# 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 'Yan Xu' _publ_contact_author_email YANXU@NJUT.EDU.CN _publ_section_title ; Solvothermal Syntheses, Crystal Structures and Luminescence Properties of Three New Lanthanide Sulfate Fluorides ; loop_ _publ_author_name 'Yan Xu' 'Lijie Han' 'Wanli Zhou' 'Dun-Ru Zhu' # Attachment 'compound_1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 758052' #TrackingRef 'compound_1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H96 F2 N18 O56 S14 Sm4' _chemical_formula_weight 2621.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1988(9) _cell_length_b 11.4073(9) _cell_length_c 16.2666(13) _cell_angle_alpha 89.9010(10) _cell_angle_beta 82.4060(10) _cell_angle_gamma 67.7570(10) _cell_volume 1903.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5727 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.88 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 3.554 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.6360 _exptl_absorpt_correction_T_max 0.6751 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _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 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9856 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7184 _reflns_number_gt 6130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7184 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.19650(3) 0.78146(3) 0.241124(19) 0.01330(12) Uani 1 1 d . . . Sm2 Sm 0.42036(3) 0.47303(3) 0.353013(18) 0.01317(12) Uani 1 1 d . . . S1 S 0.33603(14) 0.46482(14) 0.54395(9) 0.0135(3) Uani 1 1 d . . . S2 S 0.13252(15) 0.54233(14) 0.30059(10) 0.0151(3) Uani 1 1 d . . . S3 S -0.01890(15) 0.98214(14) 0.37107(10) 0.0162(3) Uani 1 1 d . . . S4 S 0.30446(18) 0.99094(16) 0.18804(10) 0.0244(4) Uani 1 1 d . . . S5 S -0.01050(16) 0.77704(15) 0.06840(10) 0.0184(3) Uani 1 1 d . . . S6 S 0.59241(16) 0.19377(15) 0.30326(10) 0.0197(3) Uani 1 1 d . . . S7 S 0.50426(14) 0.54633(15) 0.14129(9) 0.0154(3) Uani 1 1 d . . . F1 F 0.3195(3) 0.6836(3) 0.3396(2) 0.0182(8) Uani 1 1 d . . . O1 O 0.0235(5) 0.8276(5) -0.0113(3) 0.0315(12) Uani 1 1 d . . . O2 O 0.1130(5) 0.8973(5) 0.3858(3) 0.0270(11) Uani 1 1 d . . . O3 O 0.4191(5) 0.4460(5) 0.6090(3) 0.0224(10) Uani 1 1 d . . . O4 O 0.0866(5) 0.7701(5) 0.1242(3) 0.0312(12) Uani 1 1 d . . . O5 O 0.3845(4) 0.6641(4) 0.1464(3) 0.0213(10) Uani 1 1 d . . . O6 O 0.2464(4) 0.5354(4) 0.2391(3) 0.0219(10) Uani 1 1 d . . . O7 O 0.4811(5) 0.4438(5) 0.1011(3) 0.0299(12) Uani 1 1 d . . . O8 O 0.3884(5) 0.3547(4) 0.4834(3) 0.0225(10) Uani 1 1 d . . . O9 O 0.5333(5) 0.5111(5) 0.2272(3) 0.0249(11) Uani 1 1 d . . . O10 O -0.0224(5) 0.9535(4) 0.2826(3) 0.0262(11) Uani 1 1 d . . . O11 O 0.3363(6) 0.9074(6) 0.2577(3) 0.0397(14) Uani 1 1 d . . . O12 O -0.0361(5) 1.1148(5) 0.3838(3) 0.0323(12) Uani 1 1 d . . . O13 O 0.6144(5) 0.5690(5) 0.0971(3) 0.0297(12) Uani 1 1 d . . . O14 O 0.6834(5) 0.1483(5) 0.2265(3) 0.0324(12) Uani 1 1 d . . . O15 O -0.0072(5) 0.6500(5) 0.0544(4) 0.0324(12) Uani 1 1 d . . . O16 O 0.2042(4) 0.4855(5) 0.5839(3) 0.0240(10) Uani 1 1 d . . . O17 O 0.4558(4) 0.2664(5) 0.2857(3) 0.0250(11) Uani 1 1 d . . . O18 O 0.3324(5) 0.5753(4) 0.4954(3) 0.0231(10) Uani 1 1 d . . . O19 O 0.1856(4) 0.4978(4) 0.3787(3) 0.0204(10) Uani 1 1 d . . . O20 O 0.0650(5) 0.4684(5) 0.2734(3) 0.0290(11) Uani 1 1 d . . . O21 O 0.0494(5) 0.6803(4) 0.3116(3) 0.0222(10) Uani 1 1 d . . . O22 O 0.5973(5) 0.0857(4) 0.3537(3) 0.0302(12) Uani 1 1 d . . . O23 O 0.6247(5) 0.2867(4) 0.3512(3) 0.0219(10) Uani 1 1 d . . . O24 O -0.1164(5) 0.9513(5) 0.4256(3) 0.0294(11) Uani 1 1 d . . . O25 O -0.1414(5) 0.8634(5) 0.1060(3) 0.0322(12) Uani 1 1 d . . . O26 O 0.1970(5) 0.9636(5) 0.1586(3) 0.0298(12) Uani 1 1 d . . . O27 O 0.4143(6) 0.9623(6) 0.1221(4) 0.0421(14) Uani 1 1 d . . . O28 O 0.2568(8) 1.1237(5) 0.2176(4) 0.057(2) Uani 1 1 d . . . N2 N 0.2384(5) 1.0864(5) 0.4055(4) 0.0216(12) Uani 1 1 d . . . H2C H 0.1739 1.0629 0.4288 0.026 Uiso 1 1 calc R . . H2D H 0.2607 1.0555 0.3524 0.026 Uiso 1 1 calc R . . N9 N 0.5636(5) 0.7846(5) -0.1077(3) 0.0212(12) Uani 1 1 d . . . H9C H 0.5993 0.8114 -0.1529 0.025 Uiso 1 1 calc R . . H9D H 0.5539 0.7132 -0.1228 0.025 Uiso 1 1 calc R . . N8 N 0.7620(6) 0.5213(6) -0.0598(4) 0.0284(14) Uani 1 1 d . . . H8C H 0.8378 0.4579 -0.0763 