# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_zd-9 _database_code_depnum_ccdc_archive 'CCDC 875279' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(CH3)2NH2]6[H3N(CH2)2NH3][Nd2(SO4)7]' _chemical_formula_sum 'C14 H58 N8 Nd2 O28 S7' _chemical_formula_weight 1299.58 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' Nd Nd -0.1943 3.0179 '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 10.635(9) _cell_length_b 15.320(13) _cell_length_c 15.753(13) _cell_angle_alpha 82.790(9) _cell_angle_beta 73.747(9) _cell_angle_gamma 73.244(10) _cell_volume 2357(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4482 _cell_measurement_theta_min 2.683 _cell_measurement_theta_max 25.689 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 2.579 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.6983 _exptl_absorpt_correction_T_max 0.7825 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 16816 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8199 _reflns_number_gt 5748 _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^)+(0.0970P)^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 8199 _refine_ls_number_parameters 559 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1618 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.22521(4) 0.88980(3) 0.38829(3) 0.02256(16) Uani 1 1 d . . . Nd2 Nd 0.27424(4) 0.61335(3) 0.11379(3) 0.02438(16) Uani 1 1 d . . . S1 S -0.0918(2) 0.92401(14) 0.45373(14) 0.0256(5) Uani 1 1 d . . . S2 S 0.5866(2) 0.53371(15) 0.08469(15) 0.0293(5) Uani 1 1 d . . . S3 S 0.4133(2) 0.74093(15) 0.48656(15) 0.0319(5) Uani 1 1 d . . . S4 S 0.1003(3) 0.49829(19) 0.24834(18) 0.0448(6) Uani 1 1 d . . . S5 S 0.3356(2) 1.04010(16) 0.25818(17) 0.0373(6) Uani 1 1 d . . . S6 S 0.2538(2) 0.75267(12) 0.24993(13) 0.0281(5) Uani 1 1 d . . . S7 S 0.1420(3) 0.75671(18) -0.0153(2) 0.0512(7) Uani 1 1 d . . . O1 O 0.6743(7) 0.4758(5) 0.0135(4) 0.0478(18) Uani 1 1 d . . . O2 O -0.1866(6) 0.9983(4) 0.5065(5) 0.0430(17) Uani 1 1 d . . . O3 O 0.2840(7) 0.7328(5) -0.0112(5) 0.0499(18) Uani 1 1 d . . . O4 O 0.2650(6) 0.7709(5) 0.5100(5) 0.0474(18) Uani 1 1 d . . . O5 O 0.0096(6) 0.8686(4) 0.5016(4) 0.0349(15) Uani 1 1 d . . . O6 O 0.0801(6) 0.6957(5) 0.0536(4) 0.0458(18) Uani 1 1 d . . . O7 O -0.0139(6) 0.9601(4) 0.3709(4) 0.0329(14) Uani 1 1 d . . . O8 O 0.4508(7) 0.8059(5) 0.4111(5) 0.063(2) Uani 1 1 d . . . O9 O 0.1964(6) 1.0256(4) 0.2787(5) 0.0456(17) Uani 1 1 d . . . O10 O 0.4784(6) 0.4918(4) 0.1382(4) 0.0367(15) Uani 1 1 d . . . O11 O -0.1681(6) 0.8680(4) 0.4337(4) 0.0404(16) Uani 1 1 d . . . O12 O 0.5126(6) 0.6197(4) 0.0484(4) 0.0377(15) Uani 1 1 d . . . O13 O 0.6665(6) 0.5489(4) 0.1406(4) 0.0408(16) Uani 1 1 d . . . O14 O 0.4075(6) 0.9645(4) 0.3113(4) 0.0392(16) Uani 1 1 d . . . O15 O 0.1675(6) 0.7609(4) 0.3391(4) 0.0403(16) Uani 1 1 d . . . O16 O 0.4662(7) 0.7510(5) 0.5600(5) 0.0522(19) Uani 1 1 d . . . O17 O 0.4624(10) 0.6475(5) 0.4612(6) 0.080(3) Uani 1 1 d . . . O18 O 0.3468(6) 0.6624(4) 0.2353(4) 0.0412(16) Uani 1 1 d . . . O19 O 0.1724(7) 0.7670(4) 0.1849(5) 0.0516(19) Uani 1 1 d . . . O20 O 0.3246(7) 0.8243(4) 0.2383(4) 0.0504(19) Uani 1 1 d . . . O21 O 0.3972(8) 1.0322(5) 0.1666(5) 0.066(2) Uani 1 1 d . . . O22 O 0.3306(8) 1.1260(4) 0.2910(5) 0.059(2) Uani 1 1 d . . . O23 O 0.0783(10) 0.8509(5) 0.0056(7) 0.087(3) Uani 1 1 d . . . O24 O -0.0251(8) 0.4833(6) 0.2477(5) 0.072(2) Uani 1 1 d . . . O25 O 0.1314(9) 0.7377(6) -0.1001(5) 0.072(2) Uani 1 1 d . . . O26 O 0.1504(13) 0.4432(9) 0.3180(8) 0.134(4) Uani 1 1 d U . . O27 O 0.2009(8) 0.4740(5) 0.1631(7) 0.089(3) Uani 1 1 d . . . O28 O 0.0939(9) 0.5953(6) 0.2511(6) 0.093(3) Uani 1 1 d . . . N1 N 0.2425(11) 0.9376(6) 0.0826(6) 0.068(3) Uani 1 1 d . . . H1D H 0.2696 0.9325 0.1326 0.081 Uiso 1 1 calc R . . H1E H 0.2050 0.8914 0.0851 0.081 Uiso 1 1 calc R . . N2 N -0.0402(10) 0.6733(6) 0.4244(9) 0.088(4) Uani 1 1 d . . . H2D H -0.0533 0.7341 0.4233 0.106 Uiso 1 1 calc R . . H2E H 0.0107 0.6545 0.3706 0.106 Uiso 1 1 calc R . . N3 N 0.5186(8) 0.5288(5) 0.3331(5) 0.048(2) Uani 1 1 d . . . H3D H 0.5206 0.5495 0.2768 0.058 Uiso 1 1 calc R . . H3E H 0.5013 0.5772 0.3656 0.058 Uiso 1 1 calc R . . N4 N 0.0564(9) 0.8377(5) 0.6729(5) 0.049(2) Uani 1 1 d . . . H4D H 0.0896 0.8361 0.6138 0.059 Uiso 1 1 calc R . . H4E H -0.0154 0.8870 0.6844 0.059 Uiso 1 1 calc R . . N5 N 0.5537(9) 0.6871(5) -0.1353(6) 0.055(2) Uani 1 1 d . . . H5D H 0.4841 0.6890 -0.0867 0.067 Uiso 1 1 calc R . . H5E H 0.5982 0.6280 -0.1440 0.067 Uiso 1 1 calc R . . N6 N 0.4218(8) 1.1085(5) 0.4431(5) 0.045(2) Uani 1 1 d . . . H6D H 0.4523 1.1319 0.3892 0.067 Uiso 1 1 calc R . . H6E H 0.4122 1.1477 0.4832 0.067 Uiso 1 1 calc R . . H6F H 0.3419 1.0984 0.4475 0.067 Uiso 1 1 calc R . . N7 N 0.0715(8) 0.5707(6) -0.0983(5) 0.049(2) Uani 1 1 d . . . H7D H 0.0472 0.6303 -0.1117 0.073 Uiso 1 1 calc R . . H7E H 0.0660 0.5401 -0.1410 0.073 Uiso 1 1 calc R . . H7F H 0.1565 0.5545 -0.0931 0.073 Uiso 1 1 calc R . . C1 C 0.358(2) 0.9222(16) 0.0134(16) 0.180(10) Uani 1 1 d U . . H1A H 0.4166 0.8628 0.0221 0.270 Uiso 1 1 calc R . . H1B H 0.4053 0.9677 0.0113 0.270 Uiso 1 1 calc R . . H1C H 0.3338 0.9254 -0.0413 0.270 Uiso 1 1 calc R . . C2 C 0.138(2) 1.0187(13) 0.0859(13) 0.138(7) Uani 1 1 d U . . H2A H 0.0649 1.0158 0.1374 0.208 Uiso 1 1 calc R . . H2B H 0.1053 1.0262 0.0337 0.208 Uiso 1 1 calc R . . H2C H 0.1721 1.0695 0.0888 0.208 Uiso 1 1 calc R . . C3 C -0.1738(16) 0.6549(11) 0.4388(11) 0.112(5) Uani 1 1 d U . . H3A H -0.2168 0.6875 0.3938 0.168 Uiso 1 1 calc R . . H3B H -0.2300 0.6747 0.4960 0.168 Uiso 1 1 calc R . . H3C H -0.1615 0.5907 0.4361 0.168 Uiso 1 1 calc R . . C4 C 0.0397(19) 0.6305(12) 0.4902(11) 0.115(6) Uani 1 1 d . . . H4A H 0.1229 0.6484 0.4750 0.172 Uiso 1 1 calc R . . H4B H 0.0598 0.5652 0.4898 0.172 Uiso 1 1 calc R . . H4C H -0.0124 0.6502 0.5482 0.172 Uiso 1 1 calc R . . C5 C 0.6511(11) 0.4678(9) 0.3363(9) 0.077(4) Uani 1 1 d . . . H5A H 0.7196 0.5003 0.3143 0.115 Uiso 1 1 calc R . . H5B H 0.6712 0.4169 0.3003 0.115 Uiso 1 1 calc R . . H5C H 0.6498 0.4461 0.3963 0.115 Uiso 1 1 calc R . . C6 C 0.4070(13) 0.4824(9) 0.3673(9) 0.072(4) Uani 1 1 d . . . H6A H 0.3220 0.5246 0.3636 0.108 Uiso 1 1 calc R . . H6B H 0.4030 0.4617 0.4278 0.108 Uiso 1 1 calc R . . H6C H 0.4245 0.4311 0.3323 0.108 Uiso 1 1 calc R . . C7 C 0.1613(13) 0.8473(8) 0.7125(7) 0.067(3) Uani 1 1 d . . . H7A H 0.1865 0.9026 0.6891 0.100 Uiso 1 1 calc R . . H7B H 0.2395 0.7961 0.6986 0.100 Uiso 1 1 calc R . . H7C H 0.1262 0.8496 0.7755 0.100 Uiso 1 1 calc R . . C8 C 0.0101(14) 0.7548(8) 0.7063(9) 0.076(4) Uani 1 1 d . . . H8A H -0.0589 0.7524 0.6790 0.114 Uiso 1 1 calc R . . H8B H -0.0263 0.7563 0.7694 0.114 Uiso 1 1 calc R . . H8C H 0.0855 0.7018 0.6924 0.114 Uiso 1 1 calc R . . C9 C 0.6460(13) 0.7330(7) -0.1179(8) 0.068(3) Uani 1 1 d . . . H9A H 0.6758 0.7043 -0.0666 0.103 Uiso 1 1 calc R . . H9B H 0.5996 0.7960 -0.1077 0.103 Uiso 1 1 calc R . . H9C H 0.7232 0.7288 -0.1681 0.103 Uiso 1 1 calc R . . C10 C 0.4972(16) 0.7252(11) -0.2119(9) 0.088(5) Uani 1 1 d . . . H10A H 0.4373 0.6911 -0.2177 0.132 Uiso 1 1 calc R . . H10B H 0.5700 0.7212 -0.2648 0.132 Uiso 1 1 calc R . . H10C H 0.4477 0.7879 -0.2031 0.132 Uiso 1 1 calc R . . C11 C 0.5204(12) 1.0212(10) 0.4590(9) 0.083(5) Uani 1 1 d . . . H11A H 0.5336 0.9801 0.4133 0.099 Uiso 1 1 calc R . . H11B H 0.6071 1.0329 0.4540 0.099 Uiso 1 1 calc R . . C12 C -0.0199(11) 0.5495(7) -0.0140(8) 0.058(3) Uani 1 1 d . . . H12A H -0.1121 0.5658 -0.0202 0.069 Uiso 1 1 calc R . . H12B H -0.0180 0.5858 0.0316 0.069 Uiso 1 1 calc R . . C13 C -0.231(2) 0.9348(12) 0.2258(12) 0.038(4) Uani 0.50 1 d PU A 1 H13A H -0.1352 0.9270 0.2149 0.057 Uiso 0.50 1 calc PR A 1 H13B H -0.2757 0.9540 0.2850 0.057 Uiso 0.50 1 calc PR A 1 H13C H -0.2662 0.9802 0.1843 0.057 Uiso 0.50 1 calc PR A 1 C14 C -0.3580(17) 0.8362(12) 0.2252(12) 0.035(4) Uani 0.50 1 d PU A 1 H14A H -0.3501 0.7741 0.2154 0.052 Uiso 0.50 1 calc PR A 1 H14B H -0.4030 0.8762 0.1844 0.052 Uiso 0.50 1 calc PR A 1 H14C H -0.4099 0.8501 0.2847 0.052 Uiso 0.50 1 calc PR A 1 N8 N -0.257(2) 0.8458(14) 0.2151(12) 0.069(4) Uani 0.50 1 d PU A 1 H8D H -0.2105 0.8294 0.1597 0.083 Uiso 0.50 1 calc PR A 1 H8E H -0.2163 0.8044 0.2518 0.083 Uiso 0.50 1 calc PR A 1 C13A C -0.1450(15) 0.7796(12) 0.1882(12) 0.036(4) Uani 0.50 1 d PU B 2 H13D H -0.0486 0.7572 0.1647 0.054 Uiso 0.50 1 calc PR B 2 H13E H -0.1645 0.7890 0.2501 0.054 Uiso 0.50 1 calc PR B 2 H13F H -0.1778 0.8363 0.1577 0.054 Uiso 0.50 1 calc PR B 2 C14A C -0.347(2) 0.7405(16) 0.2089(16) 0.067(6) Uani 0.50 1 d PU B 2 H14D H -0.3890 0.6953 0.2016 0.100 Uiso 0.50 1 calc PR B 2 H14E H -0.3818 0.7966 0.1782 0.100 Uiso 0.50 1 calc PR B 2 H14F H -0.3662 0.7506 0.2707 0.100 Uiso 0.50 1 calc PR B 2 N8A N -0.213(2) 0.7116(15) 0.1759(13) 0.082(5) Uani 0.50 1 d PU B 2 H8AA H -0.1951 0.7027 0.1178 0.099 Uiso 0.50 1 calc PR B 2 H8AB H -0.1809 0.6580 0.2032 0.099 Uiso 0.50 1 calc PR B 2 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 0.0229(3) 0.0218(3) 0.0241(3) -0.00019(19) -0.00673(19) -0.00736(18) Nd2 0.0261(3) 0.0243(3) 0.0238(3) -0.0010(2) -0.0085(2) -0.00655(19) S1 0.0228(10) 0.0260(11) 0.0316(12) -0.0074(9) -0.0084(9) -0.0081(8) S2 0.0276(11) 0.0348(12) 0.0271(12) -0.0074(10) -0.0080(9) -0.0073(9) S3 0.0360(12) 0.0271(11) 0.0324(13) 0.0017(10) -0.0147(10) -0.0037(9) S4 0.0407(13) 0.0579(16) 0.0426(15) 0.0108(13) -0.0127(11) -0.0273(12) S5 0.0395(13) 0.0327(12) 0.0404(14) 