# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jiang-Gao Mao' _publ_contact_author_email MJG@MS.FJIRSM.AC.CN _publ_section_title ; Ln2GeB2O8 (Ln = Nd, Sm-Tb): A Series of Luminescent Lanthanide(III) Borogermanates with a Layered Structure ; loop_ _publ_author_name 'Jiang-Gao Mao' 'Pei-Xin Li' 'Jian-Han Zhang' # Attachment 'zjh-dalton-cif.CIF' data_Nd2GeB2O8 _database_code_depnum_ccdc_archive 'CCDC 760683' #TrackingRef 'zjh-dalton-cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Ge Nd2 O8' _chemical_formula_weight 510.71 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.7041(16) _cell_length_b 4.4820(5) _cell_length_c 9.4608(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 581.10(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 703 _cell_measurement_theta_min 2.1526 _cell_measurement_theta_max 27.4758 _exptl_crystal_description brick _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 22.752 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.2233 _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_type 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4002 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.51 _reflns_number_total 667 _reflns_number_gt 661 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0395P)^2^+1.9468P] 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 0.0145(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 667 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.002 _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 Nd1 Nd 0.640210(17) 0.53989(7) 0.02601(3) 0.00427(18) Uani 1 1 d . . . Ge1 Ge 0.5000 0.07566(17) 0.2500 0.0036(2) Uani 1 2 d S . . B1 B 0.2007(4) 0.4666(11) 0.2056(6) 0.0034(10) Uani 1 1 d . . . O1 O 0.1928(3) 0.4620(8) 0.0527(4) 0.0054(7) Uani 1 1 d . . . O2 O 0.1057(2) 0.3495(8) 0.2664(3) 0.0055(7) Uani 1 1 d . . . O3 O 0.2189(2) 0.7749(8) 0.2604(4) 0.0059(7) Uani 1 1 d . . . O4 O 0.4955(2) 0.2941(9) 0.1007(4) 0.0092(7) 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 Nd1 0.0015(2) 0.0048(3) 0.0065(2) 0.00052(9) 0.00064(7) 0.00022(8) Ge1 0.0009(3) 0.0052(4) 0.0047(3) 0.000 0.0002(3) 0.000 B1 0.004(2) 0.001(2) 0.005(2) 0.0002(18) 0.002(2) 0.0012(18) O1 0.0054(16) 0.0064(18) 0.0044(15) 0.0011(13) 0.0000(14) 0.0010(13) O2 0.0051(16) 0.0044(17) 0.0071(16) 0.0036(13) 0.0011(12) 0.0011(13) O3 0.0034(14) 0.0062(17) 0.0080(15) -0.0015(14) 0.0025(11) -0.0010(13) O4 0.0046(14) 0.0122(19) 0.0109(15) 0.0044(14) -0.0014(12) -0.0010(13) _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 Nd1 O4 2.334(3) 5_665 ? Nd1 O4 2.377(3) . ? Nd1 O1 2.407(4) 5_665 ? Nd1 O2 2.451(3) 6_666 ? Nd1 O1 2.461(4) 4_565 ? Nd1 O1 2.476(4) 4 ? Nd1 O3 2.580(3) 6_656 ? Nd1 B1 3.091(6) 5_665 ? Nd1 Nd1 3.7519(5) 8_765 ? Nd1 Nd1 3.7519(5) 8_755 ? Nd1 Nd1 3.8907(7) 5_665 ? Ge1 O4 1.720(4) 3_655 ? Ge1 O4 1.720(4) . ? Ge1 O2 1.775(3) 8_655 ? Ge1 O2 1.775(3) 6_656 ? B1 O1 1.450(7) . ? B1 O3 1.491(6) 8_655 ? B1 O3 1.497(6) . ? B1 O2 1.516(6) . ? B1 Nd1 3.091(6) 5_665 ? O1 Nd1 2.407(4) 5_665 ? O1 Nd1 2.461(4) 4_465 ? O1 Nd1 2.476(4) 4_455 ? O2 Ge1 1.775(3) 6_566 ? O2 Nd1 2.451(3) 6_556 ? O3 B1 1.491(6) 8_665 ? O3 Nd1 2.580(3) 6_566 ? O4 Nd1 2.334(3) 5_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 O4 Nd1 O4 68.63(15) 5_665 . ? O4 Nd1 O1 126.85(12) 5_665 5_665 ? O4 Nd1 O1 152.14(12) . 5_665 ? O4 Nd1 O2 94.45(12) 5_665 6_666 ? O4 Nd1 O2 82.14(12) . 6_666 ? O1 Nd1 O2 115.67(12) 5_665 6_666 ? O4 Nd1 O1 77.78(13) 5_665 4_565 ? O4 Nd1 O1 139.00(13) . 4_565 ? O1 Nd1 O1 68.37(11) 5_665 4_565 ? O2 Nd1 O1 77.60(12) 6_666 4_565 ? O4 Nd1 O1 111.51(13) 5_665 4 ? O4 Nd1 O1 84.90(13) . 4 ? O1 Nd1 O1 68.12(11) 5_665 4 ? O2 Nd1 O1 144.23(13) 6_666 4 ? O1 Nd1 O1 130.38(17) 4_565 4 ? O4 Nd1 O3 151.88(11) 5_665 6_656 ? O4 Nd1 O3 84.41(11) . 6_656 ? O1 Nd1 O3 80.98(12) 5_665 6_656 ? O2 Nd1 O3 73.35(11) 6_666 6_656 ? O1 Nd1 O3 122.16(12) 4_565 6_656 ? O1 Nd1 O3 72.29(12) 4 6_656 ? O4 Nd1 B1 101.59(13) 5_665 5_665 ? O4 Nd1 B1 142.67(14) . 5_665 ? O1 Nd1 B1 27.11(14) 5_665 5_665 ? O2 Nd1 B1 135.17(13) 6_666 5_665 ? O1 Nd1 B1 65.65(13) 4_565 5_665 ? O1 Nd1 B1 64.73(13) 4 5_665 ? O3 Nd1 B1 104.83(13) 6_656 5_665 ? O4 Nd1 Nd1 116.64(9) 5_665 8_765 ? O4 Nd1 Nd1 161.14(9) . 