# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ba O9 Te W2' _chemical_formula_sum 'Ba O9 Te W2' _chemical_formula_weight 776.64 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.9824(8) _cell_length_b 5.5774(3) _cell_length_c 9.8671(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 769.49(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3482 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.37 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 38.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1481 _exptl_absorpt_correction_T_max 0.2483 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX2 CCD area-detector diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5163 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.37 _reflns_number_total 871 _reflns_number_gt 842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker,2005)' _computing_cell_refinement 'APEX2 Software Suite (Bruker,2005)' _computing_data_reduction 'APEX2 Software Suite (Bruker,2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker,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^)+(0.0105P)^2^+3.1746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00418(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 871 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0370 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _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 W1 W 0.17269(2) 0.2500 0.45181(3) 0.01058(11) Uani 1 2 d S . . W2 W 0.47902(2) 0.2500 0.77034(3) 0.01010(12) Uani 1 2 d S . . Te Te 0.36884(4) 0.2500 0.20263(5) 0.01117(14) Uani 1 2 d S . . Ba Ba 0.10610(4) 0.2500 0.05890(5) 0.01364(14) Uani 1 2 d S . . O1 O 0.0863(3) 0.0034(8) 0.3327(4) 0.0166(9) Uani 1 1 d . . . O2 O 0.2361(3) 0.0095(8) 0.5191(4) 0.0201(10) Uani 1 1 d . . . O3 O 0.4183(3) 0.5007(8) 0.3101(4) 0.0163(9) Uani 1 1 d . . . O4 O 0.0712(5) 0.2500 0.5704(6) 0.0173(13) Uani 1 2 d S . . O5 O 0.2438(4) 0.2500 0.2728(6) 0.0156(13) Uani 1 2 d S . . O6 O 0.4395(4) 0.2500 0.5992(6) 0.0157(13) Uani 1 2 d S . . 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 W1 0.0107(2) 0.01139(18) 0.00968(18) 0.000 0.00011(12) 0.000 W2 0.0103(2) 0.00973(18) 0.01031(18) 0.000 -0.00018(12) 0.000 Te 0.0096(3) 0.0127(3) 0.0112(3) 0.000 0.0009(2) 0.000 Ba 0.0128(3) 0.0145(3) 0.0136(3) 0.000 -0.00137(19) 0.000 O1 0.014(2) 0.020(2) 0.015(2) -0.0021(18) 0.0022(18) -0.0030(18) O2 0.016(2) 0.023(2) 0.020(2) 0.0064(19) 0.0036(18) 0.0040(19) O3 0.015(2) 0.017(2) 0.017(2) -0.0020(18) 0.0014(17) -0.0051(18) O4 0.015(4) 0.020(3) 0.017(3) 0.000 0.001(3) 0.000 O5 0.010(3) 0.024(3) 0.013(3) 0.000 -0.001(2) 0.000 O6 0.012(3) 0.019(3) 0.016(3) 0.000 -0.002(3) 0.000 _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 W1 O2 1.739(4) 7_565 ? W1 O2 1.739(4) . ? W1 O4 1.840(6) . ? W1 