# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ye, Ning' _publ_contact_author_email nye@fjirsm.ac.cn _publ_author_name 'Ning Ye' data_Cd4GdO-BO3-3 _database_code_depnum_ccdc_archive 'CCDC 882094' #TrackingRef 'Cd4GdO-BO3-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B3 Cd4 Gd O10' _chemical_formula_weight 799.28 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 7.992(9) _cell_length_b 15.777(16) _cell_length_c 3.494(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.22(2) _cell_angle_gamma 90.00 _cell_volume 433.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 732 _cell_measurement_theta_min 2.5821 _cell_measurement_theta_max 27.4354 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 17.234 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5478 _exptl_absorpt_process_details ? _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 ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number ? _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 1626 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.46 _reflns_number_total 927 _reflns_number_gt 882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 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^)+(0.0471P)^2^+2.9631P] 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 0.0121(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(3) _refine_ls_number_reflns 927 _refine_ls_number_parameters 76 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.096 _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 Gd1 Gd 0.88522(14) 0.5000 0.8464(3) 0.0189(4) Uani 1 2 d S . . Cd1 Cd 0.53396(13) 0.61217(7) 1.1853(2) 0.0088(3) Uani 1 1 d . . . Cd2 Cd 1.15163(14) 0.32185(7) 0.4913(3) 0.0109(3) Uani 1 1 d . . . O1 O 0.710(2) 0.5000 1.261(5) 0.011(3) Uiso 1 2 d S . . O2 O 1.3479(15) 0.4229(7) 0.608(3) 0.013(2) Uani 1 1 d . . . O3 O 0.9792(15) 0.3528(8) 0.925(3) 0.019(3) Uani 1 1 d . . . O4 O 0.3604(19) 0.7303(8) 1.146(4) 0.031(4) Uani 1 1 d . . . O5 O 0.6791(18) 0.6791(9) 0.731(4) 0.030(4) Uani 1 1 d . . . O6 O 1.096(2) 0.5000 0.443(6) 0.024(4) Uiso 1 2 d S . . B1 B 1.267(3) 0.5000 0.555(8) 0.009(4) Uiso 1 2 d S . . B2 B 0.841(2) 0.6986(11) 0.937(5) 0.007(3) Uiso 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 Gd1 0.0150(6) 0.0270(7) 0.0149(6) 0.000 0.0034(4) 0.000 Cd1 0.0106(6) 0.0070(5) 0.0088(5) 0.0001(4) 0.0014(4) 0.0014(4) Cd2 0.0137(7) 0.0096(5) 0.0101(6) 0.0007(5) 0.0042(4) -0.0013(4) O2 0.019(6) 0.011(6) 0.007(5) -0.001(5) -0.002(4) 0.004(5) O3 0.011(6) 0.027(7) 0.020(6) -0.001(6) 0.008(5) -0.003(5) O4 0.050(9) 0.016(6) 0.038(8) 0.015(6) 0.037(7) 0.018(6) O5 0.029(8) 0.048(10) 0.013(6) -0.006(6) 0.006(6) -0.022(7) _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 Gd1 O1 2.186(15) . ? Gd1 O1 2.264(17) 1_554 ? Gd1 O6 2.379(19) . ? Gd1 O6 2.43(2) 1_556 ? Gd1 O3 2.441(14) 2_565 ? Gd1 O3 2.441(14) . ? Gd1 Gd1 3.494(4) 1_554 ? Gd1 Gd1 3.494(4) 1_556 ? Gd1 Cd1 3.687(3) 2_565 ? Gd1 Cd1 3.687(3) . ? Gd1 Cd1 3.748(3) 2_564 ? Gd1 Cd1 3.748(3) 1_554 ? Cd1 O1 2.247(10) . ? Cd1 O5 2.304(13) 1_556 ? Cd1 O4 2.313(12) . ? Cd1 O2 2.340(10) 2_466 ? Cd1 O2 2.350(11) 2_465 ? Cd1 O5 