8_765 ? O1 Nd1 Nd1 40.48(8) 5_665 8_765 ? O2 Nd1 Nd1 79.42(8) 6_666 8_765 ? O1 Nd1 Nd1 39.06(9) 4_565 8_765 ? O1 Nd1 Nd1 108.02(9) 4 8_765 ? O3 Nd1 Nd1 86.55(8) 6_656 8_765 ? B1 Nd1 Nd1 55.94(11) 5_665 8_765 ? O4 Nd1 Nd1 146.03(9) 5_665 8_755 ? O4 Nd1 Nd1 113.11(9) . 8_755 ? O1 Nd1 Nd1 40.12(8) 5_665 8_755 ? O2 Nd1 Nd1 119.52(8) 6_666 8_755 ? O1 Nd1 Nd1 107.89(9) 4_565 8_755 ? O1 Nd1 Nd1 39.13(9) 4 8_755 ? O3 Nd1 Nd1 52.40(8) 6_656 8_755 ? B1 Nd1 Nd1 55.15(10) 5_665 8_755 ? Nd1 Nd1 Nd1 73.352(12) 8_765 8_755 ? O4 Nd1 Nd1 34.67(9) 5_665 5_665 ? O4 Nd1 Nd1 33.96(8) . 5_665 ? O1 Nd1 Nd1 154.13(9) 5_665 5_665 ? O2 Nd1 Nd1 87.88(8) 6_666 5_665 ? O1 Nd1 Nd1 109.51(9) 4_565 5_665 ? O1 Nd1 Nd1 99.54(9) 4 5_665 ? O3 Nd1 Nd1 118.01(8) 6_656 5_665 ? B1 Nd1 Nd1 127.32(11) 5_665 5_665 ? Nd1 Nd1 Nd1 147.893(11) 8_765 5_665 ? Nd1 Nd1 Nd1 137.500(11) 8_755 5_665 ? O4 Ge1 O4 110.6(3) 3_655 . ? O4 Ge1 O2 106.44(16) 3_655 8_655 ? O4 Ge1 O2 111.54(15) . 8_655 ? O4 Ge1 O2 111.54(15) 3_655 6_656 ? O4 Ge1 O2 106.44(16) . 6_656 ? O2 Ge1 O2 110.4(2) 8_655 6_656 ? O1 B1 O3 113.2(4) . 8_655 ? O1 B1 O3 111.8(4) . . ? O3 B1 O3 106.7(4) 8_655 . ? O1 B1 O2 108.0(4) . . ? O3 B1 O2 107.6(4) 8_655 . ? O3 B1 O2 109.3(4) . . ? O1 B1 Nd1 49.2(2) . 5_665 ? O3 B1 Nd1 73.7(3) 8_655 5_665 ? O3 B1 Nd1 97.9(3) . 5_665 ? O2 B1 Nd1 150.6(3) . 5_665 ? B1 O1 Nd1 103.7(3) . 5_665 ? B1 O1 Nd1 108.1(3) . 4_465 ? Nd1 O1 Nd1 100.82(13) 5_665 4_465 ? B1 O1 Nd1 109.6(3) . 4_455 ? Nd1 O1 Nd1 100.38(13) 5_665 4_455 ? Nd1 O1 Nd1 130.38(16) 4_465 4_455 ? B1 O2 Ge1 118.0(3) . 6_566 ? B1 O2 Nd1 109.6(3) . 6_556 ? Ge1 O2 Nd1 123.40(16) 6_566 6_556 ? B1 O3 B1 122.3(4) 8_665 . ? B1 O3 Nd1 108.4(3) 8_665 6_566 ? B1 O3 Nd1 128.8(3) . 6_566 ? Ge1 O4 Nd1 129.21(17) . 5_665 ? Ge1 O4 Nd1 118.55(15) . . ? Nd1 O4 Nd1 111.37(15) 5_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.849 _refine_diff_density_min -2.168 _refine_diff_density_rms 0.372 #===end data_Sm2GeB2O8 _database_code_depnum_ccdc_archive 'CCDC 760684' #TrackingRef 'zjh-dalton-cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Ge O8 Sm2' _chemical_formula_weight 522.95 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.606(6) _cell_length_b 4.451(2) _cell_length_c 9.367(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 567.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1535 _cell_measurement_theta_min 3.7017 _cell_measurement_theta_max 27.4835 _exptl_crystal_description brick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.0800 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 25.703 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4723 _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_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3875 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.44 _reflns_number_total 642 _reflns_number_gt 627 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0263P)^2^+0.8316P] 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 0.0160(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 642 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.247 _refine_ls_restrained_S_all 1.247 _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 Sm1 Sm 0.640161(15) 0.53867(6) 0.02523(3) 0.00420(14) Uani 1 1 d . . . Ge1 Ge 0.5000 0.07429(14) 0.2500 0.00382(18) Uani 1 2 d S . . B1 B 0.2003(4) 0.4682(10) 0.2041(6) 0.0054(10) Uani 1 1 d . . . O1 O 0.1927(2) 0.4626(6) 0.0512(4) 0.0048(7) Uani 1 1 d . . . O2 O 0.1062(2) 0.3452(7) 0.2667(3) 0.0059(6) Uani 1 1 d . . . O3 O 0.2173(2) 0.7793(7) 0.2600(3) 0.0050(6) Uani 1 1 d . . . O4 O 0.49589(19) 0.2949(7) 0.0993(3) 0.0070(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 Sm1 0.00173(17) 0.00472(19) 0.0061(2) 0.00047(8) 0.00060(8) 0.00031(6) Ge1 0.0015(3) 0.0047(3) 0.0052(4) 0.000 0.0002(2) 0.000 B1 0.005(2) 0.004(2) 0.007(3) 0.0015(18) 0.004(2) -0.0003(16) O1 0.0045(14) 0.0045(14) 0.0056(19) 0.0004(11) -0.0008(13) 0.0003(11) O2 0.0042(14) 0.0048(14) 0.0087(18) 0.0026(12) 0.0015(12) -0.0002(11) O3 0.0041(13) 0.0049(14) 0.0061(17) -0.0011(12) 0.0035(11) -0.0011(11) O4 0.0047(13) 0.0088(14) 0.0075(17) 0.0031(12) -0.0001(11) -0.0009(11) _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 Sm1 O4 2.310(3) 5_665 ? Sm1 O4 2.347(3) . ? Sm1 O1 2.384(3) 5_665 ? Sm1 O2 