0.043 Uiso 1 1 calc R . . H8D H 0.7030 0.5182 -0.0905 0.043 Uiso 1 1 calc R . . H8E H 0.7355 0.5144 -0.0067 0.043 Uiso 1 1 calc R . . N3 N 0.3215(6) 0.8277(5) 0.4896(4) 0.0239(13) Uani 1 1 d . . . H3C H 0.3576 0.7436 0.4825 0.036 Uiso 1 1 calc R . . H3D H 0.2447 0.8560 0.4711 0.036 Uiso 1 1 calc R . . H3E H 0.3101 0.8501 0.5433 0.036 Uiso 1 1 calc R . . N5 N 0.2191(6) 0.4692(5) 0.7564(4) 0.0249(13) Uani 1 1 d . . . H5C H 0.1912 0.4815 0.7065 0.030 Uiso 1 1 calc R . . H5D H 0.3031 0.4607 0.7490 0.030 Uiso 1 1 calc R . . N6 N 0.2257(6) 0.1474(6) 0.7279(4) 0.0270(13) Uani 1 1 d . . . H6C H 0.2719 0.0823 0.6920 0.041 Uiso 1 1 calc R . . H6D H 0.1458 0.1849 0.7145 0.041 Uiso 1 1 calc R . . H6E H 0.2206 0.1195 0.7789 0.041 Uiso 1 1 calc R . . N1 N -0.0311(6) 1.2947(6) 0.4967(4) 0.0303(14) Uani 1 1 d . . . H1C H -0.0747 1.3348 0.5448 0.045 Uiso 1 1 calc R . . H1D H -0.0264 1.2150 0.4963 0.045 Uiso 1 1 calc R . . H1E H -0.0723 1.3341 0.4553 0.045 Uiso 1 1 calc R . . N7 N 0.2130(6) 0.9230(5) -0.0097(4) 0.0256(13) Uani 1 1 d . . . H7C H 0.1577 0.8886 0.0124 0.038 Uiso 1 1 calc R . . H7D H 0.1816 0.9687 -0.0520 0.038 Uiso 1 1 calc R . . H7E H 0.2229 0.9729 0.0286 0.038 Uiso 1 1 calc R . . N4 N 0.0673(8) 0.8176(6) 0.8096(4) 0.0409(17) Uani 1 1 d . . . H4C H 0.0495 0.8808 0.7751 0.061 Uiso 1 1 calc R . . H4D H 0.1313 0.8171 0.8369 0.061 Uiso 1 1 calc R . . H4E H -0.0035 0.8283 0.8457 0.061 Uiso 1 1 calc R . . C2 C 0.1050(7) 1.2951(6) 0.4858(5) 0.0279(16) Uani 1 1 d . . . H2A H 0.0987 1.3822 0.4873 0.033 Uiso 1 1 calc R . . H2B H 0.1479 1.2546 0.5322 0.033 Uiso 1 1 calc R . . C6 C 0.1421(7) 0.5840(6) 0.8116(4) 0.0254(15) Uani 1 1 d . . . H6A H 0.0633 0.5762 0.8390 0.031 Uiso 1 1 calc R . . H6B H 0.1926 0.5911 0.8540 0.031 Uiso 1 1 calc R . . C12 C 0.6534(7) 0.7555(7) -0.0435(4) 0.0258(15) Uani 1 1 d . . . H12A H 0.6095 0.7389 0.0080 0.031 Uiso 1 1 calc R . . H12B H 0.6742 0.8288 -0.0333 0.031 Uiso 1 1 calc R . . C11 C 0.7781(7) 0.6425(7) -0.0698(5) 0.0275(16) Uani 1 1 d . . . H11A H 0.8093 0.6483 -0.1276 0.033 Uiso 1 1 calc R . . H11B H 0.8436 0.6446 -0.0370 0.033 Uiso 1 1 calc R . . C10 C 0.3402(7) 0.8217(6) -0.0398(5) 0.0258(15) Uani 1 1 d . . . H10A H 0.3301 0.7669 -0.0816 0.031 Uiso 1 1 calc R . . H10B H 0.3745 0.7707 0.0058 0.031 Uiso 1 1 calc R . . C3 C 0.3532(6) 1.0286(6) 0.4503(4) 0.0220(14) Uani 1 1 d . . . H3A H 0.3273 1.0553 0.5087 0.026 Uiso 1 1 calc R . . H3B H 0.4202 1.0594 0.4287 0.026 Uiso 1 1 calc R . . C4 C 0.4095(7) 0.8844(7) 0.4418(4) 0.0250(15) Uani 1 1 d . . . H4A H 0.4236 0.8577 0.3836 0.030 Uiso 1 1 calc R . . H4B H 0.4933 0.8525 0.4617 0.030 Uiso 1 1 calc R . . C9 C 0.4341(6) 0.8827(6) -0.0770(4) 0.0223(14) Uani 1 1 d . . . H9A H 0.3991 0.9336 -0.1224 0.027 Uiso 1 1 calc R . . H9B H 0.4428 0.9382 -0.0350 0.027 Uiso 1 1 calc R . . C7 C 0.2125(8) 0.3527(7) 0.7859(5) 0.0298(16) Uani 1 1 d . . . H7A H 0.1220 0.3617 0.7954 0.036 Uiso 1 1 calc R . . H7B H 0.2459 0.3368 0.8386 0.036 Uiso 1 1 calc R . . C1 C 0.1879(7) 1.2286(7) 0.4064(5) 0.0268(15) Uani 1 1 d . . . H1A H 0.1372 1.2566 0.3611 0.032 Uiso 1 1 calc R . . H1B H 0.2616 1.2543 0.3962 0.032 Uiso 1 1 calc R . . C8 C 0.2896(7) 0.2390(7) 0.7254(5) 0.0315(17) Uani 1 1 d . . . H8A H 0.2969 0.2679 0.6695 0.038 Uiso 1 1 calc R . . H8B H 0.3769 0.1979 0.7396 0.038 Uiso 1 1 calc R . . C5 C 0.1068(12) 0.7001(8) 0.7632(6) 0.056(3) Uani 1 1 d . . . H5A H 0.1813 0.6921 0.7225 0.068 Uiso 1 1 calc R . . H5B H 0.0366 0.7031 0.7330 0.068 Uiso 1 1 calc R . . 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 0.01601(19) 0.01240(19) 0.00997(19) 0.00245(13) -0.00286(13) -0.00341(14) Sm2 0.01515(19) 0.01287(19) 0.00959(19) 0.00216(13) -0.00195(13) -0.00316(14) S1 0.0148(7) 0.0169(7) 0.0095(7) 0.0019(6) -0.0026(6) -0.0065(6) S2 0.0162(7) 0.0154(7) 0.0143(8) 0.0028(6) -0.0038(6) -0.0061(6) S3 0.0165(7) 0.0151(7) 0.0147(8) -0.0006(6) -0.0009(6) -0.0040(6) S4 0.0391(10) 0.0240(9) 0.0148(8) 0.0011(7) 0.0000(7) -0.0186(8) S5 0.0184(8) 0.0201(8) 0.0140(8) 0.0020(6) -0.0034(6) -0.0039(6) S6 0.0224(8) 0.0171(8) 0.0149(8) -0.0015(6) -0.0028(6) -0.0023(6) S7 0.0128(7) 0.0185(7) 0.0124(7) 0.0027(6) -0.0005(6) -0.0037(6) F1 0.0205(19) 0.0146(17) 0.0180(19) 0.0057(15) -0.0110(15) -0.0025(15) O1 0.034(3) 0.044(3) 0.014(3) 0.005(2) 0.002(2) -0.013(2) O2 0.028(3) 0.024(3) 