0.0083(10) -0.0081(11) -0.0173(10) S6 0.0370(12) 0.0246(11) 0.0253(12) -0.0024(9) -0.0101(10) -0.0095(9) S7 0.0672(18) 0.0405(14) 0.0577(18) 0.0136(13) -0.0409(15) -0.0149(13) O1 0.040(4) 0.061(5) 0.043(4) -0.018(4) -0.009(3) -0.009(3) O2 0.031(3) 0.040(4) 0.059(5) -0.024(3) 0.000(3) -0.013(3) O3 0.052(4) 0.055(4) 0.051(4) 0.008(4) -0.024(4) -0.021(3) O4 0.033(3) 0.065(5) 0.044(4) 0.006(4) -0.015(3) -0.012(3) O5 0.027(3) 0.050(4) 0.027(3) 0.002(3) -0.007(3) -0.010(3) O6 0.035(4) 0.055(4) 0.044(4) -0.006(3) -0.018(3) 0.002(3) O7 0.032(3) 0.025(3) 0.039(4) 0.008(3) -0.009(3) -0.009(3) O8 0.035(4) 0.077(5) 0.055(5) 0.029(4) -0.004(3) -0.003(4) O9 0.034(3) 0.038(4) 0.066(5) 0.021(3) -0.018(3) -0.015(3) O10 0.032(3) 0.031(3) 0.048(4) 0.001(3) -0.011(3) -0.010(3) O11 0.031(3) 0.037(3) 0.064(4) -0.025(3) -0.012(3) -0.017(3) O12 0.041(4) 0.041(4) 0.032(4) 0.007(3) -0.019(3) -0.008(3) O13 0.036(3) 0.058(4) 0.038(4) -0.014(3) -0.018(3) -0.013(3) O14 0.031(3) 0.032(3) 0.053(4) 0.014(3) -0.013(3) -0.010(3) O15 0.047(4) 0.035(3) 0.037(4) -0.011(3) 0.004(3) -0.018(3) O16 0.065(5) 0.050(4) 0.061(5) 0.003(4) -0.042(4) -0.023(4) O17 0.123(8) 0.041(4) 0.074(6) -0.017(4) -0.060(6) 0.020(5) O18 0.040(4) 0.040(4) 0.044(4) -0.014(3) -0.024(3) 0.006(3) O19 0.068(5) 0.038(4) 0.057(5) -0.007(3) -0.045(4) 0.005(3) O20 0.071(5) 0.054(4) 0.040(4) -0.016(3) 0.000(3) -0.046(4) O21 0.083(6) 0.063(5) 0.046(5) -0.004(4) 0.011(4) -0.033(4) O22 0.086(6) 0.038(4) 0.063(5) 0.006(4) -0.029(4) -0.026(4) O23 0.100(7) 0.044(5) 0.126(8) 0.011(5) -0.066(6) -0.003(5) O24 0.065(5) 0.097(6) 0.073(6) -0.009(5) -0.012(4) -0.051(5) O25 0.120(7) 0.080(6) 0.043(5) 0.025(4) -0.050(5) -0.051(5) O26 0.134(8) 0.166(8) 0.130(8) 0.052(7) -0.063(6) -0.078(7) O27 0.065(5) 0.040(4) 0.132(8) -0.019(5) 0.030(5) -0.014(4) O28 0.101(7) 0.073(6) 0.095(7) -0.042(5) 0.043(5) -0.056(5) N1 0.092(8) 0.047(6) 0.060(7) 0.007(5) -0.024(6) -0.015(5) N2 0.063(7) 0.039(6) 0.141(11) -0.013(6) 0.023(7) -0.024(5) N3 0.062(5) 0.045(5) 0.037(5) 0.007(4) -0.017(4) -0.013(4) N4 0.066(6) 0.046(5) 0.030(5) 0.003(4) -0.019(4) -0.003(4) N5 0.064(6) 0.029(4) 0.062(6) -0.002(4) 0.007(5) -0.019(4) N6 0.041(4) 0.046(5) 0.056(6) 0.003(4) -0.019(4) -0.019(4) N7 0.039(5) 0.060(6) 0.054(6) 0.012(4) -0.028(4) -0.014(4) C1 0.181(13) 0.187(13) 0.177(13) -0.028(9) -0.027(9) -0.068(9) C2 0.139(10) 0.133(10) 0.146(11) -0.007(8) -0.073(8) -0.006(8) C3 0.102(8) 0.095(8) 0.139(10) -0.005(7) -0.004(7) -0.049(7) C4 0.146(16) 0.115(14) 0.078(11) 0.023(10) -0.018(11) -0.047(13) C5 0.051(7) 0.085(9) 0.078(9) 0.011(7) -0.005(6) -0.010(7) C6 0.073(8) 0.072(8) 0.078(9) 0.011(7) -0.035(7) -0.023(7) C7 0.087(9) 0.058(7) 0.052(7) 0.012(6) -0.028(7) -0.011(6) C8 0.073(8) 0.062(8) 0.086(10) 0.024(7) -0.014(7) -0.023(7) C9 0.089(9) 0.045(7) 0.083(9) 0.006(6) -0.024(7) -0.038(6) C10 0.117(12) 0.106(12) 0.053(8) 0.028(8) -0.032(8) -0.051(10) C11 0.039(6) 0.094(10) 0.080(10) 0.026(8) -0.004(6) 0.012(6) C12 0.047(6) 0.060(7) 0.066(8) 0.002(6) -0.012(6) -0.019(6) C13 0.060(8) 0.033(7) 0.034(7) -0.009(6) -0.021(6) -0.022(6) C14 0.023(6) 0.036(7) 0.033(7) 0.004(6) 0.003(6) -0.001(6) N8 0.077(9) 0.089(9) 0.035(8) 0.011(7) -0.015(7) -0.018(8) C13A 0.014(7) 0.038(8) 0.043(9) -0.021(7) 0.003(7) 0.013(6) C14A 0.054(10) 0.069(11) 0.065(11) -0.016(10) 0.017(9) -0.022(9) N8A 0.074(9) 0.093(10) 0.060(9) 0.003(8) -0.011(8) -0.001(8) _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 O2 2.404(6) 2_576 ? Nd1 O8 2.475(7) . ? Nd1 O14 2.480(6) . ? Nd1 O15 2.496(6) . ? Nd1 O20 2.508(6) . ? Nd1 O4 2.511(7) . ? Nd1 O9 2.536(6) . ? Nd1 O7 2.537(6) . ? Nd1 O5 2.558(6) . ? Nd1 S6 3.109(3) . ? Nd1 S3 3.133(3) . ? Nd1 S1 3.143(3) . ? Nd2 O1 2.414(7) 2_665 ? Nd2 O27 2.445(8) . ? Nd2 O6 2.459(6) . ? Nd2 O12 2.480(6) . ? Nd2 O28 2.504(8) . ? Nd2 O10 2.508(6) . ? Nd2 O3 2.516(7) . ? Nd2 O18 2.518(6) . ? Nd2 O19 2.546(6) . ? Nd2 S7 3.104(3) . ? Nd2 S2 3.112(3) . ? Nd2 S4 3.125(3) . ? S1 O11 1.451(5) . ? S1 O2 1.452(6) . ? S1 O7 1.474(6) . ? S1 O5 1.490(6) . ? S2 O1 1.450(7) . ? S2 O13 1.462(6) . ? S2 O12 1.466(6) . ? S2 O10 1.481(6) . ? S3 O17 1.441(8) . ? S3 O4 1.460(7) . ? S3 O16 1.462(7) . ? S3 O8 1.493(7) . ? S4 O24 1.420(8) . ? S4 O26 1.426(12) . ? S4 O28 1.474(8) . ? S4 O27 1.475(9) . ? S5 O21 1.412(8) . ? S5 O22 1.455(7) . ? S5 O14 1.494(6) . ? S5 O9 1.500(7) . ? S6 O15 1.446(6) . ? S6 O18 1.452(6) . ? S6 O20 1.467(6) . ? S6 O19 1.476(6) . ? S7 O23 1.443(8) . ? S7 O25 1.444(7) . ? S7 O3 1.466(7) . ? S7 O6 1.478(8) . ? O1 Nd2 2.414(7) 2_665 ? O2 Nd1 2.404(6) 2_576 ? N1 C1 1.38(2) . ? N1 C2 1.403(19) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C3 1.478(16) . ? N2 C4 1.492(18) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? N3 C5 1.460(13) . ? N3 C6 1.495(14) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 C7 1.470(13) . ? N4 C8 1.476(14) . ? N4 H4D 0.9000 . ? N4 H4E 0.9000 . ? N5 C9 1.460(13) . ? N5 C10 1.478(15) . ? N5 H5D 0.9000 . ? N5 H5E 0.9000 . ? N6 C11 1.485(13) . ? N6 H6D 0.8900 . ? N6 H6E 0.8900 . ? N6 H6F 0.8900 . ? N7 C12 1.471(13) . ? N7 H7D 0.8900 . ? N7 H7E 0.8900 . ? N7 H7F 0.8900 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C11 1.39(2) 2_676 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C12 1.50(2) 2_565 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N8 1.50(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N8 1.09(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N8 H8D 0.9000 . ? N8 H8E 0.9000 . ? C13A N8A 1.49(3) . ? C13A H13D 0.9600 . ? C13A H13E 0.9600 . ? C13A H13F 0.9600 . ? C14A N8A 1.33(3) . ? C14A H14D 0.9600 . ? C14A H14E 0.9600 . ? C14A H14F 0.9600 . ? N8A H8AA 0.9000 . ? N8A H8AB 0.9000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O8 93.6(3) 2_576 . ? O2 Nd1 O14 80.4(2) 2_576 . ? O8 Nd1 O14 66.5(2) . . ? O2 Nd1 O15 151.2(2) 2_576 . ? O8 Nd1 O15 98.4(3) . . ? O14 Nd1 O15 128.4(2) . . ? O2 Nd1 O20 153.2(2) 2_576 . ? O8 Nd1 O20 83.1(3) . . ? O14 Nd1 O20 73.9(2) . . ? O15 Nd1 O20 54.89(19) . . ? O2 Nd1 O4 87.0(2) 2_576 . ? O8 Nd1 O4 55.0(2) . . ? O14 Nd1 O4 119.0(2) . . ? O15 Nd1 O4 78.8(2) . . ? O20 Nd1 O4 111.8(2) . . ? O2 Nd1 O9 84.8(2) 2_576 . ? O8 Nd1 O9 121.7(2) . . ? O14 Nd1 O9 55.71(19) . . ? O15 Nd1 O9 110.2(2) . . ? O20 Nd1 O9 74.7(2) . . ? O4 Nd1 O9 171.0(2) . . ? O2 Nd1 O7 89.3(2) 2_576 . ? O8 Nd1 O7 173.8(2) . . ? O14 Nd1 O7 119.40(19) . . ? O15 Nd1 O7 76.6(2) . . ? O20 Nd1 O7 96.7(2) . . ? O4 Nd1 O7 119.9(2) . . ? O9 Nd1 O7 63.99(19) . . ? O2 Nd1 O5 77.8(2) 2_576 . ? O8 Nd1 O5 119.9(2) . . ? O14 Nd1 O5 157.6(2) . . ? O15 Nd1 O5 73.5(2) . . ? O20 Nd1 O5 126.7(2) . . ? O4 Nd1 O5 65.1(2) . . ? O9 Nd1 O5 116.7(2) . . ? O7 Nd1 O5 55.51(19) . . ? O2 Nd1 S6 175.69(16) 2_576 . ? O8 Nd1 S6 90.7(2) . . ? O14 Nd1 S6 101.40(16) . . ? O15 Nd1 S6 27.17(14) . . ? O20 Nd1 S6 27.72(14) . . ? O4 Nd1 S6 95.45(18) . . ? O9 Nd1 S6 92.95(18) . . ? O7 Nd1 S6 86.36(14) . . ? O5 Nd1 S6 99.98(15) . . ? O2 Nd1 S3 92.28(18) 2_576 . ? O8 Nd1 S3 27.85(17) . . ? O14 Nd1 S3 93.64(15) . . ? O15 Nd1 S3 86.48(17) . . ? O20 Nd1 S3 96.65(18) . . ? O4 Nd1 S3 27.25(15) . . ? O9 Nd1 S3 149.30(15) . . ? O7 Nd1 S3 146.67(14) . . ? O5 Nd1 S3 92.36(15) . . ? S6 Nd1 S3 91.52(8) . . ? O2 Nd1 S1 83.07(15) 2_576 . ? O8 Nd1 S1 147.63(17) . . ? O14 Nd1 S1 143.10(14) . . ? O15 Nd1 S1 72.86(14) . . ? O20 Nd1 S1 113.47(16) . . ? O4 Nd1 S1 92.68(15) . . ? O9 Nd1 S1 90.20(14) . . ? O7 Nd1 S1 27.54(14) . . ? O5 Nd1 S1 27.97(14) . . ? S6 Nd1 S1 93.26(6) . . ? S3 Nd1 S1 119.86(7) . . ? O1 Nd2 O27 71.6(3) 2_665 . ? O1 Nd2 O6 81.1(2) 2_665 . ? O27 Nd2 O6 96.7(3) . . ? O1 Nd2 O12 81.3(2) 2_665 . ? O27 Nd2 O12 125.3(2) . . ? O6 Nd2 O12 125.3(2) . . ? O1 Nd2 O28 121.9(3) 2_665 . ? O27 Nd2 O28 55.0(3) . . ? O6 Nd2 O28 83.8(3) . . ? O12 Nd2 O28 147.3(3) . . ? O1 Nd2 O10 80.0(2) 2_665 . ? O27 Nd2 O10 73.2(3) . . ? O6 Nd2 O10 160.6(2) . . ? O12 Nd2 O10 55.6(2) . . ? O28 Nd2 O10 102.6(3) . . ? O1 Nd2 O3 77.9(2) 2_665 . ? O27 Nd2 O3 141.9(3) . . ? O6 Nd2 O3 55.7(2) . . ? O12 Nd2 O3 70.1(2) . . ? O28 Nd2 O3 133.1(3) . . ? O10 Nd2 O3 123.6(2) . . ? O1 Nd2 O18 150.3(2) 2_665 . ? O27 Nd2 O18 109.5(3) . . ? O6 Nd2 O18 126.9(2) . . ? O12 Nd2 O18 74.3(2) . . ? O28 Nd2 O18 75.7(3) . . ? O10 Nd2 O18 72.46(19) . . ? O3 Nd2 O18 108.4(2) . . ? O1 Nd2 O19 148.8(2) 2_665 . ? O27 Nd2 O19 126.8(3) . . ? O6 Nd2 O19 72.4(2) . . ? O12 Nd2 O19 100.6(2) . . ? O28 Nd2 O19 71.9(3) . . ? O10 Nd2 O19 126.9(2) . . ? O3 Nd2 O19 73.7(2) . . ? O18 Nd2 O19 54.78(19) . . ? O1 Nd2 S7 78.57(19) 2_665 . ? O27 Nd2 S7 121.0(3) . . ? O6 Nd2 S7 27.85(18) . . ? O12 Nd2 S7 97.72(15) . . ? O28 Nd2 S7 108.8(3) . . ? O10 Nd2 S7 148.01(15) . . ? O3 Nd2 S7 27.81(16) . . ? O18 Nd2 S7 120.77(16) . . ? O19 Nd2 S7 70.34(16) . . ? O1 Nd2 S2 79.61(16) 2_665 . ? O27 Nd2 S2 99.7(2) . . ? O6 Nd2 S2 149.20(17) . . ? O12 Nd2 S2 27.54(14) . . ? O28 Nd2 S2 126.9(3) . . ? O10 Nd2 S2 28.02(14) . . ? O3 Nd2 S2 96.72(16) . . ? O18 Nd2 S2 70.93(14) . . ? O19 Nd2 S2 116.00(16) . . ? S7 Nd2 S2 123.60(8) . . ? O1 Nd2 S4 97.34(19) 2_665 . ? O27 Nd2 S4 27.4(2) . . ? O6 Nd2 S4 91.69(19) . . ? O12 Nd2 S4 141.83(14) . . ? O28 Nd2 S4 27.63(18) . . ? O10 Nd2 S4 86.49(16) . . ? O3 Nd2 S4 147.32(16) . . ? O18 Nd2 S4 91.78(18) . . ? O19 Nd2 S4 99.57(19) . . ? S7 Nd2 S4 119.55(9) . . ? S2 Nd2 S4 114.40(8) . . ? O11 S1 O2 108.6(4) . . ? O11 S1 O7 109.9(4) . . ? O2 S1 O7 110.4(4) . . ? O11 S1 O5 110.8(4) . . ? O2 S1 O5 110.8(4) . . ? O7 S1 O5 106.3(3) . . ? O11 S1 Nd1 124.8(2) . . ? O2 S1 