# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wen-Dan Cheng' _publ_contact_author_email CWD@FJIRSM.AC.CN _publ_section_title ; Structure Determination and Characterizations of two Rare-earth Molybdenum Borate Compounds: LnMoBO6(Ln=La,Ce) ; loop_ _publ_author_name 'Wen-Dan Cheng.' 'Ming Fang.' 'Shu-Ping Hang.' 'Hao Zhang.' 'Dan Zhao.' # Attachment 'CeMoBO6.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 669425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cerium Molybdenum Borate ; _chemical_name_common 'Cerium Molybdenum Borate' _chemical_melting_point 'Not meaaured' _chemical_formula_moiety 'B Ce Mo O6' _chemical_formula_sum 'B Ce Mo O6' _chemical_formula_weight 342.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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' 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' 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 10.2404(15) _cell_length_b 4.1495(4) _cell_length_c 11.9268(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.100(9) _cell_angle_gamma 90.00 _cell_volume 455.12(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1195 _cell_measurement_theta_min 2.1945 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 5.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 12.570 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3954 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3286 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1036 _reflns_number_gt 977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0223(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1036 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Ce1 Ce 0.19653(3) 0.28091(7) 0.52922(2) 0.00677(15) Uani 1 1 d . . . Mo1 Mo 0.35455(5) 0.68761(10) 0.81901(4) 0.00573(16) Uani 1 1 d . . . O1 O -0.0044(4) 0.2691(6) 0.5852(3) 0.0074(7) Uani 1 1 d . . . O2 O 0.2586(4) 0.7779(7) 0.6528(3) 0.0100(8) Uani 1 1 d . . . O3 O 0.4604(5) 0.2674(7) 0.6094(4) 0.0152(8) Uani 1 1 d . . . O4 O 0.2654(4) 0.7264(7) 0.4144(3) 0.0133(8) Uani 1 1 d . . . O5 O 0.3382(5) 0.2684(8) 0.8036(4) 0.0181(9) Uani 1 1 d . . . O6 O -0.0305(4) -0.1603(7) 0.7002(3) 0.0091(7) Uani 1 1 d . . . B1 B -0.0041(6) 0.1664(11) 0.6910(5) 0.0087(10) 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 Ce1 0.0089(2) 0.00466(19) 0.0073(2) 0.00072(8) 0.00411(14) 