Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'William T. A. Harrison' 'J. T. S. Irvine' 'Magnus G. Johnston' 'Satish K. Tiwary' _publ_contact_author_name 'Dr William T A Harrison' _publ_contact_author_address ; Department of Chemistry University of Aberdeen Meston Walk Aberdeen Scotland AB24 3UE UNITED KINGDOM ; _publ_contact_author_email W.HARRISON@ABDN.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Lone-pair Containment in Closed Cavities. The MTe6O13 (M = Mn, Ni, Co) Family of Ternary Oxides ; data_mto _database_code_CSD 201289 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'decomposes before melting' _chemical_formula_moiety ? _chemical_formula_sum 'Mn O13 Te6' _chemical_formula_weight 1028.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.2505(5) _cell_length_b 10.2505(5) _cell_length_c 19.2195(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1748.89(15) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4318 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 32.48 _exptl_crystal_description 'faceted rhomb' _exptl_crystal_colour 'very pale pink' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2646 _exptl_absorpt_coefficient_mu 15.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.185 _exptl_absorpt_correction_T_max 0.251 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5886 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 32.49 _reflns_number_total 1417 _reflns_number_gt 1360 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0171P)^2^+16.2711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00066(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1417 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0510 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _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 Mn1 Mn 0.0000 0.0000 0.24417(4) 0.00862(16) Uani 1 3 d S . . Te1 Te 0.15413(3) 0.23722(3) 0.404036(11) 0.00994(7) Uani 1 1 d . . . Te2 Te 0.23094(2) 0.05956(3) 0.091045(11) 0.00858(7) Uani 1 1 d . . . O1 O 0.0876(3) 0.2059(3) 0.30814(13) 0.0142(5) Uani 1 1 d . . . O2 O 0.1968(3) 0.0486(3) 0.18604(13) 0.0131(5) Uani 1 1 d . . . O3 O 0.0000 0.0000 0.4113(2) 0.0115(8) Uani 1 3 d S . . O4 O 0.3335(3) -0.0819(3) 0.11389(14) 0.0141(5) Uani 1 1 d . . . O5 O 0.1289(3) 0.1822(3) 0.06988(14) 0.0128(5) 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 Mn1 0.0084(2) 0.0084(2) 0.0091(4) 0.000 0.000 0.00420(12) Te1 0.00907(11) 0.01306(11) 0.00962(11) -0.00099(7) -0.00017(7) 0.00697(8) Te2 0.00792(10) 0.00924(11) 0.00818(10) 0.00038(6) 0.00084(6) 0.00400(8) O1 0.0212(13) 0.0089(11) 0.0104(10) -0.0009(8) -0.0031(9) 0.0058(10) O2 0.0115(11) 0.0185(13) 0.0098(11) 0.0017(9) 0.0020(9) 0.0078(10) O3 0.0091(11) 0.0091(11) 