data_c:\crystal _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Th 4+)2, B O4 5-, P O4 3-' _chemical_formula_sum 'B O8 P Th2' _chemical_formula_weight 633.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4665(2) _cell_length_b 7.9552(2) _cell_length_c 8.22970(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.7460(10) _cell_angle_gamma 90.00 _cell_volume 538.42(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.0315 _exptl_crystal_size_mid 0.0252 _exptl_crystal_size_min 0.00904 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 55.478 _exptl_absorpt_correction_type 'Numerical' _exptl_absorpt_correction_T_min 0.2044 _exptl_absorpt_correction_T_max 0.6057 _exptl_absorpt_process_details 'HABITUS, W. Herrendorf, Univ. Giessen, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Apex2 (Bruker)' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15431 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 30.52 _reflns_number_total 1614 _reflns_number_gt 1245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00244(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1614 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0351 _refine_ls_wR_factor_gt 0.0334 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _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 Th1 Th 0.18301(3) 0.69330(4) 0.04140(3) 0.00646(8) Uani 1 1 d . . . Th2 Th 0.24191(3) 0.31714(4) 0.42356(3) 0.00528(8) Uani 1 1 d . . . B1 B 0.0326(10) 0.0570(11) 0.2188(10) 0.0063(15) Uiso 1 1 d . . . P1 P 0.5434(2) 0.4538(2) 0.2167(2) 0.0059(4) Uani 1 1 d . . . O1 O 0.0564(6) 0.8933(6) 0.1556(6) 0.0085(11) Uani 1 1 d . . . O2 O 0.0892(6) 0.0673(7) 0.4033(6) 0.0059(10) Uani 1 1 d . . . O3 O 0.1088(6) 0.1991(7) 0.1487(6) 0.0076(10) Uani 1 1 d . . . O4 O 0.1462(6) 0.5874(6) 0.3231(6) 0.0068(10) Uani 1 1 d . . . O5 O 0.6315(6) 0.3114(7) 0.1541(6) 0.0119(11) Uani 1 1 d . . . O6 O 0.4294(6) 0.1263(6) 0.3522(6) 0.0098(11) Uani 1 1 d . . . O7 O 0.3902(6) 0.9511(7) 0.0931(6) 0.0091(11) Uani 1 1 d . . . O8 O 0.3578(6) 0.4229(7) 0.1725(6) 0.0084(11) 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 Th1 0.00731(13) 0.00517(14) 0.00756(13) -0.00028(11) 0.00309(10) 0.00031(11) Th2 0.00504(12) 0.00538(14) 0.00527(13) -0.00025(11) 0.00094(9) -0.00012(11) P1 0.0039(8) 0.0066(9) 0.0073(9) -0.0004(7) 0.0015(7) -0.0002(7) O1 0.014(3) 0.002(3) 0.011(3) -0.001(2) 0.005(2) -0.001(2) O2 0.009(2) 0.005(3) 0.002(2) 0.001(2) -0.0015(19) -0.004(2) O3 0.010(2) 0.007(3) 0.005(2) -0.003(2) 0.0013(19) -0.002(2) O4 