2.5357(6) . . ? Pt(1) Te(2) 2.5322(6) . . ? Pt(1) Cl(1) 2.344(2) . . ? Pt(1) Cl(2) 2.356(2) . . ? Te(1) C(1) 2.164(9) . . ? Te(1) C(12) 2.159(8) . . ? Te(2) C(6) 2.156(9) . . ? Te(2) C(7) 2.161(9) . . ? O(1) C(2) 1.444(10) . . ? O(1) C(3) 1.434(11) . . ? O(2) C(4) 1.447(10) . . ? O(2) C(5) 1.432(10) . . ? O(3) C(8) 1.416(10) . . ? O(3) C(9) 1.436(10) . . ? O(4) C(10) 1.430(10) . . ? O(4) C(11) 1.426(10) . . ? C(1) C(2) 1.487(12) . . ? C(1) H(1) 0.95 . . no C(1) H(2) 0.97 . . no C(2) H(3) 0.96 . . no C(2) H(4) 0.96 . . no C(3) C(4) 1.490(12) . . ? C(3) H(5) 0.96 . . no C(3) H(6) 0.96 . . no C(4) H(7) 0.96 . . no C(4) H(8) 0.97 . . no C(5) C(6) 1.520(13) . . ? C(5) H(9) 0.96 . . no C(5) H(10) 0.95 . . no C(6) H(11) 0.97 . . no C(6) H(12) 0.94 . . no C(7) C(8) 1.515(12) . . ? C(7) H(13) 0.95 . . no C(7) H(14) 0.96 . . no C(8) H(15) 0.95 . . no C(8) H(16) 0.96 . . no C(9) C(10) 1.508(12) . . ? C(9) H(17) 0.96 . . no C(9) H(18) 0.96 . . no C(10) H(19) 0.96 . . no C(10) H(20) 0.96 . . no C(11) C(12) 1.515(12) . . ? C(11) H(21) 0.96 . . no C(11) H(22) 0.96 . . no C(12) H(23) 0.95 . . no C(12) H(24) 0.96 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te(1) Pt(1) Te(2) 88.81(2) . . . ? Te(1) Pt(1) Cl(1) 90.87(6) . . . ? Te(1) Pt(1) Cl(2) 174.96(6) . . . ? Te(2) Pt(1) Cl(1) 176.12(6) . . . ? Te(2) Pt(1) Cl(2) 89.68(5) . . . ? Cl(1) Pt(1) Cl(2) 90.97(7) . . . ? Pt(1) Te(1) C(1) 105.5(2) . . . ? Pt(1) Te(1) C(12) 101.7(2) . . . ? C(1) Te(1) C(12) 93.0(3) . . . ? Pt(1) Te(2) C(6) 101.2(3) . . . ? Pt(1) Te(2) C(7) 100.6(2) . . . ? C(6) Te(2) C(7) 95.5(3) . . . ? C(2) O(1) C(3) 112.1(6) . . . ? C(4) O(2) C(5) 113.8(6) . . . ? C(8) O(3) C(9) 114.2(7) . . . ? C(10) O(4) C(11) 113.4(7) . . . ? Te(1) C(1) C(2) 109.6(6) . . . ? Te(1) C(1) H(1) 110.8 . . . no Te(1) C(1) H(2) 109.8 . . . no C(2) C(1) H(1) 110.3 . . . no C(2) C(1) H(2) 108.6 . . . no H(1) C(1) H(2) 107.7 . . . no O(1) C(2) C(1) 112.0(7) . . . ? O(1) C(2) H(3) 108.9 . . . no O(1) C(2) H(4) 108.9 . . . no C(1) C(2) H(3) 110.3 . . . no C(1) C(2) H(4) 108.8 . . . no H(3) C(2) H(4) 108.0 . . . no O(1) C(3) C(4) 110.0(7) . . . ? O(1) C(3) H(5) 109.8 . . . no O(1) C(3) H(6) 109.4 . . . no C(4) C(3) H(5) 110.6 . . . no C(4) C(3) H(6) 109.5 . . . no H(5) C(3) H(6) 107.5 . . . no O(2) C(4) C(3) 106.8(7) . . . ? O(2) C(4) H(7) 110.5 . . . no O(2) C(4) H(8) 110.1 . . . no C(3) C(4) H(7) 111.7 . . . no C(3) C(4) H(8) 110.4 . . . no H(7) C(4) H(8) 107.3 . . . no O(2) C(5) C(6) 106.8(7) . . . ? O(2) C(5) H(9) 110.0 . . . no O(2) C(5) H(10) 111.0 . . . no C(6) C(5) H(9) 109.3 . . . no C(6) C(5) H(10) 111.5 . . . no H(9) C(5) H(10) 108.2 . . . no Te(2) C(6) C(5) 107.9(5) . . . ? Te(2) C(6) H(11) 109.9 . . . no Te(2) C(6) H(12) 111.2 . . . no C(5) C(6) H(11) 108.5 . . . no C(5) C(6) H(12) 111.0 . . . no H(11) C(6) H(12) 108.3 . . . no Te(2) C(7) C(8) 107.7(5) . . . ? Te(2) C(7) H(13) 110.6 . . . no Te(2) C(7) H(14) 110.0 . . . no C(8) C(7) H(13) 110.4 . . . no C(8) C(7) H(14) 110.1 . . . no H(13) C(7) H(14) 108.0 . . . no O(3) C(8) C(7) 107.8(7) . . . ? O(3) C(8) H(15) 110.3 . . . no O(3) C(8) H(16) 110.0 . . . no C(7) C(8) H(15) 110.4 . . . no C(7) C(8) H(16) 110.2 . . . no H(15) C(8) H(16) 108.1 . . . no O(3) C(9) C(10) 113.2(7) . . . ? O(3) C(9) H(17) 109.3 . . . no O(3) C(9) H(18) 109.7 . . . no C(10) C(9) H(17) 108.2 . . . no C(10) C(9) H(18) 108.8 . . . no H(17) C(9) H(18) 107.4 . . . no O(4) C(10) C(9) 108.5(7) . . . ? O(4) C(10) H(19) 109.8 . . . no O(4) C(10) H(20) 109.9 . . . no C(9) C(10) H(19) 109.4 . . . no C(9) C(10) H(20) 110.8 . . . no H(19) C(10) H(20) 108.5 . . . no O(4) C(11) C(12) 108.1(7) . . . ? O(4) C(11) H(21) 110.2 . . . no O(4) C(11) H(22) 110.2 . . . no C(12) C(11) H(21) 110.5 . . . no C(12) C(11) H(22) 109.7 . . . no H(21) C(11) H(22) 108.1 . . . no Te(1) C(12) C(11) 107.6(5) . . . ? Te(1) C(12) H(23) 111.0 . . . no Te(1) C(12) H(24) 110.2 . . . no C(11) C(12) H(23) 110.4 . . . no C(11) C(12) H(24) 109.0 . . . no H(23) C(12) H(24) 108.