#------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'P. Shiv Halasyamani' _publ_contact_author_address ; Department of Chemistry University of Houston Houston, Texas 77204-5003 USA ; _publ_contact_author_email psh@uh.edu _publ_contact_author_fax '1-713-743-0796' _publ_contact_author_phone '1-713-743-3278' _publ_requested_journal '' #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; ; loop_ _publ_author_name ; Hong Young Chang, Sun Woo Kim,and P. Shiv Halasyamani ; _publ_author_address ; Department of Chemistry University of Houston Houston, Texas 77204-5003 USA Department of Chemistry Chung-Ang University Seoul 155-756 Korea ; data_Rb2SeMo3O12 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'Mo3 O12 Rb2 Se' _chemical_formula_weight 729.72 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 7.2992(14) _cell_length_b 7.2992(14) _cell_length_c 11.978(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 552.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 4.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.453 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.4574 _exptl_absorpt_correction_T_max 0.7475 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_number 3445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 28.91 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 911 _reflns_number_gt 898 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0349P)^2^+0.4029P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0081(8) _refine_ls_number_reflns 911 _refine_ls_number_parameters 56 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0552 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(9) _refine_diff_density_max 1.316 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.164 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Rb1 Rb 0.3333 0.6667 0.55749(9) 0.0393(3) Uani 1 3 d S . . Rb2 Rb 0.6667 0.3333 0.43194(7) 0.0228(2) Uani 1 3 d S . . Mo1 Mo 0.33987(5) 0.13343(5) 0.76926(3) 0.00851(13) Uani 1 1 d . . . Se1 Se 0 0 0.00052(6) 0.00964(17) Uani 1 3 d S . . O1 O 0.4083(6) 0.2026(6) 0.6328(3) 0.0157(7) Uani 1 1 d . . . O2 O 0.2460(5) 0.1271(5) 0.9403(3) 0.0148(6) Uani 1 1 d . . . O3 O 0.5465(5) 0.0857(5) 0.8171(3) 0.0134(6) Uani 1 1 d . . . O4 O 0.1234(4) 0.8697(4) 0.7551(3) 0.0136(6) 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 Rb1 0.0437(4) 0.0437(4) 0.0305(6) 0 0 0.0219(2) Rb2 0.0253(3) 0.0253(3) 0.0178(4) 0 0 0.01263(14) Mo1 0.00589(17) 0.00726(18) 0.0121(2) -0.00046(14) 0.00008(13) 0.00310(12) Se1 0.0099(2) 0.0099(2) 