O5 2.026(6) . ? W1 O1 2.176(4) . ? W1 O1 2.176(4) 7_565 ? W1 Ba 3.9871(6) . ? W2 O6 1.776(6) . ? W2 O1 1.792(4) 2 ? W2 O1 1.792(4) 8_666 ? W2 O4 2.032(6) 6_657 ? W2 O3 2.150(4) 5_666 ? W2 O3 2.150(4) 3_646 ? W2 Ba 3.6805(4) 2 ? W2 Ba 3.6805(4) 2_565 ? W2 Ba 3.7029(6) 6_656 ? Te O5 1.881(6) . ? Te O3 1.886(4) . ? Te O3 1.886(4) 7_565 ? Te Ba 3.9379(8) . ? Ba O2 2.668(4) 8_665 ? Ba O2 2.668(4) 2_554 ? Ba O6 2.803(6) 6_556 ? Ba O3 2.842(4) 8_655 ? Ba O3 2.842(4) 2_564 ? Ba O5 2.856(6) . ? Ba O6 2.8883(16) 2_554 ? Ba O6 2.8883(16) 2_564 ? Ba O1 3.044(4) 7_565 ? Ba O1 3.044(4) . ? Ba O3 3.244(4) 4_455 ? Ba O3 3.244(4) 6_556 ? O1 W2 1.792(4) 2_554 ? O2 Ba 2.668(4) 2 ? O3 W2 2.150(4) 5_666 ? O3 Ba 2.842(4) 2_565 ? O3 Ba 3.244(4) 6_656 ? O4 W2 2.032(6) 6_557 ? O6 Ba 2.803(6) 6_656 ? O6 Ba 2.8883(16) 2 ? O6 Ba 2.8883(16) 2_565 ? 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 W1 O2 100.9(3) 7_565 . ? O2 W1 O4 98.65(19) 7_565 . ? O2 W1 O4 98.65(19) . . ? O2 W1 O5 94.75(18) 7_565 . ? O2 W1 O5 94.75(18) . . ? O4 W1 O5 158.9(3) . . ? O2 W1 O1 167.61(19) 7_565 . ? O2 W1 O1 90.09(19) . . ? O4 W1 O1 85.15(18) . . ? O5 W1 O1 78.53(17) . . ? O2 W1 O1 90.09(19) 7_565 7_565 ? O2 W1 O1 167.61(19) . 7_565 ? O4 W1 O1 85.15(18) . 7_565 ? O5 W1 O1 78.53(17) . 7_565 ? O1 W1 O1 78.4(2) . 7_565 ? O2 W1 Ba 119.34(15) 7_565 . ? O2 W1 Ba 119.34(15) . . ? O4 W1 Ba 116.00(19) . . ? O5 W1 Ba 42.87(17) . . ? O1 W1 Ba 49.07(11) . . ? O1 W1 Ba 49.07(11) 7_565 . ? O6 W2 O1 99.65(18) . 2 ? O6 W2 O1 99.65(17) . 8_666 ? O1 W2 O1 104.1(3) 2 8_666 ? O6 W2 O4 158.8(3) . 6_657 ? O1 W2 O4 93.32(17) 2 6_657 ? O1 W2 O4 93.32(17) 8_666 6_657 ? O6 W2 O3 81.78(19) . 5_666 ? O1 W2 O3 167.71(19) 2 5_666 ? O1 W2 O3 87.55(18) 8_666 5_666 ? O4 W2 O3 82.06(17) 6_657 5_666 ? O6 W2 O3 81.78(18) . 3_646 ? O1 W2 O3 87.55(18) 2 3_646 ? O1 W2 O3 167.71(19) 8_666 3_646 ? O4 W2 O3 82.06(17) 6_657 3_646 ? O3 W2 O3 80.6(2) 5_666 3_646 ? O6 W2 Ba 50.26(3) . 2 ? O1 W2 Ba 55.39(14) 2 2 ? O1 W2 Ba 128.85(13) 8_666 2 ? O4 W2 Ba 130.04(3) 6_657 2 ? O3 W2 Ba 119.78(11) 5_666 2 ? O3 W2 Ba 61.12(12) 3_646 2 ? O6 W2 Ba 50.26(3) . 2_565 ? O1 W2 Ba 128.85(13) 2 2_565 ? O1 W2 Ba 55.39(14) 8_666 2_565 ? O4 W2 Ba 130.04(3) 6_657 2_565 ? O3 W2 Ba 61.12(12) 5_666 2_565 ? O3 W2 Ba 119.78(11) 3_646 2_565 ? Ba W2 Ba 98.523(15) 2 2_565 ? O6 W2 Ba 46.79(19) . 6_656 ? O1 W2 Ba 123.08(14) 2 6_656 ? O1 W2 Ba 123.08(14) 8_666 6_656 ? O4 W2 Ba 111.97(18) 6_657 6_656 ? O3 W2 Ba 49.90(11) 5_666 6_656 ? O3 W2 Ba 49.90(11) 3_646 6_656 ? Ba W2 Ba 69.993(11) 2 6_656 ? Ba W2 Ba 69.993(11) 2_565 6_656 ? O5 Te O3 97.69(18) . . ? O5 Te O3 97.69(18) . 7_565 ? O3 Te O3 95.7(3) . 