Nd1 126.6(3) . . ? O7 S1 Nd1 52.7(2) . . ? O5 S1 Nd1 53.6(2) . . ? O1 S2 O13 110.0(4) . . ? O1 S2 O12 110.1(4) . . ? O13 S2 O12 111.8(4) . . ? O1 S2 O10 110.4(4) . . ? O13 S2 O10 110.3(4) . . ? O12 S2 O10 104.2(4) . . ? O1 S2 Nd2 124.8(3) . . ? O13 S2 Nd2 125.2(3) . . ? O12 S2 Nd2 51.5(3) . . ? O10 S2 Nd2 52.7(2) . . ? O17 S3 O4 111.4(5) . . ? O17 S3 O16 109.6(4) . . ? O4 S3 O16 111.0(4) . . ? O17 S3 O8 112.2(5) . . ? O4 S3 O8 102.4(4) . . ? O16 S3 O8 110.2(5) . . ? O17 S3 Nd1 121.5(3) . . ? O4 S3 Nd1 51.9(3) . . ? O16 S3 Nd1 128.9(3) . . ? O8 S3 Nd1 50.8(3) . . ? O24 S4 O26 109.6(6) . . ? O24 S4 O28 113.6(5) . . ? O26 S4 O28 112.7(7) . . ? O24 S4 O27 110.0(5) . . ? O26 S4 O27 109.1(7) . . ? O28 S4 O27 101.5(4) . . ? O24 S4 Nd2 129.2(4) . . ? O26 S4 Nd2 120.9(5) . . ? O28 S4 Nd2 52.0(3) . . ? O27 S4 Nd2 49.7(3) . . ? O21 S5 O22 113.5(5) . . ? O21 S5 O14 111.4(5) . . ? O22 S5 O14 107.7(4) . . ? O21 S5 O9 109.5(5) . . ? O22 S5 O9 111.1(4) . . ? O14 S5 O9 103.1(3) . . ? O21 S5 Nd1 125.9(3) . . ? O22 S5 Nd1 120.6(3) . . ? O14 S5 Nd1 50.5(2) . . ? O9 S5 Nd1 52.7(2) . . ? O15 S6 O18 112.5(4) . . ? O15 S6 O20 104.7(3) . . ? O18 S6 O20 112.6(4) . . ? O15 S6 O19 110.9(4) . . ? O18 S6 O19 105.5(3) . . ? O20 S6 O19 110.7(4) . . ? O15 S6 Nd1 52.0(2) . . ? O18 S6 Nd1 128.4(3) . . ? O20 S6 Nd1 52.7(2) . . ? O19 S6 Nd1 126.1(3) . . ? O15 S6 Nd2 126.3(3) . . ? O18 S6 Nd2 52.1(2) . . ? O20 S6 Nd2 128.9(3) . . ? O19 S6 Nd2 53.4(2) . . ? Nd1 S6 Nd2 178.26(7) . . ? O23 S7 O25 112.2(5) . . ? O23 S7 O3 109.5(5) . . ? O25 S7 O3 111.4(5) . . ? O23 S7 O6 110.4(5) . . ? O25 S7 O6 108.9(5) . . ? O3 S7 O6 104.1(4) . . ? O23 S7 Nd2 122.7(4) . . ? O25 S7 Nd2 125.1(4) . . ? O3 S7 Nd2 53.2(3) . . ? O6 S7 Nd2 51.0(3) . . ? S2 O1 Nd2 155.5(4) . 2_665 ? S1 O2 Nd1 148.0(4) . 2_576 ? S7 O3 Nd2 99.0(4) . . ? S3 O4 Nd1 100.8(3) . . ? S1 O5 Nd1 98.4(3) . . ? S7 O6 Nd2 101.1(3) . . ? S1 O7 Nd1 99.7(3) . . ? S3 O8 Nd1 101.4(3) . . ? S5 O9 Nd1 99.3(3) . . ? S2 O10 Nd2 99.3(3) . . ? S2 O12 Nd2 101.0(3) . . ? S5 O14 Nd1 101.9(3) . . ? S6 O15 Nd1 100.8(3) . . ? S6 O18 Nd2 100.8(3) . . ? S6 O19 Nd2 98.9(3) . . ? S6 O20 Nd1 99.6(3) . . ? S4 O27 Nd2 102.9(4) . . ? S4 O28 Nd2 100.4(4) . . ? C1 N1 C2 121.7(15) . . ? C1 N1 H1D 106.9 . . ? C2 N1 H1D 106.9 . . ? C1 N1 H1E 106.9 . . ? C2 N1 H1E 106.9 . . ? H1D N1 H1E 106.7 . . ? C3 N2 C4 117.0(13) . . ? C3 N2 H2D 108.1 . . ? C4 N2 H2D 108.1 . . ? C3 N2 H2E 108.1 . . ? C4 N2 H2E 108.1 . . ? H2D N2 H2E 107.3 . . ? C5 N3 C6 112.1(9) . . ? C5 N3 H3D 109.2 . . ? C6 N3 H3D 109.2 . . ? C5 N3 H3E 109.2 . . ? C6 N3 H3E 109.2 . . ? H3D N3 H3E 107.9 . . ? C7 N4 C8 113.0(9) . . ? C7 N4 H4D 109.0 . . ? C8 N4 H4D 109.0 . . ? C7 N4 H4E 109.0 . . ? C8 N4 H4E 109.0 . . ? H4D N4 H4E 107.8 . . ? C9 N5 C10 115.5(9) . . ? C9 N5 H5D 108.4 . . ? C10 N5 H5D 108.4 . . ? C9 N5 H5E 108.4 . . ? C10 N5 H5E 108.4 . . ? H5D N5 H5E 107.5 . . ? C11 N6 H6D 109.5 . . ? C11 N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C11 N6 H6F 109.5 . . ? H6D N6 H6F 109.5 . . ? H6E N6 H6F 109.5 . . ? C12 N7 H7D 109.5 . . ? C12 N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? C12 N7 H7F 109.5 . . ? H7D N7 H7F 109.5 . . ? H7E N7 H7F 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C11 N6 113.5(12) 2_676 . ? C11 C11 H11A 108.9 2_676 . ? N6 C11 H11A 108.9 . . ? C11 C11 H11B 108.9 2_676 . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N7 C12 C12 111.8(11) . 2_565 ? N7 C12 H12A 109.2 . . ? C12 C12 H12A 109.2 2_565 . ? N7 C12 H12B 109.2 . . ? C12 C12 H12B 109.2 2_565 . ? H12A C12 H12B 107.9 . . ? N8 C13 H13A 109.5 . . ? N8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N8 C14 H14A 109.5 . . ? N8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C14 N8 C13 124(2) . . ? C14 N8 H8D 106.4 . . ? C13 N8 H8D 106.4 . . ? C14 N8 H8E 106.4 . . ? C13 N8 H8E 106.4 . . ? H8D N8 H8E 106.5 . . ? N8A C13A H13D 109.5 . . ? N8A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? N8A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? N8A C14A H14D 109.5 . . ? N8A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? N8A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C14A N8A C13A 110.6(19) . . ? C14A N8A H8AA 109.5 . . ? C13A N8A H8AA 109.5 . . ? C14A N8A H8AB 109.5 . . ? C13A N8A H8AB 109.5 . . ? H8AA N8A H8AB 108.1 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.975 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.182 data_zd-10 _database_code_depnum_ccdc_archive 'CCDC 875280' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C2H8N)3][Eu(SO4)3]' _chemical_formula_sum 'C6 H24 Eu N3 O12 S3' _chemical_formula_weight 578.42 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' Eu Eu -0.1578 3.6682 '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 9.6036(8) _cell_length_b 10.4490(9) _cell_length_c 10.5171(9) _cell_angle_alpha 72.1640(10) _cell_angle_beta 72.6600(10) _cell_angle_gamma 75.1900(10) _cell_volume 943.18(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5795 _cell_measurement_theta_min 2.249 _cell_measurement_theta_max 26.641 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 3.717 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.6056 _exptl_absorpt_correction_T_max 0.7075 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 6662 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3291 _reflns_number_gt 3222 _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^)+(0.0277P)^2^+1.5169P] 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 3291 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _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 1.232535(18) 0.059132(18) -0.085693(18) 0.01000(8) Uani 1 1 d . . . S1 S 1.02587(10) -0.04388(10) -0.19296(10) 0.0131(2) Uani 1 1 d . . . S2 S 1.46858(10) -0.18241(9) 0.01444(10) 0.0127(2) Uani 1 1 d . . . S3 S 1.25310(11) 0.29515(10) -0.33906(10) 0.0157(2) Uani 1 1 d . . . O1 O 1.1610(3) 0.2998(3) -0.1973(3) 0.0152(6) Uani 1 1 d . . . O2 O 1.4651(3) -0.1007(3) -0.1289(3) 0.0165(6) Uani 1 1 d . . . O3 O 0.9847(3) 0.0763(3) -0.1307(3) 0.0171(6) Uani 1 1 d . . . O4 O 1.1810(3) -0.1036(3) -0.1843(3) 0.0173(6) Uani 1 1 d . . . O5 O 1.3324(3) -0.1186(3) 0.1023(3) 0.0170(6) Uani 1 1 d . . . O6 O 1.3260(3) 0.1492(3) -0.3250(3) 0.0201(6) Uani 1 1 d . . . O7 O 1.6027(3) -0.1717(3) 0.0479(3) 0.0179(6) Uani 1 1 d . . . O8 O 0.9254(3) -0.1408(3) -0.1062(3) 0.0152(6) Uani 1 1 d . . . O9 O 1.4666(3) -0.3254(3) 0.0294(3) 0.0232(7) Uani 1 1 d . . . O10 O 1.0090(3) -0.0014(3) -0.3335(3) 0.0238(7) Uani 1 1 d . . . O11 O 1.1584(4) 0.3357(3) -0.4363(3) 0.0273(7) Uani 1 1 d . . . O12 O 1.3641(3) 0.3842(3) -0.3846(3) 0.0255(7) Uani 1 1 d . . . C1 C 0.7809(6) 0.3216(5) -0.4098(5) 0.0363(12) Uani 1 1 d . . . H1C H 0.8129 0.2380 -0.4390 0.055 Uiso 1 1 calc R . . H1D H 0.7977 0.3975 -0.4882 0.055 Uiso 1 1 calc R . . H1E H 0.6771 0.3313 -0.3656 0.055 Uiso 1 1 calc R . . C2 C 0.8226(5) 0.4391(5) -0.2562(5) 0.0304(10) Uani 1 1 d . . . H2C H 0.8781 0.4268 -0.1897 0.046 Uiso 1 1 calc R . . H2D H 0.7185 0.4510 -0.2129 0.046 Uiso 1 1 calc R . . H2E H 0.8431 0.5185 -0.3295 0.046 Uiso 1 1 calc R . . C3 C 0.7995(6) -0.5538(5) 0.1034(6) 0.0368(12) Uani 1 1 d . . . H3C H 0.8374 -0.4723 0.0488 0.055 Uiso 1 1 calc R . . H3D H 0.7931 -0.6048 0.0440 0.055 Uiso 1 1 calc R . . H3E H 0.8649 -0.6086 0.1611 0.055 Uiso 1 1 calc R . . C4 C 0.5833(5) -0.6357(5) 0.2796(5) 0.0280(10) Uani 1 1 d . . . H4A H 0.4891 -0.6051 0.3361 0.042 Uiso 1 1 calc R . . H4B H 0.6479 -0.6930 0.3371 0.042 Uiso 1 1 calc R . . H4C H 0.5694 -0.6867 0.2237 0.042 Uiso 1 1 calc R . . N1 N 0.8655(4) 0.3183(4) -0.3122(4) 0.0297(9) Uani 1 1 d . . . H1A H 0.8537 0.2437 -0.2418 0.036 Uiso 1 1 calc R . . H1B H 0.9625 0.3098 -0.3549 0.036 Uiso 1 1 calc R . . N2 N 0.6500(4) -0.5163(4) 0.1902(4) 0.0225(8) Uani 1 1 d . . . H2A H 0.6564 -0.4658 0.2432 0.027 Uiso 1 1 calc R . . H2B H 0.5897 -0.4642 0.1353 0.027 Uiso 1 1 calc R . . N3 N 0.7309(4) -0.0559(4) -0.3232(4) 0.0279(9) Uani 1 1 d . . . H3A H 0.6666 -0.0449 -0.2436 0.034 Uiso 1 1 calc R . . H3B H 0.8095 -0.0186 -0.3334 0.034 Uiso 1 1 calc R . . C6 C 0.7813(6) -0.2034(6) -0.3142(6) 0.0426(14) Uani 1 1 d . . . H6A H 0.8257 -0.2455 -0.2373 0.064 Uiso 1 1 calc R . . H6B H 0.8529 -0.2163 -0.3973 0.064 Uiso 1 1 calc R . . H6C H 0.6980 -0.2445 -0.3022 0.064 Uiso 1 1 calc R . . C5 C 0.6592(5) 0.0180(6) -0.4370(5) 0.0395(13) Uani 1 1 d . . . H5A H 0.6280 0.1127 -0.4361 0.059 Uiso 1 1 calc R . . H5B H 0.5745 -0.0204 -0.4266 0.059 Uiso 1 1 calc R . . H5C H 0.7283 0.0100 -0.5228 0.059 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 Eu1 0.00797(11) 0.00860(12) 0.01201(12) -0.00144(8) -0.00348(8) 0.00086(7) S1 0.0108(4) 0.0146(5) 0.0142(5) -0.0037(4) -0.0034(4) -0.0020(4) S2 0.0098(4) 0.0088(5) 0.0184(5) -0.0002(4) -0.0059(4) -0.0005(3) S3 0.0183(5) 0.0136(5) 0.0125(5) 0.0002(4) -0.0032(4) -0.0028(4) O1 0.0153(13) 0.0121(14) 0.0142(13) -0.0017(11) -0.0028(11) 0.0016(11) O2 0.0131(13) 0.0153(14) 0.0162(14) -0.0019(12) -0.0045(11) 0.0047(11) O3 0.0137(13) 0.0127(14) 0.0250(15) -0.0056(12) -0.0089(12) 0.0032(11) O4 0.0105(13) 0.0179(15) 0.0238(15) -0.0082(12) -0.0040(12) 0.0003(11) O5 0.0126(13) 0.0173(15) 0.0151(14) 0.0007(12) -0.0021(11) 0.0003(11) O6 0.0229(15) 0.0132(15) 0.0171(14) -0.0025(12) 0.0018(12) -0.0004(12) O7 0.0123(13) 0.0159(14) 0.0242(15) 0.0000(12) -0.0092(12) -0.0007(11) O8 0.0128(13) 0.0139(14) 0.0177(14) -0.0043(11) 0.0004(11) -0.0044(11) O9 0.0240(15) 0.0093(14) 