0.00030(8) Mo1 0.0082(3) 0.0044(2) 0.0054(2) -0.00065(13) 0.00369(19) -0.00031(14) O1 0.0122(17) 0.0059(14) 0.0067(16) 0.0013(11) 0.0067(15) 0.0013(12) O2 0.0129(19) 0.0078(16) 0.0087(17) 0.0002(11) 0.0043(15) 0.0003(12) O3 0.0081(18) 0.0177(18) 0.018(2) 0.0001(13) 0.0038(15) -0.0009(13) O4 0.016(2) 0.0122(16) 0.0138(19) 0.0019(12) 0.0085(17) 0.0017(13) O5 0.025(2) 0.0091(16) 0.021(2) -0.0031(12) 0.0109(19) -0.0010(14) O6 0.0198(19) 0.0032(14) 0.0063(15) 0.0019(12) 0.0074(14) 0.0002(14) B1 0.013(3) 0.005(2) 0.008(2) -0.0020(18) 0.004(2) -0.003(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 Ce1 O1 2.427(4) . ? Ce1 O3 2.438(4) . ? Ce1 O2 2.450(3) . ? Ce1 O2 2.472(3) 1_545 ? Ce1 O6 2.556(3) 3_556 ? Ce1 O4 2.577(3) . ? Ce1 O1 2.619(3) 3_566 ? Ce1 O4 2.918(3) 1_545 ? Ce1 O1 2.929(3) 3_556 ? Ce1 O5 2.939(4) . ? Ce1 B1 3.110(5) 3_556 ? Ce1 Mo1 3.5343(6) . ? Mo1 O3 1.734(4) 2_656 ? Mo1 O5 1.750(3) . ? Mo1 O4 1.780(4) 4_576 ? Mo1 O2 1.823(4) . ? Mo1 O5 2.417(3) 1_565 ? O1 B1 1.330(6) . ? O1 Ce1 2.619(3) 3_566 ? O1 Ce1 2.929(3) 3_556 ? O2 Ce1 2.472(3) 1_565 ? O3 Mo1 1.734(4) 2_646 ? O4 Mo1 1.780(4) 4_575 ? O4 Ce1 2.918(3) 1_565 ? O5 Mo1 2.417(3) 1_545 ? O6 B1 1.386(6) 2_546 ? O6 B1 1.396(5) . ? O6 Ce1 2.556(3) 3_556 ? B1 O6 1.386(6) 2_556 ? B1 Ce1 3.110(5) 3_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 O1 Ce1 O3 144.97(13) . . ? O1 Ce1 O2 83.02(11) . . ? O3 Ce1 O2 80.44(12) . . ? O1 Ce1 O2 81.12(11) . 1_545 ? O3 Ce1 O2 78.28(12) . 1_545 ? O2 Ce1 O2 114.94(15) . 1_545 ? O1 Ce1 O6 92.60(12) . 3_556 ? O3 Ce1 O6 121.06(13) . 3_556 ? O2 Ce1 O6 133.06(11) . 3_556 ? O2 Ce1 O6 110.39(11) 1_545 3_556 ? O1 Ce1 O4 128.62(10) . . ? O3 Ce1 O4 73.13(12) . . ? O2 Ce1 O4 69.92(11) . . ? O2 Ce1 O4 149.78(12) 1_545 . ? O6 Ce1 O4 77.31(11) 3_556 . ? O1 Ce1 O1 67.93(11) . 3_566 ? O3 Ce1 O1 132.04(11) . 3_566 ? O2 Ce1 O1 69.50(11) . 3_566 ? O2 Ce1 O1 148.22(12) 1_545 3_566 ? O6 Ce1 O1 65.69(10) 3_556 3_566 ? O4 Ce1 O1 61.97(11) . 3_566 ? O1 Ce1 O4 121.48(10) . 1_545 ? O3 Ce1 O4 73.21(11) . 1_545 ? O2 Ce1 O4 153.31(12) . 1_545 ? O2 Ce1 O4 64.02(11) 1_545 1_545 ? O6 Ce1 O4 61.82(10) 3_556 1_545 ? O4 Ce1 O4 97.89(12) . 1_545 ? O1 Ce1 O4 126.80(10) 3_566 1_545 ? O1 Ce1 O1 68.62(11) . 3_556 ? O3 Ce1 O1 124.49(10) . 3_556 ? O2 Ce1 O1 151.55(12) . 3_556 ? O2 Ce1 O1 64.12(11) 1_545 3_556 ? O6 Ce1 O1 49.81(10) 3_556 3_556 ? O4 Ce1 O1 126.60(10) . 