2.423(3) 6_666 ? Sm1 O1 2.439(3) 4_565 ? Sm1 O1 2.450(3) 4 ? Sm1 O3 2.546(3) 6_656 ? Sm1 B1 3.054(6) 5_665 ? Sm1 Ge1 3.5130(10) . ? Sm1 Sm1 3.7263(12) 8_765 ? Sm1 Sm1 3.7263(12) 8_755 ? Sm1 Sm1 3.8585(17) 5_665 ? Ge1 O4 1.721(3) 3_655 ? Ge1 O4 1.721(3) . ? Ge1 O2 1.775(3) 8_655 ? Ge1 O2 1.775(3) 6_656 ? Ge1 Sm1 3.5130(10) 3_655 ? B1 O1 1.436(7) . ? B1 O3 1.496(6) 8_655 ? B1 O3 1.498(5) . ? B1 O2 1.512(6) . ? B1 Sm1 3.054(6) 5_665 ? O1 Sm1 2.384(3) 5_665 ? O1 Sm1 2.439(3) 4_465 ? O1 Sm1 2.450(3) 4_455 ? O2 Ge1 1.775(3) 6_566 ? O2 Sm1 2.423(3) 6_556 ? O3 B1 1.496(6) 8_665 ? O3 Sm1 2.546(3) 6_566 ? O4 Sm1 2.310(3) 5_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 O4 Sm1 O4 68.11(13) 5_665 . ? O4 Sm1 O1 127.86(11) 5_665 5_665 ? O4 Sm1 O1 152.27(10) . 5_665 ? O4 Sm1 O2 94.16(11) 5_665 6_666 ? O4 Sm1 O2 82.13(10) . 6_666 ? O1 Sm1 O2 115.14(10) 5_665 6_666 ? O4 Sm1 O1 78.17(11) 5_665 4_565 ? O4 Sm1 O1 138.78(11) . 4_565 ? O1 Sm1 O1 68.57(9) 5_665 4_565 ? O2 Sm1 O1 77.26(11) 6_666 4_565 ? O4 Sm1 O1 112.24(11) 5_665 4 ? O4 Sm1 O1 84.80(11) . 4 ? O1 Sm1 O1 68.39(9) 5_665 4 ? O2 Sm1 O1 143.45(11) 6_666 4 ? O1 Sm1 O1 131.12(15) 4_565 4 ? O4 Sm1 O3 151.01(10) 5_665 6_656 ? O4 Sm1 O3 84.36(10) . 6_656 ? O1 Sm1 O3 80.95(11) 5_665 6_656 ? O2 Sm1 O3 72.46(10) 6_666 6_656 ? O1 Sm1 O3 121.58(11) 4_565 6_656 ? O1 Sm1 O3 72.39(11) 4 6_656 ? O4 Sm1 B1 102.58(13) 5_665 5_665 ? O4 Sm1 B1 142.89(12) . 5_665 ? O1 Sm1 B1 27.23(14) 5_665 5_665 ? O2 Sm1 B1 134.98(12) 6_666 5_665 ? O1 Sm1 B1 66.08(12) 4_565 5_665 ? O1 Sm1 B1 65.04(12) 4 5_665 ? O3 Sm1 B1 104.96(13) 6_656 5_665 ? O4 Sm1 Ge1 93.22(8) 5_665 . ? O4 Sm1 Ge1 25.47(7) . . ? O1 Sm1 Ge1 134.13(8) 5_665 . ? O2 Sm1 Ge1 75.27(8) 6_666 . ? O1 Sm1 Ge1 150.49(8) 4_565 . ? O1 Sm1 Ge1 78.32(8) 4 . ? O3 Sm1 Ge1 58.90(7) 6_656 . ? B1 Sm1 Ge1 143.27(8) 5_665 . ? O4 Sm1 Sm1 116.83(8) 5_665 8_765 ? O4 Sm1 Sm1 161.20(8) . 8_765 ? O1 Sm1 Sm1 40.21(7) 5_665 8_765 ? O2 Sm1 Sm1 79.45(7) 6_666 8_765 ? O1 Sm1 Sm1 38.88(8) 4_565 8_765 ? O1 Sm1 Sm1 108.05(8) 4 8_765 ? O3 Sm1 Sm1 86.57(7) 6_656 8_765 ? B1 Sm1 Sm1 55.66(10) 5_665 8_765 ? Ge1 Sm1 Sm1 141.884(15) . 8_765 ? O4 Sm1 Sm1 146.54(8) 5_665 8_755 ? O4 Sm1 Sm1 113.25(8) . 8_755 ? O1 Sm1 Sm1 39.95(7) 5_665 8_755 ? O2 Sm1 Sm1 119.30(7) 6_666 8_755 ? O1 Sm1 Sm1 107.96(8) 4_565 8_755 ? O1 Sm1 Sm1 38.92(8) 4 8_755 ? O3 Sm1 Sm1 53.02(7) 6_656 8_755 ? B1 Sm1 Sm1 54.82(9) 5_665 8_755 ? Ge1 Sm1 Sm1 94.82(3) . 8_755 ? Sm1 Sm1 Sm1 73.34(3) 8_765 8_755 ? O4 Sm1 Sm1 34.37(7) 5_665 5_665 ? O4 Sm1 Sm1 33.74(7) . 5_665 ? O1 Sm1 Sm1 154.95(9) 5_665 5_665 ? O2 Sm1 Sm1 87.71(7) 6_666 5_665 ? O1 Sm1 Sm1 109.57(8) 4_565 5_665 ? O1 Sm1 Sm1 99.87(8) 4 5_665 ? O3 Sm1 Sm1 117.63(7) 6_656 5_665 ? B1 Sm1 Sm1 127.99(11) 5_665 5_665 ? Ge1 Sm1 Sm1 58.959(17) . 5_665 ? Sm1 Sm1 Sm1 147.791(16) 8_765 5_665 ? Sm1 Sm1 Sm1 137.69(2) 8_755 5_665 ? O4 Ge1 O4 110.4(2) 3_655 . ? O4 Ge1 O2 106.37(14) 3_655 8_655 ? O4 Ge1 O2 111.96(13) . 8_655 ? O4 Ge1 O2 111.95(13) 3_655 6_656 ? O4 Ge1 O2 106.37(14) . 6_656 ? O2 Ge1 O2 109.88(19) 8_655 6_656 ? O4 Ge1 Sm1 35.92(9) 3_655 3_655 ? O4 Ge1 Sm1 97.95(11) . 3_655 ? O2 Ge1 Sm1 80.98(10) 8_655 3_655 ? O2 Ge1 Sm1 146.37(10) 6_656 3_655 ? O4 Ge1 Sm1 97.95(11) 3_655 . ? O4 Ge1 Sm1 35.92(9) . . ? O2 Ge1 Sm1 146.37(10) 8_655 . ? O2 Ge1 Sm1 80.98(10) 6_656 . ? Sm1 Ge1 Sm1 107.92(3) 3_655 . ? O1 B1 O3 113.2(4) . 8_655 ? O1 B1 O3 112.1(4) . . ? O3 B1 O3 106.3(4) 8_655 . ? O1 B1 O2 108.7(4) . . ? O3 B1 O2 107.2(3) 8_655 . ? O3 B1 O2 109.3(4) . . ? O1 B1 Sm1 49.4(2) . 5_665 ? O3 B1 Sm1 73.0(2) 8_655 5_665 ? O3 B1 Sm1 98.4(3) . 5_665 ? O2 B1 Sm1 150.7(3) . 5_665 ? B1 O1 Sm1 103.3(3) . 5_665 ? B1 O1 Sm1 107.3(2) . 4_465 ? Sm1 O1 Sm1 101.17(12) 5_665 4_465 ? B1 O1 Sm1 109.1(2) . 4_455 ? Sm1 O1 Sm1 100.86(11) 5_665 4_455 ? Sm1 O1 Sm1 131.12(15) 4_465 4_455 ? B1 O2 Ge1 116.6(3) . 6_566 ? B1 O2 Sm1 110.8(3) . 6_556 ? Ge1 O2 Sm1 123.35(15) 6_566 6_556 ? B1 O3 B1 120.9(4) 8_665 . ? B1 O3 Sm1 109.3(3) 8_665 6_566 ? B1 O3 Sm1 129.2(3) . 6_566 ? Ge1 O4 Sm1 128.56(14) . 