7_565 ? O5 Te Ba 42.71(18) . . ? O3 Te Ba 122.98(13) . . ? O3 Te Ba 122.98(13) 7_565 . ? O2 Ba O2 65.71(19) 8_665 2_554 ? O2 Ba O6 127.24(13) 8_665 6_556 ? O2 Ba O6 127.24(13) 2_554 6_556 ? O2 Ba O3 103.73(13) 8_665 8_655 ? O2 Ba O3 72.94(13) 2_554 8_655 ? O6 Ba O3 54.52(13) 6_556 8_655 ? O2 Ba O3 72.94(13) 8_665 2_564 ? O2 Ba O3 103.73(13) 2_554 2_564 ? O6 Ba O3 54.52(13) 6_556 2_564 ? O3 Ba O3 58.57(17) 8_655 2_564 ? O2 Ba O5 63.36(13) 8_665 . ? O2 Ba O5 63.36(13) 2_554 . ? O6 Ba O5 166.18(17) 6_556 . ? O3 Ba O5 135.98(12) 8_655 . ? O3 Ba O5 135.98(12) 2_564 . ? O2 Ba O6 136.62(15) 8_665 2_554 ? O2 Ba O6 71.29(15) 2_554 2_554 ? O6 Ba O6 83.87(12) 6_556 2_554 ? O3 Ba O6 67.68(14) 8_655 2_554 ? O3 Ba O6 124.39(15) 2_564 2_554 ? O5 Ba O6 92.70(12) . 2_554 ? O2 Ba O6 71.29(15) 8_665 2_564 ? O2 Ba O6 136.62(15) 2_554 2_564 ? O6 Ba O6 83.87(12) 6_556 2_564 ? O3 Ba O6 124.39(15) 8_655 2_564 ? O3 Ba O6 67.68(14) 2_564 2_564 ? O5 Ba O6 92.70(12) . 2_564 ? O6 Ba O6 149.8(2) 2_554 2_564 ? O2 Ba O1 87.75(12) 8_665 7_565 ? O2 Ba O1 116.81(12) 2_554 7_565 ? O6 Ba O1 114.73(13) 6_556 7_565 ? O3 Ba O1 167.64(12) 8_655 7_565 ? O3 Ba O1 122.32(12) 2_564 7_565 ? O5 Ba O1 53.53(13) . 7_565 ? O6 Ba O1 107.10(14) 2_554 7_565 ? O6 Ba O1 54.64(14) 2_564 7_565 ? O2 Ba O1 116.81(12) 8_665 . ? O2 Ba O1 87.75(12) 2_554 . ? O6 Ba O1 114.73(13) 6_556 . ? O3 Ba O1 122.32(12) 8_655 . ? O3 Ba O1 167.64(12) 2_564 . ? O5 Ba O1 53.53(13) . . ? O6 Ba O1 54.64(14) 2_554 . ? O6 Ba O1 107.10(14) 2_564 . ? O1 Ba O1 53.73(16) 7_565 . ? O2 Ba O3 164.17(12) 8_665 4_455 ? O2 Ba O3 119.63(12) 2_554 4_455 ? O6 Ba O3 63.21(13) 6_556 4_455 ? O3 Ba O3 92.08(11) 8_655 4_455 ? O3 Ba O3 117.26(7) 2_564 4_455 ? O5 Ba O3 104.54(13) . 4_455 ? O6 Ba O3 49.46(14) 2_554 4_455 ? O6 Ba O3 100.51(14) 2_564 4_455 ? O1 Ba O3 76.56(11) 7_565 4_455 ? O1 Ba O3 51.53(11) . 4_455 ? O2 Ba O3 119.63(12) 8_665 6_556 ? O2 Ba O3 164.17(12) 2_554 6_556 ? O6 Ba O3 63.21(13) 6_556 6_556 ? O3 Ba O3 117.26(7) 8_655 6_556 ? O3 Ba O3 92.08(11) 2_564 6_556 ? O5 Ba O3 104.54(13) . 6_556 ? O6 Ba O3 100.51(14) 2_554 6_556 ? O6 Ba O3 49.46(14) 2_564 6_556 ? O1 Ba O3 51.53(11) 7_565 6_556 ? O1 Ba O3 76.56(11) . 6_556 ? O3 Ba O3 51.07(15) 4_455 6_556 ? W2 O1 W1 165.3(3) 2_554 . ? W2 O1 Ba 95.64(16) 2_554 . ? W1 O1 Ba 98.24(14) . . ? W1 O2 Ba 153.6(2) . 2 ? Te O3 W2 121.1(2) . 5_666 ? Te O3 Ba 143.5(2) . 2_565 ? W2 O3 Ba 94.74(14) 5_666 2_565 ? Te O3 Ba 101.60(17) . 6_656 ? W2 O3 Ba 83.40(13) 5_666 6_656 ? Ba O3 Ba 87.92(11) 2_565 6_656 ? W1 O4 W2 168.9(4) . 6_557 ? Te O5 W1 141.0(3) . . ? Te O5 Ba 110.8(2) . . ? W1 O5 Ba 108.3(2) . . ? W2 O6 Ba 105.7(3) . 6_656 ? W2 O6 Ba 101.51(12) . 2 ? Ba O6 Ba 96.13(12) 6_656 2 ? W2 O6 Ba 101.51(12) . 2_565 ? Ba O6 Ba 96.13(12) 6_656 2_565 ? Ba O6 Ba 149.8(2) 2 2_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.456 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.252 _database_code_depnum_ccdc_archive 'CCDC 953707'