0.0385(18) 0.0000(13) -0.0168(14) -0.0031(12) O10 0.0217(15) 0.0371(19) 0.0137(14) -0.0019(13) -0.0054(12) -0.0113(14) O11 0.0314(17) 0.0331(19) 0.0161(15) -0.0027(13) -0.0105(13) -0.0024(14) O12 0.0299(17) 0.0227(17) 0.0203(15) -0.0009(13) 0.0008(13) -0.0120(14) C1 0.040(3) 0.031(3) 0.036(3) 0.004(2) -0.019(2) -0.007(2) C2 0.026(2) 0.024(2) 0.030(3) 0.002(2) -0.002(2) -0.0017(19) C3 0.034(3) 0.032(3) 0.041(3) -0.012(2) -0.003(2) -0.002(2) C4 0.027(2) 0.025(2) 0.028(2) -0.007(2) -0.001(2) -0.0046(19) N1 0.030(2) 0.019(2) 0.030(2) 0.0094(17) -0.0136(18) 0.0014(16) N2 0.0241(19) 0.0168(19) 0.0261(19) -0.0064(16) -0.0114(16) 0.0046(15) N3 0.0219(19) 0.038(2) 0.027(2) -0.0137(18) -0.0033(16) -0.0071(17) C6 0.027(3) 0.049(3) 0.069(4) -0.043(3) -0.010(3) -0.002(2) C5 0.023(2) 0.070(4) 0.028(3) -0.015(3) -0.006(2) -0.007(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 Eu1 O7 2.378(3) 2_855 ? Eu1 O6 2.379(3) . ? Eu1 O8 2.381(3) 2_755 ? Eu1 O2 2.437(3) . ? Eu1 O1 2.442(3) . ? Eu1 O4 2.455(3) . ? Eu1 O5 2.500(3) . ? Eu1 O3 2.515(3) . ? Eu1 O3 2.870(3) 2_755 ? Eu1 S3 3.0218(10) . ? Eu1 S2 3.0802(9) . ? Eu1 S1 3.0889(9) . ? S1 O10 1.454(3) . ? S1 O4 1.479(3) . ? S1 O8 1.482(3) . ? S1 O3 1.503(3) . ? S1 Eu1 3.2177(10) 2_755 ? S2 O9 1.458(3) . ? S2 O7 1.471(3) . ? S2 O5 1.490(3) . ? S2 O2 1.493(3) . ? S3 O11 1.464(3) . ? S3 O12 1.470(3) . ? S3 O6 1.488(3) . ? S3 O1 1.498(3) . ? O3 Eu1 2.870(3) 2_755 ? O7 Eu1 2.378(3) 2_855 ? O8 Eu1 2.381(3) 2_755 ? C1 N1 1.475(6) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 N1 1.467(6) . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 N2 1.483(6) . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C3 H3E 0.9600 . ? C4 N2 1.478(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.468(6) . ? N3 C6 1.475(7) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Eu1 O6 86.91(10) 2_855 . ? O7 Eu1 O8 80.89(9) 2_855 2_755 ? O6 Eu1 O8 137.93(9) . 2_755 ? O7 Eu1 O2 79.36(9) 2_855 . ? O6 Eu1 O2 79.17(9) . . ? O8 Eu1 O2 136.33(9) 2_755 . ? O7 Eu1 O1 75.42(9) 2_855 . ? O6 Eu1 O1 58.44(9) . . ? O8 Eu1 O1 79.51(9) 2_755 . ? O2 Eu1 O1 131.09(9) . . ? O7 Eu1 O4 152.07(9) 2_855 . ? O6 Eu1 O4 78.52(10) . . ? O8 Eu1 O4 125.47(9) 2_755 . ? O2 Eu1 O4 74.60(9) . . ? O1 Eu1 O4 115.05(9) . . ? O7 Eu1 O5 78.46(9) 2_855 . ? O6 Eu1 O5 135.57(9) . . ? O8 Eu1 O5 81.00(9) 2_755 . ? O2 Eu1 O5 57.07(9) . . ? O1 Eu1 O5 149.47(9) . . ? O4 Eu1 O5 95.40(9) . . ? O7 Eu1 O3 147.42(9) 2_855 . ? O6 Eu1 O3 89.28(10) . . ? O8 Eu1 O3 80.48(9) 2_755 . ? O2 Eu1 O3 131.49(9) . . ? O1 Eu1 O3 75.07(9) . . ? O4 Eu1 O3 56.92(8) . . ? O5 Eu1 O3 124.26(9) . . ? O7 Eu1 O3 123.69(9) 2_855 2_755 ? O6 Eu1 O3 148.74(9) . 2_755 ? O8 Eu1 O3 53.36(8) 2_755 2_755 ? O2 Eu1 O3 110.20(8) . 2_755 ? O1 Eu1 O3 118.69(8) . 2_755 ? O4 Eu1 O3 75.72(9) . 2_755 ? O5 Eu1 O3 64.94(8) . 2_755 ? O3 Eu1 O3 61.80(10) . 2_755 ? O7 Eu1 S3 79.44(7) 2_855 . ? O6 Eu1 S3 28.99(7) . . ? O8 Eu1 S3 108.93(7) 2_755 . ? O2 Eu1 S3 105.16(7) . . ? O1 Eu1 S3 29.45(6) . . ? O4 Eu1 S3 97.65(7) . . ? O5 Eu1 S3 153.91(6) . . ? O3 Eu1 S3 81.67(7) . . ? O3 Eu1 S3 140.45(5) 2_755 . ? O7 Eu1 S2 77.90(7) 2_855 . ? O6 Eu1 S2 107.43(7) . . ? O8 Eu1 S2 109.03(7) 2_755 . ? O2 Eu1 S2 28.46(7) . . ? O1 Eu1 S2 150.25(6) . . ? O4 Eu1 S2 83.87(6) . . ? O5 Eu1 S2 28.62(6) . . ? O3 Eu1 S2 133.70(6) . . ? O3 Eu1 S2 87.19(5) 2_755 . ? S3 Eu1 S2 131.47(3) . . ? O7 Eu1 S1 168.18(7) 2_855 . ? O6 Eu1 S1 82.09(7) . . ? O8 Eu1 S1 104.52(6) 2_755 . ? O2 Eu1 S1 102.63(7) . . ? O1 Eu1 S1 95.04(6) . . ? O4 Eu1 S1 28.09(6) . . ? O5 Eu1 S1 112.53(7) . . ? O3 Eu1 S1 28.86(6) . . ? O3 Eu1 S1 66.87(6) 2_755 . ? S3 Eu1 S1 88.83(3) . . ? S2 Eu1 S1 109.49(3) . . ? O10 S1 O4 112.52(17) . . ? O10 S1 O8 110.25(16) . . ? O4 S1 O8 110.79(16) . . ? O10 S1 O3 110.96(18) . . ? O4 S1 O3 105.18(15) . . ? O8 S1 O3 106.88(16) . . ? O10 S1 Eu1 125.31(13) . . ? O4 S1 Eu1 51.40(11) . . ? O8 S1 Eu1 124.41(11) . . ? O3 S1 Eu1 53.85(10) . . ? O10 S1 Eu1 127.59(13) . 2_755 ? O4 S1 Eu1 119.27(12) . 2_755 ? O8 S1 Eu1 43.82(11) . 2_755 ? O3 S1 Eu1 63.12(11) . 2_755 ? Eu1 S1 Eu1 94.29(3) . 2_755 ? O9 S2 O7 109.80(16) . . ? O9 S2 O5 111.25(17) . . ? O7 S2 O5 110.88(16) . . ? O9 S2 O2 110.58(17) . . ? O7 S2 O2 109.67(16) . . ? O5 S2 O2 104.56(15) . . ? O9 S2 Eu1 124.40(12) . . ? O7 S2 Eu1 125.75(12) . . ? O5 S2 Eu1 53.50(10) . . ? O2 S2 Eu1 51.08(10) . . ? O11 S3 O12 109.96(19) . . ? O11 S3 O6 110.44(18) . . ? O12 S3 O6 110.88(18) . . ? O11 S3 O1 110.34(17) . . ? O12 S3 O1 111.04(17) . . ? O6 S3 O1 104.05(16) . . ? O11 S3 Eu1 125.71(14) . . ? O12 S3 Eu1 124.31(13) . . ? O6 S3 Eu1 50.78(11) . . ? O1 S3 Eu1 53.29(10) . . ? S3 O1 Eu1 97.26(13) . . ? S2 O2 Eu1 100.46(14) . . ? S1 O3 Eu1 97.29(13) . . ? S1 O3 Eu1 89.04(12) . 2_755 ? Eu1 O3 Eu1 118.20(10) . 2_755 ? S1 O4 Eu1 100.52(14) . . ? S2 O5 Eu1 97.88(13) . . ? S3 O6 Eu1 100.23(14) . . ? S2 O7 Eu1 156.23(17) . 2_855 ? S1 O8 Eu1 110.64(14) . 2_755 ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 H2C 109.5 . . ? N1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? N1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N2 C3 H3C 109.5 . . ? N2 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N2 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 N1 C1 114.5(4) . . ? C2 N1 H1A 108.6 . . ? C1 N1 H1A 108.6 . . ? C2 N1 H1B 108.6 . . ? C1 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C4 N2 C3 113.4(4) . . ? C4 N2 H2A 108.9 . . ? C3 N2 H2A 108.9 . . ? C4 N2 H2B 108.9 . . ? C3 N2 H2B 108.9 . . ? H2A N2 H2B 107.7 . . ? C5 N3 C6 113.8(4) . . ? C5 N3 H3A 108.8 . . ? C6 N3 H3A 108.8 . . ? C5 N3 H3B 108.8 . . ? C6 N3 H3B 108.8 . . ? H3A N3 H3B 107.7 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.718 _refine_diff_density_min -1.522 _refine_diff_density_rms 0.175 data_zd-11 _database_code_depnum_ccdc_archive 'CCDC 875281' #TrackingRef '3a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C2H8N)2(C2H10N2)0.5][Eu(SO4)3]' _chemical_formula_sum 'C5 H21 Eu N3 O12 S3' _chemical_formula_weight 563.39 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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.9333(9) _cell_length_b 10.2837(9) _cell_length_c 31.318(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3521.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5041 _cell_measurement_theta_min 2.271 _cell_measurement_theta_max 26.625 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 3.979 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.6467 _exptl_absorpt_correction_T_max 0.6917 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 24038 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3275 _reflns_number_gt 2821 _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^)+(0.0426P)^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 3275 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.003 _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 1.40112(2) 0.48224(2) 0.584931(7) 0.01553(10) Uani 1 1 d . . . S1 S 1.24740(10) 0.72831(10) 0.58470(4) 0.0190(3) Uani 1 1 d . . . S2 S 1.48407(12) 0.47194(12) 0.67864(4) 0.0281(3) Uani 1 1 d . . . S3 S 1.64411(10) 0.45307(10) 0.53628(4) 0.0174(2) Uani 1 1 d . . . O1 O 1.5912(3) 0.5735(3) 0.55459(10) 0.0219(7) Uani 1 1 d . . . O2 O 1.6498(3) 0.4587(3) 0.49004(10) 0.0267(8) Uani 1 1 d . . . O3 O 1.3833(3) 0.7200(3) 0.58420(10) 0.0223(8) Uani 1 1 d . . . O4 O 1.2026(3) 0.5930(3) 0.58651(10) 0.0253(8) Uani 1 1 d . . . O5 O 1.2038(3) 0.8043(3) 0.62135(10) 0.0274(8) Uani 1 1 d . . . O6 O 1.5590(3) 0.3463(3) 0.54980(10) 0.0210(7) Uani 1 1 d . . . O7 O 1.3771(3) 0.5454(3) 0.66030(11) 0.0337(9) Uani 1 1 d . . . O8 O 1.2027(3) 0.7978(3) 0.54678(10) 0.0242(7) Uani 1 1 d . . . O9 O 1.7653(3) 0.4316(3) 0.55478(10) 0.0278(8) Uani 1 1 d . . . O10 O 1.4425(3) 0.3620(3) 0.70395(11) 0.0367(9) Uani 1 1 d . . . O11 O 1.5474(3) 0.4267(4) 0.63907(11) 0.0390(9) Uani 1 1 d . . . O12 O 1.5604(4) 0.5580(4) 0.70338(13) 0.0586(13) Uani 1 1 d . . . N3 N 1.4718(4) 0.1739(3) 0.48381(12) 0.0238(9) Uani 1 1 d . . . H3D H 1.5188 0.2276 0.4687 0.036 Uiso 1 1 calc R . . H3E H 1.4591 0.2074 0.5096 0.036 Uiso 1 1 calc R . . H3F H 1.4005 0.1634 0.4706 0.036 Uiso 1 1 calc R . . N1 N 1.1983(4) 0.2722(4) 0.70506(13) 0.0333(10) Uani 1 1 d . . . H1D H 1.1832 0.2034 0.6881 0.040 Uiso 1 1 calc R . . H1E H 1.2721 0.3042 0.6978 0.040 Uiso 1 1 calc R . . N2 N 1.2005(5) 0.3196(5) 0.38849(16) 0.0586(16) Uani 1 1 d . . . H2D H 1.2367 0.3787 0.4055 0.070 Uiso 1 1 calc R . . H2E H 1.1636 0.2607 0.4054 0.070 Uiso 1 1 calc R . . C5 C 1.5335(6) 0.0467(5) 0.4880(2) 0.0526(18) Uani 1 1 d . . . H5A H 1.5482 0.0119 0.4597 0.063 Uiso 1 1 calc R . . H5B H 1.6123 0.0598 0.5015 0.063 Uiso 1 1 calc R . . C4 C 1.2959(6) 0.2529(6) 0.3631(2) 0.0545(17) Uani 1 1 d . . . H4A H 1.3542 0.2133 0.3820 0.082 Uiso 1 1 calc R . . H4B H 1.3368 0.3150 0.3452 0.082 Uiso 1 1 calc R . . H4C H 1.2587 0.1872 0.3457 0.082 Uiso 1 1 calc R . . C2 C 1.2024(7) 0.2286(7) 0.74938(19) 0.0616(18) Uani 1 1 d . . . H2A H 1.2650 0.1639 0.7525 0.092 Uiso 1 1 calc R . . H2B H 1.1247 0.1919 0.7571 0.092 Uiso 1 1 calc R . . H2C H 1.2200 0.3011 0.7676 0.092 Uiso 1 1 calc R . . C3 C 1.1056(7) 0.3863(7) 0.3624(2) 0.066(2) Uani 1 1 d . . . H3A H 1.0467 0.4263 0.3810 0.099 Uiso 1 1 calc R . . H3B H 1.0653 0.3240 0.3445 0.099 Uiso 1 1 calc R . . H3C H 1.1435 0.4518 0.3450 0.099 Uiso 1 1 calc R . . C1 C 1.1039(5) 0.3735(6) 0.6971(2) 0.0543(18) Uani 1 1 d . . . H1A H 1.1069 0.3996 0.6676 0.081 