0.004(2) 0.005(3) 0.009(3) 0.000(2) -0.0034(19) 0.001(2) O5 0.011(3) 0.014(3) 0.012(3) -0.005(2) 0.005(2) -0.003(2) O6 0.016(3) 0.006(3) 0.009(3) 0.001(2) 0.006(2) 0.001(2) O7 0.007(2) 0.012(3) 0.007(2) 0.000(2) -0.002(2) 0.002(2) O8 0.006(2) 0.009(3) 0.008(3) 0.001(2) -0.002(2) 0.001(2) _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 Th1 O1 2.245(5) . ? Th1 O2 2.406(5) 4_565 ? Th1 O4 2.471(5) 4_575 ? Th1 O5 2.501(5) 3_665 ? Th1 O4 2.554(5) . ? Th1 O2 2.650(5) 2 ? Th1 O7 2.666(5) . ? Th1 O8 2.688(5) . ? Th1 O3 2.729(5) 3_565 ? Th1 O5 2.786(5) 2_655 ? Th1 B1 3.163(8) 3_565 ? Th1 P1 3.3814(19) 2_655 ? Th2 O2 2.355(5) . ? Th2 O6 2.369(5) . ? Th2 O4 2.376(5) . ? Th2 O3 2.390(4) 4_566 ? Th2 O3 2.461(5) . ? Th2 O7 2.467(5) 4_576 ? Th2 O1 2.527(5) 2_545 ? Th2 O8 2.627(5) . ? Th2 O8 2.802(5) 4_566 ? Th2 B1 2.974(9) . ? Th2 B1 3.020(9) 2 ? Th2 Th1 3.8064(3) 2_545 ? B1 O1 1.434(10) 1_545 ? B1 O2 1.482(9) . ? B1 O3 1.484(10) . ? B1 O4 1.490(9) 2_545 ? B1 Th2 3.020(9) 2_545 ? B1 Th1 3.163(8) 3_565 ? P1 O5 1.512(6) . ? P1 O6 1.523(5) 2_655 ? P1 O7 1.533(5) 2_645 ? P1 O8 1.546(5) . ? P1 Th1 3.3815(19) 2_645 ? O1 B1 1.434(10) 1_565 ? O1 Th2 2.527(5) 2 ? O2 Th1 2.406(5) 4_566 ? O2 Th1 2.650(5) 2_545 ? O3 Th2 2.390(4) 4_565 ? O3 Th1 2.729(5) 3_565 ? O4 B1 1.490(9) 2 ? O4 Th1 2.471(5) 4_576 ? O5 Th1 2.501(5) 3_665 ? O5 Th1 2.786(5) 2_645 ? O6 P1 1.523(5) 2_645 ? O7 P1 1.533(5) 2_655 ? O7 Th2 2.467(5) 4_575 ? O8 Th2 2.802(5) 4_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 O1 Th1 O2 132.16(17) . 4_565 ? O1 Th1 O4 79.26(17) . 4_575 ? O2 Th1 O4 107.12(16) 4_565 4_575 ? O1 Th1 O5 135.64(18) . 3_665 ? O2 Th1 O5 82.55(16) 4_565 3_665 ? O4 Th1 O5 62.15(17) 4_575 3_665 ? O1 Th1 O4 71.39(17) . . ? O2 Th1 O4 92.68(15) 4_565 . ? O4 Th1 O4 150.65(14) 4_575 . ? O5 Th1 O4 144.03(17) 3_665 . ? O1 Th1 O2 71.03(16) . 2 ? O2 Th1 O2 63.41(17) 4_565 2 ? O4 Th1 O2 115.32(15) 4_575 2 ? O5 Th1 O2 144.03(16) 3_665 2 ? O4 Th1 O2 54.60(14) . 2 ? O1 Th1 O7 75.50(16) . . ? O2 Th1 O7 150.31(15) 4_565 . ? O4 Th1 O7 62.43(15) 4_575 . ? O5 Th1 O7 67.94(16) 3_665 . ? O4 Th1 O7 109.06(15) . . ? O2 Th1 O7 146.06(15) 2 . ? O1 Th1 O8 132.16(17) . . ? O2 Th1 O8 65.70(16) 4_565 . ? O4 Th1 O8 145.04(15) 4_575 . ? O5 Th1 O8 82.89(16) 3_665 . ? O4 Th1 O8 62.98(15) . . ? O2 Th1 O8 92.66(15) 2 . ? O7 Th1 O8 105.86(15) . . ? O1 Th1 O3 63.93(16) . 3_565 ? O2 Th1 O3 81.20(16) 4_565 3_565 ? O4 Th1 O3 54.63(15) 4_575 3_565 ? O5 Th1 O3 104.90(15) 3_665 3_565 ? O4 Th1 O3 109.56(14) . 