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(7) 3.484(9) . 4_554 no Cl(1) C(6) 3.582(9) . 4_554 no Cl(2) C(10) 3.414(9) . 4 no O(1) C(7) 3.537(11) . 3_556 no O(3) C(4) 3.447(10) . 3_556 no O(4) C(12) 3.405(10) . 3 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt(1) Te(1) C(1) C(2) . . . . 104.9(6) no Pt(1) Te(1) C(12) C(11) . . . . -51.0(6) no Pt(1) Te(2) C(6) C(5) . . . . -81.0(6) no Pt(1) Te(2) C(7) C(8) . . . . 55.6(6) no Te(1) Pt(1) Te(2) C(6) . . . . 136.5(2) no Te(1) Pt(1) Te(2) C(7) . . . . -125.6(3) no Te(1) C(1) C(2) O(1) . . . . -50.9(8) no Te(1) C(12) C(11) O(4) . . . . -47.6(8) no Te(2) Pt(1) Te(1) C(1) . . . . -126.0(2) no Te(2) Pt(1) Te(1) C(12) . . . . 137.5(2) no Te(2) C(6) C(5) O(2) . . . . 44.8(8) no Te(2) C(7) C(8) O(3) . . . . 50.7(7) no Cl(1) Pt(1) Te(1) C(1) . . . . 50.1(2) no Cl(1) Pt(1) Te(1) C(12) . . . . -46.4(2) no Cl(1) Pt(1) Te(2) C(6) . . . . 51.3(9) no Cl(1) Pt(1) Te(2) C(7) . . . . 149.2(9) no Cl(2) Pt(1) Te(1) C(1) . . . . 161.4(7) no Cl(2) Pt(1) Te(1) C(12) . . . . 64.9(7) no Cl(2) Pt(1) Te(2) C(6) . . . . -48.3(2) no Cl(2) Pt(1) Te(2) C(7) . . . . 49.6(3) no O(1) C(3) C(4) O(2) . . . . -74.6(9) no O(3) C(9) C(10) O(4) . . . . 63.5(9) no C(1) Te(1) C(12) C(11) . . . . -157.5(6) no C(1) C(2) O(1) C(3) . . . . -75.5(9) no C(2) O(1) C(3) C(4) . . . . 178.7(7) no C(2) C(1) Te(1) C(12) . . . . -152.1(6) no C(3) C(4) O(2) C(5) . . . . 168.8(7) no C(4) O(2) C(5) C(6) . . . . -179.7(7) no C(5) C(6) Te(2) C(7) . . . . 177.0(6) no C(6) Te(2) C(7) C(8) . . . . 158.1(6) no C(7) C(8) O(3) C(9) . . . . 173.9(7) no C(8) O(3) C(9) C(10) . . . . 66.9(9) no C(9) C(10) O(4) C(11) . . . . -161.6(7) no C(10) O(4) C(11) C(12) . . . . 175.9(7) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_Templatetexray.inf _database_code_CSD 207104 _audit_creation_date 2003-03-14 _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.1683(2) _cell_length_b 9.5820(2) _cell_length_c 20.5132(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1802.10(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.419 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 656.24 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H24 Cl2 O4 Pt Se2 ' _chemical_formula_moiety 'C12 H24 Cl2 O4 Pt Se2 ' _chemical_formula_structural [PtCl2([18]aneSe2O4)] _chemical_compound_source ? _exptl_crystal_F_000 1232.00 _exptl_absorpt_coefficient_mu 12.102 _exptl_absorpt_correction_type multiscan _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. The data were processed using Denzo and Scalepack, the latter applying a pseudo-emperical absorption correction." HKL - Denso & Scalepack Z. Otwinowski and W. Minor Processing of X-ray Diffraction Data Collected in Oscillation Mode, Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997, C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method - _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4118 _reflns_number_total 2381 _reflns_number_gt 2217 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05245 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 8 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.23021(4) 0.75979(4) 