3_556 ? O1 Ce1 O1 96.67(12) 3_566 3_556 ? O4 Ce1 O1 54.45(10) 1_545 3_556 ? O1 Ce1 O5 75.89(12) . . ? O3 Ce1 O5 69.13(13) . . ? O2 Ce1 O5 58.33(10) . . ? O2 Ce1 O5 56.62(10) 1_545 . ? O6 Ce1 O5 163.40(11) 3_556 . ? O4 Ce1 O5 119.20(11) . . ? O1 Ce1 O5 118.84(10) 3_566 . ? O4 Ce1 O5 113.93(10) 1_545 . ? O1 Ce1 O5 113.97(9) 3_556 . ? O1 Ce1 B1 85.49(13) . 3_556 ? O3 Ce1 B1 119.92(13) . 3_556 ? O2 Ce1 B1 155.57(13) . 3_556 ? O2 Ce1 B1 84.29(12) 1_545 3_556 ? O6 Ce1 B1 26.28(11) 3_556 3_556 ? O4 Ce1 B1 101.50(13) . 3_556 ? O1 Ce1 B1 86.21(12) 3_566 3_556 ? O4 Ce1 B1 47.73(13) 1_545 3_556 ? O1 Ce1 B1 25.22(11) 3_556 3_556 ? O5 Ce1 B1 138.47(12) . 3_556 ? O1 Ce1 Mo1 79.60(8) . . ? O3 Ce1 Mo1 71.07(9) . . ? O2 Ce1 Mo1 28.84(8) . . ? O2 Ce1 Mo1 86.17(8) 1_545 . ? O6 Ce1 Mo1 160.56(7) 3_556 . ? O4 Ce1 Mo1 93.58(8) . . ? O1 Ce1 Mo1 94.87(7) 3_566 . ? O4 Ce1 Mo1 137.23(7) 1_545 . ? O1 Ce1 Mo1 138.80(6) 3_556 . ? O5 Ce1 Mo1 29.57(6) . . ? B1 Ce1 Mo1 163.38(10) 3_556 . ? O3 Mo1 O5 105.98(18) 2_656 . ? O3 Mo1 O4 113.81(19) 2_656 4_576 ? O5 Mo1 O4 102.37(18) . 4_576 ? O3 Mo1 O2 116.47(18) 2_656 . ? O5 Mo1 O2 96.25(17) . . ? O4 Mo1 O2 118.12(17) 4_576 . ? O3 Mo1 O5 82.60(15) 2_656 1_565 ? O5 Mo1 O5 169.4(2) . 1_565 ? O4 Mo1 O5 79.10(14) 4_576 1_565 ? O2 Mo1 O5 74.10(13) . 1_565 ? O3 Mo1 Ce1 120.24(13) 2_656 . ? O5 Mo1 Ce1 56.00(14) . . ? O4 Mo1 Ce1 125.30(12) 4_576 . ? O2 Mo1 Ce1 40.41(9) . . ? O5 Mo1 Ce1 114.52(10) 1_565 . ? B1 O1 Ce1 128.2(3) . . ? B1 O1 Ce1 114.2(3) . 3_566 ? Ce1 O1 Ce1 112.07(11) . 3_566 ? B1 O1 Ce1 85.0(3) . 3_556 ? Ce1 O1 Ce1 111.38(11) . 3_556 ? Ce1 O1 Ce1 96.67(11) 3_566 3_556 ? Mo1 O2 Ce1 110.75(13) . . ? Mo1 O2 Ce1 134.12(16) . 1_565 ? Ce1 O2 Ce1 114.94(15) . 1_565 ? Mo1 O3 Ce1 168.55(19) 2_646 . ? Mo1 O4 Ce1 145.15(17) 4_575 . ? Mo1 O4 Ce1 116.07(14) 4_575 1_565 ? Ce1 O4 Ce1 97.89(12) . 1_565 ? Mo1 O5 Mo1 169.4(2) . 1_545 ? Mo1 O5 Ce1 94.43(16) . . ? Mo1 O5 Ce1 94.95(12) 1_545 . ? B1 O6 B1 126.8(3) 2_546 . ? B1 O6 Ce1 132.6(3) 2_546 3_556 ? B1 O6 Ce1 99.6(3) . 3_556 ? O1 B1 O6 127.9(4) . 2_556 ? O1 B1 O6 117.8(4) . . ? O6 B1 O6 114.1(4) 2_556 . ? O1 B1 Ce1 69.8(2) . 3_556 ? O6 B1 Ce1 155.0(4) 2_556 3_556 ? O6 B1 Ce1 54.2(2) . 3_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.892 _refine_diff_density_min -1.710 _refine_diff_density_rms 0.296 # Attachment 'LaMoBO6.