5_665 ? Ge1 O4 Sm1 118.61(13) . . ? Sm1 O4 Sm1 111.89(13) 5_665 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.936 _refine_diff_density_min -2.211 _refine_diff_density_rms 0.321 #===end data_Eu2GeB2O8 _database_code_depnum_ccdc_archive 'CCDC 760685' #TrackingRef 'zjh-dalton-cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Eu2 Ge O8' _chemical_formula_weight 526.17 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.564(7) _cell_length_b 4.435(2) _cell_length_c 9.334(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 561.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 669 _cell_measurement_theta_min 2.1817 _cell_measurement_theta_max 27.4797 _exptl_crystal_description brick _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 27.393 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4117 _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_type 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3866 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 27.46 _reflns_number_total 642 _reflns_number_gt 628 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0217P)^2^+0.5592P] 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 0.0078(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 642 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0410 _refine_ls_wR_factor_gt 0.0407 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 Eu1 Eu 0.640097(15) 0.53903(5) 0.02542(3) 0.00506(12) Uani 1 1 d . . . Ge1 Ge 0.5000 0.07409(15) 0.2500 0.00462(16) Uani 1 2 d S . . B1 B 0.1999(4) 0.4683(10) 0.2038(6) 0.0052(9) Uani 1 1 d . . . O1 O 0.1924(2) 0.4629(6) 0.0495(4) 0.0052(6) Uani 1 1 d . . . O2 O 0.1061(2) 0.3441(7) 0.2662(3) 0.0068(6) Uani 1 1 d . . . O3 O 0.2163(2) 0.7810(6) 0.2595(3) 0.0054(6) Uani 1 1 d . . . O4 O 0.49596(19) 0.2950(7) 0.0986(3) 0.0074(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 Eu1 0.00500(15) 0.00470(16) 0.00548(18) 0.00053(7) 0.00075(8) 0.00033(7) Ge1 0.0047(3) 0.0049(3) 0.0043(3) 0.000 0.0001(2) 0.000 B1 0.008(2) 0.003(2) 0.004(2) -0.0023(17) 0.0010(19) -0.0008(16) O1 0.0073(15) 0.0053(15) 0.0030(16) 0.0011(11) 0.0000(13) -0.0011(11) O2 0.0055(14) 0.0069(15) 0.0079(17) 0.0024(12) 0.0014(12) 0.0003(11) O3 0.0060(13) 0.0039(14) 0.0062(15) -0.0022(11) 0.0005(12) -0.0011(11) O4 0.0057(13) 0.0081(15) 0.0083(16) 0.0037(11) 0.0008(12) -0.0004(11) _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 Eu1 O4 2.299(3) 5_665 ? Eu1 O4 2.337(3) . ? Eu1 O1 2.378(3) 5_665 ? Eu1 O2 2.414(3) 6_666 ? Eu1 O1 2.423(3) 4_565 ? Eu1 O1 2.439(3) 4 ? Eu1 O3 2.531(3) 6_656 ? Eu1 O3 2.963(3) 4_565 ? Eu1 O3 2.996(3) 3_655 ? Eu1 B1 3.048(5) 5_665 ? Eu1 B1 3.164(5) 4_565 ? Eu1 B1 3.209(5) 4 ? Ge1 O4 1.721(3) 3_655 ? Ge1 O4 1.721(3) . ? Ge1 O2 1.770(3) 6_656 ? Ge1 O2 1.770(3) 8_655 ? Ge1 Eu1 3.5011(11) 3_655 ? Ge1 Eu1 3.6283(12) 7_566 ? Ge1 Eu1 3.6283(12) 5_665 ? Ge1 Eu1 3.6928(12) 1_545 ? Ge1 Eu1 3.6928(12) 3_645 ? B1 O1 1.444(6) . ? B1 O3 1.498(5) . ? B1 O3 1.500(6) 8_655 ? B1 O2 1.504(6) . ? B1 Eu1 3.048(5) 5_665 ? B1 Eu1 3.164(5) 4_465 ? B1 Eu1 3.209(5) 4_455 ? B1 Eu1 3.267(5) 6_556 ? O1 Eu1 2.378(3) 5_665 ? O1 Eu1 2.423(3) 4_465 ? O1 Eu1 2.439(3) 4_455 ? O2 Ge1 1.770(3) 6_566 ? O2 Eu1 2.414(3) 6_556 ? O3 B1 1.500(6) 8_665 ? O3 Eu1 2.531(3) 6_566 ? O3 Eu1 2.963(3) 4_465 ? O3 Eu1 2.996(3) 3_655 ? O4 Eu1 2.299(3) 5_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 O4 Eu1 O4 67.90(13) 5_665 . ? O4 Eu1 O1 128.32(11) 5_665 5_665 ? O4 Eu1 O1 152.13(10) . 5_665 ? O4 Eu1 O2 94.18(11) 5_665 6_666 ? O4 Eu1 O2 82.20(11) . 6_666 ? O1 Eu1 O2 114.95(10) 5_665 6_666 ? O4 Eu1 O1 78.33(11) 5_665 4_565 ? O4 Eu1 O1 138.71(10) . 4_565 ? O1 Eu1 O1 68.82(9) 5_665 4_565 ? O2 Eu1 O1 77.16(11) 6_666 4_565 ? O4 Eu1 O1 112.40(11) 5_665 4 ? O4 Eu1 O1 84.51(11) . 4 ? O1 Eu1 O1 68.55(9) 5_665 4 ? O2 Eu1 O1 142.97(11) 6_666 4 ? O1 Eu1 O1 131.62(15) 4_565 4 ? O4 Eu1 O3 150.65(10) 5_665 6_656 ? O4 Eu1 O3 84.30(10) . 6_656 ? O1 Eu1 O3 80.87(11) 5_665 6_656 ? O2 Eu1 O3 72.08(10) 6_666 6_656 ? O1 Eu1 O3 121.44(10) 4_565 6_656 ? O1 Eu1 O3 72.31(11) 4 6_656 ? O4 Eu1 O3 75.05(10) 5_665 4_565 ? O4 Eu1 O3 132.77(9) . 4_565 ? O1 Eu1 O3 53.37(10) 5_665 4_565 ? O2 Eu1 O3 129.72(10) 6_666 4_565 ? O1 Eu1 O3 52.64(10) 4_565 4_565 ? O1 Eu1 O3 83.50(10) 4 4_565 ? O3 Eu1 O3 133.71(12) 6_656 4_565 ? O4 Eu1 O3 138.11(10) 5_665 3_655 ? O4 Eu1 O3 120.93(10) . 