0.0092(3) 0 0 0.00494(10) O1 0.0128(16) 0.0150(17) 0.0176(17) 0.0014(13) 0.0007(13) 0.0056(14) O2 0.0081(14) 0.0166(15) 0.0149(17) 0.0011(12) 0.0033(13) 0.0026(12) O3 0.0096(14) 0.0142(16) 0.0174(15) 0.0002(12) -0.0009(12) 0.0067(13) O4 0.0106(12) 0.0087(13) 0.0197(16) -0.0013(13) 0.0010(13) 0.0035(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Rb1 O2 3.007(3) 5_564 ? Rb1 O2 3.007(3) 6_554 ? Rb1 O2 3.007(3) 4_664 ? Rb1 O3 3.278(4) 5_564 ? Rb1 O3 3.278(4) 4_664 ? Rb1 O3 3.278(4) 6_554 ? Rb1 O4 3.524(3) . ? Rb1 O4 3.524(3) 3_565 ? Rb1 O4 3.524(3) 2_665 ? Rb1 Mo1 4.0320(15) 5_564 ? Rb1 Mo1 4.0320(15) 4_664 ? Rb1 Mo1 4.0320(15) 6_554 ? Rb2 O1 2.908(4) 2_655 ? Rb2 O1 2.908(4) 3_665 ? Rb2 O1 2.908(4) . ? Rb2 O3 2.985(3) 4_654 ? Rb2 O3 2.985(3) 5_664 ? Rb2 O3 2.985(3) 6_554 ? Rb2 O4 3.362(3) 4_664 ? Rb2 O4 3.362(3) 6_654 ? Rb2 O4 3.362(3) 5_554 ? Rb2 Mo1 3.9044(9) 4_654 ? Rb2 Mo1 3.9044(9) 5_664 ? Rb2 Mo1 3.9044(9) 6_554 ? Mo1 O1 1.709(4) . ? Mo1 O4 1.786(3) 1_545 ? Mo1 O3 1.803(3) . ? Mo1 O4 2.117(3) 2_665 ? Mo1 O3 2.122(3) 3_665 ? Mo1 O2 2.154(3) . ? Mo1 Rb2 3.9044(9) 4_655 ? Mo1 Rb1 4.0320(15) 4_665 ? Mo1 Rb1 4.2286(11) 1_545 ? Se1 O2 1.714(3) 3_554 ? Se1 O2 1.714(3) 1_554 ? Se1 O2 1.714(3) 2_554 ? O2 Se1 1.714(3) 1_556 ? O2 Rb1 3.007(3) 4_665 ? O3 Mo1 2.122(3) 2_655 ? O3 Rb2 2.985(3) 4_655 ? O3 Rb1 3.278(4) 4_665 ? O4 Mo1 1.786(3) 1_565 ? O4 Mo1 2.117(3) 3_565 ? O4 Rb2 3.362(3) 4_665 ? 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 Rb1 O2 99.98(8) 5_564 6_554 ? O2 Rb1 O2 99.98(8) 5_564 4_664 ? O2 Rb1 O2 99.98(8) 6_554 4_664 ? O2 Rb1 O3 52.35(8) 5_564 5_564 ? O2 Rb1 O3 50.84(8) 6_554 5_564 ? O2 Rb1 O3 90.70(9) 4_664 5_564 ? O2 Rb1 O3 50.84(8) 5_564 4_664 ? O2 Rb1 O3 90.70(9) 6_554 4_664 ? O2 Rb1 O3 52.35(8) 4_664 4_664 ? O3 Rb1 O3 48.86(10) 5_564 4_664 ? O2 Rb1 O3 90.70(9) 5_564 6_554 ? O2 Rb1 O3 52.35(8) 6_554 6_554 ? O2 Rb1 O3 50.84(8) 4_664 6_554 ? O3 Rb1 O3 48.86(10) 5_564 6_554 ? O3 Rb1 O3 48.86(10) 4_664 6_554 ? O2 Rb1 O4 70.02(8) 5_564 . ? O2 Rb1 O4 128.99(7) 6_554 . ? O2 Rb1 O4 130.76(8) 4_664 . ? O3 Rb1 O4 114.55(8) 5_564 . ? O3 Rb1 O4 114.26(8) 4_664 . ? O3 Rb1 O4 160.72(8) 6_554 . ? O2 Rb1 O4 128.99(7) 5_564 3_565 ? O2 Rb1 O4 130.76(8) 6_554 3_565 ? O2 Rb1 O4 70.02(8) 4_664 3_565 ? O3 Rb1 O4 160.72(8) 5_564 3_565 ? O3 Rb1 O4 114.55(8) 4_664 3_565 ? O3 Rb1 O4 114.26(8) 6_554 3_565 ? O4 Rb1 O4 79.83(9) . 3_565 ? O2 Rb1 O4 130.76(8) 5_564 2_665 ? O2 Rb1 O4 70.02(8) 6_554 2_665 ? O2 Rb1 O4 128.99(7) 4_664 2_665 ? O3 Rb1 O4 114.26(8) 5_564 2_665 ? O3 Rb1 O4 160.72(8) 4_664 2_665 ? O3 Rb1 O4 114.55(8) 6_554 2_665 ? O4 Rb1 O4 79.83(9) . 