0.62884(2) 0.01114(10) 1.000 . Uani d ? Se(1) 0.30329(11) 0.93461(12) 0.70532(5) 0.0129(3) 1.000 . Uani d ? Se(2) 0.02879(11) 0.90870(13) 0.60363(5) 0.0159(3) 1.000 . Uani d ? Cl(1) 0.4311(3) 0.6221(3) 0.65436(13) 0.0198(7) 1.000 . Uani d ? Cl(2) 0.1535(3) 0.5936(3) 0.55308(13) 0.0217(7) 1.000 . Uani d ? O(1) 0.0918(8) 0.8431(9) 0.8034(4) 0.026(2) 1.000 . Uani d ? O(2) -0.1512(8) 0.8694(9) 0.7205(4) 0.022(2) 1.000 . Uani d ? O(3) 0.2033(8) 1.1004(9) 0.5201(3) 0.025(2) 1.000 . Uani d ? O(4) 0.4164(8) 1.1537(8) 0.6179(4) 0.024(2) 1.000 . Uani d ? C(1) 0.3494(12) 0.832(1) 0.7856(5) 0.022(3) 1.000 . Uani d ? C(2) 0.2136(11) 0.7540(13) 0.8057(5) 0.020(2) 1.000 . Uiso d ? C(3) -0.0442(12) 0.778(2) 0.8202(5) 0.035(4) 1.000 . Uani d ? C(4) -0.168(1) 0.853(1) 0.7876(6) 0.029(4) 1.000 . Uani d ? C(5) -0.1557(12) 0.745(2) 0.6836(5) 0.028(3) 1.000 . Uani d ? C(6) -0.1386(12) 0.787(1) 0.6146(6) 0.031(4) 1.000 . Uani d ? C(7) 0.033(1) 0.914(1) 0.5072(5) 0.029(4) 1.000 . Uani d ? C(8) 0.1727(13) 0.978(1) 0.4848(6) 0.026(3) 1.000 . Uani d ? C(9) 0.342(2) 1.161(2) 0.5046(6) 0.040(4) 1.000 . Uani d ? C(10) 0.3998(13) 1.235(2) 0.5583(6) 0.039(4) 1.000 . Uani d ? C(11) 0.5047(12) 1.0380(13) 0.6132(5) 0.020(3) 1.000 . Uani d ? C(12) 0.5049(11) 0.9671(12) 0.6791(5) 0.017(3) 1.000 . Uiso d ? H(1) 0.4306 0.7659 0.7770 0.028 1.000 . Uiso c ? H(2) 0.3849 0.8935 0.8188 0.028 1.000 . Uiso c ? H(3) 0.2245 0.7191 0.8490 0.023 1.000 . Uiso c ? H(4) 0.1966 0.6782 0.7769 0.023 1.000 . Uiso c ? H(5) -0.0584 0.7760 0.8670 0.044 1.000 . Uiso c ? H(6) -0.0452 0.6820 0.8057 0.044 1.000 . Uiso c ? H(7) -0.1707 0.9460 0.8076 0.035 1.000 . Uiso c ? H(8) -0.2565 0.8080 0.7978 0.035 1.000 . Uiso c ? H(9) -0.2445 0.6917 0.6906 0.034 1.000 . Uiso c ? H(10) -0.0762 0.6807 0.6962 0.034 1.000 . Uiso c ? H(11) -0.1282 0.7061 0.5874 0.034 1.000 . Uiso c ? H(12) -0.2258 0.8346 0.6019 0.034 1.000 . Uiso c ? H(13) -0.0501 0.9758 0.4899 0.038 1.000 . Uiso c ? H(14) 0.0158 0.8268 0.4868 0.038 1.000 . Uiso c ? H(15) 0.1699 1.0020 0.4386 0.031 1.000 . Uiso c ? H(16) 0.2483 0.9120 0.4907 0.031 1.000 . Uiso c ? H(17) 0.3318 1.2221 0.4678 0.045 1.000 . Uiso c ? H(18) 0.4105 1.0894 0.4930 0.045 1.000 . Uiso c ? H(19) 0.3337 1.3126 0.5676 0.051 1.000 . Uiso c ? H(20) 0.4916 1.2759 0.5465 0.051 1.000 . Uiso c ? H(21) 0.4673 0.9756 0.5801 0.025 1.000 . Uiso c ? H(22) 0.6005 1.0663 0.5995 0.025 1.000 . Uiso c ? H(23) 0.5592 0.8814 0.6770 0.022 1.000 . Uiso c ? H(24) 0.5547 1.0268 0.7102 0.022 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0120(2) 0.0110(2) 0.0104(2) 0.0002(2) -0.0007(2) 0.0000(2) Se(1) 0.0121(5) 0.0129(6) 0.0137(5) -0.0001(5) -0.0009(4) -0.0012(5) Se(2) 0.0147(5) 0.0168(7) 0.0163(5) 0.0004(5) -0.0015(5) -0.0019(5) Cl(1) 0.023(1) 0.018(2) 0.0187(13) 0.0113(13) -0.0059(13) -0.0042(12) Cl(2) 0.026(2) 0.019(2) 0.0204(13) -0.001(1) 0.0021(13) -0.0053(13) O(1) 0.023(4) 0.023(5) 0.032(5) 0.003(4) 0.023(4) 0.016(4) O(2) 0.014(4) 0.027(5) 0.024(4) -0.006(4) 0.003(4) -0.006(4) O(3) 0.022(4) 0.037(6) 0.017(4) -0.009(4) -0.008(4) -0.002(4) O(4) 0.029(4) 0.014(5) 0.029(4) -0.001(4) -0.021(4) 0.008(4) C(1) 0.024(6) 0.028(8) 0.015(6) 0.010(6) -0.006(5) -0.004(6) C(3) 0.027(6) 0.061(11) 0.016(6) -0.016(8) 0.014(5) 0.002(7) C(4) 0.033(7) 0.031(8) 0.024(7) -0.012(7) -0.017(6) 0.004(6) C(5) 0.027(6) 0.034(8) 0.023(6) -0.020(7) 0.009(5) 0.003(6) C(6) 0.013(5) 0.029(8) 0.050(8) -0.010(5) -0.002(6) 0.005(7) C(7) 0.053(8) 0.009(7) 0.024(6) 0.010(7) -0.006(7) -0.004(5) C(8) 0.029(7) 0.022(7) 0.028(7) -0.001(6) -0.005(6) 0.006(6) C(9) 0.040(8) 0.051(11) 0.030(7) 0.013(8) 0.009(7) 0.008(7) C(10) 0.034(7) 0.054(11) 0.029(7) -0.004(8) -0.001(6) 0.037(8) C(11) 0.028(6) 0.016(6) 0.015(5) -0.002(5) 0.015(5) -0.005(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; Small crystal and relatively weak data. All non-H atoms anisotropic except for C(2) and C(12) which go npd, hence isotropic. Some evidence for disorder in floppy ether unit (O(1)), but unable to identify alternative sites. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details Flack _refine_ls_abs_structure_Flack 0.0887(5) _refine_ls_number_reflns 2217 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_all 0.0650 _refine_ls_wR_factor_ref 0.0650 _refine_ls_goodness_of_fit_all 2.334 _refine_ls_goodness_of_fit_ref 2.330 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.06 _refine_diff_density_max 1.56 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) Se(1) 2.391(2) . . ? Pt(1) Se(2) 2.390(2) . . ? Pt(1) Cl(1) 2.325(4) . . ? Pt(1) Cl(2) 2.334(4) . . ? Se(1) C(1) 1.96(2) . . ? Se(1) C(12) 1.95(2) . . ? Se(2) C(6) 1.94(2) . . ? Se(2) C(7) 1.98(2) . . ? O(1) C(2) 1.41(2) . . ? O(1) C(3) 1.43(2) . . ? O(2) C(4) 1.39(2) . . ? O(2) C(5) 1.41(2) . . ? O(3) C(8) 1.41(2) . . ? O(3) C(9) 1.44(2) . . ? O(4) C(10) 1.46(2) . . ? O(4) C(11) 1.38(2) . . ? C(1) C(2) 1.51(2) . . ? C(1) H(1) 1.00 . . no C(1) H(2) 0.95 . . no C(2) H(3) 0.96 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.50(3) . . ? C(3) H(5) 0.97 . . no C(3) H(6) 0.97 . . no C(4) H(7) 0.98 . . no C(4) H(8) 0.95 . . no C(5) C(6) 1.48(2) . . ? C(5) H(9) 0.97 . . no C(5) H(10) 0.99 . . no C(6) H(11) 0.96 . . no C(6) H(12) 0.96 . . no C(7) C(8) 1.49(3) . . ? C(7) H(13) 1.03 . . no C(7) H(14) 0.95 . . no C(8) H(15) 0.97 . . no C(8) H(16) 0.95 . . no C(9) C(10) 1.41(3) . . ? C(9) H(17) 0.96 . . no C(9) H(18) 0.96 . . no C(10) H(19) 0.98 . . no C(10) H(20) 0.96 . . no C(11) C(12) 1.51(2) . . ? C(11) H(21) 0.97 . . no C(11) H(22) 0.96 . . no C(12) H(23) 0.96 . . no C(12) H(24) 0.97 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Pt(1) Se(2) 86.57(6) . . . ? Se(1) Pt(1) Cl(1) 91.59(11) . . . ? Se(1) Pt(1) Cl(2) 178.30(12) . . . ? Se(2) Pt(1) Cl(1) 177.91(12) . . . ? Se(2) Pt(1) Cl(2) 91.74(12) . . . ? Cl(1) Pt(1) Cl(2) 90.1(2) . . . ? Pt(1) Se(1) C(1) 105.2(6) . . . ? Pt(1) Se(1) C(12) 101.3(5) . . . ? C(1) Se(1) C(12) 96.1(7) . . . ? Pt(1) Se(2) C(6) 103.1(6) . . . ? Pt(1) Se(2) C(7) 102.4(5) . . . ? C(6) Se(2) C(7) 98.5(8) . . . ? C(2) O(1) C(3) 114.8(14) . . . ? C(4) O(2) C(5) 115.6(15) . . . ? C(8) O(3) C(9) 113.7(15) . . . ? C(10) O(4) C(11) 115.7(14) . . . ? Se(1) C(1) C(2) 107.4(11) . . . ? Se(1) C(1) H(1) 109.3 . . . no Se(1) C(1) H(2) 111.5 . . . no C(2) C(1) H(1) 110.2 . . . no C(2) C(1) H(2) 113.1 . . . no H(1) C(1) H(2) 105.4 . . . no O(1) C(2) C(1) 110.0(14) . . . ? O(1) C(2) H(3) 109.1 . . . no O(1) C(2) H(4) 108.3 . . . no C(1) C(2) H(3) 109.9 . . . no C(1) C(2) H(4) 110.3 . . . no H(3) C(2) H(4) 109.2 . . . no O(1) C(3) C(4) 109.9(16) . . . ? O(1) C(3) H(5) 111.5 . . . no O(1) C(3) H(6) 110.2 . . . no C(4) C(3) H(5) 110.6 . . . no C(4) C(3) H(6) 108.2 . . . no H(5) C(3) H(6) 106.3 . . . no O(2) C(4) C(3) 114.3(16) . . . ? O(2) C(4) H(7) 108.6 . . . no O(2) C(4) H(8) 111.3 . . . no C(3) C(4) H(7) 105.6 . . . no C(3) C(4) H(8) 109.2 . . . no H(7) C(4) H(8) 107.4 . . . no O(2) C(5) C(6) 106.1(16) . . . ? O(2) C(5) H(9) 112.8 . . . no O(2) C(5) H(10) 111.3 . . . no C(6) C(5) H(9) 111.9 . . . no C(6) C(5) H(10) 110.0 . . . no H(9) C(5) H(10) 104.7 . . . no Se(2) C(6) C(5) 111.0(12) . . . ? Se(2) C(6) H(11) 