0.016(2) 0.000 0.000 0.0046(6) O4 0.0141(12) 0.0158(12) 0.0167(12) 0.0016(9) 0.0040(9) 0.0106(10) O5 0.0103(11) 0.0132(11) 0.0164(12) 0.0001(9) 0.0004(9) 0.0072(10) _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 Mn1 O2 2.136(3) 3 ? Mn1 O2 2.136(3) 2 ? Mn1 O2 2.136(3) . ? Mn1 O1 2.208(3) . ? Mn1 O1 2.208(3) 3 ? Mn1 O1 2.208(3) 2 ? Te1 O4 1.853(3) 4_455 ? Te1 O1 1.936(3) . ? Te1 O3 2.1416(4) . ? Te1 O1 2.179(3) 16 ? Te1 Te1 3.2907(5) 16 ? Te2 O2 1.852(3) . ? Te2 O5 1.922(3) 3 ? Te2 O5 2.039(3) . ? Te2 O4 2.219(3) . ? Te2 O2 2.615(3) 13 ? O1 Te1 2.179(3) 16 ? O2 Te2 2.615(3) 13 ? O3 Te1 2.1416(4) 2 ? O3 Te1 2.1416(4) 3 ? O4 Te1 1.853(3) 7_544 ? O5 Te2 1.922(3) 2 ? 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 O2 Mn1 O2 95.14(10) 3 2 ? O2 Mn1 O2 95.14(10) 3 . ? O2 Mn1 O2 95.14(10) 2 . ? O2 Mn1 O1 162.05(11) 3 . ? O2 Mn1 O1 74.90(10) 2 . ? O2 Mn1 O1 100.54(11) . . ? O2 Mn1 O1 100.54(11) 3 3 ? O2 Mn1 O1 162.05(11) 2 3 ? O2 Mn1 O1 74.90(10) . 3 ? O1 Mn1 O1 92.01(10) . 3 ? O2 Mn1 O1 74.90(10) 3 2 ? O2 Mn1 O1 100.54(11) 2 2 ? O2 Mn1 O1 162.05(11) . 2 ? O1 Mn1 O1 92.01(10) . 2 ? O1 Mn1 O1 92.01(10) 3 2 ? O4 Te1 O1 101.33(12) 4_455 . ? O4 Te1 O3 83.47(10) 4_455 . ? O1 Te1 O3 82.81(14) . . ? O4 Te1 O1 91.90(12) 4_455 16 ? O1 Te1 O1 73.92(12) . 16 ? O3 Te1 O1 154.92(12) . 16 ? O4 Te1 Te1 97.90(8) 4_455 16 ? O1 Te1 Te1 39.51(8) . 16 ? O3 Te1 Te1 121.74(11) . 16 ? O1 Te1 Te1 34.41(7) 16 16 ? O2 Te2 O5 95.31(12) . 3 ? O2 Te2 O5 95.42(11) . . ? O5 Te2 O5 93.29(15) 3 . ? O2 Te2 O4 84.38(11) . . ? O5 Te2 O4 84.56(11) 3 . ? O5 Te2 O4 177.81(10) . . ? O2 Te2 O2 73.20(11) . 13 ? O5 Te2 O2 166.59(10) 3 13 ? O5 Te2 O2 94.65(10) . 13 ? O4 Te2 O2 87.39(10) . 13 ? Te1 O1 Te1 106.08(12) . 16 ? Te1 O1 Mn1 129.05(13) . . ? Te1 O1 Mn1 122.49(12) 16 . ? Te2 O2 Mn1 131.11(14) . . ? Te2 O2 Te2 106.80(11) . 13 ? Mn1 O2 Te2 110.38(11) . 13 ? Te1 O3 Te1 119.58(3) 2 . ? Te1 O3 Te1 119.58(3) 2 3 ? Te1 O3 Te1 119.58(3) . 3 ? Te1 O4 Te2 131.56(14) 7_544 . ? Te2 O5 Te2 137.13(14) 2 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.856 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.221 #===END data_cto _database_code_CSD 201290 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'decomposes before melting' _chemical_formula_moiety ? _chemical_formula_sum 'Co O13 Te6' _chemical_formula_weight 1032.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.1641(5) _cell_length_b 10.1641(5) _cell_length_c 18.9814(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1698.23(14) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3860 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 32.49 _exptl_crystal_description chunk _exptl_crystal_colour 'intense purple' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2658 _exptl_absorpt_coefficient_mu 16.