3_655 ? O1 Eu1 O3 64.99(10) 5_665 3_655 ? O2 Eu1 O3 51.93(9) 6_666 3_655 ? O1 Eu1 O3 71.14(10) 4_565 3_655 ? O1 Eu1 O3 109.29(10) 4 3_655 ? O3 Eu1 O3 50.58(6) 6_656 3_655 ? O3 Eu1 O3 106.15(4) 4_565 3_655 ? O4 Eu1 B1 102.79(13) 5_665 5_665 ? O4 Eu1 B1 142.75(12) . 5_665 ? O1 Eu1 B1 27.49(13) 5_665 5_665 ? O2 Eu1 B1 135.05(11) 6_666 5_665 ? O1 Eu1 B1 66.33(11) 4_565 5_665 ? O1 Eu1 B1 65.28(11) 4 5_665 ? O3 Eu1 B1 105.14(13) 6_656 5_665 ? O3 Eu1 B1 28.86(11) 4_565 5_665 ? O3 Eu1 B1 90.66(12) 3_655 5_665 ? O4 Eu1 B1 69.17(12) 5_665 4_565 ? O4 Eu1 B1 137.06(12) . 4_565 ? O1 Eu1 B1 63.79(12) 5_665 4_565 ? O2 Eu1 B1 101.94(12) 6_666 4_565 ? O1 Eu1 B1 25.86(12) 4_565 4_565 ? O1 Eu1 B1 111.21(12) 4 4_565 ? O3 Eu1 B1 138.05(12) 6_656 4_565 ? O3 Eu1 B1 28.05(10) 4_565 4_565 ? O3 Eu1 B1 92.23(11) 3_655 4_565 ? B1 Eu1 B1 49.45(12) 5_665 4_565 ? O4 Eu1 B1 95.26(13) 5_665 4 ? O4 Eu1 B1 94.69(12) . 4 ? O1 Eu1 B1 63.87(12) 5_665 4 ? O2 Eu1 B1 168.11(12) 6_666 4 ? O1 Eu1 B1 111.87(13) 4_565 4 ? O1 Eu1 B1 25.21(12) 4 4 ? O3 Eu1 B1 96.23(12) 6_656 4 ? O3 Eu1 B1 60.13(11) 4_565 4 ? O3 Eu1 B1 122.25(11) 3_655 4 ? B1 Eu1 B1 49.03(12) 5_665 4 ? B1 Eu1 B1 88.18(14) 4_565 4 ? O4 Ge1 O4 110.6(2) 3_655 . ? O4 Ge1 O2 111.86(13) 3_655 6_656 ? O4 Ge1 O2 106.49(14) . 6_656 ? O4 Ge1 O2 106.49(14) 3_655 8_655 ? O4 Ge1 O2 111.86(13) . 8_655 ? O2 Ge1 O2 109.6(2) 6_656 8_655 ? O4 Ge1 Eu1 98.00(11) 3_655 . ? O4 Ge1 Eu1 35.91(9) . . ? O2 Ge1 Eu1 81.20(10) 6_656 . ? O2 Ge1 Eu1 146.27(10) 8_655 . ? O4 Ge1 Eu1 35.91(9) 3_655 3_655 ? O4 Ge1 Eu1 98.00(11) . 3_655 ? O2 Ge1 Eu1 146.27(10) 6_656 3_655 ? O2 Ge1 Eu1 81.20(10) 8_655 3_655 ? Eu1 Ge1 Eu1 107.83(4) . 3_655 ? O4 Ge1 Eu1 29.77(9) 3_655 7_566 ? O4 Ge1 Eu1 109.23(11) . 7_566 ? O2 Ge1 Eu1 84.68(10) 6_656 7_566 ? O2 Ge1 Eu1 129.62(10) 8_655 7_566 ? Eu1 Ge1 Eu1 82.04(4) . 7_566 ? Eu1 Ge1 Eu1 65.26(3) 3_655 7_566 ? O4 Ge1 Eu1 109.23(11) 3_655 5_665 ? O4 Ge1 Eu1 29.77(9) . 5_665 ? O2 Ge1 Eu1 129.62(10) 6_656 5_665 ? O2 Ge1 Eu1 84.68(10) 8_655 5_665 ? Eu1 Ge1 Eu1 65.26(3) . 5_665 ? Eu1 Ge1 Eu1 82.04(4) 3_655 5_665 ? Eu1 Ge1 Eu1 123.55(4) 7_566 5_665 ? O4 Ge1 Eu1 144.67(9) 3_655 1_545 ? O4 Ge1 Eu1 85.18(11) . 1_545 ? O2 Ge1 Eu1 33.18(10) 6_656 1_545 ? O2 Ge1 Eu1 95.54(11) 8_655 1_545 ? Eu1 Ge1 Eu1 76.07(4) . 1_545 ? Eu1 Ge1 Eu1 176.097(17) 3_655 1_545 ? Eu1 Ge1 Eu1 115.89(3) 7_566 1_545 ? Eu1 Ge1 Eu1 99.85(4) 5_665 1_545 ? O4 Ge1 Eu1 85.18(11) 3_655 3_645 ? O4 Ge1 Eu1 144.67(9) . 3_645 ? O2 Ge1 Eu1 95.54(11) 6_656 3_645 ? O2 Ge1 Eu1 33.18(10) 8_655 3_645 ? Eu1 Ge1 Eu1 176.097(17) . 3_645 ? Eu1 Ge1 Eu1 76.07(4) 3_655 3_645 ? Eu1 Ge1 Eu1 99.85(4) 7_566 3_645 ? Eu1 Ge1 Eu1 115.89(3) 5_665 3_645 ? Eu1 Ge1 Eu1 100.03(4) 1_545 3_645 ? O1 B1 O3 111.8(4) . . ? O1 B1 O3 113.0(4) . 8_655 ? O3 B1 O3 106.3(3) . 8_655 ? O1 B1 O2 108.7(4) . . ? O3 B1 O2 109.3(4) . . ? O3 B1 O2 107.7(3) 8_655 . ? O1 B1 Eu1 49.5(2) . 5_665 ? O3 B1 Eu1 98.5(3) . 5_665 ? O3 B1 Eu1 72.4(2) 8_655 5_665 ? O2 B1 Eu1 150.5(3) . 5_665 ? O1 B1 Eu1 47.05(19) . 4_465 ? O3 B1 Eu1 68.5(2) . 4_465 ? O3 B1 Eu1 144.2(3) 8_655 4_465 ? O2 B1 Eu1 107.3(3) . 4_465 ? Eu1 B1 Eu1 73.45(12) 5_665 4_465 ? O1 B1 Eu1 46.01(18) . 4_455 ? O3 B1 Eu1 156.7(3) . 4_455 ? O3 B1 Eu1 92.0(2) 8_655 4_455 ? O2 B1 Eu1 77.7(2) . 4_455 ? Eu1 B1 Eu1 72.81(12) 5_665 4_455 ? Eu1 B1 Eu1 88.18(14) 4_465 4_455 ? O1 B1 Eu1 138.1(3) . 6_556 ? O3 B1 Eu1 107.9(3) . 6_556 ? O3 B1 Eu1 66.3(2) 8_655 6_556 ? O2 B1 Eu1 43.69(19) . 6_556 ? Eu1 B1 Eu1 135.56(16) 5_665 6_556 ? Eu1 B1 Eu1 149.54(18) 4_465 6_556 ? Eu1 B1 Eu1 92.55(12) 4_455 6_556 ? B1 O1 Eu1 103.0(3) . 5_665 ? B1 O1 Eu1 107.1(2) . 4_465 ? Eu1 O1 Eu1 101.42(11) 5_665 4_465 ? B1 O1 Eu1 108.8(2) . 4_455 ? Eu1 O1 Eu1 100.96(11) 5_665 4_455 ? Eu1 O1 Eu1 131.62(14) 4_465 4_455 ? B1 O2 Ge1 116.4(3) . 6_566 ? B1 O2 Eu1 110.8(3) . 6_556 ? Ge1 O2 Eu1 123.16(15) 6_566 6_556 ? B1 O3 B1 120.3(4) . 8_665 ? B1 O3 Eu1 129.3(3) . 6_566 ? B1 O3 Eu1 109.5(2) 8_665 6_566 ? B1 O3 Eu1 83.5(2) . 4_465 ? B1 O3 Eu1 78.7(2) 8_665 4_465 ? Eu1 O3 Eu1 116.59(11) 6_566 4_465 ? B1 O3 Eu1 89.8(2) . 3_655 ? B1 O3 Eu1 86.5(2) 8_665 3_655 ? Eu1 O3 Eu1 84.04(9) 6_566 3_655 ? Eu1 O3 Eu1 157.64(11) 4_465 3_655 ? Ge1 O4 Eu1 128.41(14) . 