3_565 ? O2 Th1 O3 60.75(15) 2 3_565 ? O7 Th1 O3 108.77(15) . 3_565 ? O8 Th1 O3 144.91(16) . 3_565 ? O1 Th1 O5 66.90(17) . 2_655 ? O2 Th1 O5 140.16(16) 4_565 2_655 ? O4 Th1 O5 111.26(16) 4_575 2_655 ? O5 Th1 O5 106.13(17) 3_665 2_655 ? O4 Th1 O5 57.26(15) . 2_655 ? O2 Th1 O5 107.49(14) 2 2_655 ? O7 Th1 O5 52.27(15) . 2_655 ? O8 Th1 O5 76.70(16) . 2_655 ? O3 Th1 O5 130.55(15) 3_565 2_655 ? O1 Th1 B1 65.30(19) . 3_565 ? O2 Th1 B1 98.55(19) 4_565 3_565 ? O4 Th1 B1 27.31(17) 4_575 3_565 ? O5 Th1 B1 85.62(18) 3_665 3_565 ? O4 Th1 B1 130.27(18) . 3_565 ? O2 Th1 B1 88.19(18) 2 3_565 ? O7 Th1 B1 82.92(19) . 3_565 ? O8 Th1 B1 161.54(18) . 3_565 ? O3 Th1 B1 27.96(18) 3_565 3_565 ? O5 Th1 B1 120.6(2) 2_655 3_565 ? O1 Th1 P1 69.38(13) . 2_655 ? O2 Th1 P1 155.39(12) 4_565 2_655 ? O4 Th1 P1 86.89(12) 4_575 2_655 ? O5 Th1 P1 86.62(12) 3_665 2_655 ? O4 Th1 P1 83.23(11) . 2_655 ? O2 Th1 P1 129.26(10) 2 2_655 ? O7 Th1 P1 26.10(11) . 2_655 ? O8 Th1 P1 91.11(11) . 2_655 ? O3 Th1 P1 123.07(12) 3_565 2_655 ? O5 Th1 P1 26.18(11) 2_655 2_655 ? B1 Th1 P1 102.60(16) 3_565 2_655 ? O2 Th2 O6 80.24(17) . . ? O2 Th2 O4 127.08(16) . . ? O6 Th2 O4 133.38(17) . . ? O2 Th2 O3 69.95(17) . 4_566 ? O6 Th2 O3 128.65(17) . 4_566 ? O4 Th2 O3 97.72(17) . 4_566 ? O2 Th2 O3 59.28(16) . . ? O6 Th2 O3 73.46(17) . . ? O4 Th2 O3 88.93(17) . . ? O3 Th2 O3 119.64(18) 4_566 . ? O2 Th2 O7 150.17(16) . 4_576 ? O6 Th2 O7 109.76(17) . 4_576 ? O4 Th2 O7 66.82(17) . 4_576 ? O3 Th2 O7 82.67(17) 4_566 4_576 ? O3 Th2 O7 149.88(17) . 4_576 ? O2 Th2 O1 71.70(16) . 2_545 ? O6 Th2 O1 141.01(17) . 2_545 ? O4 Th2 O1 57.06(16) . 2_545 ? O3 Th2 O1 65.56(16) 4_566 2_545 ? O3 Th2 O1 69.10(16) . 2_545 ? O7 Th2 O1 108.03(16) 4_576 2_545 ? O2 Th2 O8 121.04(16) . . ? O6 Th2 O8 67.23(16) . . ? O4 Th2 O8 66.21(16) . . ? O3 Th2 O8 163.74(17) 4_566 . ? O3 Th2 O8 64.80(16) . . ? O7 Th2 O8 88.31(15) 4_576 . ? O1 Th2 O8 104.93(15) 2_545 . ? O2 Th2 O8 64.38(16) . 4_566 ? O6 Th2 O8 66.78(16) . 4_566 ? O4 Th2 O8 154.48(16) . 4_566 ? O3 Th2 O8 62.86(15) 4_566 4_566 ? O3 Th2 O8 114.61(16) . 4_566 ? O7 Th2 O8 93.04(15) 4_576 4_566 ? O1 Th2 O8 120.43(15) 2_545 4_566 ? O8 Th2 O8 131.45(17) . 4_566 ? O2 Th2 B1 29.48(18) . . ? O6 Th2 B1 76.0(2) . . ? O4 Th2 B1 108.9(2) . . ? O3 Th2 B1 94.26(19) 4_566 . ? O3 Th2 B1 29.84(19) . . ? O7 Th2 B1 174.2(2) 4_576 . ? O1 Th2 B1 66.2(2) 2_545 . ? O8 Th2 B1 93.48(18) . . ? O8 Th2 B1 89.90(19) 4_566 . ? O2 Th2 B1 98.4(2) . 2 ? O6 Th2 B1 143.90(19) . 2 ? O4 Th2 B1 29.1(2) . 2 ? O3 Th2 B1 82.75(18) 4_566 2 ? O3 Th2 B1 75.1(2) . 