0.019(3) -0.004(2) -0.004(2) 0.002(2) O3 0.026(3) 0.030(3) 0.014(2) 0.004(2) -0.0111(19) -0.012(2) O4 0.045(3) 0.032(3) 0.020(3) 0.002(2) -0.016(2) -0.015(3) O5 0.011(2) 0.023(2) 0.020(2) 0.0066(19) 0.0037(18) 0.0023(18) O6 0.020(2) 0.032(3) 0.014(2) -0.002(2) 0.0059(19) -0.013(2) O7 0.035(3) 0.026(3) 0.028(3) -0.003(2) -0.008(2) -0.010(2) O8 0.032(3) 0.015(2) 0.016(2) -0.0018(19) -0.003(2) -0.005(2) O9 0.030(3) 0.030(3) 0.010(2) 0.010(2) -0.0027(19) -0.007(2) O10 0.039(3) 0.020(2) 0.014(2) 0.0006(19) -0.008(2) -0.004(2) O11 0.061(4) 0.052(4) 0.025(3) 0.020(3) -0.019(3) -0.038(3) O12 0.042(3) 0.018(2) 0.033(3) -0.002(2) -0.004(2) -0.009(2) O13 0.020(3) 0.046(3) 0.023(3) 0.015(2) -0.006(2) -0.012(2) O14 0.032(3) 0.037(3) 0.020(3) -0.008(2) 0.004(2) -0.007(2) O15 0.020(3) 0.029(3) 0.052(4) 0.001(2) -0.011(2) -0.012(2) O16 0.019(2) 0.031(3) 0.017(2) 0.004(2) 0.0019(19) -0.005(2) O17 0.016(2) 0.029(3) 0.029(3) -0.003(2) -0.009(2) -0.006(2) O18 0.035(3) 0.017(2) 0.014(2) 0.0012(19) -0.001(2) -0.007(2) O19 0.018(2) 0.024(2) 0.020(2) 0.0070(19) -0.0079(19) -0.0083(19) O20 0.031(3) 0.031(3) 0.032(3) 0.001(2) -0.012(2) -0.018(2) O21 0.024(2) 0.015(2) 0.025(3) 0.0053(19) -0.005(2) -0.0038(19) O22 0.039(3) 0.016(2) 0.027(3) 0.004(2) 0.003(2) -0.003(2) O23 0.024(2) 0.019(2) 0.020(2) -0.0017(19) -0.006(2) -0.0038(19) O24 0.023(3) 0.036(3) 0.029(3) 0.003(2) 0.004(2) -0.012(2) O25 0.024(3) 0.030(3) 0.027(3) 0.008(2) 0.007(2) 0.002(2) O26 0.033(3) 0.027(3) 0.035(3) 0.014(2) -0.011(2) -0.016(2) O27 0.049(4) 0.043(3) 0.034(3) 0.001(3) 0.017(3) -0.026(3) O28 0.107(6) 0.025(3) 0.040(4) -0.009(3) 0.015(4) -0.033(4) N2 0.022(3) 0.018(3) 0.024(3) 0.001(2) -0.005(2) -0.005(2) N9 0.020(3) 0.028(3) 0.017(3) 0.002(2) -0.001(2) -0.012(2) N8 0.017(3) 0.034(3) 0.027(3) -0.001(3) -0.005(2) -0.001(3) N3 0.032(3) 0.017(3) 0.022(3) 0.007(2) -0.010(3) -0.008(2) N5 0.033(3) 0.022(3) 0.016(3) 0.002(2) 0.002(2) -0.008(3) N6 0.032(3) 0.026(3) 0.025(3) -0.002(3) 0.004(3) -0.016(3) N1 0.033(3) 0.023(3) 0.025(3) -0.005(3) -0.006(3) 0.001(3) N7 0.027(3) 0.023(3) 0.023(3) 0.007(2) -0.004(3) -0.004(3) N4 0.054(5) 0.030(4) 0.029(4) 0.002(3) -0.004(3) -0.006(3) C2 0.034(4) 0.018(3) 0.033(4) 0.000(3) -0.013(3) -0.008(3) C6 0.032(4) 0.025(4) 0.018(4) 0.006(3) -0.006(3) -0.009(3) C12 0.030(4) 0.026(4) 0.023(4) 0.006(3) -0.011(3) -0.010(3) C11 0.021(3) 0.034(4) 0.027(4) 0.003(3) -0.007(3) -0.009(3) C10 0.029(4) 0.019(3) 0.025(4) 0.003(3) -0.003(3) -0.005(3) C3 0.022(3) 0.027(4) 0.022(4) 0.005(3) -0.004(3) -0.013(3) C4 0.023(4) 0.028(4) 0.018(4) 0.001(3) -0.001(3) -0.004(3) C9 0.023(3) 0.023(3) 0.019(3) 0.002(3) -0.002(3) -0.007(3) C7 0.044(4) 0.027(4) 0.021(4) 0.002(3) 0.001(3) -0.018(3) C1 0.033(4) 0.026(4) 0.025(4) 0.008(3) -0.005(3) -0.014(3) C8 0.030(4) 0.028(4) 0.038(5) -0.003(3) 0.010(3) -0.016(3) C5 0.097(8) 0.022(4) 0.037(5) 0.006(4) -0.004(5) -0.010(5) _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 F1 2.263(3) . ? Sm1 O5 2.370(4) . ? Sm1 O4 2.427(5) . ? Sm1 O26 2.474(5) . ? Sm1 O10 2.498(5) . ? Sm1 O21 2.509(5) . ? Sm1 O11 2.530(5) . ? Sm1 O2 2.579(5) . ? Sm1 O6 2.646(5) . ? Sm1 S4 3.1341(17) . ? Sm1 S3 3.1648(15) . ? Sm1 S2 3.1901(15) . ? Sm2 F1 2.259(3) . ? Sm2 O9 2.388(5) . ? Sm2 O3 2.454(4) 2_666 ? Sm2 O23 2.461(4) . ? Sm2 O17 2.470(5) . ? Sm2 O18 2.496(5) . ? Sm2 O19 2.513(4) . ? Sm2 O8 2.570(5) . ? Sm2 O6 2.763(5) . ? Sm2 S6 3.0766(16) . ? Sm2 S1 3.1366(15) . ? Sm2 S2 3.2462(15) . ? S1 O3 1.462(4) . ? S1 O16 1.464(5) . ? S1 O18 1.477(5) . ? S1 O8 1.479(5) . ? S2 O20 1.432(5) . ? S2 O19 1.481(5) . ? S2 O6 1.490(5) . ? S2 O21 1.491(5) . ? S3 O24 1.462(5) . ? S3 O12 1.463(5) . ? S3 O2 1.479(5) . ? S3 O10 1.485(5) . ? S4 O27 1.456(6) . ? S4 O28 1.460(6) . ? S4 O11 1.471(6) . ? S4 O26 1.487(5) . ? S5 O15 1.453(5) . ? S5 O25 1.472(5) . ? S5 O1 1.480(5) . ? S5 O4 1.486(5) . ? S6 O14 1.461(5) . ? S6 O22 1.467(5) . ? S6 O23 1.494(5) . ? S6 O17 1.505(5) . ? S7 O13 1.453(5) . ? S7 O7 1.462(5) . ? S7 O5 1.489(4) . ? S7 O9 1.497(5) . ? O3 Sm2 2.454(4) 2_666 ? N2 C3 1.491(8) . ? N2 C1 1.501(9) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N9 C9 1.479(8) . ? N9 C12 1.494(8) . ? N9 H9C 0.9000 . ? N9 H9D 0.9000 . ? N8 C11 1.465(9) . ? N8 H8C 0.8900 . ? N8 H8D 0.8900 . ? N8 H8E 0.8900 . ? N3 C4 1.507(9) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N5 