Uiso 1 1 calc R . . H1B H 1.1194 0.4474 0.7150 0.081 Uiso 1 1 calc R . . H1C H 1.0244 0.3388 0.7034 0.081 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 Eu1 0.01448(16) 0.01490(14) 0.01723(16) 0.00081(8) 0.00073(9) 0.00012(8) S1 0.0186(6) 0.0184(5) 0.0201(6) 0.0000(4) -0.0002(5) 0.0044(4) S2 0.0308(8) 0.0326(6) 0.0208(7) 0.0045(5) -0.0071(6) -0.0083(5) S3 0.0144(6) 0.0199(5) 0.0179(6) 0.0019(4) 0.0006(5) 0.0004(4) O1 0.0199(19) 0.0206(16) 0.0254(19) 0.0006(14) 0.0044(14) -0.0003(13) O2 0.030(2) 0.0348(18) 0.0150(18) 0.0031(14) 0.0026(15) 0.0034(16) O3 0.0146(18) 0.0191(17) 0.033(2) 0.0046(13) -0.0038(15) 0.0023(12) O4 0.0180(18) 0.0202(16) 0.038(2) 0.0017(13) 0.0042(15) 0.0008(13) O5 0.035(2) 0.0276(17) 0.0200(19) -0.0020(13) 0.0006(16) 0.0094(15) O6 0.0196(17) 0.0194(15) 0.0241(18) -0.0005(13) 0.0041(15) -0.0013(13) O7 0.049(2) 0.0303(19) 0.022(2) -0.0040(15) -0.0053(17) 0.0138(16) O8 0.0257(19) 0.0281(16) 0.0188(18) 0.0033(13) -0.0016(15) 0.0108(14) O9 0.0127(18) 0.0397(19) 0.031(2) 0.0009(16) -0.0037(15) 0.0030(14) O10 0.041(2) 0.042(2) 0.027(2) 0.0131(16) -0.0106(18) -0.0106(18) O11 0.028(2) 0.063(3) 0.027(2) 0.0059(18) -0.0002(17) 0.0076(19) O12 0.077(3) 0.061(3) 0.038(3) 0.007(2) -0.025(2) -0.037(3) N3 0.028(2) 0.0186(18) 0.025(2) 0.0023(16) -0.0019(18) -0.0012(16) N1 0.033(3) 0.037(2) 0.030(3) -0.0070(19) 0.002(2) -0.006(2) N2 0.094(5) 0.046(3) 0.036(3) 0.007(2) -0.008(3) -0.033(3) C5 0.033(4) 0.036(3) 0.089(5) 0.019(3) -0.012(4) 0.004(3) C4 0.050(4) 0.071(4) 0.042(4) 0.004(3) 0.002(3) -0.018(3) C2 0.064(5) 0.092(5) 0.029(4) 0.006(3) -0.001(3) 0.004(4) C3 0.099(6) 0.043(4) 0.057(5) 0.004(3) -0.011(4) 0.001(4) C1 0.053(4) 0.058(4) 0.052(4) 0.001(3) 0.008(3) 0.016(3) _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 O11 2.400(3) . ? Eu1 O5 2.443(3) 8_855 ? Eu1 O4 2.452(3) . ? Eu1 O3 2.453(3) . ? Eu1 O7 2.462(3) . ? Eu1 O1 2.470(3) . ? Eu1 O6 2.478(3) . ? Eu1 O2 2.488(3) 5_866 ? Eu1 O8 2.513(3) 8_855 ? Eu1 S1 3.0378(11) . ? Eu1 S2 3.0735(13) . ? Eu1 S1 3.0751(11) 8_855 ? S1 O5 1.468(3) . ? S1 O8 1.470(3) . ? S1 O4 1.476(3) . ? S1 O3 1.488(3) . ? S1 Eu1 3.0751(11) 8_865 ? S2 O12 1.442(4) . ? S2 O10 1.453(3) . ? S2 O11 1.494(4) . ? S2 O7 1.506(4) . ? S3 O2 1.451(3) . ? S3 O9 1.462(3) . ? S3 O1 1.483(3) . ? S3 O6 1.500(3) . ? O2 Eu1 2.488(3) 5_866 ? O5 Eu1 2.443(3) 8_865 ? O8 Eu1 2.513(3) 8_865 ? N3 C5 1.478(6) . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N3 H3F 0.8900 . ? N1 C2 1.460(7) . ? N1 C1 1.487(7) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C4 1.480(8) . ? N2 C3 1.488(8) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? C5 C5 1.422(11) 5_856 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 O11 Eu1 O5 78.75(12) . 8_855 ? O11 Eu1 O4 133.35(12) . . ? O5 Eu1 O4 85.57(11) 8_855 . ? O11 Eu1 O3 107.27(12) . . ? O5 Eu1 O3 135.54(10) 8_855 . ? O4 Eu1 O3 57.77(10) . . ? O11 Eu1 O7 57.09(12) . . ? O5 Eu1 O7 72.52(11) 8_855 . ? O4 Eu1 O7 76.33(11) . . ? O3 Eu1 O7 74.78(11) . . ? O11 Eu1 O1 78.56(12) . . ? O5 Eu1 O1 149.26(11) 8_855 . ? O4 Eu1 O1 125.16(10) . . ? O3 Eu1 O1 71.60(10) . . ? O7 Eu1 O1 111.00(12) . . ? O11 Eu1 O6 73.45(11) . . ? O5 Eu1 O6 96.44(10) 8_855 . ? O4 Eu1 O6 152.55(10) . . ? O3 Eu1 O6 127.82(10) . . ? O7 Eu1 O6 130.44(11) . . ? O1 Eu1 O6 57.16(10) . . ? O11 Eu1 O2 150.92(12) . 5_866 ? O5 Eu1 O2 121.22(11) 8_855 5_866 ? O4 Eu1 O2 72.98(11) . 5_866 ? O3 Eu1 O2 74.34(10) . 5_866 ? O7 Eu1 O2 144.71(11) . 5_866 ? O1 Eu1 O2 74.49(11) . 5_866 ? O6 Eu1 O2 82.80(11) . 5_866 ? O11 Eu1 O8 117.21(12) . 8_855 ? O5 Eu1 O8 56.24(10) 8_855 8_855 ? O4 Eu1 O8 87.73(10) . 8_855 ? O3 Eu1 O8 135.41(10) . 8_855 ? O7 Eu1 O8 127.35(11) . 8_855 ? O1 Eu1 O8 118.94(10) . 8_855 ? O6 Eu1 O8 71.21(10) . 8_855 ? O2 Eu1 O8 68.56(10) 5_866 8_855 ? O11 Eu1 S1 124.67(9) . . ? O5 Eu1 S1 111.42(8) 8_855 . ? O4 Eu1 S1 28.74(7) . . ? O3 Eu1 S1 29.04(7) . . ? O7 Eu1 S1 73.95(8) . . ? O1 Eu1 S1 98.51(7) . . ? O6 Eu1 S1 148.64(7) . . ? O2 Eu1 S1 70.76(8) 5_866 . ? O8 Eu1 S1 112.19(8) 8_855 . ? O11 Eu1 S2 28.43(9) . . ? O5 Eu1 S2 70.54(8) 8_855 . ? O4 Eu1 S2 104.95(8) . . ? O3 Eu1 S2 93.82(8) . . ? O7 Eu1 S2 28.98(8) . . ? O1 Eu1 S2 97.60(8) . . ? O6 Eu1 S2 101.48(8) . . ? O2 Eu1 S2 167.27(8) 5_866 . ? O8 Eu1 S2 124.15(7) 8_855 . ? S1 Eu1 S2 101.20(3) . . ? O11 Eu1 S1 98.71(10) . 8_855 ? O5 Eu1 S1 27.98(7) 8_855 8_855 ? O4 Eu1 S1 85.82(7) . 8_855 ? O3 Eu1 S1 143.56(7) . 8_855 ? O7 Eu1 S1 99.78(9) . 8_855 ? O1 Eu1 S1 140.00(8) . 8_855 ? O6 Eu1 S1 83.56(7) . 8_855 ? O2 Eu1 S1 94.98(8) 5_866 8_855 ? O8 Eu1 S1 28.27(7) 8_855 8_855 ? S1 Eu1 S1 114.533(9) . 8_855 ? S2 Eu1 S1 97.40(3) . 8_855 ? O5 S1 O8 105.38(19) . . ? O5 S1 O4 111.35(19) . . ? O8 S1 O4 112.26(19) . . ? O5 S1 O3 111.26(19) . . ? O8 S1 O3 110.57(19) . . ? O4 S1 O3 106.13(19) . . ? O5 S1 Eu1 128.40(13) . . ? O8 S1 Eu1 126.22(13) . . ? O4 S1 Eu1 53.01(13) . . ? O3 S1 Eu1 53.13(13) . . ? O5 S1 Eu1 51.30(13) . 8_865 ? O8 S1 Eu1 54.09(12) . 8_865 ? O4 S1 Eu1 128.69(14) . 8_865 ? O3 S1 Eu1 125.16(14) . 8_865 ? Eu1 S1 Eu1 178.26(4) . 8_865 ? O12 S2 O10 111.4(2) . . ? O12 S2 O11 111.6(3) . . ? O10 S2 O11 110.8(2) . . ? O12 S2 O7 110.3(3) . . ? O10 S2 O7 110.8(2) . . ? O11 S2 O7 101.5(2) . . ? O12 S2 Eu1 131.50(18) . . ? O10 S2 Eu1 117.09(15) . . ? O11 S2 Eu1 49.87(14) . . ? O7 S2 Eu1 52.38(14) . . ? O2 S3 O9 111.3(2) . . ? O2 S3 O1 111.69(19) . . ? O9 S3 O1 109.05(19) . . ? O2 S3 O6 109.74(19) . . ? O9 S3 O6 109.87(19) . . ? O1 S3 O6 105.06(18) . . ? O2 S3 Eu1 121.84(15) . . ? O9 S3 Eu1 126.90(14) . . ? O1 S3 Eu1 52.41(12) . . ? O6 S3 Eu1 52.84(12) . . ? S3 O1 Eu1 99.19(15) . . ? S3 O2 Eu1 160.4(2) . 5_866 ? S1 O3 Eu1 97.83(16) . . ? S1 O4 Eu1 98.24(16) . . ? S1 O5 Eu1 100.72(16) . 8_865 ? S3 O6 Eu1 98.33(14) . . ? S2 O7 Eu1 98.64(17) . . ? S1 O8 Eu1 97.64(15) . 8_865 ? S2 O11 Eu1 101.70(18) . . ? C5 N3 H3D 109.5 . . ? C5 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C5 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? C2 N1 C1 113.4(5) . . ? C2 N1 H1D 108.9 . . ? C1 N1 H1D 108.9 . . ? C2 N1 H1E 108.9 . . ? C1 N1 H1E 108.9 . . ? H1D N1 H1E 107.7 . . ? C4 N2 C3 114.3(5) . . ? C4 N2 H2D 108.7 . . ? C3 N2 H2D 108.7 . . ? C4 N2 H2E 108.7 . . ? C3 N2 H2E 108.7 . . ? H2D N2 H2E 107.6 . . ? C5 C5 N3 114.2(7) 5_856 . ? C5 C5 H5A 108.7 5_856 . ? N3 C5 H5A 108.7 . . ? C5 C5 H5B 108.7 5_856 . ? N3 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.974 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.117 data_zd-8 _database_code_depnum_ccdc_archive 'CCDC 875282' #TrackingRef '3b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C2H8N)2(C2H10N2)0.5][Gd(SO4)3]' _chemical_formula_sum 'C5 H21 Gd N3 O12 S3' _chemical_formula_weight 568.68 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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.9321(17) _cell_length_b 10.2720(16) _cell_length_c 31.325(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3517.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2724 _cell_measurement_theta_min 2.269 _cell_measurement_theta_max 25.304 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 4.188 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.5917 _exptl_absorpt_correction_T_max 0.6795 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 15969 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3258 _reflns_number_gt 2555 _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^)+(0.0326P)^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 3258 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.004 _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 1.40036(2) 0.48291(2) 0.584457(8) 0.01723(9) Uani 1 1 d . . . S1 S 1.24786(11) 0.72906(11) 0.58419(4) 0.0206(3) Uani 1 1 d . . . S2 S 1.48289(13) 0.47361(13) 0.67803(5) 0.0311(3) Uani 1 1 d . . . S3 S 1.64295(11) 0.45289(11) 0.53623(4) 0.0192(3) Uani 1 1 d . . . O1 O 1.5898(3) 0.5734(3) 0.55467(11) 0.0243(8) Uani 1 1 d . . . O2 O 1.6488(3) 0.4579(3) 0.49019(11) 0.0284(8) Uani 1 1 d . . . O3 O 1.3830(3) 0.7194(3) 0.58429(11) 0.0240(8) Uani 1 1 d . . . O4 O 1.2036(3) 0.5939(3) 0.58601(11) 0.0259(8) Uani 1 1 d . . . O5 O 1.2039(3) 0.8050(3) 0.62091(11) 0.0285(9) Uani 1 1 d . . . O6 O 1.5574(3) 0.3462(3) 0.54988(11) 0.0242(8) Uani 1 1 d . . . O7 O 1.3748(4) 0.5452(3) 0.66004(12) 0.0371(10) Uani 1 1 d . . . O8 O 1.2041(3) 0.7992(3) 0.54613(11) 0.0266(8) Uani 1 1 d . . . O9 O 1.7637(3) 0.4306(3) 0.55443(11) 0.0302(9) Uani 1 1 d . . . O10 O 1.4422(4) 0.3632(4) 0.70301(13) 0.0411(10) Uani 1 1 d . . . O11 O 1.5458(4) 0.4289(4) 0.63856(12) 0.0429(10) Uani 1 1 d . . . O12 O 1.5584(4) 0.5607(4) 0.70277(14) 0.0627(14) Uani 1 1 d . . . N3 N 1.4702(4) 0.1735(4) 0.48377(14) 0.0271(10) Uani 1 1 d . . . H3D H 1.5172 0.2272 0.4686 0.041 Uiso 1 1 calc R . . H3E H 1.4558 0.2082 0.5093 0.041 Uiso 1 1 calc R . . H3F H 1.3997 0.1612 0.4702 0.041 Uiso 1 1 calc R . . N1 N 1.1971(4) 0.2737(4) 0.70465(15) 0.0399(12) Uani 1 1 d . . . H1D H 1.1815 0.2043 0.6880 0.048 Uiso 1 1 calc R . . H1E H 1.2706 0.3055 0.6970 0.048 Uiso 1 1 calc R . . N2 N 1.1992(6) 0.3198(5) 0.38833(19) 0.0681(19) Uani 1 1 d . . . H2D H 1.2351 0.3787 0.4055 0.082 Uiso 1 1 calc R . . H2E H 1.1629 0.2601 0.4052 0.082 Uiso 1 1 calc R . . C5 C 1.5327(6) 0.0486(5) 0.4890(3) 0.056(2) Uani 1 1 d . . . H5A H 1.5531 0.0155 0.4609 0.068 Uiso 1 1 calc R . . H5B H 1.6090 0.0638 0.5040 0.068 Uiso 1 1 calc R . . C4 C 1.2938(6) 0.2551(7) 0.3636(2) 0.067(2) Uani 1 1 d . . . H4A H 1.3519 