2_665 ? O4 Rb1 O4 79.83(9) 3_565 2_665 ? O2 Rb1 Mo1 31.57(6) 5_564 5_564 ? O2 Rb1 Mo1 76.79(6) 6_554 5_564 ? O2 Rb1 Mo1 83.20(7) 4_664 5_564 ? O3 Rb1 Mo1 26.03(5) 5_564 5_564 ? O3 Rb1 Mo1 31.66(5) 4_664 5_564 ? O3 Rb1 Mo1 59.53(6) 6_554 5_564 ? O4 Rb1 Mo1 101.24(6) . 5_564 ? O4 Rb1 Mo1 143.54(5) 3_565 5_564 ? O4 Rb1 Mo1 136.54(5) 2_665 5_564 ? O2 Rb1 Mo1 76.79(6) 5_564 4_664 ? O2 Rb1 Mo1 83.20(7) 6_554 4_664 ? O2 Rb1 Mo1 31.57(6) 4_664 4_664 ? O3 Rb1 Mo1 59.53(6) 5_564 4_664 ? O3 Rb1 Mo1 26.03(5) 4_664 4_664 ? O3 Rb1 Mo1 31.66(5) 6_554 4_664 ? O4 Rb1 Mo1 136.54(5) . 4_664 ? O4 Rb1 Mo1 101.24(6) 3_565 4_664 ? O4 Rb1 Mo1 143.54(5) 2_665 4_664 ? Mo1 Rb1 Mo1 53.15(2) 5_564 4_664 ? O2 Rb1 Mo1 83.20(7) 5_564 6_554 ? O2 Rb1 Mo1 31.57(6) 6_554 6_554 ? O2 Rb1 Mo1 76.79(6) 4_664 6_554 ? O3 Rb1 Mo1 31.66(5) 5_564 6_554 ? O3 Rb1 Mo1 59.53(6) 4_664 6_554 ? O3 Rb1 Mo1 26.03(5) 6_554 6_554 ? O4 Rb1 Mo1 143.54(5) . 6_554 ? O4 Rb1 Mo1 136.54(5) 3_565 6_554 ? O4 Rb1 Mo1 101.24(6) 2_665 6_554 ? Mo1 Rb1 Mo1 53.15(2) 5_564 6_554 ? Mo1 Rb1 Mo1 53.15(2) 4_664 6_554 ? O1 Rb2 O1 58.20(12) 2_655 3_665 ? O1 Rb2 O1 58.20(12) 2_655 . ? O1 Rb2 O1 58.20(12) 3_665 . ? O1 Rb2 O3 98.02(10) 2_655 4_654 ? O1 Rb2 O3 151.61(10) 3_665 4_654 ? O1 Rb2 O3 97.18(10) . 4_654 ? O1 Rb2 O3 97.18(10) 2_655 5_664 ? O1 Rb2 O3 98.02(10) 3_665 5_664 ? O1 Rb2 O3 151.61(10) . 5_664 ? O3 Rb2 O3 100.44(8) 4_654 5_664 ? O1 Rb2 O3 151.61(10) 2_655 6_554 ? O1 Rb2 O3 97.18(10) 3_665 6_554 ? O1 Rb2 O3 98.02(9) . 6_554 ? O3 Rb2 O3 100.44(8) 4_654 6_554 ? O3 Rb2 O3 100.44(8) 5_664 6_554 ? O1 Rb2 O4 94.89(9) 2_655 4_664 ? O1 Rb2 O4 137.59(9) 3_665 4_664 ? O1 Rb2 O4 137.77(9) . 4_664 ? O3 Rb2 O4 51.45(7) 4_654 4_664 ? O3 Rb2 O4 49.71(7) 5_664 4_664 ? O3 Rb2 O4 113.49(10) 6_554 4_664 ? O1 Rb2 O4 137.59(9) 2_655 6_654 ? O1 Rb2 O4 137.77(9) 3_665 6_654 ? O1 Rb2 O4 94.89(9) . 6_654 ? O3 Rb2 O4 49.71(7) 4_654 6_654 ? O3 Rb2 O4 113.49(10) 5_664 6_654 ? O3 Rb2 O4 51.45(7) 6_554 6_654 ? O4 Rb2 O4 84.52(9) 4_664 6_654 ? O1 Rb2 O4 137.77(9) 2_655 5_554 ? O1 Rb2 O4 94.89(9) 3_665 5_554 ? O1 Rb2 O4 137.59(9) . 5_554 ? O3 Rb2 O4 113.49(10) 4_654 5_554 ? O3 Rb2 O4 51.45(7) 5_664 5_554 ? O3 Rb2 O4 49.71(7) 6_554 5_554 ? O4 Rb2 O4 84.52(9) 4_664 5_554 ? O4 Rb2 O4 84.52(9) 6_654 5_554 ? O1 Rb2 Mo1 89.78(7) 2_655 4_654 ? O1 Rb2 Mo1 147.03(7) 3_665 4_654 ? O1 Rb2 Mo1 113.81(7) . 