2.374(13) . ? Cd1 Gd1 3.748(3) 1_556 ? Cd2 O2 2.223(12) . ? Cd2 O3 2.255(13) 1_554 ? Cd2 O3 2.275(11) . ? Cd2 O4 2.372(12) 2_664 ? Cd2 O5 2.399(15) 3_545 ? Cd2 B2 2.767(18) 3_545 ? O1 Cd1 2.247(10) 2_565 ? O1 Gd1 2.264(17) 1_556 ? O2 B1 1.376(17) . ? O2 Cd1 2.340(10) 2_664 ? O2 Cd1 2.350(11) 2_665 ? O3 B2 1.38(2) 2_565 ? O3 Cd2 2.255(13) 1_556 ? O4 B2 1.33(2) 4_465 ? O4 Cd2 2.372(12) 2_466 ? O5 B2 1.40(2) . ? O5 Cd1 2.304(13) 1_554 ? O5 Cd2 2.399(15) 3_455 ? O6 B1 1.35(3) . ? O6 Gd1 2.43(2) 1_554 ? B1 O2 1.376(17) 2_565 ? B2 O4 1.33(2) 4_565 ? B2 O3 1.38(2) 2_565 ? B2 Cd2 2.767(18) 3_455 ? 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 Gd1 O1 103.5(7) . 1_554 ? O1 Gd1 O6 175.0(7) . . ? O1 Gd1 O6 81.5(6) 1_554 . ? O1 Gd1 O6 81.9(6) . 1_556 ? O1 Gd1 O6 174.6(6) 1_554 1_556 ? O6 Gd1 O6 93.1(7) . 1_556 ? O1 Gd1 O3 98.4(3) . 2_565 ? O1 Gd1 O3 103.3(3) 1_554 2_565 ? O6 Gd1 O3 80.3(3) . 2_565 ? O6 Gd1 O3 75.6(3) 1_556 2_565 ? O1 Gd1 O3 98.4(3) . . ? O1 Gd1 O3 103.3(3) 1_554 . ? O6 Gd1 O3 80.3(3) . . ? O6 Gd1 O3 75.6(3) 1_556 . ? O3 Gd1 O3 144.1(6) 2_565 . ? O1 Gd1 Gd1 140.9(4) . 1_554 ? O1 Gd1 Gd1 37.5(4) 1_554 1_554 ? O6 Gd1 Gd1 44.1(5) . 1_554 ? O6 Gd1 Gd1 137.2(4) 1_556 1_554 ? O3 Gd1 Gd1 93.3(3) 2_565 1_554 ? O3 Gd1 Gd1 93.3(3) . 1_554 ? O1 Gd1 Gd1 39.1(4) . 1_556 ? O1 Gd1 Gd1 142.5(4) 1_554 1_556 ? O6 Gd1 Gd1 135.9(5) . 1_556 ? O6 Gd1 Gd1 42.8(4) 1_556 1_556 ? O3 Gd1 Gd1 86.7(3) 2_565 1_556 ? O3 Gd1 Gd1 86.7(3) . 1_556 ? Gd1 Gd1 Gd1 180.00(7) 1_554 1_556 ? O1 Gd1 Cd1 34.3(2) . 2_565 ? O1 Gd1 Cd1 84.6(3) 1_554 2_565 ? O6 Gd1 Cd1 148.1(2) . 2_565 ? O6 Gd1 Cd1 100.1(4) 1_556 2_565 ? O3 Gd1 Cd1 131.1(3) 2_565 2_565 ? O3 Gd1 Cd1 75.2(3) . 2_565 ? Gd1 Gd1 Cd1 117.14(4) 1_554 2_565 ? Gd1 Gd1 Cd1 62.86(4) 1_556 2_565 ? O1 Gd1 Cd1 34.3(2) . . ? O1 Gd1 Cd1 84.6(3) 1_554 . ? O6 Gd1 Cd1 148.1(2) . . ? O6 Gd1 Cd1 100.1(4) 1_556 . ? O3 Gd1 Cd1 75.2(3) 2_565 . ? O3 Gd1 Cd1 131.1(3) . . ? Gd1 Gd1 Cd1 117.14(4) 1_554 . ? Gd1 Gd1 Cd1 62.86(4) 1_556 . ? Cd1 Gd1 Cd1 57.37(8) 2_565 . ? O1 Gd1 Cd1 84.9(4) . 2_564 ? O1 Gd1 Cd1 33.7(2) 1_554 2_564 ? O6 Gd1 Cd1 99.5(4) . 2_564 ? O6 Gd1 Cd1 148.84(18) 1_556 2_564 ? O3 Gd1 Cd1 134.5(3) 2_565 2_564 ? O3 Gd1 Cd1 78.6(3) . 2_564 ? Gd1 Gd1 Cd1 61.09(5) 1_554 2_564 ? Gd1 Gd1 Cd1 118.91(5) 1_556 2_564 ? Cd1 Gd1 Cd1 56.06(7) 2_565 2_564 ? Cd1 Gd1 Cd1 83.96(8) . 2_564 ? O1 Gd1 Cd1 84.9(4) . 1_554 ? O1 Gd1 Cd1 33.7(2) 1_554 1_554 ? O6 Gd1 Cd1 99.5(4) . 1_554 ? O6 Gd1 Cd1 148.84(18) 1_556 1_554 ? O3 Gd1 Cd1 78.6(3) 2_565 1_554 ? O3 Gd1 Cd1 134.5(3) . 1_554 ? Gd1 Gd1 Cd1 61.09(5) 1_554 1_554 ? Gd1 Gd1 Cd1 118.91(5) 1_556 1_554 ? Cd1 Gd1 Cd1 83.96(8) 2_565 1_554 ? Cd1 Gd1 Cd1 56.06(7) . 1_554 ? Cd1 Gd1 Cd1 56.35(7) 2_564 1_554 ? O1 Cd1 O5 92.9(5) . 1_556 ? O1 Cd1 O4 176.4(6) . . ? O5 Cd1 O4 83.6(6) 1_556 . ? O1 Cd1 O2 101.2(5) . 2_466 ? O5 Cd1 O2 82.5(4) 1_556 2_466 ? O4 Cd1 O2 77.7(4) . 2_466 ? O1 Cd1 O2 101.7(5) . 2_465 ? O5 Cd1 O2 165.3(5) 1_556 2_465 ? O4 Cd1 O2 81.8(5) . 