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.078 _exptl_absorpt_correction_T_max 0.135 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4461 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 32.50 _reflns_number_total 1364 _reflns_number_gt 1340 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0145P)^2^+19.3233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'from analogue' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00176(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1364 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 1.384 _refine_ls_restrained_S_all 1.384 _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 Co1 Co 0.0000 0.0000 0.24401(4) 0.00644(15) Uani 1 3 d S . . Te1 Te 0.15564(3) 0.23755(3) 0.404936(11) 0.00779(8) Uani 1 1 d . . . Te2 Te 0.23254(2) 0.06187(3) 0.090712(11) 0.00650(8) Uani 1 1 d . . . O1 O 0.0895(3) 0.2034(3) 0.30747(13) 0.0111(5) Uani 1 1 d . . . O2 O 0.1942(3) 0.0519(3) 0.18688(13) 0.0101(4) Uani 1 1 d . . . O3 O 0.0000 0.0000 0.4139(2) 0.0087(7) Uani 1 3 d S . . O4 O 0.3328(3) -0.0818(3) 0.11516(14) 0.0116(5) Uani 1 1 d . . . O5 O 0.1291(3) 0.1837(3) 0.06907(14) 0.0105(4) 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 Co1 0.0071(2) 0.0071(2) 0.0052(3) 0.000 0.000 0.00353(11) Te1 0.00760(11) 0.01182(11) 0.00576(11) -0.00065(6) -0.00009(6) 0.00620(8) Te2 0.00703(11) 0.00795(11) 0.00417(11) 0.00024(6) 0.00054(6) 0.00348(8) O1 0.0174(12) 0.0089(11) 0.0051(9) 0.0001(8) -0.0021(9) 0.0051(9) O2 0.0112(11) 0.0157(12) 0.0038(10) -0.0005(8) 0.0017(8) 0.0070(10) O3 0.0074(11) 0.0074(11) 0.0111(18) 0.000 0.000 0.0037(5) O4 0.0129(11) 0.0147(12) 0.0118(11) 0.0023(9) 0.0044(9) 0.0104(10) O5 0.0090(11) 0.0121(11) 0.0127(11) 0.0025(9) 0.0020(8) 0.0069(9) _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 Co1 O2 2.076(3) 3 ? Co1 O2 2.076(3) 2 ? Co1 O2 2.076(3) . ? Co1 O1 2.161(3) . ? Co1 O1 2.161(3) 2 ? Co1 O1 2.161(3) 3 ? Te1 O4 1.857(3) 4_455 ? Te1 O1 1.939(2) . ? Te1 O3 2.1311(4) . ? Te1 O1 2.183(3) 16 ? Te1 O4 2.927(3) 17 ? Te2 O2 1.859(2) . ? Te2 O5 1.923(3) 3 ? Te2 O5 2.027(3) . ? Te2 O4 2.208(3) . ? Te2 O2 2.570(3) 13 ? O1 Te1 2.183(3) 16 ? O2 Te2 2.570(3) 13 ? O3 Te1 2.1311(4) 2 ? O3 Te1 2.1311(4) 3 ? O4 Te1 1.857(3) 7_544 ? O4 Te1 2.927(3) 18_545 ? O5 Te2 1.923(3) 2 ? 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 O2 Co1 O2 95.20(10) 3 2 ? O2 Co1 O2 95.20(10) 3 . ? O2 Co1 O2 95.20(10) 2 . ? O2 Co1 O1 163.87(11) 3 . ? O2 Co1 O1 75.93(10) 2 . ? O2 Co1 O1 98.97(11) . . ? O2 Co1 O1 75.93(10) 3 2 ? O2 Co1 O1 98.97(11) 2 2 ? O2 Co1 O1 163.87(11) . 2 ? O1 Co1 O1 91.95(10) . 2 ? O2 Co1 O1 98.97(11) 3 3 ? O2 Co1 O1 163.87(11) 2 3 ? O2 Co1 O1 75.93(10) . 