0.2156 0.3825 0.100 Uiso 1 1 calc R . . H4B H 1.3347 0.3178 0.3459 0.100 Uiso 1 1 calc R . . H4C H 1.2573 0.1893 0.3459 0.100 Uiso 1 1 calc R . . C2 C 1.2035(7) 0.2303(8) 0.7490(2) 0.077(2) Uani 1 1 d . . . H2A H 1.2665 0.1657 0.7519 0.116 Uiso 1 1 calc R . . H2B H 1.1263 0.1936 0.7573 0.116 Uiso 1 1 calc R . . H2C H 1.2221 0.3032 0.7671 0.116 Uiso 1 1 calc R . . C3 C 1.1045(7) 0.3858(7) 0.3636(3) 0.080(3) Uani 1 1 d . . . H3A H 1.0465 0.4251 0.3827 0.120 Uiso 1 1 calc R . . H3B H 1.0634 0.3238 0.3457 0.120 Uiso 1 1 calc R . . H3C H 1.1413 0.4519 0.3462 0.120 Uiso 1 1 calc R . . C1 C 1.1036(6) 0.3736(7) 0.6965(3) 0.066(2) Uani 1 1 d . . . H1A H 1.1070 0.3994 0.6670 0.099 Uiso 1 1 calc R . . H1B H 1.1188 0.4479 0.7143 0.099 Uiso 1 1 calc R . . H1C H 1.0241 0.3388 0.7027 0.099 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 Gd1 0.01618(15) 0.01636(13) 0.01913(15) 0.00073(10) 0.00069(11) 0.00029(9) S1 0.0199(7) 0.0191(6) 0.0227(7) 0.0004(5) 0.0017(6) 0.0049(5) S2 0.0339(9) 0.0366(7) 0.0228(8) 0.0065(6) -0.0085(6) -0.0099(6) S3 0.0162(7) 0.0213(6) 0.0202(7) 0.0017(5) 0.0017(5) 0.0009(5) O1 0.023(2) 0.0196(16) 0.030(2) -0.0002(15) 0.0069(17) 0.0000(14) O2 0.030(2) 0.036(2) 0.019(2) 0.0040(16) 0.0024(17) 0.0006(17) O3 0.018(2) 0.0196(17) 0.034(2) -0.0006(15) -0.0022(17) 0.0012(13) O4 0.024(2) 0.0195(17) 0.034(2) 0.0005(15) 0.0028(17) 0.0015(14) O5 0.035(2) 0.0269(18) 0.024(2) -0.0012(15) 0.0042(18) 0.0111(16) O6 0.023(2) 0.0215(17) 0.028(2) 0.0022(15) 0.0059(17) -0.0034(14) O7 0.054(3) 0.035(2) 0.022(2) -0.0082(17) -0.0072(19) 0.0127(18) O8 0.032(2) 0.0265(18) 0.021(2) 0.0028(15) -0.0013(17) 0.0104(16) O9 0.015(2) 0.043(2) 0.033(2) 0.0038(18) -0.0054(17) 0.0034(16) O10 0.043(3) 0.047(2) 0.033(2) 0.0164(19) -0.010(2) -0.0150(19) O11 0.031(2) 0.070(3) 0.028(2) 0.004(2) -0.0043(19) 0.009(2) O12 0.081(4) 0.073(3) 0.034(3) 0.005(2) -0.021(3) -0.043(3) N3 0.032(3) 0.021(2) 0.028(3) -0.0001(18) -0.003(2) -0.0014(19) N1 0.042(3) 0.052(3) 0.026(3) -0.006(2) 0.005(2) -0.010(2) N2 0.107(6) 0.052(3) 0.046(4) 0.001(3) -0.002(4) -0.033(4) C5 0.032(4) 0.035(4) 0.102(6) 0.024(4) -0.013(4) 0.003(3) C4 0.076(6) 0.077(5) 0.047(5) 0.001(4) 0.011(4) -0.028(5) C2 0.078(6) 0.116(7) 0.037(5) 0.014(5) 0.004(4) 0.007(5) C3 0.110(8) 0.055(5) 0.075(6) 0.012(4) -0.013(5) 0.001(5) C1 0.063(5) 0.072(5) 0.064(5) -0.003(4) 0.012(4) 0.014(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 O11 2.389(4) . ? Gd1 O4 2.435(3) . ? Gd1 O3 2.437(3) . ? Gd1 O5 2.438(3) 8_855 ? Gd1 O1 2.454(3) . ? Gd1 O7 2.468(4) . ? Gd1 O6 2.469(3) . ? Gd1 O2 2.475(3) 5_866 ? Gd1 O8 2.511(3) 8_855 ? Gd1 S1 3.0286(12) . ? Gd1 S3 3.0677(13) . ? Gd1 S2 3.0683(15) . ? S1 O5 1.471(3) . ? S1 O4 1.472(3) . ? S1 O8 1.473(3) . ? S1 O3 1.480(3) . ? S1 Gd1 3.0700(12) 8_865 ? S2 O12 1.443(4) . ? S2 O10 1.448(4) . ? S2 O11 1.487(4) . ? S2 O7 1.502(4) . ? S3 O2 1.444(4) . ? S3 O9 1.456(3) . ? S3 O1 1.485(3) . ? S3 O6 1.503(3) . ? O2 Gd1 2.475(3) 5_866 ? O5 Gd1 2.438(3) 8_865 ? O8 Gd1 2.511(3) 8_865 ? N3 C5 1.463(6) . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N3 H3F 0.8900 . ? N1 C2 1.461(8) . ? N1 C1 1.471(7) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C4 1.454(8) . ? N2 C3 1.460(9) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? C5 C5 1.409(11) 5_856 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 O11 Gd1 O4 133.03(13) . . ? O11 Gd1 O3 106.54(13) . . ? O4 Gd1 O3 57.62(11) . . ? O11 Gd1 O5 78.76(13) . 8_855 ? O4 Gd1 O5 85.89(11) . 8_855 ? O3 Gd1 O5 135.38(11) . 8_855 ? O11 Gd1 O1 78.23(13) . . ? O4 Gd1 O1 125.15(11) . . ? O3 Gd1 O1 71.78(11) . . ? O5 Gd1 O1 148.94(11) 8_855 . ? O11 Gd1 O7 56.99(13) . . ? O4 Gd1 O7 76.08(12) . . ? O3 Gd1 O7 74.62(12) . . ? O5 Gd1 O7 72.06(12) 8_855 . ? O1 Gd1 O7 111.23(12) . . ? O11 Gd1 O6 73.52(12) . . ? O4 Gd1 O6 152.82(12) . . ? O3 Gd1 O6 128.35(11) . . ? O5 Gd1 O6 95.99(11) 8_855 . ? O1 Gd1 O6 57.44(10) . . ? O7 Gd1 O6 130.33(12) . . ? O11 Gd1 O2 150.66(13) . 5_866 ? O4 Gd1 O2 73.25(12) . 5_866 ? O3 Gd1 O2 74.69(11) . 5_866 ? O5 Gd1 O2 121.67(11) 8_855 5_866 ? O1 Gd1 O2 74.40(12) . 5_866 ? O7 Gd1 O2 144.86(12) . 5_866 ? O6 Gd1 O2 82.90(11) . 5_866 ? O11 Gd1 O8 117.87(13) . 8_855 ? O4 Gd1 O8 87.68(11) . 8_855 ? O3 Gd1 O8 135.45(11) . 8_855 ? O5 Gd1 O8 56.49(11) 8_855 8_855 ? O1 Gd1 O8 119.12(11) . 8_855 ? O7 Gd1 O8 126.99(12) . 8_855 ? O6 Gd1 O8 71.28(11) . 8_855 ? O2 Gd1 O8 68.55(11) 5_866 8_855 ? O11 Gd1 S1 124.20(10) . . ? O4 Gd1 S1 28.71(8) . . ? O3 Gd1 S1 28.93(8) . . ? O5 Gd1 S1 111.69(9) 8_855 . ? O1 Gd1 S1 98.46(8) . . ? O7 Gd1 S1 73.97(9) . . ? O6 Gd1 S1 148.94(8) . . ? O2 Gd1 S1 70.89(8) 5_866 . ? O8 Gd1 S1 112.06(8) 8_855 . ? O11 Gd1 S3 75.56(10) . . ? O4 Gd1 S3 145.15(8) . . ? O3 Gd1 S3 99.59(8) . . ? O5 Gd1 S3 124.03(8) 8_855 . ? O1 Gd1 S3 28.53(8) . . ? O7 Gd1 S3 126.62(10) . . ? O6 Gd1 S3 29.01(7) . . ? O2 Gd1 S3 75.36(9) 5_866 . ? O8 Gd1 S3 94.72(8) 8_855 . ? S1 Gd1 S3 123.95(3) . . ? O11 Gd1 S2 28.29(10) . . ? O4 Gd1 S2 104.79(9) . . ? O3 Gd1 S2 93.21(8) . . ? O5 Gd1 S2 70.53(8) 8_855 . ? O1 Gd1 S2 97.29(9) . . ? O7 Gd1 S2 28.97(9) . . ? O6 Gd1 S2 101.36(9) . . ? O2 Gd1 S2 166.90(8) 5_866 . ? O8 Gd1 S2 124.54(8) 8_855 . ? S1 Gd1 S2 100.98(4) . . ? S3 Gd1 S2 102.31(4) . . ? O5 S1 O4 111.3(2) . . ? O5 S1 O8 105.5(2) . . ? O4 S1 O8 112.7(2) . . ? O5 S1 O3 111.1(2) . . ? O4 S1 O3 105.37(19) . . ? O8 S1 O3 111.0(2) . . ? O5 S1 Gd1 128.36(15) . . ? O4 S1 Gd1 52.64(13) . . ? O8 S1 Gd1 126.12(14) . . ? O3 S1 Gd1 52.78(13) . . ? O5 S1 Gd1 51.30(14) . 8_865 ? O4 S1 Gd1 128.89(15) . 8_865 ? O8 S1 Gd1 54.21(13) . 8_865 ? O3 S1 Gd1 125.68(14) . 8_865 ? Gd1 S1 Gd1 178.42(5) . 8_865 ? O12 S2 O10 111.8(3) . . ? O12 S2 O11 111.9(3) . . ? O10 S2 O11 110.5(3) . . ? O12 S2 O7 110.4(3) . . ? O10 S2 O7 110.1(2) . . ? O11 S2 O7 101.7(2) . . ? O12 S2 Gd1 131.45(19) . . ? O10 S2 Gd1 116.76(17) . . ? O11 S2 Gd1 49.58(15) . . ? O7 S2 Gd1 52.76(14) . . ? O2 S3 O9 110.9(2) . . ? O2 S3 O1 112.1(2) . . ? O9 S3 O1 109.5(2) . . ? O2 S3 O6 109.7(2) . . ? O9 S3 O6 109.8(2) . . ? O1 S3 O6 104.70(19) . . ? O2 S3 Gd1 121.78(16) . . ? O9 S3 Gd1 127.35(16) . . ? O1 S3 Gd1 52.12(13) . . ? O6 S3 Gd1 52.79(13) . . ? S3 O1 Gd1 99.35(16) . . ? S3 O2 Gd1 160.4(2) . 5_866 ? S1 O3 Gd1 98.29(16) . . ? S1 O4 Gd1 98.65(17) . . ? S1 O5 Gd1 100.61(18) . 8_865 ? S3 O6 Gd1 98.20(15) . . ? S2 O7 Gd1 98.27(18) . . ? S1 O8 Gd1 97.38(17) . 8_865 ? S2 O11 Gd1 102.1(2) . . ? C5 N3 H3D 109.5 . . ? C5 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C5 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? C2 N1 C1 114.3(5) . . ? C2 N1 H1D 108.7 . . ? C1 N1 H1D 108.7 . . ? C2 N1 H1E 108.7 . . ? C1 N1 H1E 108.7 . . ? H1D N1 H1E 107.6 . . ? C4 N2 C3 115.7(6) . . ? C4 N2 H2D 108.4 . . ? C3 N2 H2D 108.4 . . ? C4 N2 H2E 108.4 . . ? C3 N2 H2E 108.4 . . ? H2D N2 H2E 107.4 . . ? C5 C5 N3 116.0(7) 5_856 . ? C5 C5 H5A 108.3 5_856 . ? N3 C5 H5A 108.3 . . ? C5 C5 H5B 108.3 5_856 . ? N3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.759 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.129 data_zd-19 _database_code_depnum_ccdc_archive 'CCDC 875283' #TrackingRef '3c.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C2H8N)2(C2H10N2)0.5][Tb(SO4)3]' _chemical_formula_sum 'C5 H21 N3 O12 S3 Tb' _chemical_formula_weight 570.35 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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.919(4) _cell_length_b 10.236(3) _cell_length_c 31.206(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3488(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4835 _cell_measurement_theta_min 2.265 _cell_measurement_theta_max 25.532 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 4.476 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.5730 _exptl_absorpt_correction_T_max 0.6631 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 23618 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3247 _reflns_number_gt 2662 _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^)+(0.0426P)^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 3247 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.013 _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 Tb1 Tb 1.399888(18) 0.483186(19) 0.584388(6) 0.01703(9) Uani 1 1 d . . . S1 S 1.24812(9) 0.72919(10) 0.58398(3) 0.0202(2) Uani 1 1 d . . . S2 S 1.48181(11) 0.47418(12) 0.67778(4) 0.0307(3) Uani 1 1 d . . . S3 S 1.64151(9) 0.45302(10) 0.53626(3) 0.0184(2) Uani 1 1 d . . . O1 O 1.5891(2) 0.5734(3) 0.55459(9) 0.0238(7) Uani 1 1 d . . . O2 O 1.6473(3) 0.4586(3) 0.48996(9) 0.0289(7) Uani 1 1 d . . . O3 O 1.3834(3) 0.7195(3) 0.58449(9) 0.0235(7) Uani 1 1 d . . . O4 O 1.2034(3) 0.5932(3) 0.58553(9) 0.0266(7) Uani 1 1 d . . . O5 O 1.2029(3) 0.8049(3) 0.62049(9) 0.0292(7) Uani 1 1 d . . . O6 O 1.5559(3) 0.3470(3) 0.54995(9) 0.0231(7) Uani 1 1 d . . . O7 O 1.3733(3) 0.5449(3) 0.65953(10) 0.0354(8) Uani 1 1 d . . . O8 O 1.2050(3) 0.7996(3) 0.54599(9) 0.0263(7) Uani 1 1 d . . . O9 O 1.7625(3) 0.4303(3) 0.55467(10) 0.0296(7) Uani 1 1 d . . . O10 O 1.4425(3) 0.3632(3) 0.70295(11) 0.0419(9) Uani 1 1 d . . . O11 O 1.5455(3) 0.4303(4) 0.63820(10) 0.0410(9) Uani 1 1 d . . . O12 O 1.5568(4) 0.5617(4) 0.70255(12) 0.0624(12) Uani 1 1 d . . . N3 N 1.4700(3) 0.1741(3) 0.48363(12) 0.0276(9) Uani 1 1 d . . . H3D H 1.5171 0.2280 0.4685 0.041 Uiso 1 1 calc R . . H3E H 1.4558 0.2087 0.5093 0.041 Uiso 1 1 calc R . . H3F H 1.3992 0.1622 0.4700 0.041 Uiso 1 1 calc R . . N1 N 1.1978(4) 