5_665 ? Ge1 O4 Eu1 118.50(14) . . ? Eu1 O4 Eu1 112.10(13) 5_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.715 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.272 #===end data_Gd2GeB2O8 _database_code_depnum_ccdc_archive 'CCDC 760686' #TrackingRef 'zjh-dalton-cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Gd2 Ge O8' _chemical_formula_weight 536.73 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' Ge Ge 0.1547 1.8001 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.506(15) _cell_length_b 4.417(5) _cell_length_c 9.302(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 555.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1413 _cell_measurement_theta_min 2.1893 _cell_measurement_theta_max 27.4487 _exptl_crystal_description brick _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 29.017 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5995 _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_type 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3310 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.53 _reflns_number_total 620 _reflns_number_gt 605 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1320P)^2^+15.8609P] 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 0.0031(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 620 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Gd1 Gd 0.64009(5) 0.54021(18) 0.02614(8) 0.0113(5) Uani 1 1 d . . . Ge1 Ge 0.5000 0.0740(5) 0.2500 0.0111(6) Uani 1 2 d S . . B1 B 0.1994(12) 0.474(3) 0.200(2) 0.009(3) Uiso 1 1 d . . . O1 O 0.1914(8) 0.464(2) 0.0490(13) 0.011(2) Uani 1 1 d . . . O2 O 0.1066(7) 0.345(2) 0.2668(11) 0.0125(19) Uani 1 1 d . . . O3 O 0.2162(8) 0.781(2) 0.2593(11) 0.015(2) Uani 1 1 d . . . O4 O 0.4946(7) 0.294(3) 0.0987(10) 0.0152(19) 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 Gd1 0.0129(7) 0.0060(7) 0.0151(8) 0.0009(2) 0.0011(2) 0.00015(18) Ge1 0.0146(12) 0.0049(10) 0.0139(10) 0.000 0.0006(8) 0.000 O1 0.010(5) 0.006(4) 0.018(5) 0.004(3) -0.005(4) -0.006(3) O2 0.010(5) 0.008(4) 0.019(5) -0.001(4) 0.000(4) -0.005(3) O3 0.015(5) 0.011(5) 0.017(5) 0.003(4) 0.002(3) 0.007(4) O4 0.018(5) 0.017(4) 0.011(4) -0.001(4) -0.006(3) -0.008(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 Gd1 O4 2.279(10) 5_665 ? Gd1 O4 2.346(10) . ? Gd1 O1 2.380(12) 5_665 ? Gd1 O2 2.392(10) 6_666 ? Gd1 O1 2.402(10) 4_565 ? Gd1 O1 2.435(9) 4 ? Gd1 O3 2.521(10) 6_656 ? Gd1 B1 3.021(18) 5_665 ? Gd1 B1 3.109(16) 4_565 ? Gd1 Ge1 3.487(3) . ? Gd1 Gd1 3.700(3) 8_765 ? Gd1 Gd1 3.700(3) 8_755 ? Ge1 O4 1.712(11) 3_655 ? Ge1 O4 1.712(11) . ? Ge1 O2 1.767(10) 8_655 ? Ge1 O2 1.767(10) 6_656 ? Ge1 Gd1 3.487(3) 3_655 ? B1 O1 1.41(2) . ? B1 O3 1.479(18) . ? B1 O2 1.512(18) . ? B1 O3 1.528(19) 8_655 ? B1 Gd1 3.021(18) 5_665 ? B1 Gd1 3.109(16) 4_465 ? O1 Gd1 2.380(12) 5_665 ? O1 Gd1 2.402(10) 4_465 ? O1 Gd1 2.435(9) 4_455 ? O2 Ge1 1.767(10) 6_566 ? O2 Gd1 2.392(10) 6_556 ? O3 B1 1.528(19) 8_665 ? O3 Gd1 2.521(10) 6_566 ? O4 Gd1 2.279(10) 5_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 O4 Gd1 O4 68.1(4) 5_665 . ? O4 Gd1 O1 128.0(4) 5_665 5_665 ? O4 Gd1 O1 151.9(3) . 5_665 ? O4 Gd1 O2 94.5(4) 5_665 6_666 ? O4 Gd1 O2 82.6(3) . 6_666 ? O1 Gd1 O2 114.9(3) 5_665 6_666 ? O4 Gd1 O1 77.8(4) 5_665 4_565 ? O4 Gd1 O1 138.5(4) . 4_565 ? O1 Gd1 O1 69.2(3) 5_665 4_565 ? O2 Gd1 O1 77.0(4) 6_666 4_565 ? O4 Gd1 O1 112.1(4) 5_665 4 ? O4 Gd1 O1 84.1(4) . 4 ? O1 Gd1 O1 68.7(3) 5_665 4 ? O2 Gd1 O1 143.1(4) 6_666 4 ? O1 Gd1 O1 131.9(5) 4_565 4 ? O4 Gd1 O3 151.1(4) 5_665 6_656 ? O4 Gd1 O3 84.4(4) . 6_656 ? O1 Gd1 O3 80.7(4) 5_665 6_656 ? O2 Gd1 O3 72.3(3) 6_666 6_656 ? O1 Gd1 O3 121.8(4) 4_565 6_656 ? O1 Gd1 O3 72.2(4) 4 6_656 ? O4 Gd1 B1 103.0(4) 5_665 5_665 ? O4 Gd1 B1 142.3(4) . 5_665 ? O1 Gd1 B1 27.1(4) 5_665 5_665 ? O2 Gd1 B1 135.1(4) 6_666 5_665 ? O1 Gd1 B1 67.0(4) 4_565 5_665 ? O1 Gd1 B1 64.9(4) 4 5_665 ? O3 Gd1 B1 104.4(4) 6_656 5_665 ? O4 Gd1 B1 68.9(4) 5_665 4_565 ? O4 Gd1 B1 136.9(4) . 4_565 ? O1 Gd1 B1 63.9(4) 5_665 4_565 ? O2 Gd1 B1 101.9(4) 6_666 4_565 ? O1 Gd1 B1 25.8(4) 4_565 4_565 ? O1 Gd1 B1 111.3(4) 4 4_565 ? O3 Gd1 B1 138.1(4) 6_656 4_565 ? B1 Gd1 B1 50.1(4) 5_665 4_565 ? O4 Gd1 Ge1 93.5(3) 5_665 . ? O4 Gd1 Ge1 25.8(2) . . ? O1 Gd1 Ge1 133.6(2) 5_665 . ? O2 Gd1 Ge1 75.5(2) 6_666 . ? O1 Gd1 Ge1 150.4(3) 4_565 . ? O1 Gd1 Ge1 77.6(3) 4 . ? O3 Gd1 Ge1 58.7(3) 6_656 . ? B1 Gd1 Ge1 142.4(3) 5_665 . ? B1 Gd1 Ge1 162.1(3) 4_565 . ? O4 Gd1 Gd1 116.6(3) 5_665 8_765 ? O4 Gd1 Gd1 161.7(2) . 