3 ? O1 Co1 O1 91.95(10) . 3 ? O1 Co1 O1 91.95(10) 2 3 ? O4 Te1 O1 101.86(12) 4_455 . ? O4 Te1 O3 82.68(10) 4_455 . ? O1 Te1 O3 83.02(14) . . ? O4 Te1 O1 90.81(11) 4_455 16 ? O1 Te1 O1 74.47(12) . 16 ? O3 Te1 O1 154.76(11) . 16 ? O4 Te1 O4 81.30(7) 4_455 17 ? O1 Te1 O4 172.97(10) . 17 ? O3 Te1 O4 91.23(12) . 17 ? O1 Te1 O4 111.94(8) 16 17 ? O2 Te2 O5 95.11(12) . 3 ? O2 Te2 O5 94.22(11) . . ? O5 Te2 O5 93.46(16) 3 . ? O2 Te2 O4 84.90(11) . . ? O5 Te2 O4 83.64(11) 3 . ? O5 Te2 O4 176.87(11) . . ? O2 Te2 O2 74.04(11) . 13 ? O5 Te2 O2 165.88(10) 3 13 ? O5 Te2 O2 96.29(10) . 13 ? O4 Te2 O2 86.36(10) . 13 ? Te1 O1 Co1 130.20(14) . . ? Te1 O1 Te1 105.53(12) . 16 ? Co1 O1 Te1 122.61(11) . 16 ? Te2 O2 Co1 132.36(14) . . ? Te2 O2 Te2 105.96(11) . 13 ? Co1 O2 Te2 111.99(10) . 13 ? Te1 O3 Te1 119.38(3) 2 . ? Te1 O3 Te1 119.38(3) 2 3 ? Te1 O3 Te1 119.38(3) . 3 ? Te1 O4 Te2 130.68(14) 7_544 . ? Te1 O4 Te1 120.50(12) 7_544 18_545 ? Te2 O4 Te1 105.85(9) . 18_545 ? Te2 O5 Te2 136.76(14) 2 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.965 _refine_diff_density_min -1.352 _refine_diff_density_rms 0.244 #===END data_nto _database_code_CSD 201291 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'decomposes before melting' _chemical_formula_moiety ? _chemical_formula_sum 'Ni O13 Te6' _chemical_formula_weight 1032.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.1522(5) _cell_length_b 10.1522(5) _cell_length_c 18.8669(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1684.04(14) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4127 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 32.50 _exptl_crystal_description rhomb _exptl_crystal_colour 'yellowish green' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 17.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.280 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5768 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 32.56 _reflns_number_total 1356 _reflns_number_gt 1294 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0184P)^2^+21.5925P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'from analogue' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00061(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1356 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.24353(4) 0.00699(15) Uani 1 3 d S . . Te1 Te 0.15581(3) 0.23779(3) 0.405279(12) 0.00829(8) Uani 1 1 d . . . Te2 Te 0.23294(2) 0.06277(3) 0.090528(12) 0.00716(8) Uani 1 1 d . . . O1 O 0.0924(3) 0.2028(3) 0.30678(14) 0.0114(5) Uani 1 1 d . . . O2 O 0.1937(3) 0.0542(3) 0.18726(14) 0.0104(5) Uani 1 1 d . . . O3 O 0.0000 0.0000 0.4142(2) 0.0092(8) Uani 1 3 d S . . O4 O 0.3316(3) -0.0832(3) 0.11542(15) 0.0125(5) Uani 1 1 d . . . O5 O 0.1287(3) 