# ic980716j.cif # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. Boris \2sigma(I) _computing_data_collection 'IPDS package (Stoe, 1995)' _computing_cell_refinement 'IPDS package (Stoe, 1995)' _computing_data_reduction 'IPDS package (Stoe, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1990)' _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 w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.1985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1171 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La La 0.43971(3) 0.7500 0.06436(3) 0.01557(12) Uani 1 d S . . F1 F 0.4004(3) 0.62462(18) -0.0794(3) 0.0389(7) Uani 1 d . . . H1 H 0.383(7) 0.591(4) -0.073(8) 0.06(2) Uiso 1 d . . . As1 As 0.56153(5) 0.7500 -0.38566(6) 0.02009(16) Uani 1 d S . . F2 F 0.4115(4) 0.7500 -0.3005(5) 0.0380(8) Uani 1 d S . . F3 F 0.6110(3) 0.7500 -0.1674(4) 0.0347(8) Uani 1 d S . . F4 F 0.7192(3) 0.7500 -0.4570(4) 0.0343(8) Uani 1 d S . . F5 F 0.5113(4) 0.7500 -0.5977(4) 0.0443(10) Uani 1 d S . . F6 F 0.5659(3) 0.65344(15) -0.3845(3) 0.0423(7) Uani 1 d . . . As2 As 0.22952(4) 0.58873(2) 0.34659(4) 0.02023(14) Uani 1 d . . . F7 F 0.3211(3) 0.66586(15) 0.2602(3) 0.0394(6) Uani 1 d . . . F8 F 0.1781(3) 0.57115(16) 0.1443(3) 0.0413(7) Uani 1 d . . . F9 F 0.3500(3) 0.52705(18) 0.3236(3) 0.0507(8) Uani 1 d . . . F10 F 0.2742(3) 0.61510(18) 0.5464(3) 0.0417(7) Uani 1 d . . . F11 F 0.1057(3) 0.65812(14) 0.3643(3) 0.0357(6) Uani 1 d . . . F12 F 0.1290(3) 0.52033(15) 0.4306(3) 0.0440(7) Uani 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 La 0.0151(2) 0.01552(17) 0.01605(17) 0.000 0.00125(9) 0.000 F1 0.056(2) 0.0222(14) 0.0382(14) -0.0081(11) 0.0017(12) -0.0108(13) As1 0.0182(3) 0.0270(3) 0.0151(3) 0.000 0.00386(18) 0.000 F2 0.022(2) 0.040(2) 0.052(2) 0.000 0.0141(15) 0.000 F3 0.035(2) 0.054(2) 0.0153(14) 0.000 -0.0001(13) 0.000 F4 0.022(2) 0.053(2) 0.0288(15) 0.000 0.0065(13) 0.000 F5 0.037(2) 0.072(3) 0.0241(15) 0.000 -0.0082(15) 0.000 F6 0.053(2) 0.0275(13) 0.0468(14) -0.0055(12) 0.0184(12) 0.0038(12) As2 0.0232(3) 0.0172(2) 0.0203(2) 0.00248(13) 0.00284(14) 0.00181(15) F7 0.0401(17) 0.0400(14) 0.0382(12) 0.0078(11) 0.0097(11) -0.0127(12) F8 0.058(2) 0.0389(15) 0.0265(12) -0.0081(10) -0.0086(11) 0.0014(13) F9 0.046(2) 0.0476(16) 0.0581(15) 0.0022(14) 0.0064(13) 0.0268(14) F10 0.0496(18) 0.0505(17) 0.0249(11) -0.0007(11) -0.0072(10) -0.0055(14) F11 0.0352(16) 0.0313(13) 0.0404(13) -0.0005(11) 0.0042(10) 0.0128(11) F12 0.052(2) 0.0230(14) 0.0574(16) 0.0103(11) 0.0083(12) -0.0085(12) _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 La F11 2.433(2) 4_565 ? La F11 2.433(2) 6_656 ? La F7 2.443(2) 7_575 ? La F7 2.443(2) . ? La F1 2.466(3) 7_575 ? La F1 2.466(3) . ? La F4 2.482(3) 6 ? La F3 2.547(3) . ? La F5 2.711(3) 1_556 ? La F2 2.826(4) . ? F1 H1 0.61(7) . ? As1 F6 1.667(3) 7_575 ? As1 F6 1.667(3) . ? As1 F5 1.718(3) . ? As1 F2 1.722(4) . ? As1 F4 1.760(3) . ? As1 F3 1.760(3) . ? F4 La 2.482(3) 6_655 ? F5 La 2.711(3) 1_554 ? As2 F10 1.673(2) . ? As2 F9 1.673(3) . ? As2 F8 1.678(2) . ? As2 F12 1.717(3) . ? As2 F7 1.777(2) . ? As2 F11 1.783(2) . ? F11 La 2.433(2) 6_556 ? 