4_654 ? O3 Rb2 Mo1 26.25(6) 4_654 4_654 ? O3 Rb2 Mo1 76.80(6) 5_664 4_654 ? O3 Rb2 Mo1 115.79(7) 6_554 4_654 ? O4 Rb2 Mo1 27.16(5) 4_664 4_654 ? O4 Rb2 Mo1 70.78(5) 6_654 4_654 ? O4 Rb2 Mo1 105.99(6) 5_554 4_654 ? O1 Rb2 Mo1 113.81(7) 2_655 5_664 ? O1 Rb2 Mo1 89.78(7) 3_665 5_664 ? O1 Rb2 Mo1 147.03(7) . 5_664 ? O3 Rb2 Mo1 115.79(7) 4_654 5_664 ? O3 Rb2 Mo1 26.25(6) 5_664 5_664 ? O3 Rb2 Mo1 76.80(6) 6_554 5_664 ? O4 Rb2 Mo1 70.78(5) 4_664 5_664 ? O4 Rb2 Mo1 105.99(6) 6_654 5_664 ? O4 Rb2 Mo1 27.16(5) 5_554 5_664 ? Mo1 Rb2 Mo1 97.26(2) 4_654 5_664 ? O1 Rb2 Mo1 147.03(7) 2_655 6_554 ? O1 Rb2 Mo1 113.81(7) 3_665 6_554 ? O1 Rb2 Mo1 89.78(7) . 6_554 ? O3 Rb2 Mo1 76.80(6) 4_654 6_554 ? O3 Rb2 Mo1 115.79(7) 5_664 6_554 ? O3 Rb2 Mo1 26.25(6) 6_554 6_554 ? O4 Rb2 Mo1 105.99(6) 4_664 6_554 ? O4 Rb2 Mo1 27.16(5) 6_654 6_554 ? O4 Rb2 Mo1 70.78(5) 5_554 6_554 ? Mo1 Rb2 Mo1 97.26(2) 4_654 6_554 ? Mo1 Rb2 Mo1 97.26(2) 5_664 6_554 ? O1 Mo1 O4 101.41(17) . 1_545 ? O1 Mo1 O3 102.21(16) . . ? O4 Mo1 O3 101.36(14) 1_545 . ? O1 Mo1 O4 88.03(16) . 2_665 ? O4 Mo1 O4 90.33(18) 1_545 2_665 ? O3 Mo1 O4 162.45(15) . 2_665 ? O1 Mo1 O3 89.68(16) . 3_665 ? O4 Mo1 O3 164.23(14) 1_545 3_665 ? O3 Mo1 O3 87.00(19) . 3_665 ? O4 Mo1 O3 78.76(12) 2_665 3_665 ? O1 Mo1 O2 163.44(14) . . ? O4 Mo1 O2 88.11(14) 1_545 . ? O3 Mo1 O2 88.95(14) . . ? O4 Mo1 O2 78.30(13) 2_665 . ? O3 Mo1 O2 78.61(12) 3_665 . ? O1 Mo1 Rb2 127.53(13) . 4_655 ? O4 Mo1 Rb2 59.26(10) 1_545 4_655 ? O3 Mo1 Rb2 47.10(10) . 4_655 ? O4 Mo1 Rb2 134.89(9) 2_665 4_655 ? O3 Mo1 Rb2 121.90(9) 3_665 4_655 ? O2 Mo1 Rb2 69.00(8) . 4_655 ? O1 Mo1 Rb1 132.76(12) . 4_665 ? O4 Mo1 Rb1 121.07(11) 1_545 4_665 ? O3 Mo1 Rb1 52.93(11) . 4_665 ? O4 Mo1 Rb1 109.76(9) 2_665 4_665 ? O3 Mo1 Rb1 54.17(9) 3_665 4_665 ? O2 Mo1 Rb1 46.95(9) . 4_665 ? Rb2 Mo1 Rb1 68.615(17) 4_655 4_665 ? O1 Mo1 Rb1 63.17(13) . 1_545 ? O4 Mo1 Rb1 55.04(10) 1_545 1_545 ? O3 Mo1 Rb1 73.04(11) . 1_545 ? O4 Mo1 Rb1 124.50(9) 2_665 1_545 ? O3 Mo1 Rb1 140.73(9) 3_665 1_545 ? O2 Mo1 Rb1 132.70(8) . 1_545 ? Rb2 Mo1 Rb1 66.80(3) 4_655 1_545 ? Rb1 Mo1 Rb1 124.854(16) 4_665 1_545 ? O2 Se1 O2 103.58(13) 3_554 1_554 ? O2 Se1 O2 103.58(13) 3_554 2_554 ? O2 Se1 O2 103.58(13) 1_554 2_554 ? Mo1 O1 Rb2 158.99(19) . . ? Se1 O2 Mo1 130.35(17) 1_556 . ? Se1 O2 Rb1 127.29(15) 1_556 4_665 ? Mo1 O2 Rb1 101.48(12) . 4_665 ? Mo1 O3 Mo1 133.46(18) . 2_655 ? Mo1 O3 Rb2 106.65(12) . 4_655 ? Mo1 O3 Rb2 116.84(12) 2_655 4_655 ? Mo1 O3 Rb1 101.04(13) . 