109.8 . . . no Se(2) C(6) H(12) 110.0 . . . no C(5) C(6) H(11) 110.2 . . . no C(5) C(6) H(12) 107.6 . . . no H(11) C(6) H(12) 108.2 . . . no Se(2) C(7) C(8) 109.7(13) . . . ? Se(2) C(7) H(13) 110.1 . . . no Se(2) C(7) H(14) 114.6 . . . no C(8) C(7) H(13) 107.0 . . . no C(8) C(7) H(14) 111.8 . . . no H(13) C(7) H(14) 103.3 . . . no O(3) C(8) C(7) 110.8(16) . . . ? O(3) C(8) H(15) 108.1 . . . no O(3) C(8) H(16) 110.2 . . . no C(7) C(8) H(15) 111.9 . . . no C(7) C(8) H(16) 108.1 . . . no H(15) C(8) H(16) 107.6 . . . no O(3) C(9) C(10) 111.3(16) . . . ? O(3) C(9) H(17) 109.5 . . . no O(3) C(9) H(18) 110.0 . . . no C(10) C(9) H(17) 110.3 . . . no C(10) C(9) H(18) 107.9 . . . no H(17) C(9) H(18) 107.8 . . . no O(4) C(10) C(9) 115.2(19) . . . ? O(4) C(10) H(19) 107.9 . . . no O(4) C(10) H(20) 109.7 . . . no C(9) C(10) H(19) 107.5 . . . no C(9) C(10) H(20) 109.7 . . . no H(19) C(10) H(20) 106.4 . . . no O(4) C(11) C(12) 107.4(13) . . . ? O(4) C(11) H(21) 109.8 . . . no O(4) C(11) H(22) 109.3 . . . no C(12) C(11) H(21) 110.5 . . . no C(12) C(11) H(22) 112.7 . . . no H(21) C(11) H(22) 107.1 . . . no Se(1) C(12) C(11) 108.5(11) . . . ? Se(1) C(12) H(23) 111.6 . . . no Se(1) C(12) H(24) 111.1 . . . no C(11) C(12) H(23) 110.0 . . . no C(11) C(12) H(24) 108.8 . . . no H(23) C(12) H(24) 106.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(7) 3.46(2) . 3_566 no O(2) C(12) 3.40(2) . 1_455 no O(3) C(10) 3.58(2) . 3_476 no O(4) C(1) 3.39(2) . 4_656 no O(4) C(4) 3.55(2) . 4_556 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt(1) Se(1) C(1) C(2) . . . . -58.7(12) no Pt(1) Se(1) C(12) C(11) . . . . 68.9(12) no Pt(1) Se(2) C(6) C(5) . . . . 66.1(14) no Pt(1) Se(2) C(7) C(8) . . . . -62.7(13) no Se(1) Pt(1) Se(2) C(6) . . . . -126.7(6) no Se(1) Pt(1) Se(2) C(7) . . . . 131.4(6) no Se(1) C(1) C(2) O(1) . . . . -47.6(16) no Se(1) C(12) C(11) O(4) . . . . 53.1(15) no Se(2) Pt(1) Se(1) C(1) . . . . 133.4(5) no Se(2) Pt(1) Se(1) C(12) . . . . -127.0(5) no Se(2) C(6) C(5) O(2) . . . . 50.6(17) no Se(2) C(7) C(8) O(3) . . . . -46.1(17) no Cl(1) Pt(1) Se(1) C(1) . . . . -47.7(5) no Cl(1) Pt(1) Se(1) C(12) . . . . 52.0(5) no Cl(1) Pt(1) Se(2) C(6) . . . . -155.4(31) no Cl(1) Pt(1) Se(2) C(7) . . . . 102.7(31) no Cl(2) Pt(1) Se(1) C(1) . . . . 140.0(38) no Cl(2) Pt(1) Se(1) C(12) . . . . -120.3(39) no Cl(2) Pt(1) Se(2) C(6) . . . . 53.5(6) no Cl(2) Pt(1) Se(2) C(7) . . . . -48.4(6) no O(1) C(3) C(4) O(2) . . . . 52.6(22) no O(3) C(9) C(10) O(4) . . . . 56.6(23) no C(1) Se(1) C(12) C(11) . . . . 175.8(12) no C(1) C(2) O(1) C(3) . . . . 178.7(13) no C(2) O(1) C(3) C(4) . . . . -153.3(15) no C(2) C(1) Se(1) C(12) . . . . -162.2(12) no C(3) C(4) O(2) C(5) . . . . 66.9(20) no C(4) O(2) C(5) C(6) . . . . 179.1(14) no C(5) C(6) Se(2) C(7) . . . . 171.0(14) no C(6) Se(2) C(7) C(8) . . . . -168.2(13) no C(7) C(8) O(3) C(9) . . . . 175.2(14) no C(8) O(3) C(9) C(10) . . . . -151.3(17) no C(9) C(10) O(4) C(11) . . . . 58.8(22) no C(10) O(4) C(11) C(12) . . . . -178.8(14) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_03mlm030[PdCl2([18]aneTe2 _database_code_CSD 207105 _audit_creation_date 2003-03-12 _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 10.5109(3) _cell_length_b 15.9002(5) _cell_length_c 10.9837(3) _cell_angle_alpha 90 _cell_angle_beta 96.8439(11) _cell_angle_gamma 90 _cell_volume 1822.58(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.423 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 664.83 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H24 Cl2 O4 Pd Te2 ' _chemical_formula_moiety 