C7 1.437(9) . ? N5 C6 1.487(9) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 C8 1.472(9) . ? N6 H6C 0.8900 . ? N6 H6D 0.8900 . ? N6 H6E 0.8900 . ? N1 C2 1.513(10) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N7 C10 1.475(9) . ? N7 H7C 0.8900 . ? N7 H7D 0.8900 . ? N7 H7E 0.8900 . ? N4 C5 1.424(10) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.502(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C6 C5 1.486(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C12 C11 1.508(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C10 C9 1.529(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C3 C4 1.520(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C7 C8 1.525(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 F1 Sm1 O5 84.60(14) . . ? F1 Sm1 O4 149.81(15) . . ? O5 Sm1 O4 82.42(17) . . ? F1 Sm1 O26 130.23(15) . . ? O5 Sm1 O26 84.37(17) . . ? O4 Sm1 O26 75.35(17) . . ? F1 Sm1 O10 119.93(14) . . ? O5 Sm1 O10 154.46(16) . . ? O4 Sm1 O10 78.72(17) . . ? O26 Sm1 O10 74.34(17) . . ? F1 Sm1 O21 81.85(14) . . ? O5 Sm1 O21 121.66(15) . . ? O4 Sm1 O21 82.01(17) . . ? O26 Sm1 O21 142.83(16) . . ? O10 Sm1 O21 72.57(15) . . ? F1 Sm1 O11 75.28(15) . . ? O5 Sm1 O11 79.81(19) . . ? O4 Sm1 O11 128.40(17) . . ? O26 Sm1 O11 55.02(17) . . ? O10 Sm1 O11 98.65(19) . . ? O21 Sm1 O11 147.03(17) . . ? F1 Sm1 O2 66.59(14) . . ? O5 Sm1 O2 144.90(16) . . ? O4 Sm1 O2 132.37(17) . . ? O26 Sm1 O2 98.82(18) . . ? O10 Sm1 O2 54.78(15) . . ? O21 Sm1 O2 75.29(16) . . ? O11 Sm1 O2 73.96(18) . . ? F1 Sm1 O6 67.87(13) . . ? O5 Sm1 O6 67.98(15) . . ? O4 Sm1 O6 81.99(16) . . ? O26 Sm1 O6 146.30(16) . . ? O10 Sm1 O6 125.36(15) . . ? O21 Sm1 O6 54.32(14) . . ? O11 Sm1 O6 132.40(17) . . ? O2 Sm1 O6 114.88(15) . . ? F1 Sm1 S4 102.56(10) . . ? O5 Sm1 S4 78.53(12) . . ? O4 Sm1 S4 101.39(13) . . ? O26 Sm1 S4 27.69(12) . . ? O10 Sm1 S4 88.44(12) . . ? O21 Sm1 S4 159.80(11) . . ? O11 Sm1 S4 27.55(12) . . ? O2 Sm1 S4 88.26(13) . . ? O6 Sm1 S4 145.66(10) . . ? F1 Sm1 S3 93.24(10) . . ? O5 Sm1 S3 166.28(12) . . ? O4 Sm1 S3 105.41(13) . . ? O26 Sm1 S3 86.75(14) . . ? O10 Sm1 S3 27.31(11) . . ? O21 Sm1 S3 71.21(11) . . ? O11 Sm1 S3 86.53(15) . . ? O2 Sm1 S3 27.49(11) . . ? O6 Sm1 S3 123.66(10) . . ? S4 Sm1 S3 88.77(4) . . ? F1 Sm1 S2 69.72(9) . . ? O5 Sm1 S2 95.60(12) . . ? O4 Sm1 S2 84.55(13) . . ? O26 Sm1 S2 159.75(12) . . ? O10 Sm1 S2 99.56(12) . . ? O21 Sm1 S2 27.12(10) . . ? O11 Sm1 S2 144.98(13) . . ? O2 Sm1 S2 92.81(12) . . ? O6 Sm1 S2 27.63(10) . . ? S4 Sm1 S2 170.90(5) . . ? S3 Sm1 S2 96.35(4) . . ? F1 Sm2 O9 76.20(15) . . ? F1 Sm2 O3 78.00(14) . 2_666 ? O9 Sm2 O3 72.51(16) . 2_666 ? F1 Sm2 O23 148.79(15) . . ? O9 Sm2 O23 82.41(16) . . ? O3 Sm2 O23 74.00(16) 2_666 . ? F1 Sm2 O17 141.30(14) . . ? O9 Sm2 O17 86.36(17) . . ? O3 Sm2 O17 129.31(15) 2_666 . ? O23 Sm2 O17 57.56(15) . . ? F1 Sm2 O18 72.38(14) . . ? O9 Sm2 O18 137.98(16) . . ? O3 Sm2 O18 74.22(16) 2_666 . ? O23 Sm2 O18 112.03(15) . . ? O17 Sm2 O18 135.18(16) . . ? F1 Sm2 O19 79.23(14) . . ? O9 Sm2 O19 126.55(16) . . ? O3 Sm2 O19 144.96(15) 2_666 . ? O23 Sm2 O19 131.99(15) . . ? O17 Sm2 O19 84.26(15) . . ? O18 Sm2 O19 73.69(16) . . ? F1 Sm2 O8 125.22(14) . . ? O9 Sm2 O8 156.44(16) . . ? O3 Sm2 O8 100.47(15) 2_666 . ? O23 Sm2 O8 74.03(16) . . ? O17 Sm2 O8 81.02(16) . . ? O18 Sm2 O8 55.36(14) . . ? O19 Sm2 O8 72.02(15) . . ? F1 Sm2 O6 65.77(13) . . ? O9 Sm2 O6 73.53(15) . . ? O3 Sm2 O6 134.95(15) 2_666 . ? O23 Sm2 O6 128.97(14) . . ? O17 Sm2 O6 76.29(14) . . ? O18 Sm2 O6 116.02(15) . . ? O19 Sm2 O6 53.11(14) . . ? O8 Sm2 O6 121.83(14) . . ? F1 Sm2 S6 158.69(10) . . ? O9 Sm2 S6 83.32(12) . . ? O3 Sm2 S6 101.57(12) 2_666 . ? O23 Sm2 S6 28.64(11) . . ? O17 Sm2 S6 28.92(10) . . ? O18 Sm2 S6 128.40(11) . . ? O19 Sm2 S6 109.21(11) . . ? O8 Sm2 S6 76.01(10) . . ? O6 Sm2 S6 102.95(10) . . ? F1 Sm2 S1 98.76(10) . . ? O9 Sm2 S1 159.43(12) . . ? O3 Sm2 S1 86.96(11) 2_666 . ? O23 Sm2 S1 93.31(11) . . ? O17 Sm2 S1 108.37(13) . . ? O18 Sm2 S1 27.52(11) . . ? O19 Sm2 S1 70.62(11) . . ? O8 Sm2 S1 27.84(10) . . ? O6 Sm2 S1 123.09(9) . . ? S6 Sm2 S1 102.50(4) . . ? F1 Sm2 S2 68.62(9) . . ? O9 Sm2 S2 100.51(12) . . ? O3 Sm2 S2 146.57(11) 2_666 . ? O23 Sm2 S2 138.65(11) . . ? O17 Sm2 S2 81.32(11) . . ? O18 Sm2 S2 93.33(12) . . ? O19 Sm2 S2 26.04(11) . . ? O8 