2_465 ? O2 Cd1 O2 96.3(4) 2_466 2_465 ? O1 Cd1 O5 93.4(5) . . ? O5 Cd1 O5 96.6(5) 1_556 . ? O4 Cd1 O5 87.8(5) . . ? O2 Cd1 O5 165.4(5) 2_466 . ? O2 Cd1 O5 80.8(4) 2_465 . ? O1 Cd1 Gd1 33.2(4) . . ? O5 Cd1 Gd1 100.7(4) 1_556 . ? O4 Cd1 Gd1 148.3(3) . . ? O2 Cd1 Gd1 134.0(3) 2_466 . ? O2 Cd1 Gd1 90.7(3) 2_465 . ? O5 Cd1 Gd1 60.5(4) . . ? O1 Cd1 Gd1 34.0(4) . 1_556 ? O5 Cd1 Gd1 59.6(4) 1_556 1_556 ? O4 Cd1 Gd1 142.4(4) . 1_556 ? O2 Cd1 Gd1 89.4(3) 2_466 1_556 ? O2 Cd1 Gd1 135.1(3) 2_465 1_556 ? O5 Cd1 Gd1 102.8(4) . 1_556 ? Gd1 Cd1 Gd1 56.06(7) . 1_556 ? O2 Cd2 O3 107.9(4) . 1_554 ? O2 Cd2 O3 102.4(4) . . ? O3 Cd2 O3 101.0(5) 1_554 . ? O2 Cd2 O4 78.7(4) . 2_664 ? O3 Cd2 O4 90.3(5) 1_554 2_664 ? O3 Cd2 O4 167.6(5) . 2_664 ? O2 Cd2 O5 126.3(5) . 3_545 ? O3 Cd2 O5 120.9(5) 1_554 3_545 ? O3 Cd2 O5 89.9(4) . 3_545 ? O4 Cd2 O5 79.8(5) 2_664 3_545 ? O2 Cd2 B2 96.0(5) . 3_545 ? O3 Cd2 B2 146.5(5) 1_554 3_545 ? O3 Cd2 B2 96.3(5) . 3_545 ? O4 Cd2 B2 71.3(5) 2_664 3_545 ? O5 Cd2 B2 30.3(5) 3_545 3_545 ? Gd1 O1 Cd1 112.5(5) . 2_565 ? Gd1 O1 Cd1 112.5(5) . . ? Cd1 O1 Cd1 103.9(6) 2_565 . ? Gd1 O1 Gd1 103.5(7) . 1_556 ? Cd1 O1 Gd1 112.4(5) 2_565 1_556 ? Cd1 O1 Gd1 112.4(5) . 1_556 ? B1 O2 Cd2 107.9(12) . . ? B1 O2 Cd1 117.5(12) . 2_664 ? Cd2 O2 Cd1 102.8(4) . 2_664 ? B1 O2 Cd1 122.4(13) . 2_665 ? Cd2 O2 Cd1 107.8(4) . 2_665 ? Cd1 O2 Cd1 96.3(4) 2_664 2_665 ? B2 O3 Cd2 102.4(9) 2_565 1_556 ? B2 O3 Cd2 118.6(10) 2_565 . ? Cd2 O3 Cd2 101.0(5) 1_556 . ? B2 O3 Gd1 109.2(10) 2_565 . ? Cd2 O3 Gd1 115.6(5) 1_556 . ? Cd2 O3 Gd1 109.9(5) . . ? B2 O4 Cd1 136.2(10) 4_465 . ? B2 O4 Cd2 123.0(10) 4_465 2_466 ? Cd1 O4 Cd2 99.1(5) . 2_466 ? B2 O5 Cd1 144.3(11) . 1_554 ? B2 O5 Cd1 105.6(10) . . ? Cd1 O5 Cd1 96.6(5) 1_554 . ? B2 O5 Cd2 89.6(10) . 3_455 ? Cd1 O5 Cd2 98.1(5) 1_554 3_455 ? Cd1 O5 Cd2 128.7(6) . 3_455 ? B1 O6 Gd1 127.7(15) . . ? B1 O6 Gd1 139.2(15) . 1_554 ? Gd1 O6 Gd1 93.1(7) . 1_554 ? O6 B1 O2 117.9(11) . . ? O6 B1 O2 117.9(11) . 2_565 ? O2 B1 O2 124(2) . 2_565 ? O4 B2 O3 119.6(15) 4_565 2_565 ? O4 B2 O5 118.5(15) 4_565 . ? O3 B2 O5 121.9(15) 2_565 . ? O4 B2 Cd2 73.6(10) 4_565 3_455 ? O3 B2 Cd2 139.2(11) 2_565 3_455 ? O5 B2 Cd2 60.1(9) . 3_455 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.962 _refine_diff_density_min -2.309 _refine_diff_density_rms 0.472 # Attachment 'Cd4LuO-BO3-3.cif' data_Cd4LuO-BO3-3 _database_code_depnum_ccdc_archive 'CCDC 882095' #TrackingRef 'Cd4LuO-BO3-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B3 Cd4 Lu O10' _chemical_formula_weight 817.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 7.937(5) _cell_length_b 15.778(10) _cell_length_c 3.436(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.972(10) _cell_angle_gamma 90.00 _cell_volume 423.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 686 _cell_measurement_theta_min 2.9082 _cell_measurement_theta_max 27.5438 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 21.458 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5946 _exptl_absorpt_process_details ? _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 ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2017 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1005 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.41 _reflns_number_total 954 _reflns_number_gt 