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 669426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lanthanum molybdenum Borate ; _chemical_name_common 'Lanthanum molybdenum Borate' _chemical_melting_point 'Not measured' _chemical_formula_moiety 'B La Mo O6' _chemical_formula_sum 'B La Mo O6' _chemical_formula_weight 341.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' 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' 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 10.2968(8) _cell_length_b 4.1636(3) _cell_length_c 23.8587(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.367(3) _cell_angle_gamma 90.00 _cell_volume 924.24(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2482 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 25.02 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 11.773 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.439011 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4214 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.76 _reflns_number_total 1716 _reflns_number_gt 1340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0497P)^2^+11.2392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0153(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1716 _refine_ls_number_parameters 164 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.091 _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 La1 La 0.16948(6) 0.71951(12) -0.01458(2) 0.0090(2) Uani 1 1 d . . . La2 La 0.33106(6) 0.24650(11) 0.26419(2) 0.0091(2) Uani 1 1 d . . . Mo1 Mo 0.03429(9) 0.19089(18) 0.33940(4) 0.0083(3) Uani 1 1 d . . . Mo2 Mo 0.46656(8) -0.33058(19) 0.41015(3) 0.0078(3) Uani 1 1 d . . . O1 O 0.4082(7) 0.7670(13) 0.2073(3) 0.0108(14) Uani 1 1 d . . . O2 O 0.3996(8) -0.2416(13) 0.3278(3) 0.0129(15) Uani 1 1 d . . . O3 O 0.0894(7) 1.2675(13) 0.0426(3) 0.0119(14) Uani 1 1 d . . . O4 O 0.1022(7) 0.2799(13) 0.4222(3) 0.0116(15) Uani 1 1 d . . . O5 O 0.2297(7) 0.8401(13) 0.1001(3) 0.0108(13) Uani 1 1 d . . . O6 O -0.1496(7) 0.2828(14) 0.2912(3) 0.0160(15) Uani 1 1 d . . . O7 O 0.3500(8) 0.7469(14) -0.0558(3) 0.0176(16) Uani 1 1 d . . . O8 O 0.6516(7) -0.2418(14) 0.4590(3) 0.0143(15) Uani 1 1 d . . . O9 O 0.4699(9) -0.7480(14) 0.4030(4) 0.0214(17) Uani 1 1 d . . . O10 O 0.1506(8) 0.2753(14) 0.3058(3) 0.0162(15) Uani 1 1 d . . . O11 O 0.0320(8) -0.2256(14) 0.3463(4) 0.0202(17) Uani 1 1 d . . . O12 O 0.2681(6) 0.3386(14) 0.1487(3) 0.0118(13) Uani 1 1 d U . . B1 B 0.3051(11) 0.666(2) 0.1540(5) 0.011(2) Uani 1 1 d . . . B2 B 0.1930(10) 1.166(2) 0.0952(4) 0.0080(18) Uani 1 1 d U . . 