Sm2 S2 97.16(11) . . ? O6 Sm2 S2 27.22(9) . . ? S6 Sm2 S2 110.17(4) . . ? S1 Sm2 S2 95.97(4) . . ? O3 S1 O16 108.0(3) . . ? O3 S1 O18 111.7(3) . . ? O16 S1 O18 109.3(3) . . ? O3 S1 O8 110.5(3) . . ? O16 S1 O8 111.9(3) . . ? O18 S1 O8 105.6(3) . . ? O3 S1 Sm2 126.3(2) . . ? O16 S1 Sm2 125.6(2) . . ? O18 S1 Sm2 51.33(18) . . ? O8 S1 Sm2 54.24(19) . . ? O20 S2 O19 111.9(3) . . ? O20 S2 O6 112.4(3) . . ? O19 S2 O6 105.7(3) . . ? O20 S2 O21 112.6(3) . . ? O19 S2 O21 109.3(3) . . ? O6 S2 O21 104.4(3) . . ? O20 S2 Sm1 137.5(2) . . ? O19 S2 Sm1 110.58(19) . . ? O6 S2 Sm1 55.42(19) . . ? O21 S2 Sm1 50.08(19) . . ? O20 S2 Sm2 133.9(2) . . ? O19 S2 Sm2 48.14(18) . . ? O6 S2 Sm2 58.02(19) . . ? O21 S2 Sm2 113.35(19) . . ? Sm1 S2 Sm2 78.21(3) . . ? O24 S3 O12 111.6(3) . . ? O24 S3 O2 109.4(3) . . ? O12 S3 O2 110.2(3) . . ? O24 S3 O10 110.9(3) . . ? O12 S3 O10 110.2(3) . . ? O2 S3 O10 104.1(3) . . ? O24 S3 Sm1 122.6(2) . . ? O12 S3 Sm1 125.7(2) . . ? O2 S3 Sm1 53.64(19) . . ? O10 S3 Sm1 50.50(19) . . ? O27 S4 O28 110.5(4) . . ? O27 S4 O11 112.5(4) . . ? O28 S4 O11 110.4(4) . . ? O27 S4 O26 110.7(3) . . ? O28 S4 O26 109.7(4) . . ? O11 S4 O26 102.8(3) . . ? O27 S4 Sm1 120.0(2) . . ? O28 S4 Sm1 129.4(3) . . ? O11 S4 Sm1 52.7(2) . . ? O26 S4 Sm1 50.6(2) . . ? O15 S5 O25 110.8(3) . . ? O15 S5 O1 110.1(3) . . ? O25 S5 O1 108.2(3) . . ? O15 S5 O4 108.3(3) . . ? O25 S5 O4 110.1(3) . . ? O1 S5 O4 109.2(3) . . ? O14 S6 O22 109.4(3) . . ? O14 S6 O23 110.8(3) . . ? O22 S6 O23 110.0(3) . . ? O14 S6 O17 111.3(3) . . ? O22 S6 O17 110.6(3) . . ? O23 S6 O17 104.7(3) . . ? O14 S6 Sm2 125.4(2) . . ? O22 S6 Sm2 125.2(2) . . ? O23 S6 Sm2 52.14(18) . . ? O17 S6 Sm2 52.56(18) . . ? O13 S7 O7 112.2(3) . . ? O13 S7 O5 109.8(3) . . ? O7 S7 O5 108.9(3) . . ? O13 S7 O9 107.8(3) . . ? O7 S7 O9 108.9(3) . . ? O5 S7 O9 109.1(3) . . ? Sm2 F1 Sm1 127.74(16) . . ? S3 O2 Sm1 98.9(2) . . ? S1 O3 Sm2 137.3(3) . 2_666 ? S5 O4 Sm1 165.6(4) . . ? S7 O5 Sm1 140.1(3) . . ? S2 O6 Sm1 97.0(2) . . ? S2 O6 Sm2 94.8(2) . . ? Sm1 O6 Sm2 97.25(14) . . ? S1 O8 Sm2 97.9(2) . . ? S7 O9 Sm2 137.0(3) . . ? S3 O10 Sm1 102.2(2) . . ? S4 O11 Sm1 99.7(3) . . ? S6 O17 Sm2 98.5(2) . . ? S1 O18 Sm2 101.2(2) . . ? S2 O19 Sm2 105.8(2) . . ? S2 O21 Sm1 102.8(2) . . ? S6 O23 Sm2 99.2(2) . . ? S4 O26 Sm1 101.7(3) . . ? C3 N2 C1 113.9(5) . . ? C3 N2 H2C 108.8 . . ? C1 N2 H2C 108.8 . . ? C3 N2 H2D 108.8 . . ? C1 N2 H2D 108.8 . . ? H2C N2 H2D 107.7 . . ? C9 N9 C12 112.1(5) . . ? C9 N9 H9C 109.2 . . ? C12 N9 H9C 109.2 . . ? C9 N9 H9D 109.2 . . ? C12 N9 H9D 109.2 . . ? H9C N9 H9D 107.9 . . ? C11 N8 H8C 109.5 . . ? C11 N8 H8D 109.5 . . ? H8C N8 H8D 109.5 . . ? C11 N8 H8E 109.5 . . ? H8C N8 H8E 109.5 . . ? H8D N8 H8E 109.5 . . ? C4 N3 H3C 109.5 . . ? C4 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C4 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C7 N5 C6 115.3(5) . . ? C7 N5 H5C 108.4 . . ? C6 N5 H5C 108.4 . . ? C7 N5 H5D 108.4 . . ? C6 N5 H5D 108.4 . . ? H5C N5 H5D 107.5 . . ? C8 N6 H6C 109.5 . . ? C8 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C8 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C2 N1 H1C 109.5 . . ? C2 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C2 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C10 N7 H7C 109.5 . . ? C10 N7 H7D 109.5 . . ? H7C N7 H7D 109.5 . . ? C10 N7 H7E 109.5 . . ? H7C N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? C5 N4 H4C 109.5 . . ? C5 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C5 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C1 C2 N1 114.0(6) . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? N1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C5 C6 N5 110.8(6) . . ? C5 C6 H6A 109.5 . . ? N5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? N5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N9 C12 C11 112.3(6) . . ? N9 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? N9 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N8 C11 C12 112.9(6) . . ? N8 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N8 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N7 C10 C9 108.7(5) . . ? N7 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N7 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N2 C3 C4 112.6(5) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 