8_765 ? O1 Gd1 Gd1 40.3(2) 5_665 8_765 ? O2 Gd1 Gd1 79.4(2) 6_666 8_765 ? O1 Gd1 Gd1 39.1(3) 4_565 8_765 ? O1 Gd1 Gd1 108.5(3) 4 8_765 ? O3 Gd1 Gd1 86.8(3) 6_656 8_765 ? B1 Gd1 Gd1 55.7(3) 5_665 8_765 ? B1 Gd1 Gd1 51.8(3) 4_565 8_765 ? Ge1 Gd1 Gd1 141.99(4) . 8_765 ? O4 Gd1 Gd1 146.3(3) 5_665 8_755 ? O4 Gd1 Gd1 113.3(3) . 8_755 ? O1 Gd1 Gd1 39.5(2) 5_665 8_755 ? O2 Gd1 Gd1 119.2(2) 6_666 8_755 ? O1 Gd1 Gd1 108.2(3) 4_565 8_755 ? O1 Gd1 Gd1 39.2(3) 4 8_755 ? O3 Gd1 Gd1 53.2(2) 6_656 8_755 ? B1 Gd1 Gd1 54.0(3) 5_665 8_755 ? B1 Gd1 Gd1 101.8(3) 4_565 8_755 ? Ge1 Gd1 Gd1 94.75(7) . 8_755 ? Gd1 Gd1 Gd1 73.29(9) 8_765 8_755 ? O4 Ge1 O4 110.9(7) 3_655 . ? O4 Ge1 O2 106.7(5) 3_655 8_655 ? O4 Ge1 O2 111.3(4) . 8_655 ? O4 Ge1 O2 111.3(4) 3_655 6_656 ? O4 Ge1 O2 106.7(5) . 6_656 ? O2 Ge1 O2 110.1(6) 8_655 6_656 ? O4 Ge1 Gd1 36.6(3) 3_655 3_655 ? O4 Ge1 Gd1 97.6(4) . 3_655 ? O2 Ge1 Gd1 81.0(3) 8_655 3_655 ? O2 Ge1 Gd1 146.5(3) 6_656 3_655 ? O4 Ge1 Gd1 97.6(4) 3_655 . ? O4 Ge1 Gd1 36.6(3) . . ? O2 Ge1 Gd1 146.5(3) 8_655 . ? O2 Ge1 Gd1 81.0(3) 6_656 . ? Gd1 Ge1 Gd1 107.59(10) 3_655 . ? O1 B1 O3 114.4(11) . . ? O1 B1 O2 109.5(12) . . ? O3 B1 O2 108.7(12) . . ? O1 B1 O3 113.5(13) . 8_655 ? O3 B1 O3 105.3(11) . 8_655 ? O2 B1 O3 105.0(11) . 8_655 ? O1 B1 Gd1 50.2(7) . 5_665 ? O3 B1 Gd1 99.8(8) . 5_665 ? O2 B1 Gd1 150.8(10) . 5_665 ? O3 B1 Gd1 72.8(7) 8_655 5_665 ? O1 B1 Gd1 47.8(6) . 4_465 ? O3 B1 Gd1 70.2(7) . 4_465 ? O2 B1 Gd1 109.0(8) . 4_465 ? O3 B1 Gd1 145.4(10) 8_655 4_465 ? Gd1 B1 Gd1 74.2(4) 5_665 4_465 ? B1 O1 Gd1 102.7(9) . 5_665 ? B1 O1 Gd1 106.4(8) . 4_465 ? Gd1 O1 Gd1 101.4(4) 5_665 4_465 ? B1 O1 Gd1 109.7(8) . 4_455 ? Gd1 O1 Gd1 100.4(4) 5_665 4_455 ? Gd1 O1 Gd1 131.9(5) 4_465 4_455 ? B1 O2 Ge1 115.0(8) . 6_566 ? B1 O2 Gd1 112.8(8) . 6_556 ? Ge1 O2 Gd1 123.2(5) 6_566 6_556 ? B1 O3 B1 119.5(12) . 8_665 ? B1 O3 Gd1 130.5(9) . 6_566 ? B1 O3 Gd1 109.6(8) 8_665 6_566 ? Ge1 O4 Gd1 129.5(5) . 5_665 ? Ge1 O4 Gd1 117.6(5) . . ? Gd1 O4 Gd1 111.9(4) 5_665 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.500 _refine_diff_density_min -2.765 _refine_diff_density_rms 1.032 #===end data_Tb2GeB2O8 _database_code_depnum_ccdc_archive 'CCDC 760687' #TrackingRef 'zjh-dalton-cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Ge O8 Tb2' _chemical_formula_weight 540.09 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.484(6) _cell_length_b 4.4107(19) _cell_length_c 9.264(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 550.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1343 _cell_measurement_theta_min 2.1984 _cell_measurement_theta_max 27.4565 _exptl_crystal_description brick _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 30.819 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5436 _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 'Mercury2 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3672 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.40 _diffrn_reflns_theta_max 27.49 _reflns_number_total 624 _reflns_number_gt 541 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0217P)^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 0.0082(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 624 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.002 _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 Tb1 Tb 0.64002(3) 0.53848(8) 0.02535(4) 0.00528(17) Uani 1 1 d . . . Ge1 Ge 0.5000 0.0738(3) 0.2500 0.0050(3) Uani 1 2 d S . . B1 B 0.2003(6) 0.4688(17) 0.2032(8) 0.0037(15) Uiso 1 1 d . . . O1 O 0.1925(4) 0.4622(11) 0.0485(5) 0.0058(11) Uani 1 1 d . . . O2 O 0.1063(4) 0.3419(12) 0.2671(5) 0.0068(11) Uiso 1 1 d . . . O3 O 0.2146(4) 0.7845(11) 0.2586(5) 0.0061(11) Uani 1 1 d . . . O4 O 0.4952(4) 0.2957(12) 0.0977(5) 0.0080(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 Tb1 0.0049(2) 0.0036(2) 0.0073(2) 0.00051(13) 0.00067(14) 0.00034(13) Ge1 0.0053(6) 0.0029(5) 0.0068(5) 0.000 0.0000(4) 0.000 O1 0.007(3) 0.004(2) 0.007(3) 0.0006(18) -0.001(2) -0.001(2) O3 0.008(3) 0.002(2) 0.009(2) 0.0016(18) 0.002(2) 0.002(2) O4 0.008(3) 0.006(3) 0.010(2) 0.005(2) 0.002(2) 0.002(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 Tb1 O4 2.271(5) 5_665 ? Tb1 O4 2.326(5) . ? Tb1 