4_665 ? Mo1 O3 Rb1 94.16(10) 2_655 4_665 ? Rb2 O3 Rb1 91.07(9) 4_655 4_665 ? Mo1 O4 Mo1 147.66(17) 1_565 3_565 ? Mo1 O4 Rb2 93.58(12) 1_565 4_665 ? Mo1 O4 Rb2 103.60(11) 3_565 4_665 ? Mo1 O4 Rb1 100.42(12) 1_565 . ? Mo1 O4 Rb1 109.06(11) 3_565 . ? Rb2 O4 Rb1 81.25(7) 4_665 . ? #===END data_Tl2SeMo3O12 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'Mo3 O12 Se Tl2' _chemical_formula_weight 967.52 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P31c' _cell_length_a 7.2867(10) _cell_length_b 7.2867(10) _cell_length_c 11.794(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 542.33(18) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 5.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 36.398 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.1588 _exptl_absorpt_correction_T_max 0.3238 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0579 _diffrn_reflns_number 893 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 28.85 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 893 _reflns_number_gt 811 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0216P)^2^+0.9220P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0125(6) _refine_ls_number_reflns 893 _refine_ls_number_parameters 56 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(11) _refine_diff_density_max 2.732 _refine_diff_density_min -1.697 _refine_diff_density_rms 0.24 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tl1 Tl 0.3333 0.6667 0.34467(11) 0.0561(4) Uani 1 3 d S . . Tl2 Tl 0.6667 0.3333 0.22930(6) 0.0271(3) Uani 1 3 d S . . Mo1 Mo 0.33987(12) 0.13365(13) 0.56590(8) 0.0072(2) Uani 1 1 d . . . Se1 Se 0 0 0.30084(17) 0.0085(3) Uani 1 3 d S . . O1 O 0.4102(12) 0.2049(13) 0.4276(6) 0.0128(15) Uani 1 1 d . . . O2 O 0.2429(11) 0.1235(12) 0.7402(6) 0.0102(15) Uani 1 1 d . . . O3 O 0.5462(11) 0.0853(11) 0.6156(7) 0.0121(15) Uani 1 1 d . . . O4 O 0.1210(12) 0.8680(12) 0.5506(8) 0.0119(14) 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 Tl1 0.0709(6) 0.0709(6) 0.0266(5) 0 0 0.0354(3) Tl2 0.0295(4) 0.0295(4) 0.0224(4) 0 0 0.01473(18) Mo1 0.0056(4) 0.0062(4) 0.0099(4) -0.0006(3) 0.0001(3) 0.0030(3) Se1 0.0099(5) 0.0099(5) 0.0058(8) 0 0 0.0050(2) O1 0.011(4) 0.022(4) 0.009(4) 0.004(3) 0.003(3) 0.011(3) O2 0.002(3) 0.016(4) 0.009(4) -0.004(3) -0.003(3) 0.002(3) O3 0.007(3) 0.004(3) 0.021(4) -0.002(3) 0.000(3) -0.001(3) O4 0.010(4) 0.008(3) 0.016(4) 0.004(3) 0.003(3) 0.003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Tl1 O2 2.944(7) 5_564 ? Tl1 O2 2.944(7) 4_554 ? Tl1 O2 2.944(7) 6_664 ? Tl1 O3 3.123(8) 4_554 ? Tl1 O3 3.123(8) 5_564 ? Tl1 O3 3.123(8) 6_664 ? Tl1 O4 3.566(9) . ? Tl1 O4 3.566(9) 3_565 ? Tl1 O4 3.566(9) 2_665 ? Tl2 O1 2.844(7) 2_655 ? Tl2 O1 2.844(7) 3_665 ? Tl2 O1 2.844(7) . ? Tl2 O3 2.963(7) 5_554 ? Tl2 O3 2.963(7) 4_654 ? Tl2 O3 2.963(7) 6_664 ? Tl2 O4 3.355(8) 4_554 ? Tl2 O4 3.355(8) 5_664 ? Tl2 O4 3.355(8) 6_654 ? Mo1 O1 1.711(7) . ? Mo1 O4 1.799(8) 1_545 ? Mo1 O3 1.805(7) . ? Mo1 O4 2.098(8) 2_665 ? Mo1 O3 2.123(7) 3_665 ? Mo1 O2 2.163(7) . ? Se1 O2 1.692(7) 6_554 ? Se1 O2 1.692(7) 4_554 ? Se1 O2 1.692(7) 5_554 ? O2 Se1 1.692(7) 4 ? O2 Tl1 2.944(7) 4 ? O2 Tl2 3.676(8) 4 ? O2 Tl2 3.704(8) 4_545 ? O3 Mo1 2.123(7) 2_655 ? O3 Tl2 2.963(7) 4_545 ? O3 Tl1 3.123(8) 4 ? O4 Mo1 1.799(8) 1_565 ? O4 Mo1 2.098(8) 3_565 ? O4 Tl2 3.355(8) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tl1 O2 103.73(17) 5_564 4_554 ? O2 Tl1 O2 103.73(17) 5_564 6_664 ? O2 Tl1 O2 103.73(17) 4_554 6_664 ? O2 Tl1 O3 53.24(19) 5_564 4_554 ? O2 Tl1 O3 54.5(2) 4_554 4_554 ? O2 Tl1 O3 95.35(19) 6_664 4_554 ? O2 Tl1 O3 54.5(2) 5_564 5_564 ? O2 Tl1 O3 95.35(19) 4_554 5_564 ? O2 Tl1 O3 53.24(19) 6_664 5_564 ? O3 Tl1 O3 51.5(2) 4_554 5_564 ? O2 Tl1 O3 95.35(19) 5_564 6_664 ? O2 Tl1 O3 53.24(19) 4_554 6_664 ? O2 Tl1 O3 54.5(2) 6_664 6_664 ? O3 Tl1 O3 51.5(2) 4_554 6_664 ? O3 Tl1 O3 51.5(2) 5_564 6_664 ? O2 Tl1 O4 67.68(19) 5_564 . ? O2 Tl1 O4 127.72(19) 4_554 . ? O2 Tl1 O4 128.55(19) 6_664 . ? O3 Tl1 O4 113.32(18) 4_554 . ? O3 Tl1 O4 114.60(18) 5_564 . ? O3 Tl1 O4 162.99(19) 6_664 . ? O2 Tl1 O4 127.72(19) 5_564 3_565 ? O2 Tl1 O4 128.55(19) 4_554 3_565 ? O2 Tl1 O4 67.68(19) 6_664 3_565 ? O3 Tl1 O4 162.99(19) 4_554 3_565 ? O3 Tl1 O4 113.32(18) 5_564 3_565 ? O3 Tl1 O4 114.60(18) 6_664 3_565 ? O4 Tl1 O4 78.69(19) . 3_565 ? O2 Tl1 O4 128.55(19) 5_564 2_665 ? O2 Tl1 O4 67.68(19) 4_554 2_665 ? O2 Tl1 O4 127.72(19) 6_664 2_665 ? O3 Tl1 O4 114.60(18) 4_554 2_665 ? O3 Tl1 O4 162.99(19) 5_564 2_665 ? O3 Tl1 O4 113.32(18) 6_664 2_665 ? O4 Tl1 O4 78.69(19) . 2_665 ? O4 Tl1 O4 78.69(19) 3_565 2_665 ? O2 Tl1 Mo1 33.41(14) 5_564 5_564 ? O2 Tl1 Mo1 86.71(15) 4_554 5_564 ? O2 Tl1 Mo1 80.28(15) 6_664 5_564 ? O3 Tl1 Mo1 32.99(13) 4_554 5_564 ? O3 Tl1 Mo1 27.11(13) 5_564 5_564 ? O3 Tl1 Mo1 62.29(14) 6_664 5_564 ? O4 Tl1 Mo1 100.87(13) . 5_564 ? O4 Tl1 Mo1 136.15(13) 3_565 5_564 ? O4 Tl1 Mo1 144.85(12) 2_665 5_564 ? O2 Tl1 Mo1 80.28(15) 5_564 4_554 ? O2 Tl1 Mo1 33.41(14) 4_554 4_554 ? O2 Tl1 Mo1 86.71(15) 6_664 4_554 ? O3 Tl1 Mo1 27.11(13) 4_554 4_554 ? O3 Tl1 Mo1 62.29(14) 5_564 4_554 ? O3 Tl1 Mo1 32.99(13) 6_664 4_554 ? O4 Tl1 Mo1 136.15(13) . 