112.4(6) . . ? N3 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N3 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N9 C9 C10 110.7(5) . . ? N9 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N9 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N5 C7 C8 112.9(6) . . ? N5 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N5 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N2 C1 C2 114.8(6) . . ? N2 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N2 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? N6 C8 C7 111.0(6) . . ? N6 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N6 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N4 C5 C6 116.4(8) . . ? N4 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N4 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1C O19 2_576 0.889 2.131 2.948(8) 152.5 y N1 H1D O12 . 0.889 2.196 2.777(8) 122.5 y N1 H1D O2 2_576 0.889 2.589 3.215(8) 128.1 y N1 H1C O21 2_576 0.889 2.388 3.104(8) 137.7 y N1 H1D O24 2_576 0.889 2.451 3.038(8) 124.0 y N1 H1E O16 2_576 0.889 2.183 2.957(8) 145.0 y N2 H2c O2 . 0.900 2.373 3.024(8) 129.2 y N2 H2c O12 . 0.900 2.412 3.035(9) 126.5 y N2 H2c O24 2_576 0.900 2.393 3.008(8) 125.7 y N2 H2D O11 . 0.900 2.127 2.963(8) 154.0 y N2 H2D O28 . 0.900 2.326 3.076(9) 140.8 y N3 H3D O2 . 0.890 2.082 2.927(9) 158.1 y N3 H3D O24 2_576 0.890 2.589 2.885(8) 100.4 y N3 H3E O22 2_666 0.890 2.336 3.099(8) 143.8 y N3 H3E O23 2_666 0.890 2.318 2.929(9) 125.8 y N3 H3E O24 2_576 0.890 2.467 2.885(8) 109.2 y N4 H4C O10 2_576 0.890 2.045 2.918(8) 166.2 y N4 H4D O1 1_556 0.890 2.583 2.885(8) 100.8 y N4 H4D O14 2_666 0.890 2.362 2.946(11) 123.3 y N4 H4E O1 1_556 0.890 2.385 2.885(8) 115.7 y N4 H4E O26 2_576 0.890 2.546 3.044(10) 116.1 y N5 H5C O16 . 0.900 1.982 2.835(8) 157.6 y N5 H5D O3 . 0.900 2.441 2.995(9) 120.1 y N5 H5D O9 2_666 0.900 2.060 2.912(9) 157.4 y N6 H6C O22 2_656 0.900 1.991 2.844(8) 160.3 y N6 H6D O21 2_566 0.900 2.241 3.115(9) 167.0 y N6 H6E O25 2_566 0.900 1.939 2.760(8) 152.5 y N7 H7C O1 . 0.900 1.959 2.730(9) 144.1 y N7 H7C O4 . 0.900 2.488 3.291(8) 150.3 y N7 H7D O25 2_575 0.900 2.022 2.806(8) 146.2 y N7 H7E O26 . 0.900 2.104 2.748(8) 128.6 y N8 H8C O4 2_665 0.890 2.501 3.209(8) 137.0 y N8 H8C O15 2_665 0.890 1.911 2.714(9) 149.4 y N8 H8D O6 2_665 0.890 2.443 3.010(8) 122.8 y N8 H8D O7 2_665 0.890 1.971 2.772(9) 148.9 y N8 H8E O13 . 0.890 1.959 2.784(8) 153.8 y N9 H9D O7 2_665 0.900 1.995 2.832(8) 154.2 y N9 H9C O28 2_675 0.900 2.169 2.995(10) 152.5 y _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.870 _refine_diff_density_min -1.696 _refine_diff_density_rms 0.234 # Attachment 'compound_2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 758053' #TrackingRef 'compound_2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 F O5 S Tb' _chemical_formula_weight 292.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.0014(7) _cell_length_b 7.3769(11) _cell_length_c 11.6508(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.692(2) _cell_angle_gamma 90.00 _cell_volume 426.93(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 831 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 25.99 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 17.003 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.1717 _exptl_absorpt_correction_T_max 0.2348 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _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 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2182 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.99 _reflns_number_total 831 _reflns_number_gt 794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+1.1793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 831 _refine_ls_number_parameters 79 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0471 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.175 _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 0.21505(4) 0.78923(3) 0.187168(18) 0.00848(11) Uani 1 1 d . . . S1 S -0.2112(2) 0.64010(17) 0.38476(9) 0.0073(2) Uani 1 1 d . . . O1W O -0.1334(8) 0.6222(5) 0.0775(3) 0.0172(8) Uani 1 1 d D . . H1WB H -0.274(8) 0.673(8) 0.045(5) 0.021 Uiso 1 1 d D . . H1WA H -0.139(13) 0.507(3) 0.076(5) 0.021 Uiso 1 1 d D . . O1 O 0.0425(6) 0.5965(5) 0.3349(3) 0.0109(7) Uani 