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 La1 0.0128(4) 0.0076(3) 0.0085(4) 0.00056(16) 0.0064(3) 0.00010(16) La2 0.0126(4) 0.0083(4) 0.0078(4) -0.00007(16) 0.0058(3) -0.00028(17) Mo1 0.0118(5) 0.0075(4) 0.0069(4) 0.0003(3) 0.0052(3) 0.0002(3) Mo2 0.0114(4) 0.0073(4) 0.0060(4) -0.0002(3) 0.0049(3) -0.0004(3) O1 0.016(4) 0.008(3) 0.008(3) 0.001(2) 0.004(3) 0.000(2) O2 0.025(4) 0.008(3) 0.010(3) -0.003(2) 0.012(3) -0.001(2) O3 0.014(4) 0.016(3) 0.010(3) -0.001(2) 0.009(3) -0.001(2) O4 0.017(4) 0.010(3) 0.007(3) 0.002(2) 0.004(3) 0.003(2) O5 0.020(3) 0.003(3) 0.005(3) 0.000(2) 0.002(3) 0.000(2) O6 0.015(4) 0.016(3) 0.018(4) 0.004(2) 0.008(3) 0.001(2) O7 0.016(4) 0.023(4) 0.020(4) 0.006(2) 0.013(3) 0.007(2) O8 0.008(4) 0.019(4) 0.012(4) -0.002(2) 0.001(3) 0.000(2) O9 0.027(4) 0.010(3) 0.026(4) 0.002(2) 0.011(4) -0.001(2) O10 0.017(4) 0.017(3) 0.020(4) 0.001(2) 0.013(3) 0.002(2) O11 0.022(4) 0.012(3) 0.026(4) -0.002(2) 0.009(3) 0.001(2) O12 0.0124(15) 0.0108(15) 0.0118(15) 0.0006(10) 0.0048(10) 0.0001(10) B1 0.020(5) 0.005(4) 0.016(5) 0.000(4) 0.014(4) 0.002(4) B2 0.008(2) 0.008(2) 0.008(2) -0.0004(10) 0.0038(12) 0.0004(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 La1 O7 2.450(7) . ? La1 O3 2.455(7) 3_575 ? La1 O4 2.486(6) 4_565 ? La1 O4 2.491(6) 4_575 ? La1 O5 2.582(6) . ? La1 O8 2.598(6) 2_655 ? La1 O3 2.655(6) 1_545 ? La1 O8 2.844(6) 2_665 ? La1 O3 2.952(6) . ? La1 O11 2.999(8) 4_565 ? La1 B2 3.136(10) . ? La1 Mo1 3.5832(10) 4_565 ? La2 O2 2.452(6) . ? La2 O10 2.457(7) . ? La2 O1 2.472(7) 2_645 ? La2 O2 2.535(6) 1_565 ? La2 O12 2.576(6) . ? La2 O6 2.617(6) 2_545 ? La2 O1 2.717(6) 1_545 ? La2 O1 2.845(6) . ? La2 O6 2.847(6) 2 ? La2 O9 2.993(8) 1_565 ? La2 B1 3.071(10) . ? La2 Mo2 3.6073(10) 1_565 ? Mo1 O10 1.738(7) . ? Mo1 O11 1.743(6) . ? Mo1 O6 1.786(7) . ? Mo1 O4 1.829(7) . ? Mo1 O11 2.436(6) 1_565 ? Mo1 La1 3.5832(10) 4_566 ? Mo2 O7 1.748(7) 4_566 ? Mo2 O9 1.748(6) . ? Mo2 O8 1.795(7) . ? Mo2 O2 1.821(7) . ? Mo2 O9 2.433(6) 1_565 ? Mo2 La2 3.6073(10) 1_545 ? O1 B1 