865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 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^)+(0.0693P)^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 0.0100(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(3) _refine_ls_number_reflns 954 _refine_ls_number_parameters 56 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _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 Cd1 Cd 0.06243(19) 0.11207(9) 0.9295(3) 0.0011(4) Uiso 1 1 d . . . Cd2 Cd 0.4479(2) 0.17790(11) 0.6264(4) 0.0099(5) Uani 1 1 d . . . Lu2 Lu -0.2945(2) 0.0000 1.2629(4) 0.0155(5) Uani 1 2 d S . . O1 O -0.119(3) 0.0000 0.847(8) 0.011(5) Uiso 1 2 d S . . O2 O -0.080(3) 0.1782(12) 1.385(6) 0.015(4) Uani 1 1 d . . . O3 O 0.249(2) 0.0767(13) 0.509(5) 0.010(4) Uiso 1 1 d . . . O4 O -0.377(2) -0.1413(13) 1.186(6) 0.013(4) Uiso 1 1 d . . . O5 O 0.234(3) 0.2282(13) 0.962(6) 0.020(4) Uiso 1 1 d . . . O6 O -0.486(5) 0.0000 1.683(10) 0.030(8) Uiso 1 2 d S . . B1 B -0.243(4) 0.2000(18) 1.188(8) 0.006(5) Uiso 1 1 d . . . B2 B 0.318(5) 0.0000 0.549(10) 0.002(6) Uiso 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 Cd2 0.0116(10) 0.0062(8) 0.0125(9) 0.0010(7) 0.0037(7) 0.0000(7) Lu2 0.0167(9) 0.0139(9) 0.0163(8) 0.000 0.0041(6) 0.000 O2 0.008(9) 0.012(9) 0.023(10) -0.003(8) -0.006(8) 0.004(7) _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 Cd1 O2 2.27(2) 1_554 ? Cd1 O1 2.269(17) . ? Cd1 O5 2.28(2) . ? Cd1 O3 2.310(16) . ? Cd1 O2 2.33(2) . ? Cd1 O3 2.333(19) 1_556 ? Cd1 Cd1 3.436(2) 1_554 ? Cd1 Cd1 3.436(2) 1_556 ? Cd1 Lu2 3.687(2) . ? Cd2 O3 2.23(2) . ? Cd2 O4 2.24(2) 2_655 ? Cd2 O4 2.297(18) 2_654 ? Cd2 O5 2.348(19) . ? Cd2 O2 2.415(19) 4_554 ? Cd2 B1 2.73(3) 4_554 ? Cd2 Cd2 3.436(2) 1_556 ? Cd2 Cd2 3.436(2) 1_554 ? Lu2 O1 2.16(2) . ? Lu2 O1 2.24(3) 1_556 ? Lu2 O6 2.27(3) . ? Lu2 O6 2.29(4) 1_554 ? Lu2 O4 2.33(2) . ? Lu2 O4 2.33(2) 2 ? Lu2 Lu2 3.436(2) 1_556 ? Lu2 Lu2 3.436(2) 1_554 ? Lu2 Cd1 3.687(2) 2 ? O1 Lu2 2.24(3) 1_554 ? O1 Cd1 2.269(17) 2 ? O2 B1 1.39(3) . ? O2 Cd1 2.27(2) 1_556 ? O2 Cd2 2.415(19) 4_456 ? O3 B2 1.33(3) . ? O3 Cd1 2.333(18) 1_554 ? O4 B1 1.41(3) 2 ? O4 Cd2 2.24(2) 2_455 ? O4 Cd2 2.297(18) 2_456 ? O5 B1 1.37(4) 4 ? O6 B2 1.54(5) 1_456 ? O6 Lu2 2.29(4) 1_556 ? B1 O5 1.37(3) 4_455 ? B1 O4 1.41(3) 2 ? B1 Cd2 2.73(3) 4_456 ? B2 O3 1.33(3) 2 ? B2 O6 1.54(5) 1_654 ? 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 Cd1 O1 92.3(8) 1_554 . ? O2 Cd1 O5 83.1(7) 1_554 . ? O1 Cd1 O5 175.3(9) . . ? O2 Cd1 O3 83.0(7) 1_554 . ? O1 Cd1 O3 101.4(7) . . ? O5 Cd1 O3 77.4(7) . . ? O2 Cd1 O2 96.7(7) 1_554 . ? O1 Cd1 O2 93.4(8) . . ? O5 Cd1 O2 87.9(7) . . ? O3 Cd1 O2 165.2(7) . . ? O2 Cd1 O3 165.2(7) 1_554 1_556 ? O1 Cd1 O3 102.5(8) . 1_556 ? O5 Cd1 O3 82.2(7) . 1_556 ? O3 Cd1 O3 95.4(7) . 1_556 ? O2 Cd1 O3 81.1(6) . 1_556 ? O2 Cd1 Cd1 42.4(5) 1_554 1_554 ? O1 Cd1 Cd1 89.2(6) . 1_554 ? O5 Cd1 Cd1 86.9(5) . 1_554 ? O3 Cd1 Cd1 42.5(5) . 1_554 ? O2 Cd1 Cd1 139.1(5) . 1_554 ? O3 Cd1 Cd1 138.0(4) 1_556 1_554 ? O2 Cd1 Cd1 137.6(5) 1_554 1_556 ? O1 Cd1 Cd1 90.8(6) . 1_556 ? O5 Cd1 Cd1 93.1(5) . 1_556 ? O3 Cd1 Cd1 137.5(5) . 1_556 ? O2 Cd1 Cd1 40.9(5) . 