1 1 d . . . O2 O -0.1396(7) 0.7217(5) 0.5004(3) 0.0129(8) Uani 1 1 d . . . O3 O -0.3650(8) 0.7727(5) 0.3084(3) 0.0140(8) Uani 1 1 d . . . O4 O -0.3652(7) 0.4747(5) 0.3958(3) 0.0122(7) Uani 1 1 d . . . F1 F 0.1545(5) 0.9948(4) 0.3236(2) 0.0124(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 Tb1 0.00923(15) 0.00823(17) 0.00772(15) 0.00001(8) -0.00003(10) 0.00074(9) S1 0.0069(5) 0.0079(6) 0.0070(5) 0.0001(5) 0.0005(4) 0.0000(5) O1W 0.0147(18) 0.0096(19) 0.026(2) -0.0011(17) -0.0045(15) 0.0038(16) O1 0.0105(16) 0.0111(19) 0.0118(16) 0.0001(14) 0.0046(13) 0.0028(14) O2 0.0146(18) 0.015(2) 0.0093(18) -0.0040(15) 0.0021(14) -0.0025(15) O3 0.0161(19) 0.0077(18) 0.0162(19) 0.0026(15) -0.0066(15) 0.0014(15) O4 0.0135(16) 0.0104(18) 0.0123(16) 0.0039(14) 0.0004(13) -0.0038(15) F1 0.0128(14) 0.0127(15) 0.0122(13) -0.0001(12) 0.0030(11) -0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 F1 2.243(3) . ? Tb1 F1 2.275(3) 2_545 ? Tb1 O4 2.340(3) 2_455 ? Tb1 O2 2.375(4) 4_675 ? Tb1 O1W 2.381(4) . ? Tb1 O3 2.393(4) 1_655 ? Tb1 O1 2.465(3) . ? Tb1 O1 2.598(4) 2 ? Tb1 Tb1 3.9688(5) 2 ? Tb1 Tb1 3.9688(5) 2_545 ? S1 O4 1.457(4) . ? S1 O3 1.477(4) . ? S1 O2 1.481(4) . ? S1 O1 1.491(3) . ? O1W H1WB 0.85(2) . ? O1W H1WA 0.85(2) . ? O1 Tb1 2.598(4) 2_545 ? O2 Tb1 2.375(4) 4_576 ? O3 Tb1 2.393(4) 1_455 ? O4 Tb1 2.340(3) 2_445 ? F1 Tb1 2.275(3) 2 ? 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 F1 Tb1 F1 138.40(6) . 2_545 ? F1 Tb1 O4 75.01(11) . 2_455 ? F1 Tb1 O4 137.80(11) 2_545 2_455 ? F1 Tb1 O2 138.88(12) . 4_675 ? F1 Tb1 O2 78.27(11) 2_545 4_675 ? O4 Tb1 O2 86.28(12) 2_455 4_675 ? F1 Tb1 O1W 125.41(12) . . ? F1 Tb1 O1W 70.92(12) 2_545 . ? O4 Tb1 O1W 67.38(13) 2_455 . ? O2 Tb1 O1W 76.92(13) 4_675 . ? F1 Tb1 O3 78.34(12) . 1_655 ? F1 Tb1 O3 75.31(11) 2_545 1_655 ? O4 Tb1 O3 146.74(13) 2_455 1_655 ? O2 Tb1 O3 101.40(13) 4_675 1_655 ? O1W Tb1 O3 145.83(13) . 1_655 ? F1 Tb1 O1 78.92(11) . . ? F1 Tb1 O1 67.30(10) 2_545 . ? O4 Tb1 O1 108.67(11) 2_455 . ? O2 Tb1 O1 142.19(12) 4_675 . ? O1W Tb1 O1 77.44(12) . . ? O3 Tb1 O1 85.01(12) 1_655 . ? F1 Tb1 O1 65.37(10) . 2 ? F1 Tb1 O1 133.42(10) 2_545 2 ? O4 Tb1 O1 77.53(12) 2_455 2 ? O2 Tb1 O1 75.07(12) 4_675 2 ? O1W Tb1 O1 135.99(12) . 2 ? O3 Tb1 O1 73.46(12) 1_655 2 ? O1 Tb1 O1 141.07(8) . 2 ? F1 Tb1 Tb1 28.78(7) . 2 ? F1 Tb1 Tb1 153.37(7) 2_545 2 ? O4 Tb1 Tb1 68.81(9) 2_455 2 ? O2 Tb1 Tb1 110.26(9) 4_675 2 ? O1W Tb1 Tb1 134.95(9) . 2 ? O3 Tb1 Tb1 78.24(9) 1_655 2 ? O1 Tb1 Tb1 107.53(8) . 2 ? O1 Tb1 Tb1 37.20(7) 2 2 ? F1 Tb1 Tb1 112.36(8) . 2_545 ? F1 Tb1 Tb1 28.33(7) 2_545 2_545 ? O4 Tb1 Tb1 136.50(9) 2_455 2_545 ? O2 Tb1 Tb1 106.46(9) 4_675 2_545 ? O1W Tb1 Tb1 75.20(10) . 2_545 ? O3 Tb1 Tb1 72.63(9) 1_655 2_545 ? O1 Tb1 Tb1 39.58(8) . 2_545 ? O1 Tb1 Tb1 145.64(8) 2 2_545 ? Tb1 Tb1 Tb1 136.673(14) 2 2_545 ? O4 S1 O3 111.4(2) . . ? O4 S1 O2 109.5(2) . . ? O3 S1 O2 109.4(2) . . ? O4 S1 O1 109.7(2) . . ? O3 S1 O1 108.4(2) . . ? O2 S1 O1 108.4(2) . . ? Tb1 O1W H1WB 122(5) . . ? Tb1 O1W H1WA 123(4) . . ? H1WB O1W H1WA 114(6) . . ? S1 O1 Tb1 122.1(2) . . ? S1 O1 Tb1 130.9(2) . 2_545 ? Tb1 O1 Tb1 103.22(11) . 2_545 ? S1 O2 Tb1 138.8(2) . 4_576 ? S1 O3 Tb1 138.5(2) . 1_455 ? S1 O4 Tb1 146.2(2) . 2_445 ? Tb1 F1 Tb1 122.89(12) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1W H1WB O2 4_575 0.85(5) 2.00(5) 2.831(5) 167(5) y O1W H1WA O2 2_445 0.85(2) 2.49(4) 3.256(5) 150(5) y O1W H1WA O3 2_445 0.85(2) 2.19(4) 2.901(5) 141(5) y _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.587 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.205 # Attachment 'compound_3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 758054' #TrackingRef 'compound_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 F Nd O5 S' _chemical_formula_weight 277.