2 ? O7 Th2 B1 89.3(2) 4_576 2 ? O1 Th2 B1 28.22(19) 2_545 2 ? O8 Th2 B1 83.65(18) . 2 ? O8 Th2 B1 144.85(17) 4_566 2 ? B1 Th2 B1 85.40(4) . 2 ? O2 Th2 Th1 43.46(12) . 2_545 ? O6 Th2 Th1 123.64(12) . 2_545 ? O4 Th2 Th1 90.59(11) . 2_545 ? O3 Th2 Th1 45.49(12) 4_566 2_545 ? O3 Th2 Th1 74.71(11) . 2_545 ? O7 Th2 Th1 120.90(11) 4_576 2_545 ? O1 Th2 Th1 34.62(11) 2_545 2_545 ? O8 Th2 Th1 132.74(11) . 2_545 ? O8 Th2 Th1 86.63(10) 4_566 2_545 ? B1 Th2 Th1 54.28(15) . 2_545 ? B1 Th2 Th1 62.54(15) 2 2_545 ? O1 B1 O2 112.5(6) 1_545 . ? O1 B1 O3 116.0(6) 1_545 . ? O2 B1 O3 106.9(6) . . ? O1 B1 O4 106.6(6) 1_545 2_545 ? O2 B1 O4 106.9(5) . 2_545 ? O3 B1 O4 107.4(6) . 2_545 ? O1 B1 Th2 136.2(5) 1_545 . ? O2 B1 Th2 51.5(3) . . ? O3 B1 Th2 55.6(3) . . ? O4 B1 Th2 117.0(5) 2_545 . ? O1 B1 Th2 56.4(4) 1_545 2_545 ? O2 B1 Th2 117.6(4) . 2_545 ? O3 B1 Th2 134.1(5) . 2_545 ? O4 B1 Th2 50.7(3) 2_545 2_545 ? Th2 B1 Th2 163.6(3) . 2_545 ? O1 B1 Th1 115.6(5) 1_545 3_565 ? O2 B1 Th1 130.8(5) . 3_565 ? O3 B1 Th1 59.5(3) . 3_565 ? O4 B1 Th1 49.5(3) 2_545 3_565 ? Th2 B1 Th1 96.7(2) . 3_565 ? Th2 B1 Th1 82.4(2) 2_545 3_565 ? O5 P1 O6 114.7(3) . 2_655 ? O5 P1 O7 104.3(3) . 2_645 ? O6 P1 O7 110.0(3) 2_655 2_645 ? O5 P1 O8 110.9(3) . . ? O6 P1 O8 106.9(3) 2_655 . ? O7 P1 O8 110.1(3) 2_645 . ? O5 P1 Th1 54.3(2) . 2_645 ? O6 P1 Th1 128.9(2) 2_655 2_645 ? O7 P1 Th1 49.9(2) 2_645 2_645 ? O8 P1 Th1 123.8(2) . 2_645 ? B1 O1 Th1 156.5(5) 1_565 . ? B1 O1 Th2 95.3(4) 1_565 2 ? Th1 O1 Th2 105.64(19) . 2 ? B1 O2 Th2 99.1(4) . . ? B1 O2 Th1 115.3(4) . 4_566 ? Th2 O2 Th1 125.4(2) . 4_566 ? B1 O2 Th1 96.5(4) . 2_545 ? Th2 O2 Th1 98.84(18) . 2_545 ? Th1 O2 Th1 116.59(17) 4_566 2_545 ? B1 O3 Th2 126.0(4) . 4_565 ? B1 O3 Th2 94.6(4) . . ? Th2 O3 Th2 122.40(19) 4_565 . ? B1 O3 Th1 92.5(4) . 3_565 ? Th2 O3 Th1 95.85(16) 4_565 3_565 ? Th2 O3 Th1 124.2(2) . 3_565 ? B1 O4 Th2 100.2(4) 2 . ? B1 O4 Th1 103.2(4) 2 4_576 ? Th2 O4 Th1 114.34(19) . 4_576 ? B1 O4 Th1 100.4(4) 2 . ? Th2 O4 Th1 120.64(19) . . ? Th1 O4 Th1 113.93(19) 4_576 . ? P1 O5 Th1 131.8(3) . 3_665 ? P1 O5 Th1 99.5(2) . 2_645 ? Th1 O5 Th1 105.52(18) 3_665 2_645 ? P1 O6 Th2 147.1(3) 2_645 . ? P1 O7 Th2 125.5(3) 2_655 4_575 ? P1 O7 Th1 104.0(3) 2_655 . ? Th2 O7 Th1 104.92(17) 4_575 . ? P1 O8 Th2 114.5(3) . . ? P1 O8 Th1 113.5(3) . . ? Th2 O8 Th1 107.41(16) . . ? P1 O8 Th2 116.1(2) . 4_565 ? Th2 O8 Th2 103.04(17) . 4_565 ? Th1 O8 Th2 100.85(16) . 4_565 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.853 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.386