'C12 H24 Cl2 O4 Pd Te2 ' _chemical_formula_structural [PdCl2([18]aneTe2O4)] _chemical_compound_source CH2Cl2 _exptl_crystal_F_000 1248.00 _exptl_absorpt_coefficient_mu 4.460 _exptl_absorpt_correction_type multiscan _exptl_special_details ; max. and min transmission factors: 0.95882, 0.60512 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 7470 _reflns_number_total 4281 _reflns_number_gt 3811 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02219 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 8 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Te(1) -0.10571(2) 0.57426(2) 0.79401(2) 0.00929(7) 1.000 . Uani d ? Te(2) 0.08966(2) 0.60157(2) 0.55470(2) 0.00909(7) 1.000 . Uani d ? Pd(1) -0.02727(3) 0.70198(2) 0.68278(2) 0.00793(8) 1.000 . Uani d ? Cl(1) -0.15124(10) 0.79045(6) 0.79275(9) 0.0160(3) 1.000 . Uani d ? Cl(2) 0.07034(9) 0.81548(6) 0.59076(8) 0.0133(2) 1.000 . Uani d ? O(1) 0.1411(3) 0.5879(2) 0.9625(3) 0.0163(8) 1.000 . Uani d ? O(2) 0.2974(3) 0.5714(2) 0.7672(3) 0.0132(7) 1.000 . Uani d ? O(3) -0.1702(3) 0.6397(2) 0.4243(2) 0.0140(7) 1.000 . Uani d ? O(4) -0.3211(3) 0.5356(2) 0.5749(2) 0.0144(7) 1.000 . Uani d ? C(1) -0.0741(4) 0.6178(3) 0.9811(3) 0.0141(10) 1.000 . Uani d ? C(2) 0.0595(4) 0.6483(3) 1.0091(3) 0.0134(10) 1.000 . Uani d ? C(3) 0.2732(4) 0.6126(3) 0.9790(4) 0.0157(10) 1.000 . Uani d ? C(4) 0.3436(4) 0.5591(3) 0.8951(4) 0.0157(10) 1.000 . Uani d ? C(5) 0.3216(4) 0.6542(2) 0.7208(4) 0.0143(10) 1.000 . Uani d ? C(6) 0.2803(3) 0.6514(2) 0.5852(4) 0.0119(10) 1.000 . Uani d ? C(7) 0.0409(4) 0.6559(3) 0.3759(3) 0.0136(10) 1.000 . Uani d ? C(8) -0.0938(4) 0.6303(2) 0.3281(3) 0.0130(10) 1.000 . Uani d ? C(9) -0.3017(4) 0.6154(3) 0.3928(4) 0.0155(10) 1.000 . Uani d ? C(10) -0.3635(4) 0.6106(3) 0.5086(4) 0.0147(10) 1.000 . Uani d ? C(11) -0.3729(4) 0.5298(3) 0.6878(4) 0.0164(11) 1.000 . Uani d ? C(12) -0.3105(4) 0.5890(3) 0.7850(4) 0.0132(10) 1.000 . Uani d ? H(1) -0.1316 0.6616 0.9939 0.016 1.000 . Uiso c ? H(2) -0.0872 0.5720 1.0357 0.016 1.000 . Uiso c ? H(3) 0.0811 0.6534 1.0965 0.018 1.000 . Uiso c ? H(4) 0.0682 0.7015 0.9728 0.018 1.000 . Uiso c ? H(5) 0.2817 0.6700 0.9593 0.019 1.000 . Uiso c ? H(6) 0.3082 0.6034 1.0624 0.019 1.000 . Uiso c ? H(7) 0.3361 0.5013 0.9159 0.020 1.000 . Uiso c ? H(8) 0.4340 0.5736 0.9082 0.020 1.000 . Uiso c ? H(9) 0.2743 0.6956 0.7574 0.016 1.000 . Uiso c ? H(10) 0.4111 0.6671 0.7365 0.016 1.000 . Uiso c ? H(11) 0.3381 0.6146 0.5474 0.014 1.000 . Uiso c ? H(12) 0.2841 0.7052 0.5509 0.014 1.000 . Uiso c ? H(13) 0.0462 0.7164 0.3814 0.018 1.000 . Uiso c ? H(14) 0.1003 0.6377 0.3217 0.018 1.000 . Uiso c ? H(15) -0.0944 0.5728 0.3007 0.017 1.000 . Uiso c ? H(16) -0.1264 0.6645 0.2596 0.017 1.000 . Uiso c ? H(17) -0.3451 0.6549 0.3374 0.017 1.000 . Uiso c ? H(18) -0.3064 0.5610 0.3533 0.017 1.000 . Uiso c ? H(19) -0.4550 0.6092 0.4890 0.018 1.000 . Uiso c ? H(20) -0.3410 0.6591 0.5569 0.018 1.000 . Uiso c ? H(21) -0.4633 0.5412 0.6736 0.018 1.000 . Uiso c ? H(22) -0.3633 0.4725 0.7174 0.018 1.000 . Uiso c ? H(23) -0.3366 0.5765 0.8634 0.016 1.000 . Uiso c ? H(24) -0.3329 0.6456 0.7642 0.016 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te(1) 0.0103(1) 0.0088(2) 0.0094(1) 0.00043(10) 0.00358(10) 0.00012(9) Te(2) 0.0099(1) 0.0096(2) 0.00814(13) -0.00009(10) 0.00266(10) -0.00060(9) Pd(1) 0.0087(2) 0.0083(2) 0.0070(2) 0.00083(11) 0.00188(11) 0.00004(10) Cl(1) 0.0214(5) 0.0114(5) 0.0169(5) 0.0052(4) 0.0091(4) 0.0001(4) Cl(2) 0.0159(5) 0.0100(5) 0.0139(5) -0.0014(4) 0.0021(4) 0.0022(4) O(1) 0.015(2) 0.013(1) 0.021(2) 