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.9948(5) _cell_length_b 7.3684(7) _cell_length_c 11.6366(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.6720(10) _cell_angle_gamma 90.00 _cell_volume 425.37(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 563 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.50 _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 12.645 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.2705 _exptl_absorpt_correction_T_max 0.3645 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _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 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2083 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 785 _reflns_number_gt 749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+1.1793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 785 _refine_ls_number_parameters 79 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.21511(6) 0.78935(4) 0.18719(3) 0.00677(15) Uani 1 1 d . . . S1 S -0.2110(3) 0.6402(2) 0.38485(12) 0.0120(3) Uani 1 1 d . . . O1W O -0.1323(9) 0.6222(7) 0.0777(4) 0.0232(11) Uani 1 1 d D . . H1WB H -0.264(11) 0.661(11) 0.031(5) 0.028 Uiso 1 1 d D . . H1WA H -0.194(15) 0.514(5) 0.080(7) 0.028 Uiso 1 1 d D . . O1 O 0.0435(8) 0.5967(6) 0.3347(4) 0.0167(10) Uani 1 1 d . . . O2 O -0.1393(9) 0.7213(7) 0.5001(4) 0.0183(10) Uani 1 1 d . . . O3 O -0.3636(10) 0.7725(7) 0.3087(4) 0.0193(11) Uani 1 1 d . . . O4 O -0.3648(9) 0.4743(6) 0.3959(4) 0.0175(10) Uani 1 1 d . . . F1 F 0.1546(7) 0.9948(5) 0.3236(3) 0.0178(8) 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 0.0097(2) 0.0045(2) 0.0057(2) 0.00014(11) -0.00076(13) 0.00063(11) S1 0.0146(7) 0.0103(8) 0.0108(7) 0.0001(6) 0.0004(5) 0.0001(6) O1W 0.019(2) 0.016(3) 0.032(3) 0.001(2) -0.006(2) -0.004(2) O1 0.017(2) 0.015(3) 0.018(2) -0.0015(18) 0.0016(17) -0.0003(18) O2 0.019(2) 0.021(3) 0.016(3) -0.0029(19) 0.0046(19) -0.0023(19) O3 0.021(3) 0.015(3) 0.021(3) 0.0021(19) -0.003(2) -0.001(2) O4 0.021(2) 0.014(3) 0.016(2) 0.0016(19) -0.0006(17) -0.003(2) F1 0.0217(19) 0.014(2) 0.0175(19) -0.0004(15) 0.0021(14) -0.0006(16) _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 F1 2.239(4) . ? Nd1 F1 2.274(4) 2_545 ? Nd1 O4 2.337(4) 2_455 ? Nd1 O1W 2.375(5) . ? Nd1 O2 2.375(5) 4_675 ? Nd1 O3 2.398(5) 1_655 ? Nd1 O1 2.457(4) . ? Nd1 O1 2.592(5) 2 ? Nd1 Nd1 3.9640(4) 2 ? Nd1 Nd1 3.9640(4) 2_545 ? S1 O4 1.457(5) . ? S1 O3 1.470(5) . ? S1 O2 1.474(5) . ? S1 O1 1.494(4) . ? O1W H1WB 0.86(2) . ? O1W H1WA 0.85(2) . ? O1 Nd1 2.592(5) 2_545 ? O2 Nd1 2.375(5) 4_576 ? O3 Nd1 2.398(5) 1_455 ? O4 Nd1 2.337(4) 2_445 ? F1 Nd1 2.274(4) 2 ? 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 F1 Nd1 F1 138.38(8) . 2_545 ? F1 Nd1 O4 75.10(14) . 2_455 ? F1 Nd1 O4 137.67(14) 2_545 2_455 ? F1 Nd1 O1W 125.49(15) . . ? F1 Nd1 O1W 70.80(16) 2_545 . ? O4 Nd1 O1W 67.37(17) 2_455 . ? F1 Nd1 O2 138.85(15) . 4_675 ? F1 Nd1 O2 78.33(15) 2_545 4_675 ? O4 Nd1 O2 86.23(15) 2_455 4_675 ? O1W Nd1 O2 76.92(17) . 4_675 ? F1 Nd1 O3 78.38(15) . 1_655 ? F1 Nd1 O3 75.29(15) 2_545 1_655 ? O4 Nd1 O3 146.90(16) 2_455 1_655 ? O1W Nd1 O3 145.69(17) . 1_655 ? O2 Nd1 O3 101.39(17) 4_675 1_655 ? F1 Nd1 O1 78.95(14) . . ? F1 Nd1 O1 67.20(13) 2_545 . ? O4 Nd1 O1 108.70(15) 2_455 . ? O1W Nd1 O1 77.44(16) . . ? O2 Nd1 O1 142.18(15) 4_675 . ? O3 Nd1 O1 84.94(15) 1_655 . ? F1 Nd1 O1 65.28(13) . 2 ? F1 Nd1 O1 133.57(13) 2_545 2 ? O4 Nd1 O1 77.55(15) 2_455 2 ? O1W Nd1 O1 136.05(16) . 2 ? O2 Nd1 O1 75.13(15) 4_675 2 ? O3 Nd1 O1 73.55(15) 1_655 2 ? O1 Nd1 O1 141.02(10) . 2 ? F1 Nd1 Nd1 28.80(9) . 2 ? F1 Nd1 Nd1 153.41(9) 2_545 2 ? O4 Nd1 Nd1 68.90(11) 2_455 2 ? O1W Nd1 Nd1 135.03(13) . 2 ? O2 Nd1 Nd1 110.21(12) 4_675 2 ? O3 Nd1 Nd1 78.30(12) 1_655 2 ? O1 Nd1 Nd1 107.59(11) . 2 ? O1 Nd1 Nd1 37.08(9) 2 2 ? F1 Nd1 Nd1 112.33(10) . 2_545 ? F1 Nd1 Nd1 28.32(9) 2_545 2_545 ? O4 Nd1 Nd1 136.40(12) 2_455 2_545 ? O1W Nd1 Nd1 75.12(13) . 2_545 ? O2 Nd1 Nd1 106.51(11) 4_675 2_545 ? O3 Nd1 Nd1 72.60(12) 1_655 2_545 ? O1 Nd1 Nd1 39.50(10) . 2_545 ? O1 Nd1 Nd1 145.72(9) 2 2_545 ? Nd1 Nd1 Nd1 136.685(16) 2 2_545 ? O4 S1 O3 111.6(3) . . ? O4 S1 O2 109.6(3) . . ? O3 S1 O2 109.5(3) . . ? O4 S1 O1 109.6(3) . . ? O3 S1 O1 108.2(3) . . ? O2 S1 O1 108.3(3) . . ? Nd1 O1W H1WB 129(6) . . ? Nd1 O1W H1WA 135(5) . . ? H1WB O1W H1WA 95(7) . . ? S1 O1 Nd1 122.1(3) . . ? S1 O1 Nd1 130.7(3) . 2_545 ? Nd1 O1 Nd1 103.42(15) . 2_545 ? S1 O2 Nd1 138.8(3) . 4_576 ? S1 O3 Nd1 138.4(3) . 1_455 ? S1 O4 Nd1 146.1(3) . 2_445 ? Nd1 F1 Nd1 122.88(15) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1W H1WB O2 4_575 0.85(6) 2.06(6) 2.833(7) 151(5) y O1W H1WA O2 2_445 0.85(4) 2.46(5) 3.257(7) 156(5) y O1W H1WA O3 2_445 0.85(4) 2.20(6) 2.897(7) 138(5) y _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.804 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.249