1.327(12) . ? O1 La2 2.472(7) 2_655 ? O1 La2 2.717(6) 1_565 ? O2 La2 2.535(6) 1_545 ? O3 B2 1.319(11) . ? O3 La1 2.455(7) 3_575 ? O3 La1 2.655(6) 1_565 ? O4 La1 2.486(6) 4_566 ? O4 La1 2.491(6) 4_576 ? O5 B1 1.388(11) . ? O5 B2 1.401(11) . ? O6 La2 2.617(6) 2 ? O6 La2 2.847(6) 2_545 ? O7 Mo2 1.748(7) 4_565 ? O8 La1 2.598(6) 2_645 ? O8 La1 2.844(6) 2_635 ? O9 Mo2 2.433(6) 1_545 ? O9 La2 2.993(8) 1_545 ? O11 Mo1 2.436(6) 1_545 ? O11 La1 2.999(8) 4_566 ? O12 B2 1.377(11) 1_545 ? O12 B1 1.408(11) . ? B2 O12 1.377(11) 1_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 O7 La1 O3 144.2(2) . 3_575 ? O7 La1 O4 81.8(2) . 4_565 ? O3 La1 O4 82.3(2) 3_575 4_565 ? O7 La1 O4 77.3(2) . 4_575 ? O3 La1 O4 80.1(2) 3_575 4_575 ? O4 La1 O4 113.6(3) 4_565 4_575 ? O7 La1 O5 122.5(2) . . ? O3 La1 O5 91.4(2) 3_575 . ? O4 La1 O5 133.1(2) 4_565 . ? O4 La1 O5 110.91(19) 4_575 . ? O7 La1 O8 75.2(2) . 2_655 ? O3 La1 O8 127.2(2) 3_575 2_655 ? O4 La1 O8 69.1(2) 4_565 2_655 ? O4 La1 O8 151.7(2) 4_575 2_655 ? O5 La1 O8 78.9(2) . 2_655 ? O7 La1 O3 134.1(2) . 1_545 ? O3 La1 O3 67.4(2) 3_575 1_545 ? O4 La1 O3 69.6(2) 4_565 1_545 ? O4 La1 O3 146.9(2) 4_575 1_545 ? O5 La1 O3 65.14(19) . 1_545 ? O8 La1 O3 61.5(2) 2_655 1_545 ? O7 La1 O8 72.5(2) . 2_665 ? O3 La1 O8 121.37(19) 3_575 2_665 ? O4 La1 O8 154.0(2) 4_565 2_665 ? O4 La1 O8 65.09(19) 4_575 2_665 ? O5 La1 O8 62.56(19) . 2_665 ? O8 La1 O8 99.7(2) 2_655 2_665 ? O3 La1 O8 126.95(19) 1_545 2_665 ? O7 La1 O3 124.06(19) . . ? O3 La1 O3 67.9(2) 3_575 . ? O4 La1 O3 150.1(2) 4_565 . ? O4 La1 O3 64.7(2) 4_575 . ? O5 La1 O3 49.27(18) . . ? O8 La1 O3 127.8(2) 2_655 . ? O3 La1 O3 95.8(2) 1_545 . ? O8 La1 O3 55.14(18) 2_665 . ? O7 La1 O11 68.6(2) . 4_565 ? O3 La1 O11 75.8(2) 3_575 4_565 ? O4 La1 O11 57.26(19) 4_565 4_565 ? O4 La1 O11 56.36(19) 4_575 4_565 ? O5 La1 O11 162.97(19) . 4_565 ? O8 La1 O11 117.8(2) 2_655 4_565 ? O3 La1 O11 118.15(19) 1_545 4_565 ? O8 La1 O11 114.42(18) 2_665 4_565 ? O3 La1 O11 114.36(18) . 4_565 ? O7 La1 B2 120.5(2) . . ? O3 La1 B2 84.3(2) 3_575 . ? O4 La1 B2 154.7(2) 4_565 . ? O4 La1 B2 84.9(2) 4_575 . ? O5 La1 B2 26.1(2) . . ? O8 La1 B2 103.2(2) 2_655 . ? O3 La1 B2 85.5(2) 1_545 . ? O8 La1 B2 48.7(2) 2_665 . ? O3 La1 B2 24.8(2) . . ? O11 La1 B2 138.6(2) 4_565 . ? O7 La1 Mo1 71.18(17) . 