4_554 ? O4 Tl1 Mo1 144.85(12) 3_565 4_554 ? O4 Tl1 Mo1 100.87(13) 2_665 4_554 ? Mo1 Tl1 Mo1 55.14(3) 5_564 4_554 ? O2 Tl1 Mo1 86.71(15) 5_564 6_664 ? O2 Tl1 Mo1 80.28(15) 4_554 6_664 ? O2 Tl1 Mo1 33.41(14) 6_664 6_664 ? O3 Tl1 Mo1 62.29(14) 4_554 6_664 ? O3 Tl1 Mo1 32.99(13) 5_564 6_664 ? O3 Tl1 Mo1 27.11(13) 6_664 6_664 ? O4 Tl1 Mo1 144.85(12) . 6_664 ? O4 Tl1 Mo1 100.87(13) 3_565 6_664 ? O4 Tl1 Mo1 136.15(13) 2_665 6_664 ? Mo1 Tl1 Mo1 55.14(3) 5_564 6_664 ? Mo1 Tl1 Mo1 55.14(3) 4_554 6_664 ? O1 Tl2 O1 59.1(3) 2_655 3_665 ? O1 Tl2 O1 59.1(3) 2_655 . ? O1 Tl2 O1 59.1(3) 3_665 . ? O1 Tl2 O3 96.6(2) 2_655 5_554 ? O1 Tl2 O3 151.6(2) 3_665 5_554 ? O1 Tl2 O3 97.0(2) . 5_554 ? O1 Tl2 O3 97.0(2) 2_655 4_654 ? O1 Tl2 O3 96.6(2) 3_665 4_654 ? O1 Tl2 O3 151.6(2) . 4_654 ? O3 Tl2 O3 101.10(18) 5_554 4_654 ? O1 Tl2 O3 151.6(2) 2_655 6_664 ? O1 Tl2 O3 97.0(2) 3_665 6_664 ? O1 Tl2 O3 96.6(2) . 6_664 ? O3 Tl2 O3 101.10(19) 5_554 6_664 ? O3 Tl2 O3 101.10(19) 4_654 6_664 ? O1 Tl2 O4 94.2(2) 2_655 4_554 ? O1 Tl2 O4 138.1(2) 3_665 4_554 ? O1 Tl2 O4 137.0(2) . 4_554 ? O3 Tl2 O4 49.73(19) 5_554 4_554 ? O3 Tl2 O4 51.97(19) 4_654 4_554 ? O3 Tl2 O4 114.2(2) 6_664 4_554 ? O1 Tl2 O4 138.1(2) 2_655 5_664 ? O1 Tl2 O4 137.0(2) 3_665 5_664 ? O1 Tl2 O4 94.2(2) . 5_664 ? O3 Tl2 O4 51.97(19) 5_554 5_664 ? O3 Tl2 O4 114.2(2) 4_654 5_664 ? O3 Tl2 O4 49.73(19) 6_664 5_664 ? O4 Tl2 O4 84.7(2) 4_554 5_664 ? O1 Tl2 O4 137.0(2) 2_655 6_654 ? O1 Tl2 O4 94.2(2) 3_665 6_654 ? O1 Tl2 O4 138.1(2) . 6_654 ? O3 Tl2 O4 114.2(2) 5_554 6_654 ? O3 Tl2 O4 49.73(19) 4_654 6_654 ? O3 Tl2 O4 51.97(19) 6_664 6_654 ? O4 Tl2 O4 84.7(2) 4_554 6_654 ? O4 Tl2 O4 84.7(2) 5_664 6_654 ? O1 Tl2 O2 55.98(18) 2_655 6_654 ? O1 Tl2 O2 114.4(2) 3_665 6_654 ? O1 Tl2 O2 93.39(18) . 6_654 ? O3 Tl2 O2 46.94(17) 5_554 6_654 ? O3 Tl2 O2 83.47(18) 4_654 6_654 ? O3 Tl2 O2 147.58(18) 6_664 6_654 ? O4 Tl2 O2 44.94(17) 4_554 6_654 ? O4 Tl2 O2 98.89(17) 5_664 6_654 ? O4 Tl2 O2 128.27(18) 6_654 6_654 ? O1 Tl2 O2 93.39(19) 2_655 5_664 ? O1 Tl2 O2 55.98(18) 3_665 5_664 ? O1 Tl2 O2 114.4(2) . 5_664 ? O3 Tl2 O2 147.58(18) 5_554 5_664 ? O3 Tl2 O2 46.94(17) 4_654 5_664 ? O3 Tl2 O2 83.47(18) 6_664 5_664 ? O4 Tl2 O2 98.89(17) 4_554 5_664 ? O4 Tl2 O2 128.27(18) 5_664 5_664 ? O4 Tl2 O2 44.94(17) 6_654 5_664 ? O2 Tl2 O2 119.878(14) 6_654 5_664 ? O1 Tl2 O2 114.4(2) 2_655 4_554 ? O1 Tl2 O2 93.39(18) 3_665 4_554 ? O1 Tl2 O2 55.98(18) . 4_554 ? O3 Tl2 O2 83.47(18) 5_554 4_554 ? O3 Tl2 O2 147.58(18) 4_654 4_554 ? O3 Tl2 O2 46.94(17) 6_664 4_554 ? O4 Tl2 O2 128.27(18) 4_554 4_554 ? O4 Tl2 O2 44.94(17) 5_664 4_554 ? O4 Tl2 O2 98.89(17) 6_654 4_554 ? O2 Tl2 O2 119.878(14) 6_654 4_554 ? O2 Tl2 O2 119.878(13) 5_664 4_554 ? O1 Mo1 O4 101.6(4) . 