1_556 ? O3 Cd1 Cd1 42.0(4) 1_556 1_556 ? Cd1 Cd1 Cd1 180.00(5) 1_554 1_556 ? O2 Cd1 Lu2 100.1(5) 1_554 . ? O1 Cd1 Lu2 32.7(6) . . ? O5 Cd1 Lu2 149.0(5) . . ? O3 Cd1 Lu2 133.6(5) . . ? O2 Cd1 Lu2 61.1(5) . . ? O3 Cd1 Lu2 91.7(4) 1_556 . ? Cd1 Cd1 Lu2 116.35(4) 1_554 . ? Cd1 Cd1 Lu2 63.65(4) 1_556 . ? O3 Cd2 O4 106.5(7) . 2_655 ? O3 Cd2 O4 100.9(7) . 2_654 ? O4 Cd2 O4 98.4(7) 2_655 2_654 ? O3 Cd2 O5 77.4(7) . . ? O4 Cd2 O5 93.4(7) 2_655 . ? O4 Cd2 O5 168.1(7) 2_654 . ? O3 Cd2 O2 126.1(8) . 4_554 ? O4 Cd2 O2 122.9(7) 2_655 4_554 ? O4 Cd2 O2 92.3(7) 2_654 4_554 ? O5 Cd2 O2 79.5(7) . 4_554 ? O3 Cd2 B1 95.6(8) . 4_554 ? O4 Cd2 B1 148.7(8) 2_655 4_554 ? O4 Cd2 B1 98.8(7) 2_654 4_554 ? O5 Cd2 B1 69.8(7) . 4_554 ? O2 Cd2 B1 30.5(7) 4_554 4_554 ? O3 Cd2 Cd2 93.4(4) . 1_556 ? O4 Cd2 Cd2 41.4(5) 2_655 1_556 ? O4 Cd2 Cd2 139.8(5) 2_654 1_556 ? O5 Cd2 Cd2 52.0(5) . 1_556 ? O2 Cd2 Cd2 109.1(5) 4_554 1_556 ? B1 Cd2 Cd2 117.1(5) 4_554 1_556 ? O3 Cd2 Cd2 86.6(4) . 1_554 ? O4 Cd2 Cd2 138.6(5) 2_655 1_554 ? O4 Cd2 Cd2 40.2(5) 2_654 1_554 ? O5 Cd2 Cd2 128.0(5) . 1_554 ? O2 Cd2 Cd2 70.9(5) 4_554 1_554 ? B1 Cd2 Cd2 62.9(5) 4_554 1_554 ? Cd2 Cd2 Cd2 180.00(11) 1_556 1_554 ? O1 Lu2 O1 102.9(11) . 1_556 ? O1 Lu2 O6 178.2(12) . . ? O1 Lu2 O6 78.9(11) 1_556 . ? O1 Lu2 O6 80.2(11) . 1_554 ? O1 Lu2 O6 177.0(11) 1_556 1_554 ? O6 Lu2 O6 98.0(13) . 1_554 ? O1 Lu2 O4 97.3(5) . . ? O1 Lu2 O4 102.8(5) 1_556 . ? O6 Lu2 O4 82.3(5) . . ? O6 Lu2 O4 76.6(5) 1_554 . ? O1 Lu2 O4 97.3(5) . 2 ? O1 Lu2 O4 102.8(5) 1_556 2 ? O6 Lu2 O4 82.3(5) . 2 ? O6 Lu2 O4 76.6(5) 1_554 2 ? O4 Lu2 O4 146.8(10) . 2 ? O1 Lu2 Lu2 140.6(7) . 1_556 ? O1 Lu2 Lu2 37.7(6) 1_556 1_556 ? O6 Lu2 Lu2 41.2(9) . 1_556 ? O6 Lu2 Lu2 139.2(8) 1_554 1_556 ? O4 Lu2 Lu2 93.7(5) . 1_556 ? O4 Lu2 Lu2 93.7(5) 2 1_556 ? O1 Lu2 Lu2 39.4(7) . 1_554 ? O1 Lu2 Lu2 142.3(6) 1_556 1_554 ? O6 Lu2 Lu2 138.8(9) . 1_554 ? O6 Lu2 Lu2 40.8(8) 1_554 1_554 ? O4 Lu2 Lu2 86.3(5) . 1_554 ? O4 Lu2 Lu2 86.3(5) 2 1_554 ? Lu2 Lu2 Lu2 180.000(1) 1_556 1_554 ? O1 Lu2 Cd1 34.6(4) . . ? O1 Lu2 Cd1 83.5(6) 1_556 . ? O6 Lu2 Cd1 146.4(5) . . ? O6 Lu2 Cd1 99.1(7) 1_554 . ? O4 Lu2 Cd1 129.9(4) . . ? O4 Lu2 Cd1 73.9(4) 2 . ? Lu2 Lu2 Cd1 116.35(4) 1_556 . ? Lu2 Lu2 Cd1 63.65(4) 1_554 . ? O1 Lu2 Cd1 34.6(4) . 2 ? O1 Lu2 Cd1 83.5(6) 1_556 2 ? O6 Lu2 Cd1 146.4(5) . 2 ? O6 Lu2 Cd1 99.1(7) 1_554 2 ? O4 Lu2 Cd1 73.9(4) . 2 ? O4 Lu2 Cd1 129.9(4) 2 2 ? Lu2 Lu2 Cd1 116.35(4) 1_556 2 ? Lu2 Lu2 Cd1 63.65(4) 1_554 2 ? Cd1 Lu2 Cd1 57.32(6) . 2 ? Lu2 O1 Lu2 102.9(11) . 1_554 ? Lu2 O1 Cd1 112.7(8) . . ? Lu2 O1 Cd1 113.2(8) 1_554 . ? Lu2 O1 Cd1 112.7(8) . 2 ? Lu2 O1 Cd1 113.2(8) 1_554 2 ? Cd1 O1 Cd1 102.4(10) . 2 ? B1 O2 Cd1 143.5(17) . 1_556 ? B1 O2 Cd1 107.6(15) . . ? Cd1 O2 Cd1 96.7(7) 1_556 . ? B1 O2 Cd2 87.5(15) . 4_456 ? Cd1 O2 Cd2 98.4(7) 1_556 4_456 ? Cd1 O2 Cd2 128.6(9) . 4_456 ? B2 O3 Cd2 111.5(19) . . ? B2 O3 Cd1 117.1(17) . . ? Cd2 O3 Cd1 102.9(7) . . ? B2 O3 Cd1 119.8(19) . 1_554 ? Cd2 O3 Cd1 108.0(8) . 1_554 ? Cd1 O3 Cd1 95.4(7) . 1_554 ? B1 O4 Cd2 101.1(14) 2 2_455 ? B1 O4 Cd2 112.0(14) 2 2_456 ? Cd2 O4 Cd2 98.4(7) 2_455 2_456 ? B1 O4 Lu2 115.4(16) 2 . ? Cd2 O4 Lu2 117.7(9) 2_455 . ? Cd2 O4 Lu2 110.9(8) 2_456 . ? B1 O5 Cd1 135.7(16) 4 . ? B1 O5 Cd2 121.4(16) 4 . ? Cd1 O5 Cd2 100.4(8) . . ? B2 O6 Lu2 124(2) 1_456 . ? B2 O6 Lu2 138(2) 1_456 1_556 ? Lu2 O6 Lu2 98.0(13) . 