4_565 ? O3 La1 Mo1 79.70(15) 3_575 4_565 ? O4 La1 Mo1 28.40(15) 4_565 4_565 ? O4 La1 Mo1 85.36(15) 4_575 4_565 ? O5 La1 Mo1 160.02(13) . 4_565 ? O8 La1 Mo1 92.22(15) 2_655 4_565 ? O3 La1 Mo1 94.88(14) 1_545 4_565 ? O8 La1 Mo1 137.18(14) 2_665 4_565 ? O3 La1 Mo1 138.52(13) . 4_565 ? O11 La1 Mo1 29.01(11) 4_565 4_565 ? B2 La1 Mo1 162.49(18) . 4_565 ? O2 La2 O10 81.8(2) . . ? O2 La2 O1 82.4(2) . 2_645 ? O10 La2 O1 143.9(2) . 2_645 ? O2 La2 O2 113.2(3) . 1_565 ? O10 La2 O2 77.4(2) . 1_565 ? O1 La2 O2 79.3(2) 2_645 1_565 ? O2 La2 O12 131.2(2) . . ? O10 La2 O12 122.5(2) . . ? O1 La2 O12 92.0(2) 2_645 . ? O2 La2 O12 113.1(2) 1_565 . ? O2 La2 O6 69.8(2) . 2_545 ? O10 La2 O6 74.9(2) . 2_545 ? O1 La2 O6 128.4(2) 2_645 2_545 ? O2 La2 O6 151.4(2) 1_565 2_545 ? O12 La2 O6 76.8(2) . 2_545 ? O2 La2 O1 68.4(2) . 1_545 ? O10 La2 O1 132.2(2) . 1_545 ? O1 La2 O1 69.35(18) 2_645 1_545 ? O2 La2 O1 148.3(2) 1_565 1_545 ? O12 La2 O1 64.43(19) . 1_545 ? O6 La2 O1 60.3(2) 2_545 1_545 ? O2 La2 O1 149.5(2) . . ? O10 La2 O1 124.74(19) . . ? O1 La2 O1 67.21(19) 2_645 . ? O2 La2 O1 65.3(2) 1_565 . ? O12 La2 O1 50.94(18) . . ? O6 La2 O1 127.3(2) 2_545 . ? O1 La2 O1 96.9(2) 1_545 . ? O2 La2 O6 153.5(2) . 2 ? O10 La2 O6 71.9(2) . 2 ? O1 La2 O6 121.33(19) 2_645 2 ? O2 La2 O6 65.0(2) 1_565 2 ? O12 La2 O6 64.69(19) . 2 ? O6 La2 O6 99.2(2) 2_545 2 ? O1 La2 O6 128.23(19) 1_545 2 ? O1 La2 O6 56.16(19) . 2 ? O2 La2 O9 56.44(19) . 1_565 ? O10 La2 O9 68.8(2) . 1_565 ? O1 La2 O9 75.4(2) 2_645 1_565 ? O2 La2 O9 56.82(19) 1_565 1_565 ? O12 La2 O9 164.8(2) . 1_565 ? O6 La2 O9 117.6(2) 2_545 1_565 ? O1 La2 O9 117.08(19) 1_545 1_565 ? O1 La2 O9 115.06(18) . 1_565 ? O6 La2 O9 114.50(19) 2 1_565 ? O2 La2 B1 153.9(2) . . ? O10 La2 B1 121.0(2) . . ? O1 La2 B1 84.4(2) 2_645 . ? O2 La2 B1 86.2(2) 1_565 . ? O12 La2 B1 27.1(2) . . ? O6 La2 B1 101.9(2) 2_545 . ? O1 La2 B1 85.9(2) 1_545 . ? O1 La2 B1 25.6(2) . . ? O6 La2 B1 50.0(2) 2 . ? O9 La2 B1 140.2(2) 1_565 . ? O2 La2 Mo2 85.27(15) . 1_565 ? O10 La2 Mo2 68.45(17) . 1_565 ? O1 La2 Mo2 78.02(14) 2_645 1_565 ? O2 La2 Mo2 28.16(15) 1_565 1_565 ? O12 La2 Mo2 140.93(13) . 1_565 ? O6 La2 Mo2 138.12(15) 2_545 1_565 ? O1 La2 Mo2 139.99(14) 1_545 1_565 ? O1 La2 Mo2 90.98(13) . 1_565 ? O6 La2 Mo2 88.31(13) 2 1_565 ? O9 La2 Mo2 28.84(12) 1_565 1_565 ? B1 La2 Mo2 113.83(19) . 