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 F11 La F11 81.37(13) 4_565 6_656 ? F11 La F7 81.13(9) 4_565 7_575 ? F11 La F7 128.40(8) 6_656 7_575 ? F11 La F7 128.40(8) 4_565 . ? F11 La F7 81.13(9) 6_656 . ? F7 La F7 72.97(13) 7_575 . ? F11 La F1 69.63(10) 4_565 7_575 ? F11 La F1 142.75(11) 6_656 7_575 ? F7 La F1 70.61(9) 7_575 7_575 ? F7 La F1 135.36(10) . 7_575 ? F11 La F1 142.75(10) 4_565 . ? F11 La F1 69.62(10) 6_656 . ? F7 La F1 135.36(10) 7_575 . ? F7 La F1 70.61(9) . . ? F1 La F1 122.68(14) 7_575 . ? F11 La F4 139.27(7) 4_565 6 ? F11 La F4 139.27(7) 6_656 6 ? F7 La F4 73.74(9) 7_575 6 ? F7 La F4 73.74(9) . 6 ? F1 La F4 71.99(9) 7_575 6 ? F1 La F4 71.99(9) . 6 ? F11 La F3 69.02(8) 4_565 . ? F11 La F3 69.02(8) 6_656 . ? F7 La F3 143.14(7) 7_575 . ? F7 La F3 143.14(7) . . ? F1 La F3 78.83(8) 7_575 . ? F1 La F3 78.83(8) . . ? F4 La F3 116.04(10) 6 . ? F11 La F5 65.19(8) 4_565 1_556 ? F11 La F5 65.19(8) 6_656 1_556 ? F7 La F5 63.37(9) 7_575 1_556 ? F7 La F5 63.37(9) . 1_556 ? F1 La F5 118.57(7) 7_575 1_556 ? F1 La F5 118.57(7) . 1_556 ? F4 La F5 125.74(11) 6 1_556 ? F3 La F5 118.22(12) . 1_556 ? F11 La F2 107.54(8) 4_565 . ? F11 La F2 107.54(8) 6_656 . ? F7 La F2 124.00(8) 7_575 . ? F7 La F2 124.00(8) . . ? F1 La F2 62.35(7) 7_575 . ? F1 La F2 62.35(7) . . ? F4 La F2 64.45(10) 6 . ? F3 La F2 51.59(11) . . ? F5 La F2 169.81(11) 1_556 . ? La F1 H1 148(6) . . ? F6 As1 F6 176.8(2) 7_575 . ? F6 As1 F5 90.78(10) 7_575 . ? F6 As1 F5 90.78(10) . . ? F6 As1 F2 91.36(9) 7_575 . ? F6 As1 F2 91.36(9) . . ? F5 As1 F2 94.31(18) . . ? F6 As1 F4 88.58(9) 7_575 . ? F6 As1 F4 88.58(9) . . ? F5 As1 F4 89.89(17) . . ? F2 As1 F4 175.80(17) . . ? F6 As1 F3 89.24(10) 7_575 . ? F6 As1 F3 89.24(10) . . ? F5 As1 F3 179.26(18) . . ? F2 As1 F3 84.95(17) . . ? F4 As1 F3 90.85(15) . . ? As1 F2 La 106.29(17) . . ? As1 F3 La 117.16(17) . . ? As1 F4 La 178.72(17) . 6_655 ? As1 F5 La 178.2(2) . 1_554 ? F10 As2 F9 93.10(14) . . ? F10 As2 F8 174.23(14) . . ? F9 As2 F8 92.00(14) . . ? F10 As2 F12 90.96(13) . . ? F9 As2 F12 94.41(16) . . ? F8 As2 F12 91.34(13) . . ? F10 As2 F7 89.17(13) . . ? F9 As2 F7 91.11(15) . . ? F8 As2 F7 88.03(13) . . ? F12 As2 F7 174.47(13) . . ? F10 As2 F11 87.47(13) . . ? F9 As2 F11 176.92(14) . . ? F8 As2 F11 87.30(13) . . ? F12 As2 F11 88.60(13) . . ? F7 As2 F11 85.88(13) . . ? As2 F7 La 163.35(14) . . ? As2 F11 La 171.32(12) . 6_556 ? _diffrn_measured_fraction_theta_max 0.823 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.823 _refine_diff_density_max 0.552 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.108