1_556 ? O5 B1 O2 120(2) 4_455 . ? O5 B1 O4 121(2) 4_455 2 ? O2 B1 O4 118(2) . 2 ? O5 B1 Cd2 74.8(15) 4_455 4_456 ? O2 B1 Cd2 61.9(13) . 4_456 ? O4 B1 Cd2 144.2(16) 2 4_456 ? O3 B2 O3 132(3) 2 . ? O3 B2 O6 114.1(18) 2 1_654 ? O3 B2 O6 114.1(18) . 1_654 ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 3.568 _refine_diff_density_min -3.173 _refine_diff_density_rms 0.641 # Attachment 'Cd4YO-BO3-3.cif' data_Cd4YO-BO3-3 _database_code_depnum_ccdc_archive 'CCDC 882096' #TrackingRef 'Cd4YO-BO3-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B3 Cd4 O10 Y' _chemical_formula_weight 730.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 7.9627(10) _cell_length_b 15.793(2) _cell_length_c 3.4706(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.088(7) _cell_angle_gamma 90.00 _cell_volume 429.71(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 719 _cell_measurement_theta_min 2.9008 _cell_measurement_theta_max 27.4123 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 16.460 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5875 _exptl_absorpt_process_details ? _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 ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number ? _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 2379 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1019 _reflns_number_gt 977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 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^)+(0.0590P)^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 0.0283(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.246(19) _refine_ls_number_reflns 1019 _refine_ls_number_parameters 53 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.005 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 Cd1 Cd 0.38419(12) 0.11205(6) 0.22190(18) 0.0086(3) Uani 1 1 d . . . Cd2 Cd 1.00048(14) -0.17854(7) -0.4741(2) 0.0132(3) Uani 1 1 d . . . Y1 Y 0.7380(2) 0.0000 -0.1142(4) 0.0028(4) Uiso 1 2 d S . . O1 O 0.5606(16) 0.0000 0.310(3) 0.003(2) Uiso 1 2 d S . . O2 O 0.9406(17) 0.0000 -0.524(4) 0.009(3) Uiso 1 2 d S . . O3 O 0.5261(16) 0.1791(7) 0.772(4) 0.021(2) Uiso 1 1 d . . . O4 O 0.1995(11) 0.0763(6) 0.650(2) 0.0047(18) Uiso 1 1 d . . . O5 O 0.8224(12) -0.1422(6) -0.036(3) 0.0064(18) Uiso 1 1 d . . . O6 O 0.2103(18) 0.2302(9) 0.187(4) 0.031(3) Uiso 1 1 d . . . B1 B 1.112(3) 0.0000 -0.409(6) 0.005(4) Uiso 1 2 d S . . B2 B 0.687(2) 0.1980(12) 0.961(4) 0.011(3) Uiso 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 Cd1 0.0091(5) 0.0056(5) 0.0122(5) 0.0006(4) 0.0048(3) 0.0011(4) Cd2 0.0151(6) 0.0117(6) 0.0141(5) 0.0016(4) 0.0064(4) 0.0002(4) _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 Cd1 O1 2.247(8) . ? Cd1 O3 2.300(12) . ? Cd1 O6 2.314(14) . ? Cd1 O4 2.323(8) 1_554 ? Cd1 O3 2.335(13) 1_554 ? Cd1 O4 2.336(9) . ? Cd1 Cd1 3.4706(4) 1_554 ? Cd1 Cd1 3.4706(4) 1_556 ? Cd1 Y1 3.6852(17) . ? Cd1 Y1 3.7555(16) 1_556 ? Cd2 O4 2.251(10) 2_654 ? Cd2 O5 2.276(9) 