0.0009(12) 0.0044(12) 0.0008(12) O(2) 0.019(2) 0.009(1) 0.0114(13) -0.0008(12) 0.0007(12) 0.0006(11) O(3) 0.0104(13) 0.023(2) 0.0087(13) 0.0035(12) 0.0021(11) -0.0031(12) O(4) 0.016(1) 0.017(2) 0.0111(13) 0.0023(12) 0.0036(11) -0.0005(11) C(1) 0.017(2) 0.017(2) 0.010(2) 0.002(2) 0.004(2) 0.002(2) C(2) 0.019(2) 0.013(2) 0.008(2) -0.002(2) 0.001(2) -0.000(2) C(3) 0.014(2) 0.017(2) 0.015(2) -0.006(2) -0.002(2) -0.000(2) C(4) 0.013(2) 0.019(2) 0.014(2) -0.001(2) -0.005(2) 0.000(2) C(5) 0.012(2) 0.007(2) 0.023(2) 0.001(2) -0.002(2) 0.000(2) C(6) 0.004(2) 0.015(2) 0.017(2) 0.001(2) 0.002(2) 0.000(2) C(7) 0.017(2) 0.016(2) 0.009(2) 0.006(2) 0.005(2) 0.005(2) C(8) 0.020(2) 0.009(2) 0.011(2) 0.001(2) 0.007(2) 0.000(2) C(9) 0.014(2) 0.020(2) 0.012(2) 0.000(2) -0.002(2) -0.003(2) C(10) 0.012(2) 0.020(2) 0.011(2) 0.005(2) -0.004(2) 0.001(2) C(11) 0.011(2) 0.018(2) 0.021(2) -0.002(2) 0.002(2) 0.003(2) C(12) 0.010(2) 0.017(2) 0.014(2) -0.001(2) 0.006(2) -0.003(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3811 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_all 0.0470 _refine_ls_wR_factor_ref 0.0470 _refine_ls_goodness_of_fit_all 1.647 _refine_ls_goodness_of_fit_ref 1.650 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -2.47 _refine_diff_density_max 1.33 #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te(1) Pd(1) 2.5567(5) . . ? Te(1) C(1) 2.157(5) . . ? Te(1) C(12) 2.156(5) . . ? Te(2) Pd(1) 2.5398(5) . . ? Te(2) C(6) 2.144(5) . . ? Te(2) C(7) 2.151(5) . . ? Pd(1) Cl(1) 2.3474(13) . . ? Pd(1) Cl(2) 2.3618(12) . . ? O(1) C(2) 1.423(6) . . ? O(1) C(3) 1.433(6) . . ? O(2) C(4) 1.444(6) . . ? O(2) C(5) 1.446(6) . . ? O(3) C(8) 1.409(6) . . ? O(3) C(9) 1.438(6) . . ? O(4) C(10) 1.440(6) . . ? O(4) C(11) 1.415(6) . . ? C(1) C(2) 1.483(7) . . ? C(1) H(1) 0.94 . . no C(1) H(2) 0.96 . . no C(2) H(3) 0.96 . . no C(2) H(4) 0.94 . . no C(3) C(4) 1.512(8) . . ? C(3) H(5) 0.95 . . no C(3) H(6) 0.96 . . no C(4) H(7) 0.95 . . no C(4) H(8) 0.97 . . no C(5) C(6) 1.501(7) . . ? C(5) H(9) 0.94 . . no C(5) H(10) 0.96 . . no C(6) H(11) 0.97 . . no C(6) H(12) 0.94 . . no C(7) C(8) 1.507(7) . . ? C(7) H(13) 0.97 . . no C(7) H(14) 0.96 . . no C(8) H(15) 0.96 . . no C(8) H(16) 0.96 . . no C(9) C(10) 1.498(7) . . ? C(9) H(17) 0.95 . . no C(9) H(18) 0.97 . . no C(10) H(19) 0.96 . . no C(10) H(20) 0.95 . . no C(11) C(12) 1.513(7) . . ? C(11) H(21) 0.96 . . no C(11) H(22) 0.97 . . no C(12) H(23) 0.96 . . no C(12) H(24) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd(1) Te(1) C(1) 100.3(1) . . . ? Pd(1) Te(1) C(12) 105.6(1) . . . ? C(1) Te(1) C(12) 92.8(2) . . . ? Pd(1) Te(2) C(6) 100.73(13) . . . ? Pd(1) Te(2) C(7) 100.09(13) . . . ? C(6) Te(2) C(7) 96.4(2) . . . ? Te(1) Pd(1) Te(2) 88.29(2) . . . ? Te(1) Pd(1) Cl(1) 89.98(3) . . . ? Te(1) Pd(1) Cl(2) 173.07(3) . . . ? Te(2) Pd(1) Cl(1) 175.27(4) . . . ? Te(2) Pd(1) Cl(2) 88.84(3) . . . ? Cl(1) Pd(1) Cl(2) 93.35(4) . . . ? C(2) O(1) C(3) 112.7(4) . . . ? C(4) O(2) C(5) 114.4(4) . . . ? C(8) O(3) C(9) 114.1(4) . . . ? C(10) O(4) C(11) 111.6(4) . . . ? Te(1) C(1) C(2) 109.7(3) . . . ? Te(1) C(1) H(1) 110.5 . . . no Te(1) C(1) H(2) 109.4 . . . no C(2) C(1) H(1) 109.7 . . . no C(2) C(1) H(2) 108.6 . . . no H(1) C(1) H(2) 108.9 . . . no O(1) C(2) C(1) 107.6(4) . . . ? O(1) C(2) H(3) 109.6 . . . no O(1) C(2) H(4) 111.1 . . . no C(1) C(2) H(3) 109.8 . . . no C(1) C(2) H(4) 109.9 . . . no H(3) C(2) H(4) 108.8 . . . no O(1) C(3) C(4) 107.8(4) . . . ? O(1) C(3) H(5) 110.7 . . . no O(1) C(3) H(6) 109.6 . . . no C(4) C(3) H(5) 109.7 . . . no C(4) C(3) H(6) 109.7 . . . no H(5) C(3) H(6) 109.3 . . . no O(2) C(4) C(3) 112.6(4) . . . ? O(2) C(4) H(7) 109.6 . . . no O(2) C(4) H(8) 108.8 . . . no C(3) C(4) H(7) 109.6 . . . no C(3) C(4) H(8) 108.5 . . . no H(7) C(4) H(8) 107.5 . . . no O(2) C(5) C(6) 106.3(4) . . . ? O(2) C(5) H(9) 111.1 . . . no O(2) C(5) H(10) 109.9 . . . no C(6) C(5) H(9) 109.8 . . . no C(6) C(5) H(10) 110.3 . . . no H(9) C(5) H(10) 109.4 . . . no Te(2) C(6) C(5) 108.7(3) . . . ? Te(2) C(6) H(11) 109.3 . . . no Te(2) C(6) H(12) 111.0 . . . no C(5) C(6) H(11) 108.7 . . . no C(5) C(6) H(12) 110.5 . . . no H(11) C(6) H(12) 108.6 . . . no Te(2) C(7) C(8) 108.8(3) . . . ? Te(2) C(7) H(13) 109.7 . . . no Te(2) C(7) H(14) 110.2 . . . no C(8) C(7) H(13) 109.6 . . . no C(8) C(7) H(14) 111.0 . . . no H(13) C(7) H(14) 107.6 . . . no O(3) C(8) C(7) 107.8(4) . . . ? O(3) C(8) H(15) 110.7 . . . no O(3) C(8) H(16) 110.3 . . . no C(7) C(8) H(15) 109.6 . . . no C(7) C(8) H(16) 110.7 . . . no H(15) C(8) H(16) 107.8 . . . no O(3) C(9) C(10) 108.1(4) . . . ? O(3) C(9) H(17) 110.5 . . . no O(3) C(9) H(18) 110.2 . . . no C(10) C(9) H(17) 110.7 . . . no C(10) C(9) H(18) 109.3 . . . no H(17) C(9) H(18) 108.0 . . . no O(4) C(10) C(9) 109.4(4) . . . ? O(4) C(10) H(19) 109.6 . . . no O(4) C(10) H(20) 110.4 . . . no C(9) C(10) H(19) 109.5 . . . no C(9) C(10) H(20) 109.2 . . . no H(19) C(10) H(20) 108.7 . . . no O(4) C(11) C(12) 113.4(4) . . . ? O(4) C(11) H(21) 108.8 . . . no O(4) C(11) H(22) 108.6 . . . no C(12) C(11) H(21) 109.6 . . . no C(12) C(11) H(22) 109.2 . . . no H(21) C(11) H(22) 107.0 . . . no Te(1) C(12) C(11) 108.1(3) . . . ? Te(1) C(12) H(23) 109.1 . . . no Te(1) C(12) H(24) 109.4 . . . no C(11) C(12) H(23) 111.1 . . . no C(11) C(12) H(24) 110.2 . . . no H(23) C(12) H(24) 108.9 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(6) 3.499(5) . 4_465 no Cl(1) C(7) 3.569(5) . 4_465 no Cl(2) C(3) 3.414(5) . 4_464 no Cl(2) C(9) 3.600(5) . 4_565 no O(1) C(1) 3.418(6) . 3_567 no O(2) C(9) 3.454(6) . 3_566 no O(4) C(6) 3.507(6) . 3_566 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Te(1) Pd(1) Te(2) C(6) . . . . -125.71(13) no Te(1) Pd(1) Te(2) C(7) . . . . 135.8(1) no Te(1) C(1) C(2) O(1) . . . . -45.4(4) no Te(1) C(12) C(11) O(4) . . . . -49.8(5) no Te(2) Pd(1) Te(1) C(1) . . . . 135.8(1) no Te(2) Pd(1) Te(1) C(12) . . . . -128.3(1) no Te(2) C(6) C(5) O(2) . . . . 51.0(4) no Te(2) C(7) C(8) O(3) . . . . 44.2(4) no Pd(1) Te(1) C(1) C(2) . . . . -51.9(3) no Pd(1) Te(1) C(12) C(11) . . . . 103.3(3) no Pd(1) Te(2) C(6) C(5) . . . . 55.6(3) no Pd(1) Te(2) C(7) C(8) . . . . -78.2(3) no Cl(1) Pd(1) Te(1) C(1) . . . . -48.6(1) no Cl(1) Pd(1) Te(1) C(12) . . . . 47.2(1) no Cl(1) Pd(1) Te(2) C(6) . . . . 165.6(4) no Cl(1) Pd(1) Te(2) C(7) . . . . 67.1(4) no Cl(2) Pd(1) Te(1) C(1) . . . . 70.2(3) no Cl(2) Pd(1) Te(1) C(12) . . . . 166.1(3) no Cl(2) Pd(1) Te(2) C(6) . . . . 48.0(1) no Cl(2) Pd(1) Te(2) C(7) . . . . -50.5(1) no O(1) C(3) C(4) O(2) . . . . 62.0(5) no O(3) C(9) C(10) O(4) . . . . -74.9(5) no C(1) Te(1) C(12) C(11) . . . . -155.2(3) no C(1) C(2) O(1) C(3) . . . . 177.2(4) no C(2) O(1) C(3) C(4) . . . . -163.3(4) no C(2) C(1) Te(1) C(12) . . . . -158.3(3) no C(3) C(4) O(2) C(5) . . . . 66.4(5) no C(4) O(2) C(5) C(6) . . . . 173.9(4) no C(5) C(6) Te(2) C(7) . . . . 157.2(3) no C(6) Te(2) C(7) C(8) . . . . 179.7(3) no C(7) C(8) O(3) C(9) . . . . -178.5(4) no C(8) O(3) C(9) C(10) . . . . 167.9(4) no C(9) C(10) O(4) C(11) . . . . 177.7(4) no C(10) O(4) C(11) C(12) . . . . -74.9(5) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================