0.1840(3) 0.06876(15) 0.0115(5) 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 Ni1 0.0079(2) 0.0079(2) 0.0053(3) 0.000 0.000 0.00393(10) Te1 0.00837(11) 0.01241(12) 0.00566(12) -0.00054(7) -0.00003(7) 0.00638(8) Te2 0.00801(11) 0.00882(11) 0.00432(11) 0.00021(7) 0.00046(7) 0.00397(8) O1 0.0184(13) 0.0091(11) 0.0045(10) -0.0005(8) -0.0021(9) 0.0053(10) O2 0.0104(11) 0.0167(12) 0.0046(10) 0.0015(9) 0.0023(9) 0.0072(10) O3 0.0095(11) 0.0095(11) 0.009(2) 0.000 0.000 0.0048(6) O4 0.0138(12) 0.0151(12) 0.0137(12) 0.0022(10) 0.0037(9) 0.0110(10) O5 0.0116(11) 0.0116(11) 0.0130(12) 0.0025(9) 0.0025(9) 0.0071(10) _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 Ni1 O2 2.053(3) 3 ? Ni1 O2 2.053(3) . ? Ni1 O2 2.053(3) 2 ? Ni1 O1 2.148(3) . ? Ni1 O1 2.148(3) 3 ? Ni1 O1 2.148(3) 2 ? Te1 O4 1.857(3) 4_455 ? Te1 O1 1.940(3) . ? Te1 O3 2.1306(4) . ? Te1 O1 2.183(3) 16 ? Te1 O4 2.896(3) 17 ? Te2 O2 1.861(3) . ? Te2 O5 1.922(3) 3 ? Te2 O5 2.026(3) . ? Te2 O4 2.214(3) . ? Te2 O2 2.551(3) 13 ? O1 Te1 2.183(3) 16 ? O2 Te2 2.551(3) 13 ? O3 Te1 2.1306(4) 2 ? O3 Te1 2.1306(4) 3 ? O4 Te1 1.857(3) 7_544 ? O4 Te1 2.896(3) 18_545 ? O5 Te2 1.922(3) 2 ? 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 O2 Ni1 O2 95.67(10) 3 . ? O2 Ni1 O2 95.67(10) 3 2 ? O2 Ni1 O2 95.67(10) . 2 ? O2 Ni1 O1 165.28(11) 3 . ? O2 Ni1 O1 97.44(11) . . ? O2 Ni1 O1 76.43(11) 2 . ? O2 Ni1 O1 97.44(11) 3 3 ? O2 Ni1 O1 76.43(11) . 3 ? O2 Ni1 O1 165.28(11) 2 3 ? O1 Ni1 O1 92.12(10) . 3 ? O2 Ni1 O1 76.43(11) 3 2 ? O2 Ni1 O1 165.28(11) . 2 ? O2 Ni1 O1 97.44(11) 2 2 ? O1 Ni1 O1 92.12(10) . 2 ? O1 Ni1 O1 92.12(10) 3 2 ? O4 Te1 O1 102.54(13) 4_455 . ? O4 Te1 O3 82.25(10) 4_455 . ? O1 Te1 O3 82.99(14) . . ? O4 Te1 O1 90.22(12) 4_455 16 ? O1 Te1 O1 74.77(12) . 16 ? O3 Te1 O1 154.38(12) . 16 ? O4 Te1 O4 81.45(7) 4_455 17 ? O1 Te1 O4 172.37(10) . 17 ? O3 Te1 O4 91.20(13) . 17 ? O1 Te1 O4 111.95(9) 16 17 ? O2 Te2 O5 95.26(12) . 3 ? O2 Te2 O5 93.57(12) . . ? O5 Te2 O5 93.42(16) 3 . ? O2 Te2 O4 85.35(11) . . ? O5 Te2 O4 83.01(11) 3 . ? O5 Te2 O4 176.15(11) . . ? O2 Te2 O2 74.18(11) . 13 ? O5 Te2 O2 165.43(11) 3 13 ? O5 Te2 O2 97.17(10) . 13 ? O4 Te2 O2 86.10(10) . 13 ? Te1 O1 Ni1 130.80(14) . . ? Te1 O1 Te1 105.23(12) . 16 ? Ni1 O1 Te1 122.93(12) . 16 ? Te2 O2 Ni1 132.37(15) . . ? Te2 O2 Te2 105.82(11) . 13 ? Ni1 O2 Te2 113.14(11) . 13 ? Te1 O3 Te1 119.38(3) 2 . ? Te1 O3 Te1 119.38(3) 2 3 ? Te1 O3 Te1 119.38(3) . 3 ? Te1 O4 Te2 130.14(14) 7_544 . ? Te1 O4 Te1 120.46(12) 7_544 18_545 ? Te2 O4 Te1 106.06(10) . 18_545 ? Te2 O5 Te2 136.78(15) 2 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.56 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.331 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.233 # end of file