1_554 ? Cd2 O5 2.324(10) . ? Cd2 O6 2.351(14) 2_654 ? Cd2 O3 2.402(12) 3_544 ? Cd2 B2 2.740(17) 3_544 ? Cd2 Cd2 3.4706(4) 1_554 ? Cd2 Cd2 3.4706(4) 1_556 ? Y1 O1 2.212(13) . ? Y1 O1 2.235(12) 1_554 ? Y1 O2 2.329(13) . ? Y1 O5 2.346(10) 2 ? Y1 O5 2.346(10) . ? Y1 O2 2.376(13) 1_556 ? Y1 Y1 3.4706(4) 1_556 ? Y1 Y1 3.4706(4) 1_554 ? Y1 Cd1 3.6852(17) 2 ? Y1 Cd1 3.7555(16) 2_554 ? Y1 Cd1 3.7555(16) 1_554 ? O1 Y1 2.235(12) 1_556 ? O1 Cd1 2.247(8) 2 ? O2 B1 1.35(3) . ? O2 Y1 2.376(13) 1_554 ? O3 B2 1.368(19) . ? O3 Cd1 2.335(13) 1_556 ? O3 Cd2 2.402(12) 3_456 ? O4 B1 1.389(14) 1_456 ? O4 Cd2 2.251(10) 2_456 ? O4 Cd1 2.323(8) 1_556 ? O5 B2 1.39(2) 2_554 ? O5 Cd2 2.276(9) 1_556 ? O6 B2 1.37(2) 4_454 ? O6 Cd2 2.351(14) 2_456 ? B1 O4 1.389(14) 1_654 ? B1 O4 1.389(14) 2_654 ? B2 O6 1.37(2) 4_556 ? B2 O5 1.39(2) 2_556 ? B2 Cd2 2.740(17) 3_456 ? 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 Cd1 O3 92.6(4) . . ? O1 Cd1 O6 175.1(5) . . ? O3 Cd1 O6 82.8(5) . . ? O1 Cd1 O4 102.3(4) . 1_554 ? O3 Cd1 O4 165.2(4) . 1_554 ? O6 Cd1 O4 82.4(4) . 1_554 ? O1 Cd1 O3 94.8(4) . 1_554 ? O3 Cd1 O3 97.0(5) . 1_554 ? O6 Cd1 O3 87.4(4) . 1_554 ? O4 Cd1 O3 81.2(4) 1_554 1_554 ? O1 Cd1 O4 99.9(4) . . ? O3 Cd1 O4 81.7(4) . . ? O6 Cd1 O4 77.9(4) . . ? O4 Cd1 O4 96.3(3) 1_554 . ? O3 Cd1 O4 165.3(4) 1_554 . ? O1 Cd1 Cd1 91.5(3) . 1_554 ? O3 Cd1 Cd1 138.1(3) . 1_554 ? O6 Cd1 Cd1 93.0(3) . 1_554 ? O4 Cd1 Cd1 42.0(2) 1_554 1_554 ? O3 Cd1 Cd1 41.1(3) 1_554 1_554 ? O4 Cd1 Cd1 138.3(2) . 1_554 ? O1 Cd1 Cd1 88.5(3) . 1_556 ? O3 Cd1 Cd1 41.9(3) . 1_556 ? O6 Cd1 Cd1 87.0(3) . 1_556 ? O4 Cd1 Cd1 138.0(2) 1_554 1_556 ? O3 Cd1 Cd1 138.9(3) 1_554 1_556 ? O4 Cd1 Cd1 41.7(2) . 1_556 ? Cd1 Cd1 Cd1 180.00(3) 1_554 1_556 ? O1 Cd1 Y1 34.0(3) . . ? O3 Cd1 Y1 101.1(3) . . ? O6 Cd1 Y1 148.7(3) . . ? O4 Cd1 Y1 91.0(2) 1_554 . ? O3 Cd1 Y1 61.3(3) 1_554 . ? O4 Cd1 Y1 133.4(2) . . ? Cd1 Cd1 Y1 63.23(3) 1_554 . ? Cd1 Cd1 Y1 116.77(3) 1_556 . ? O1 Cd1 Y1 33.0(3) . 1_556 ? O3 Cd1 Y1 60.0(3) . 1_556 ? O6 Cd1 Y1 142.2(3) . 1_556 ? O4 Cd1 Y1 134.8(2) 1_554 1_556 ? O3 Cd1 Y1 103.0(3) 1_554 1_556 ? O4 Cd1 Y1 89.1(2) . 1_556 ? Cd1 Cd1 Y1 118.82(3) 1_554 1_556 ? Cd1 Cd1 Y1 61.18(3) 1_556 1_556 ? Y1 Cd1 Y1 55.60(2) . 1_556 ? O4 Cd2 O5 107.2(3) 2_654 1_554 ? O4 Cd2 O5 100.8(3) 2_654 . ? O5 Cd2 O5 98.0(3) 1_554 . ? O4 Cd2 O6 78.8(4) 2_654 2_654 ? O5 Cd2 O6 92.8(4) 1_554 2_654 ? O5 Cd2 O6 168.8(4) . 2_654 ? O4 Cd2 O3 126.2(4) 2_654 3_544 ? O5 Cd2 O3 122.9(4) 1_554 3_544 ? O5 Cd2 O3 91.3(4) . 3_544 ? O6 Cd2 O3 80.2(5) 2_654 3_544 ? O4 Cd2 B2 96.3(4) 2_654 3_544 ? O5 Cd2 B2 148.1(4) 1_554 3_544 ? O5 Cd2 B2 98.6(4) . 3_544 ? O6 Cd2 B2 70.4(5) 2_654 3_544 ? O3 Cd2 B2 29.9(5) 3_544 3_544 ? O4 Cd2 Cd2 93.9(2) 2_654 1_554 ? O5 Cd2 Cd2 41.5(2) 1_554 1_554 ? O5 Cd2 Cd2 139.5(2) . 1_554 ? O6 Cd2 Cd2 51.3(3) 2_654 1_554 ? O3 Cd2 Cd2 109.9(3) 3_544 1_554 ? B2 Cd2 Cd2 117.1(3) 3_544 1_554 ? O4 Cd2 Cd2 86.1(2) 2_654 1_556 ? O5 Cd2 Cd2 138.5(2) 1_554 1_556 ? O5 Cd2 Cd2 40.5(2) . 1_556 ? O6 Cd2 Cd2 128.7(3) 2_654 1_556 ? O3 Cd2 Cd2 70.1(3) 3_544 1_556 ? B2 Cd2 Cd2 62.9(3) 3_544 1_556 ? Cd2 Cd2 Cd2 180.0 1_554 1_556 ? O1 Y1 O1 102.6(5) . 