1_545 ? O1 Mo1 O3 102.5(3) . . ? O4 Mo1 O3 101.5(3) 1_545 . ? O1 Mo1 O4 87.8(4) . 2_665 ? O4 Mo1 O4 90.1(4) 1_545 2_665 ? O3 Mo1 O4 162.5(3) . 2_665 ? O1 Mo1 O3 89.6(3) . 3_665 ? O4 Mo1 O3 164.0(3) 1_545 3_665 ? O3 Mo1 O3 86.9(4) . 3_665 ? O4 Mo1 O3 78.9(3) 2_665 3_665 ? O1 Mo1 O2 163.7(3) . . ? O4 Mo1 O2 87.7(4) 1_545 . ? O3 Mo1 O2 88.5(3) . . ? O4 Mo1 O2 78.7(3) 2_665 . ? O3 Mo1 O2 78.9(3) 3_665 . ? O1 Mo1 Tl2 127.5(3) . 4_545 ? O4 Mo1 Tl2 59.4(2) 1_545 4_545 ? O3 Mo1 Tl2 46.8(2) . 4_545 ? O4 Mo1 Tl2 135.2(2) 2_665 4_545 ? O3 Mo1 Tl2 121.8(2) 3_665 4_545 ? O2 Mo1 Tl2 68.8(2) . 4_545 ? O1 Mo1 Tl1 131.1(3) . 4 ? O4 Mo1 Tl1 122.3(3) 1_545 4 ? O3 Mo1 Tl1 52.0(2) . 4 ? O4 Mo1 Tl1 110.6(2) 2_665 4 ? O3 Mo1 Tl1 53.2(2) 3_665 4 ? O2 Mo1 Tl1 48.53(19) . 4 ? Tl2 Mo1 Tl1 69.26(2) 4_545 4 ? O1 Mo1 Tl1 62.7(3) . 1_545 ? O4 Mo1 Tl1 55.3(3) 1_545 1_545 ? O3 Mo1 Tl1 73.8(2) . 1_545 ? O4 Mo1 Tl1 123.7(2) 2_665 1_545 ? O3 Mo1 Tl1 140.7(2) 3_665 1_545 ? O2 Mo1 Tl1 132.9(2) . 1_545 ? Tl2 Mo1 Tl1 67.37(3) 4_545 1_545 ? Tl1 Mo1 Tl1 125.13(2) 4 1_545 ? O1 Mo1 Tl2 106.6(3) . 4 ? O4 Mo1 Tl2 127.2(3) 1_545 4 ? O3 Mo1 Tl2 114.3(2) . 4 ? O4 Mo1 Tl2 48.4(2) 2_665 4 ? O3 Mo1 Tl2 37.3(2) 3_665 4 ? O2 Mo1 Tl2 57.4(2) . 4 ? Tl2 Mo1 Tl2 124.04(3) 4_545 4 ? Tl1 Mo1 Tl2 64.547(17) 4 4 ? Tl1 Mo1 Tl2 168.52(3) 1_545 4 ? O2 Se1 O2 103.4(3) 6_554 4_554 ? O2 Se1 O2 103.4(3) 6_554 5_554 ? O2 Se1 O2 103.4(3) 4_554 5_554 ? O2 Se1 Tl1 120.6(3) 6_554 1_545 ? O2 Se1 Tl1 119.6(3) 4_554 1_545 ? O2 Se1 Tl1 32.0(2) 5_554 1_545 ? O2 Se1 Tl1 119.6(3) 6_554 . ? O2 Se1 Tl1 32.0(2) 4_554 . ? O2 Se1 Tl1 120.6(3) 5_554 . ? Tl1 Se1 Tl1 118.535(14) 1_545 . ? O2 Se1 Tl1 32.0(2) 6_554 1_445 ? O2 Se1 Tl1 120.6(3) 4_554 1_445 ? O2 Se1 Tl1 119.6(3) 5_554 1_445 ? Tl1 Se1 Tl1 118.535(14) 1_545 1_445 ? Tl1 Se1 Tl1 118.535(14) . 1_445 ? Mo1 O1 Tl2 158.7(4) . . ? Se1 O2 Mo1 131.1(4) 4 . ? Se1 O2 Tl1 130.3(3) 4 4 ? Mo1 O2 Tl1 98.1(3) . 4 ? Se1 O2 Tl2 99.4(3) 4 4 ? Mo1 O2 Tl2 92.9(2) . 4 ? Tl1 O2 Tl2 83.03(17) 4 4 ? Se1 O2 Tl2 98.4(3) 4 4_545 ? Mo1 O2 Tl2 78.2(2) . 4_545 ? Tl1 O2 Tl2 82.52(17) 4 4_545 ? Tl2 O2 Tl2 161.8(2) 4 4_545 ? Mo1 O3 Mo1 132.8(4) . 2_655 ? Mo1 O3 Tl2 106.8(3) . 4_545 ? Mo1 O3 Tl2 117.0(3) 2_655 4_545 ? Mo1 O3 Tl1 100.8(3) . 4 ? Mo1 O3 Tl1 93.8(2) 2_655 4 ? Tl2 O3 Tl1 93.2(2) 4_545 4 ? Mo1 O4 Mo1 147.6(4) 1_565 3_565 ? Mo1 O4 Tl2 93.1(3) 1_565 4 ? Mo1 O4 Tl2 103.7(3) 3_565 4 ? Mo1 O4 Tl1 100.2(3) 1_565 . ? Mo1 O4 Tl1 109.4(3) 3_565 . ? Tl2 O4 Tl1 81.85(16) 4 . ? #===END