O1 2.360(6) 5_665 ? Tb1 O2 2.386(5) 6_666 ? Tb1 O1 2.412(5) 4_565 ? Tb1 O1 2.418(5) 4 ? Tb1 O3 2.505(5) 6_656 ? Tb1 B1 3.020(8) 5_665 ? Tb1 Ge1 3.4779(11) . ? Tb1 Tb1 3.6959(13) 8_765 ? Tb1 Tb1 3.6959(13) 8_755 ? Tb1 Tb1 3.8203(18) 5_665 ? Ge1 O4 1.718(5) 3_655 ? Ge1 O4 1.718(5) . ? Ge1 O2 1.768(6) 8_655 ? Ge1 O2 1.768(6) 6_656 ? Ge1 Tb1 3.4779(12) 3_655 ? B1 O1 1.437(9) . ? B1 O3 1.497(10) 8_655 ? B1 O3 1.497(9) . ? B1 O2 1.506(10) . ? B1 Tb1 3.020(8) 5_665 ? O1 Tb1 2.360(6) 5_665 ? O1 Tb1 2.412(5) 4_465 ? O1 Tb1 2.418(5) 4_455 ? O2 Ge1 1.768(6) 6_566 ? O2 Tb1 2.386(5) 6_556 ? O3 B1 1.497(10) 8_665 ? O3 Tb1 2.505(5) 6_566 ? O4 Tb1 2.271(5) 5_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 O4 Tb1 O4 67.6(2) 5_665 . ? O4 Tb1 O1 128.55(18) 5_665 5_665 ? O4 Tb1 O1 152.44(18) . 5_665 ? O4 Tb1 O2 94.05(18) 5_665 6_666 ? O4 Tb1 O2 82.30(19) . 6_666 ? O1 Tb1 O2 114.63(18) 5_665 6_666 ? O4 Tb1 O1 78.40(19) 5_665 4_565 ? O4 Tb1 O1 138.44(18) . 4_565 ? O1 Tb1 O1 68.80(16) 5_665 4_565 ? O2 Tb1 O1 76.84(17) 6_666 4_565 ? O4 Tb1 O1 112.76(19) 5_665 4 ? O4 Tb1 O1 84.63(19) . 4 ? O1 Tb1 O1 68.71(16) 5_665 4 ? O2 Tb1 O1 142.76(17) 6_666 4 ? O1 Tb1 O1 131.9(2) 4_565 4 ? O4 Tb1 O3 150.17(18) 5_665 6_656 ? O4 Tb1 O3 84.32(18) . 6_656 ? O1 Tb1 O3 81.19(18) 5_665 6_656 ? O2 Tb1 O3 71.56(18) 6_666 6_656 ? O1 Tb1 O3 121.16(17) 4_565 6_656 ? O1 Tb1 O3 72.55(17) 4 6_656 ? O4 Tb1 B1 102.9(2) 5_665 5_665 ? O4 Tb1 B1 142.7(2) . 5_665 ? O1 Tb1 B1 27.7(2) 5_665 5_665 ? O2 Tb1 B1 135.0(2) 6_666 5_665 ? O1 Tb1 B1 66.53(19) 4_565 5_665 ? O1 Tb1 B1 65.38(19) 4 5_665 ? O3 Tb1 B1 105.6(2) 6_656 5_665 ? O4 Tb1 Ge1 93.11(13) 5_665 . ? O4 Tb1 Ge1 25.90(12) . . ? O1 Tb1 Ge1 133.82(12) 5_665 . ? O2 Tb1 Ge1 75.22(13) 6_666 . ? O1 Tb1 Ge1 150.10(12) 4_565 . ? O1 Tb1 Ge1 77.87(13) 4 . ? O3 Tb1 Ge1 58.42(13) 6_656 . ? B1 Tb1 Ge1 143.16(15) 5_665 . ? O4 Tb1 Tb1 116.88(13) 5_665 8_765 ? O4 Tb1 Tb1 161.54(13) . 8_765 ? O1 Tb1 Tb1 39.89(12) 5_665 8_765 ? O2 Tb1 Tb1 79.53(13) 6_666 8_765 ? O1 Tb1 Tb1 38.74(13) 4_565 8_765 ? O1 Tb1 Tb1 108.08(14) 4 8_765 ? O3 Tb1 Tb1 86.82(13) 6_656 8_765 ? B1 Tb1 Tb1 55.54(15) 5_665 8_765 ? Ge1 Tb1 Tb1 141.930(16) . 8_765 ? O4 Tb1 Tb1 146.76(13) 5_665 8_755 ? O4 Tb1 Tb1 113.52(13) . 8_755 ? O1 Tb1 Tb1 39.76(12) 5_665 8_755 ? O2 Tb1 Tb1 119.19(13) 6_666 8_755 ? O1 Tb1 Tb1 108.04(14) 4_565 8_755 ? O1 Tb1 Tb1 38.77(13) 4 8_755 ? O3 Tb1 Tb1 53.90(12) 6_656 8_755 ? B1 Tb1 Tb1 54.66(15) 5_665 8_755 ? Ge1 Tb1 Tb1 94.82(3) . 8_755 ? Tb1 Tb1 Tb1 73.27(4) 8_765 8_755 ? O4 Tb1 Tb1 34.25(13) 5_665 5_665 ? O4 Tb1 Tb1 33.34(13) . 5_665 ? O1 Tb1 Tb1 155.53(12) 5_665 5_665 ? O2 Tb1 Tb1 87.73(13) 6_666 5_665 ? O1 Tb1 Tb1 109.63(14) 4_565 5_665 ? O1 Tb1 Tb1 99.97(14) 4 5_665 ? O3 Tb1 Tb1 117.10(13) 6_656 5_665 ? B1 Tb1 Tb1 128.14(16) 5_665 5_665 ? Ge1 Tb1 Tb1 58.977(19) . 5_665 ? Tb1 Tb1 Tb1 147.801(19) 8_765 5_665 ? Tb1 Tb1 Tb1 137.74(2) 8_755 5_665 ? O4 Ge1 O4 110.6(4) 3_655 . ? O4 Ge1 O2 106.6(2) 3_655 8_655 ? O4 Ge1 O2 111.9(2) . 8_655 ? O4 Ge1 O2 111.9(2) 3_655 6_656 ? O4 Ge1 O2 106.6(2) . 6_656 ? O2 Ge1 O2 109.3(4) 8_655 6_656 ? O4 Ge1 Tb1 36.25(17) 3_655 3_655 ? O4 Ge1 Tb1 97.78(18) . 3_655 ? O2 Ge1 Tb1 81.21(17) 8_655 3_655 ? O2 Ge1 Tb1 146.59(16) 6_656 3_655 ? O4 Ge1 Tb1 97.78(18) 3_655 . ? O4 Ge1 Tb1 36.25(17) . . ? O2 Ge1 Tb1 146.59(16) 8_655 . ? O2 Ge1 Tb1 81.21(17) 6_656 . ? Tb1 Ge1 Tb1 107.79(4) 3_655 . ? O1 B1 O3 112.8(6) . 8_655 ? O1 B1 O3 111.7(6) . . ? O3 B1 O3 106.8(5) 8_655 . ? O1 B1 O2 108.8(6) . . ? O3 B1 O2 108.0(6) 8_655 . ? O3 B1 O2 108.7(6) . . ? O1 B1 Tb1 49.7(4) . 5_665 ? O3 B1 Tb1 71.8(4) 8_655 5_665 ? O3 B1 Tb1 99.1(4) . 5_665 ? O2 B1 Tb1 150.6(5) . 5_665 ? B1 O1 Tb1 102.7(5) . 5_665 ? B1 O1 Tb1 106.6(4) . 4_465 ? Tb1 O1 Tb1 101.50(19) 5_665 4_465 ? B1 O1 Tb1 108.8(4) . 4_455 ? Tb1 O1 Tb1 101.34(19) 5_665 4_455 ? Tb1 O1 Tb1 131.9(2) 4_465 4_455 ? B1 O2 Ge1 115.6(4) . 6_566 ? B1 O2 Tb1 111.4(4) . 6_556 ? Ge1 O2 Tb1 123.5(3) 6_566 6_556 ? B1 O3 B1 119.1(5) 8_665 . ? B1 O3 Tb1 109.8(4) 8_665 6_566 ? B1 O3 Tb1 129.7(4) . 6_566 ? Ge1 O4 Tb1 128.7(3) . 5_665 ? Ge1 O4 Tb1 117.9(3) . . ? Tb1 O4 Tb1 112.4(2) 5_665 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.248 _refine_diff_density_min -1.518 _refine_diff_density_rms 0.385 #===end