0.2735(4) 0.70451(13) 0.0392(10) Uani 1 1 d . . . H1D H 1.1818 0.2036 0.6879 0.047 Uiso 1 1 calc R . . H1E H 1.2716 0.3048 0.6968 0.047 Uiso 1 1 calc R . . N2 N 1.1994(5) 0.3203(5) 0.38856(15) 0.0604(15) Uani 1 1 d . . . H2D H 1.2359 0.3800 0.4054 0.072 Uiso 1 1 calc R . . H2E H 1.1638 0.2608 0.4058 0.072 Uiso 1 1 calc R . . C5 C 1.5324(5) 0.0480(5) 0.4887(2) 0.0547(17) Uani 1 1 d . . . H5A H 1.5512 0.0142 0.4604 0.066 Uiso 1 1 calc R . . H5B H 1.6096 0.0631 0.5033 0.066 Uiso 1 1 calc R . . C4 C 1.2931(5) 0.2552(6) 0.3632(2) 0.0617(18) Uani 1 1 d . . . H4A H 1.3518 0.2152 0.3820 0.093 Uiso 1 1 calc R . . H4B H 1.3335 0.3180 0.3453 0.093 Uiso 1 1 calc R . . H4C H 1.2557 0.1893 0.3456 0.093 Uiso 1 1 calc R . . C2 C 1.2032(6) 0.2314(7) 0.74927(19) 0.074(2) Uani 1 1 d . . . H2A H 1.2660 0.1666 0.7525 0.111 Uiso 1 1 calc R . . H2B H 1.1257 0.1950 0.7575 0.111 Uiso 1 1 calc R . . H2C H 1.2215 0.3052 0.7672 0.111 Uiso 1 1 calc R . . C3 C 1.1034(6) 0.3858(7) 0.3636(2) 0.074(2) Uani 1 1 d . . . H3A H 1.0453 0.4251 0.3828 0.111 Uiso 1 1 calc R . . H3B H 1.0624 0.3229 0.3458 0.111 Uiso 1 1 calc R . . H3C H 1.1396 0.4520 0.3459 0.111 Uiso 1 1 calc R . . C1 C 1.1040(5) 0.3749(6) 0.6962(2) 0.0600(17) Uani 1 1 d . . . H1A H 1.1074 0.4007 0.6667 0.090 Uiso 1 1 calc R . . H1B H 1.1195 0.4493 0.7141 0.090 Uiso 1 1 calc R . . H1C H 1.0243 0.3403 0.7025 0.090 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 Tb1 0.01604(13) 0.01577(13) 0.01928(13) 0.00075(8) 0.00047(8) 0.00023(8) S1 0.0196(6) 0.0186(6) 0.0224(6) 0.0001(4) 0.0000(5) 0.0038(4) S2 0.0341(7) 0.0352(7) 0.0229(6) 0.0054(5) -0.0081(5) -0.0098(5) S3 0.0158(5) 0.0203(5) 0.0190(5) 0.0013(4) 0.0008(4) 0.0000(4) O1 0.0231(17) 0.0195(16) 0.0289(17) -0.0018(13) 0.0040(13) -0.0002(12) O2 0.0336(18) 0.0335(18) 0.0196(16) 0.0028(13) 0.0003(14) 0.0013(15) O3 0.0204(17) 0.0203(17) 0.0297(18) 0.0011(13) 0.0003(13) 0.0005(12) O4 0.0228(16) 0.0220(17) 0.0348(18) -0.0017(13) 0.0025(14) -0.0009(13) O5 0.0367(19) 0.0275(17) 0.0233(18) -0.0038(13) 0.0017(14) 0.0114(14) O6 0.0224(16) 0.0191(16) 0.0279(17) 0.0010(13) 0.0039(14) -0.0020(12) O7 0.051(2) 0.0323(19) 0.0231(18) -0.0020(15) -0.0054(15) 0.0100(16) O8 0.0248(16) 0.0298(17) 0.0243(17) 0.0023(13) -0.0029(13) 0.0101(13) O9 0.0166(16) 0.0418(19) 0.0305(18) 0.0018(15) -0.0037(13) 0.0032(14) O10 0.045(2) 0.048(2) 0.033(2) 0.0172(16) -0.0116(17) -0.0110(17) O11 0.0289(19) 0.069(3) 0.0255(18) 0.0062(17) -0.0019(15) 0.0094(18) O12 0.078(3) 0.073(3) 0.036(2) 0.006(2) -0.023(2) -0.044(2) N3 0.031(2) 0.022(2) 0.030(2) 0.0011(16) -0.0013(17) -0.0012(16) N1 0.037(2) 0.045(3) 0.036(3) -0.011(2) 0.007(2) -0.008(2) N2 0.091(4) 0.053(3) 0.038(3) 0.002(2) -0.006(3) -0.029(3) C5 0.033(3) 0.036(3) 0.096(5) 0.024(3) -0.012(3) 0.000(2) C4 0.065(4) 0.072(5) 0.048(4) 0.008(3) 0.002(3) -0.027(4) C2 0.076(5) 0.113(6) 0.033(3) 0.008(4) 0.003(3) 0.002(4) C3 0.108(6) 0.057(5) 0.058(4) 0.003(4) -0.015(4) -0.005(4) C1 0.049(4) 0.061(4) 0.069(5) -0.005(3) 0.005(3) 0.009(3) _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 O11 2.375(3) . ? Tb1 O5 2.420(3) 8_855 ? Tb1 O4 2.423(3) . ? Tb1 O3 2.426(3) . ? Tb1 O7 2.446(3) . ? Tb1 O1 2.446(3) . ? Tb1 O6 2.449(3) . ? Tb1 O2 2.450(3) 5_866 ? Tb1 O8 2.506(3) 8_855 ? Tb1 S1 3.0145(13) . ? Tb1 S2 3.0500(15) . ? Tb1 S3 3.0515(13) . ? S1 O5 1.464(3) . ? S1 O8 1.465(3) . ? S1 O4 1.476(3) . ? S1 O3 1.480(3) . ? S1 Tb1 3.0613(13) 8_865 ? S2 O12 1.439(4) . ? S2 O10 1.446(3) . ? S2 O11 1.487(3) . ? S2 O7 1.501(3) . ? S3 O2 1.447(3) . ? S3 O9 1.459(3) . ? S3 O1 1.475(3) . ? S3 O6 1.495(3) . ? O2 Tb1 2.450(3) 5_866 ? O5 Tb1 2.420(3) 8_865 ? O8 Tb1 2.506(3) 8_865 ? N3 C5 1.469(6) . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N3 H3F 0.8900 . ? N1 C2 1.463(7) . ? N1 C1 1.480(6) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C4 1.455(7) . ? N2 C3 1.467(7) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? C5 C5 1.402(10) 5_856 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 O11 Tb1 O5 79.01(12) . 8_855 ? O11 Tb1 O4 133.48(11) . . ? O5 Tb1 O4 86.15(10) 8_855 . ? O11 Tb1 O3 106.02(11) . . ? O5 Tb1 O3 135.79(10) 8_855 . ? O4 Tb1 O3 58.05(10) . . ? O11 Tb1 O7 57.33(11) . . ? O5 Tb1 O7 72.16(11) 8_855 . ? O4 Tb1 O7 76.16(10) . . ? O3 Tb1 O7 74.46(10) . . ? O11 Tb1 O1 77.86(11) . . ? O5 Tb1 O1 148.55(10) 8_855 . ? O4 Tb1 O1 125.29(10) . . ? O3 Tb1 O1 71.74(10) . . ? O7 Tb1 O1 111.52(11) . . ? O11 Tb1 O6 73.46(11) . . ? O5 Tb1 O6 95.60(10) 8_855 . ? O4 Tb1 O6 152.44(10) . . ? O3 Tb1 O6 128.31(9) . . ? O7 Tb1 O6 130.56(10) . . ? O1 Tb1 O6 57.39(9) . . ? O11 Tb1 O2 149.98(11) . 5_866 ? O5 Tb1 O2 121.78(10) 8_855 5_866 ? O4 Tb1 O2 73.42(10) . 5_866 ? O3 Tb1 O2 75.10(10) . 5_866 ? O7 Tb1 O2 145.08(11) . 5_866 ? O1 Tb1 O2 74.09(10) . 5_866 ? O6 Tb1 O2 82.49(10) . 5_866 ? O11 Tb1 O8 118.25(12) . 8_855 ? O5 Tb1 O8 56.32(10) 8_855 8_855 ? O4 Tb1 O8 87.18(10) . 8_855 ? O3 Tb1 O8 135.60(9) . 8_855 ? O7 Tb1 O8 126.74(11) . 8_855 ? O1 Tb1 O8 119.17(9) . 8_855 ? O6 Tb1 O8 71.40(9) . 8_855 ? O2 Tb1 O8 68.50(10) 5_866 8_855 ? O11 Tb1 S1 124.14(9) . . ? O5 Tb1 S1 112.14(8) 8_855 . ? O4 Tb1 S1 28.98(7) . . ? O3 Tb1 S1 29.09(7) . . ? O7 Tb1 S1 73.92(8) . . ? O1 Tb1 S1 98.46(7) . . ? O6 Tb1 S1 148.85(7) . . ? O2 Tb1 S1 71.16(8) 5_866 . ? O8 Tb1 S1 111.91(7) 8_855 . ? O11 Tb1 S2 28.49(8) . . ? O5 Tb1 S2 70.63(7) 8_855 . ? O4 Tb1 S2 105.05(7) . . ? O3 Tb1 S2 92.91(7) . . ? O7 Tb1 S2 29.13(8) . . ? O1 Tb1 S2 97.29(7) . . ? O6 Tb1 S2 101.43(7) . . ? O2 Tb1 S2 166.86(8) 5_866 . ? O8 Tb1 S2 124.64(7) 8_855 . ? S1 Tb1 S2 100.99(3) . . ? O11 Tb1 S3 75.30(8) . . ? O5 Tb1 S3 123.62(8) 8_855 . ? O4 Tb1 S3 145.06(7) . . ? O3 Tb1 S3 99.54(7) . . ? O7 Tb1 S3 126.90(8) . . ? O1 Tb1 S3 28.49(7) . . ? O6 Tb1 S3 28.99(7) . . ? O2 Tb1 S3 74.96(8) 5_866 . ? O8 Tb1 S3 94.81(7) 8_855 . ? S1 Tb1 S3 123.90(3) . . ? S2 Tb1 S3 102.34(4) . . ? O5 S1 O8 105.11(18) . . ? O5 S1 O4 111.25(18) . . ? O8 S1 O4 112.61(18) . . ? O5 S1 O3 111.32(18) . . ? O8 S1 O3 111.24(17) . . ? O4 S1 O3 105.46(18) . . ? O5 S1 Tb1 128.65(13) . . ? O8 S1 Tb1 126.24(13) . . ? O4 S1 Tb1 52.68(12) . . ? O3 S1 Tb1 52.83(12) . . ? O5 S1 Tb1 50.86(12) . 8_865 ? O8 S1 Tb1 54.26(12) . 8_865 ? O4 S1 Tb1 128.78(13) . 8_865 ? O3 S1 Tb1 125.68(13) . 8_865 ? Tb1 S1 Tb1 178.44(4) . 8_865 ? O12 S2 O10 111.5(2) . . ? O12 S2 O11 111.6(2) . . ? O10 S2 O11 110.7(2) . . ? O12 S2 O7 110.6(2) . . ? O10 S2 O7 110.5(2) . . ? O11 S2 O7 101.50(19) . . ? O12 S2 Tb1 131.39(17) . . ? O10 S2 Tb1 117.09(14) . . ? O11 S2 Tb1 49.64(13) . . ? O7 S2 Tb1 52.50(13) . . ? O2 S3 O9 111.08(19) . . ? O2 S3 O1 111.82(18) . . ? O9 S3 O1 109.39(18) . . ? O2 S3 O6 109.94(18) . . ? O9 S3 O6 109.75(18) . . ? O1 S3 O6 104.66(17) . . ? O2 S3 Tb1 121.69(14) . . ? O9 S3 Tb1 127.23(13) . . ? O1 S3 Tb1 52.32(11) . . ? O6 S3 Tb1 52.55(11) . . ? S3 O1 Tb1 99.19(15) . . ? S3 O2 Tb1 161.0(2) . 5_866 ? S1 O3 Tb1 98.09(15) . . ? S1 O4 Tb1 98.34(15) . . ? S1 O5 Tb1 101.15(15) . 8_865 ? S3 O6 Tb1 98.46(14) . . ? S2 O7 Tb1 98.37(16) . . ? S1 O8 Tb1 97.41(15) . 8_865 ? S2 O11 Tb1 101.88(17) . . ? C5 N3 H3D 109.5 . . ? C5 N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C5 N3 H3F 109.5 . . ? H3D N3 H3F 109.5 . . ? H3E N3 H3F 109.5 . . ? C2 N1 C1 113.6(5) . . ? C2 N1 H1D 108.8 . . ? C1 N1 H1D 108.8 . . ? C2 N1 H1E 108.8 . . ? C1 N1 H1E 108.8 . . ? H1D N1 H1E 107.7 . . ? C4 N2 C3 115.0(5) . . ? C4 N2 H2D 108.5 . . ? C3 N2 H2D 108.5 . . ? C4 N2 H2E 108.5 . . ? C3 N2 H2E 108.5 . . ? H2D N2 H2E 107.5 . . ? C5 C5 N3 115.8(6) 5_856 . ? C5 C5 H5A 108.3 5_856 . ? N3 C5 H5A 108.3 . . ? C5 C5 H5B 108.3 5_856 . ? N3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.792 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.109 data_zd-28 _database_code_depnum_ccdc_archive 'CCDC 875284' #TrackingRef '4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(CH3)2NH2]4[Dy2(SO4)5]' _chemical_formula_sum 'C8 H32 Dy2 N4 O20 S5' _chemical_formula_weight 989.68 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' Dy Dy -0.1892 4.4098 '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 9.832(5) _cell_length_b 11.001(6) _cell_length_c 15.288(8) _cell_angle_alpha 70.555(6) _cell_angle_beta 75.366(7) _cell_angle_gamma 67.367(5) _cell_volume 1424.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2608 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.07 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 5.