1_554 ? O1 Y1 O2 176.0(4) . . ? O1 Y1 O2 81.5(5) 1_554 . ? O1 Y1 O5 97.3(2) . 2 ? O1 Y1 O5 103.1(2) 1_554 2 ? O2 Y1 O5 81.7(2) . 2 ? O1 Y1 O5 97.3(2) . . ? O1 Y1 O5 103.1(2) 1_554 . ? O2 Y1 O5 81.7(2) . . ? O5 Y1 O5 146.3(5) 2 . ? O1 Y1 O2 80.9(4) . 1_556 ? O1 Y1 O2 176.5(5) 1_554 1_556 ? O2 Y1 O2 95.1(5) . 1_556 ? O5 Y1 O2 76.3(2) 2 1_556 ? O5 Y1 O2 76.3(2) . 1_556 ? O1 Y1 Y1 38.9(3) . 1_556 ? O1 Y1 Y1 141.5(3) 1_554 1_556 ? O2 Y1 Y1 137.0(3) . 1_556 ? O5 Y1 Y1 86.3(2) 2 1_556 ? O5 Y1 Y1 86.3(2) . 1_556 ? O2 Y1 Y1 41.9(3) 1_556 1_556 ? O1 Y1 Y1 141.1(3) . 1_554 ? O1 Y1 Y1 38.5(3) 1_554 1_554 ? O2 Y1 Y1 43.0(3) . 1_554 ? O5 Y1 Y1 93.7(2) 2 1_554 ? O5 Y1 Y1 93.7(2) . 1_554 ? O2 Y1 Y1 138.1(3) 1_556 1_554 ? Y1 Y1 Y1 180.0 1_556 1_554 ? O1 Y1 Cd1 34.57(16) . . ? O1 Y1 Cd1 83.4(3) 1_554 . ? O2 Y1 Cd1 147.43(14) . . ? O5 Y1 Cd1 73.9(2) 2 . ? O5 Y1 Cd1 130.0(2) . . ? O2 Y1 Cd1 99.7(3) 1_556 . ? Y1 Y1 Cd1 63.23(3) 1_556 . ? Y1 Y1 Cd1 116.77(3) 1_554 . ? O1 Y1 Cd1 34.57(16) . 2 ? O1 Y1 Cd1 83.4(3) 1_554 2 ? O2 Y1 Cd1 147.43(14) . 2 ? O5 Y1 Cd1 130.0(2) 2 2 ? O5 Y1 Cd1 73.9(2) . 2 ? O2 Y1 Cd1 99.7(3) 1_556 2 ? Y1 Y1 Cd1 63.23(3) 1_556 2 ? Y1 Y1 Cd1 116.77(3) 1_554 2 ? Cd1 Y1 Cd1 57.40(4) . 2 ? O1 Y1 Cd1 84.9(3) . 2_554 ? O1 Y1 Cd1 33.18(17) 1_554 2_554 ? O2 Y1 Cd1 98.7(3) . 2_554 ? O5 Y1 Cd1 133.7(2) 2 2_554 ? O5 Y1 Cd1 77.8(2) . 2_554 ? O2 Y1 Cd1 148.46(14) 1_556 2_554 ? Y1 Y1 Cd1 118.82(3) 1_556 2_554 ? Y1 Y1 Cd1 61.18(3) 1_554 2_554 ? Cd1 Y1 Cd1 83.54(4) . 2_554 ? Cd1 Y1 Cd1 55.60(2) 2 2_554 ? O1 Y1 Cd1 84.9(3) . 1_554 ? O1 Y1 Cd1 33.18(17) 1_554 1_554 ? O2 Y1 Cd1 98.7(3) . 1_554 ? O5 Y1 Cd1 77.8(2) 2 1_554 ? O5 Y1 Cd1 133.7(2) . 1_554 ? O2 Y1 Cd1 148.46(14) 1_556 1_554 ? Y1 Y1 Cd1 118.82(3) 1_556 1_554 ? Y1 Y1 Cd1 61.18(3) 1_554 1_554 ? Cd1 Y1 Cd1 55.60(2) . 1_554 ? Cd1 Y1 Cd1 83.54(4) 2 1_554 ? Cd1 Y1 Cd1 56.23(4) 2_554 1_554 ? Y1 O1 Y1 102.6(5) . 1_556 ? Y1 O1 Cd1 111.5(4) . . ? Y1 O1 Cd1 113.8(4) 1_556 . ? Y1 O1 Cd1 111.5(4) . 2 ? Y1 O1 Cd1 113.8(4) 1_556 2 ? Cd1 O1 Cd1 103.9(5) . 2 ? B1 O2 Y1 126.3(11) . . ? B1 O2 Y1 138.6(11) . 1_554 ? Y1 O2 Y1 95.1(5) . 1_554 ? B2 O3 Cd1 141.4(11) . . ? B2 O3 Cd1 107.6(10) . 1_556 ? Cd1 O3 Cd1 97.0(5) . 1_556 ? B2 O3 Cd2 88.9(10) . 3_456 ? Cd1 O3 Cd2 97.8(4) . 3_456 ? Cd1 O3 Cd2 129.9(5) 1_556 3_456 ? B1 O4 Cd2 106.1(9) 1_456 2_456 ? B1 O4 Cd1 124.3(9) 1_456 1_556 ? Cd2 O4 Cd1 108.0(4) 2_456 1_556 ? B1 O4 Cd1 118.1(10) 1_456 . ? Cd2 O4 Cd1 101.9(4) 2_456 . ? Cd1 O4 Cd1 96.3(3) 1_556 . ? B2 O5 Cd2 102.2(8) 2_554 1_556 ? B2 O5 Cd2 113.5(9) 2_554 . ? Cd2 O5 Cd2 98.0(3) 1_556 . ? B2 O5 Y1 113.6(9) 2_554 . ? Cd2 O5 Y1 117.6(4) 1_556 . ? Cd2 O5 Y1 110.9(4) . . ? B2 O6 Cd1 135.6(11) 4_454 . ? B2 O6 Cd2 122.5(11) 4_454 2_456 ? Cd1 O6 Cd2 99.5(5) . 2_456 ? O2 B1 O4 119.8(8) . 1_654 ? O2 B1 O4 119.8(8) . 2_654 ? O4 B1 O4 120.4(17) 1_654 2_654 ? O3 B2 O6 118.3(15) . 4_556 ? O3 B2 O5 121.7(14) . 2_556 ? O6 B2 O5 119.7(13) 4_556 2_556 ? O3 B2 Cd2 61.2(8) . 3_456 ? O6 B2 Cd2 74.5(9) 4_556 3_456 ? O5 B2 Cd2 143.1(10) 2_556 3_456 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.023 _refine_diff_density_min -1.595 _refine_diff_density_rms 0.415