1_565 ? O10 Mo1 O11 106.5(3) . . ? O10 Mo1 O6 114.1(3) . . ? O11 Mo1 O6 102.8(3) . . ? O10 Mo1 O4 115.9(3) . . ? O11 Mo1 O4 96.5(3) . . ? O6 Mo1 O4 117.5(3) . . ? O10 Mo1 O11 81.8(3) . 1_565 ? O11 Mo1 O11 170.1(4) . 1_565 ? O6 Mo1 O11 78.0(3) . 1_565 ? O4 Mo1 O11 74.6(3) . 1_565 ? O10 Mo1 La1 119.2(2) . 4_566 ? O11 Mo1 La1 56.6(3) . 4_566 ? O6 Mo1 La1 126.3(2) . 4_566 ? O4 Mo1 La1 40.26(18) . 4_566 ? O11 Mo1 La1 114.88(18) 1_565 4_566 ? O7 Mo2 O9 106.8(3) 4_566 . ? O7 Mo2 O8 114.0(3) 4_566 . ? O9 Mo2 O8 102.0(3) . . ? O7 Mo2 O2 116.3(3) 4_566 . ? O9 Mo2 O2 96.4(3) . . ? O8 Mo2 O2 117.7(3) . . ? O7 Mo2 O9 82.3(3) 4_566 1_565 ? O9 Mo2 O9 169.5(4) . 1_565 ? O8 Mo2 O9 78.3(3) . 1_565 ? O2 Mo2 O9 74.4(3) . 1_565 ? O7 Mo2 La2 119.2(2) 4_566 1_545 ? O9 Mo2 La2 55.7(3) . 1_545 ? O8 Mo2 La2 126.3(2) . 1_545 ? O2 Mo2 La2 41.08(18) . 1_545 ? O9 Mo2 La2 115.50(19) 1_565 1_545 ? B1 O1 La2 125.5(6) . 2_655 ? B1 O1 La2 115.1(6) . 1_565 ? La2 O1 La2 113.8(2) 2_655 1_565 ? B1 O1 La2 86.8(5) . . ? La2 O1 La2 109.6(2) 2_655 . ? La2 O1 La2 96.9(2) 1_565 . ? Mo2 O2 La2 135.4(3) . . ? Mo2 O2 La2 110.8(3) . 1_545 ? La2 O2 La2 113.2(3) . 1_545 ? B2 O3 La1 127.4(6) . 3_575 ? B2 O3 La1 114.4(5) . 1_565 ? La1 O3 La1 112.6(2) 3_575 1_565 ? B2 O3 La1 85.4(5) . . ? La1 O3 La1 112.1(2) 3_575 . ? La1 O3 La1 95.8(2) 1_565 . ? Mo1 O4 La1 111.3(3) . 4_566 ? Mo1 O4 La1 134.6(3) . 4_576 ? La1 O4 La1 113.6(3) 4_566 4_576 ? B1 O5 B2 127.3(7) . . ? B1 O5 La1 131.8(5) . . ? B2 O5 La1 99.6(5) . . ? Mo1 O6 La2 144.5(3) . 2 ? Mo1 O6 La2 115.8(3) . 2_545 ? La2 O6 La2 99.2(2) 2 2_545 ? Mo2 O7 La1 170.3(3) 4_565 . ? Mo2 O8 La1 143.8(3) . 2_645 ? Mo2 O8 La1 115.8(3) . 2_635 ? La1 O8 La1 99.7(2) 2_645 2_635 ? Mo2 O9 Mo2 169.5(4) . 1_545 ? Mo2 O9 La2 95.5(3) . 1_545 ? Mo2 O9 La2 93.2(2) 1_545 1_545 ? Mo1 O10 La2 165.1(3) . . ? Mo1 O11 Mo1 170.1(4) . 1_545 ? Mo1 O11 La1 94.4(3) . 4_566 ? Mo1 O11 La1 94.0(2) 1_545 4_566 ? B2 O12 B1 127.8(7) 1_545 . ? B2 O12 La2 134.3(5) 1_545 . ? B1 O12 La2 96.5(5) . . ? O1 B1 O5 128.6(8) . . ? O1 B1 O12 117.9(8) . . ? O5 B1 O12 113.5(8) . . ? O1 B1 La2 67.6(5) . . ? O5 B1 La2 154.1(7) . . ? O12 B1 La2 56.4(4) . . ? O3 B2 O12 128.2(8) . 1_565 ? O3 B2 O5 117.9(8) . . ? O12 B2 O5 113.8(7) 1_565 . ? O3 B2 La1 69.8(5) . . ? O12 B2 La1 153.5(6) 1_565 . ? O5 B2 La1 54.3(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.901 _refine_diff_density_min -1.441 _refine_diff_density_rms 0.309