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5047 _exptl_absorpt_correction_T_max 0.6015 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 9470 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0926 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4892 _reflns_number_gt 3444 _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^)+(0.0930P)^2^+22.6014P] 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 4892 _refine_ls_number_parameters 352 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1834 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _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 Dy1 Dy 0.72096(8) 0.08322(7) 0.45225(5) 0.0253(3) Uani 1 1 d . . . Dy2 Dy 0.75746(8) 0.44351(7) 0.05268(5) 0.0280(3) Uani 1 1 d . . . S1 S 0.7469(5) 0.2576(4) 0.2517(3) 0.0265(9) Uani 1 1 d . . . S2 S 0.8690(5) 0.0630(4) 0.6087(3) 0.0295(10) Uani 1 1 d . . . S3 S 0.3957(4) 0.1980(4) 0.5201(3) 0.0268(9) Uani 1 1 d . . . S4 S 0.8556(4) 0.6755(4) 0.0380(3) 0.0297(10) Uani 1 1 d . . . S5 S 0.6394(5) 0.3618(4) -0.0743(3) 0.0316(10) Uani 1 1 d . . . O1 O 0.7675(14) 0.8104(12) 0.0514(10) 0.047(3) Uani 1 1 d . . . O2 O 0.8316(14) 0.5657(12) 0.1217(8) 0.038(3) Uani 1 1 d . . . O3 O 0.8129(13) 0.6468(11) -0.0377(8) 0.033(3) Uani 1 1 d . . . O4 O 1.0104(13) 0.6592(13) 0.0193(9) 0.042(3) Uani 1 1 d . . . O5 O 0.6839(12) 0.2829(11) 0.0199(8) 0.035(3) Uani 1 1 d . . . O6 O 0.4791(12) 0.3898(12) -0.0672(9) 0.036(3) Uani 1 1 d . . . O7 O 0.6754(14) 0.4884(12) -0.0929(8) 0.039(3) Uani 1 1 d . . . O8 O 0.7217(14) 0.2904(16) -0.1445(10) 0.054(4) Uani 1 1 d . . . O9 O 0.8774(13) 0.2581(12) 0.1813(9) 0.038(3) Uani 1 1 d . . . O10 O 0.6236(13) 0.3654(11) 0.2046(8) 0.033(3) Uani 1 1 d . . . O11 O 0.7262(13) 0.1214(11) 0.2850(8) 0.034(3) Uani 1 1 d . . . O12 O 0.7600(13) 0.2848(11) 0.3366(8) 0.034(3) Uani 1 1 d . . . O13 O 0.7995(13) 0.0952(14) 0.6965(8) 0.042(3) Uani 1 1 d . . . O14 O 1.0329(14) 0.0207(13) 0.6049(8) 0.040(3) Uani 1 1 d . . . O15 O 0.8239(13) 0.1798(11) 0.5256(8) 0.031(3) Uani 1 1 d . . . O16 O 0.8277(13) -0.0436(11) 0.5949(8) 0.035(3) Uani 1 1 d . . . O17 O 0.3018(14) 0.1173(13) 0.5362(10) 0.048(4) Uani 1 1 d . . . O18 O 0.3086(14) 0.3262(12) 0.5406(10) 0.049(4) Uani 1 1 d . . . O19 O 0.5213(14) 0.1208(13) 0.5752(9) 0.045(3) Uani 1 1 d . . . O20 O 0.4704(13) 0.2143(12) 0.4218(9) 0.040(3) Uani 1 1 d . . . N1 N 0.461(3) 0.628(3) 0.2852(19) 0.114(10) Uani 1 1 d . . . H1D H 0.3776 0.6932 0.2649 0.137 Uiso 1 1 calc R . . H1E H 0.4943 0.5703 0.2487 0.137 Uiso 1 1 calc R . . N2 N 1.0189(18) 0.0834(16) 0.7913(12) 0.047(4) Uani 1 1 d . . . H2D H 0.9261 0.1084 0.7783 0.057 Uiso 1 1 calc R . . H2E H 1.0776 0.0175 0.7627 0.057 Uiso 1 1 calc R . . N3 N 0.4437(18) 0.1844(16) 0.1312(12) 0.048(4) Uani 1 1 d . . . H3D H 0.3592 0.2466 0.1106 0.057 Uiso 1 1 calc R . . H3E H 0.5152 0.2236 0.1103 0.057 Uiso 1 1 calc R . . N4 N 1.0193(19) 0.3317(16) 0.3628(14) 0.057(5) Uani 1 1 d . . . H4D H 0.9351 0.3159 0.3651 0.069 Uiso 1 1 calc R . . H4E H 1.0905 0.2501 0.3779 0.069 Uiso 1 1 calc R . . C1 C 0.421(4) 0.557(4) 0.374(2) 0.114(12) Uani 1 1 d U . . H1A H 0.3469 0.5208 0.3737 0.171 Uiso 1 1 calc R . . H1B H 0.3811 0.6172 0.4147 0.171 Uiso 1 1 calc R . . H1C H 0.5068 0.4837 0.3969 0.171 Uiso 1 1 calc R . . C2 C 0.568(4) 0.693(4) 0.268(2) 0.115(12) Uani 1 1 d U . . H2A H 0.5836 0.7368 0.2026 0.172 Uiso 1 1 calc R . . H2B H 0.6600 0.6254 0.2869 0.172 Uiso 1 1 calc R . . H2C H 0.5333 0.7591 0.3035 0.172 Uiso 1 1 calc R . . C3 C 1.017(3) 0.028(2) 0.8888(16) 0.068(7) Uani 1 1 d . . . H3A H 0.9813 -0.0487 0.9085 0.103 Uiso 1 1 calc R . . H3B H 0.9520 0.0957 0.9205 0.103 Uiso 1 1 calc R . . H3C H 1.1157 -0.0023 0.9038 0.103 Uiso 1 1 calc R . . C4 C 1.071(3) 0.200(3) 0.751(2) 0.094(10) Uani 1 1 d . . . H4A H 1.0675 0.2316 0.6851 0.142 Uiso 1 1 calc R . . H4B H 1.1713 0.1744 0.7625 0.142 Uiso 1 1 calc R . . H4C H 1.0079 0.2725 0.7801 0.142 Uiso 1 1 calc R . . C5 C 0.488(3) 0.066(2) 0.091(2) 0.090(10) Uani 1 1 d . . . H5A H 0.5011 0.0971 0.0240 0.136 Uiso 1 1 calc R . . H5B H 0.4111 0.0248 0.1121 0.136 Uiso 1 1 calc R . . H5C H 0.5793 0.0003 0.1116 0.136 Uiso 1 1 calc R . . C6 C 0.420(3) 0.145(3) 0.2355(17) 0.078(8) Uani 1 1 d . . . H6A H 0.3928 0.2252 0.2574 0.117 Uiso 1 1 calc R . . H6B H 0.5103 0.0801 0.2581 0.117 Uiso 1 1 calc R . . H6C H 0.3418 0.1061 0.2583 0.117 Uiso 1 1 calc R . . C7 C 1.063(3) 0.402(3) 0.2668(19) 0.080(9) Uani 1 1 d . . . H7A H 1.0771 0.3466 0.2260 0.121 Uiso 1 1 calc R . . H7B H 1.1539 0.4177 0.2627 0.121 Uiso 1 1 calc R . . H7C H 0.9860 0.4877 0.2485 0.121 Uiso 1 1 calc R . . C8 C 0.995(3) 0.401(2) 0.4329(19) 0.069(7) Uani 1 1 d . . . H8A H 0.9662 0.3459 0.4932 0.104 Uiso 1 1 calc R . . H8B H 0.9171 0.4871 0.4190 0.104 Uiso 1 1 calc R . . H8C H 1.0848 0.4152 0.4334 0.104 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 Dy1 0.0231(5) 0.0169(4) 0.0361(5) -0.0066(3) -0.0118(3) -0.0023(3) Dy2 0.0233(5) 0.0206(4) 0.0380(5) -0.0060(3) -0.0121(4) -0.0018(3) S1 0.029(2) 0.0156(18) 0.031(2) -0.0053(15) -0.0077(17) -0.0011(16) S2 0.024(2) 0.027(2) 0.039(2) -0.0126(18) -0.0119(18) -0.0013(17) S3 0.020(2) 0.0161(18) 0.048(3) -0.0139(17) -0.0094(18) -0.0024(16) S4 0.018(2) 0.023(2) 0.052(3) -0.0176(19) -0.0095(19) -0.0017(17) S5 0.021(2) 0.033(2) 0.044(3) -0.0170(19) -0.0107(19) -0.0026(18) O1 0.029(7) 0.028(7) 0.086(10) -0.033(7) -0.004(7) 0.000(5) O2 0.040(8) 0.039(7) 0.034(7) -0.017(5) 0.000(5) -0.010(6) O3 0.034(7) 0.026(6) 0.039(7) -0.006(5) -0.014(5) -0.008(5) O4 0.029(7) 0.041(7) 0.063(9) -0.023(6) -0.013(6) -0.008(6) O5 0.025(6) 0.025(6) 0.049(7) -0.007(5) -0.015(5) 0.002(5) O6 0.019(6) 0.042(7) 0.055(8) -0.017(6) -0.012(5) -0.010(5) O7 0.036(7) 0.035(7) 0.043(7) 0.000(6) -0.013(6) -0.012(6) O8 0.028(7) 0.076(10) 0.059(9) -0.041(8) -0.013(6) 0.007(7) O9 0.028(7) 0.037(7) 0.049(8) -0.002(6) -0.015(6) -0.013(6) O10 0.030(7) 0.025(6) 0.037(7) -0.002(5) -0.011(5) -0.002(5) O11 0.031(7) 0.019(6) 0.046(7) -0.009(5) -0.016(5) 0.002(5) O12 0.035(7) 0.030(6) 0.042(7) -0.005(5) -0.013(6) -0.015(5) O13 0.030(7) 0.064(9) 0.038(7) -0.030(6) -0.005(6) -0.008(6) O14 0.040(8) 0.048(8) 0.031(7) -0.016(6) -0.011(6) -0.006(6) O15 0.030(7) 0.027(6) 0.049(7) -0.018(5) -0.015(5) -0.010(5) O16 0.039(7) 0.023(6) 0.050(8) -0.017(5) -0.015(6) -0.006(5) O17 0.036(8) 0.029(7) 0.079(10) -0.027(7) -0.004(7) -0.002(6) O18 0.036(8) 0.022(6) 0.088(10) -0.031(7) -0.001(7) 0.001(6) O19 0.028(7) 0.048(8) 0.059(9) -0.020(7) -0.014(6) -0.003(6) O20 0.028(7) 0.030(6) 0.056(8) -0.007(6) -0.015(6) -0.001(5) N1 0.12(2) 0.10(2) 0.11(2) 0.020(17) -0.058(18) -0.044(19) N2 0.035(9) 0.039(9) 0.074(13) -0.019(9) -0.021(9) -0.008(8) N3 0.036(10) 0.034(9) 0.063(11) -0.003(8) -0.010(8) -0.008(7) N4 0.039(10) 0.025(8) 0.114(16) -0.028(10) -0.017(10) -0.004(8) C1 0.112(14) 0.105(14) 0.116(14) -0.023(9) -0.007(9) -0.037(9) C2 0.115(15) 0.118(15) 0.121(14) -0.041(9) -0.018(9) -0.041(10) C3 0.069(17) 0.056(14) 0.065(16) -0.026(12) -0.010(13) 0.005(12) C4 0.09(2) 0.071(19) 0.09(2) -0.020(15) -0.004(17) 0.005(16) C5 0.11(2) 0.045(14) 0.11(2) -0.040(15) -0.040(19) 0.012(15) C6 0.063(17) 0.11(2) 0.075(18) -0.019(16) -0.024(14) -0.040(16) C7 0.10(2) 0.072(17) 0.09(2) 0.007(15) -0.051(17) -0.052(17) C8 0.057(15) 0.050(14) 0.12(2) -0.028(14) -0.020(14) -0.027(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 Dy1 O17 2.247(13) 2_656 ? Dy1 O14 2.322(12) 2_756 ? Dy1 O19 2.363(13) . ? Dy1 O15 2.368(10) . ? Dy1 O20 2.401(11) . ? Dy1 O16 2.410(11) . ? Dy1 O12 2.428(11) . ? Dy1 O11 2.440(12) . ? Dy1 S3 2.997(4) . ? Dy1 S2 3.007(4) . ? Dy1 S1 3.035(4) . ? Dy2 O4 2.296(12) 2_765 ? Dy2 O6 2.356(11) 2_665 ? Dy2 O2 2.354(12) . ? Dy2 O5 2.377(12) . ? Dy2 O3 2.389(12) . ? Dy2 O7 2.392(12) . ? Dy2 O10 2.421(11) . ? Dy2 O9 2.463(11) . ? Dy2 S4 2.983(4) . ? Dy2 S5 3.005(4) . ? Dy2 S1 3.052(4) . ? S1 O9 1.453(13) . ? S1 O10 1.470(11) . ? S1 O12 1.469(12) . ? S1 O11 1.490(12) . ? S2 O13 1.435(12) . ? S2 O16 1.470(12) . ? S2 O14 1.487(13) . ? S2 O15 1.490(12) . ? S3 O18 1.432(12) . ? S3 O17 1.439(14) . ? S3 O20 1.480(13) . ? S3 O19 1.483(13) . ? S4 O4 1.426(13) . ? S4 O1 1.455(12) . ? S4 O2 1.479(13) . ? S4 O3 1.486(12) . ? S5 O8 1.433(13) . ? S5 O6 1.467(11) . ? S5 O5 1.488(12) . ? S5 O7 1.487(13) . ? O4 Dy2 2.296(12) 2_765 ? O6 Dy2 2.356(11) 2_665 ? O14 Dy1 2.322(12) 2_756 ? O17 Dy1 2.247(13) 2_656 ? N1 C1 1.37(3) . ? N1 C2 1.41(4) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C3 1.41(3) . ? N2 C4 1.45(3) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? N3 C5 1.49(3) . ? N3 C6 1.49(3) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 C8 1.43(3) . ? N4 C7 1.45(3) . ? N4 H4D 0.9000 . ? N4 H4E 0.9000 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O17 Dy1 O14 83.4(5) 2_656 2_756 ? O17 Dy1 O19 90.6(5) 2_656 . ? O14 Dy1 O19 152.5(4) 2_756 . ? O17 Dy1 O15 140.5(5) 2_656 . ? O14 Dy1 O15 84.5(4) 2_756 . ? O19 Dy1 O15 83.2(4) . . ? O17 Dy1 O20 94.3(5) 2_656 . ? O14 Dy1 O20 148.6(4) 2_756 . ? O19 Dy1 O20 58.4(4) . . ? O15 Dy1 O20 114.7(4) . . ? O17 Dy1 O16 82.6(4) 2_656 . ? O14 Dy1 O16 78.2(4) 2_756 . ? O19 Dy1 O16 74.4(4) . . ? O15 Dy1 O16 58.1(4) . . ? O20 Dy1 O16 132.7(4) . . ? O17 Dy1 O12 141.4(5) 2_656 . ? O14 Dy1 O12 82.9(4) 2_756 . ? O19 Dy1 O12 116.6(4) . . ? O15 Dy1 O12 73.4(4) . . ? O20 Dy1 O12 79.6(4) . . ? O16 Dy1 O12 129.1(4) . . ? O17 Dy1 O11 83.9(5) 2_656 . ? O14 Dy1 O11 74.4(4) 2_756 . ? O19 Dy1 O11 131.8(4) . . ? O15 Dy1 O11 128.2(4) . . ? O20 Dy1 O11 74.2(4) . . ? O16 Dy1 O11 150.6(4) . . ? O12 Dy1 O11 57.6(4) . . ? O17 Dy1 S3 91.4(3) 2_656 . ? O14 Dy1 S3 174.3(3) 2_756 . ? O19 Dy1 S3 29.2(3) . . ? O15 Dy1 S3 101.0(3) . . ? O20 Dy1 S3 29.3(3) . . ? O16 Dy1 S3 103.5(3) . . ? O12 Dy1 S3 99.9(3) . . ? O11 Dy1 S3 102.9(3) . . ? O17 Dy1 S2 111.4(4) 2_656 . ? O14 Dy1 S2 80.6(3) 2_756 . ? O19 Dy1 S2 76.6(3) . . ? O15 Dy1 S2 29.2(3) . . ? O20 Dy1 S2 128.3(3) . . ? O16 Dy1 S2 28.9(3) . . ? O12 Dy1 S2 101.7(3) . . ? O11 Dy1 S2 149.0(3) . . ? S3 Dy1 S2 103.45(12) . . ? O17 Dy1 S1 113.0(4) 2_656 . ? O14 Dy1 S1 78.1(3) 2_756 . ? O19 Dy1 S1 128.5(3) . . ? O15 Dy1 S1 101.0(3) . . ? O20 Dy1 S1 74.1(3) . . ? O16 Dy1 S1 149.7(3) . . ? O12 Dy1 S1 28.5(3) . . ? O11 Dy1 S1 29.1(3) . . ? S3 Dy1 S1 102.01(11) . . ? S2 Dy1 S1 127.48(13) . . ? O4 Dy2 O6 157.1(5) 2_765 2_665 ? O4 Dy2 O2 96.8(4) 2_765 . ? O6 Dy2 O2 85.1(4) 2_665 . ? O4 Dy2 O5 85.7(4) 2_765 . ? O6 Dy2 O5 98.0(4) 2_665 . ? O2 Dy2 O5 166.1(4) . . ? O4 Dy2 O3 82.5(4) 2_765 . ? O6 Dy2 O3 79.0(4) 2_665 . ? O2 Dy2 O3 58.8(4) . . ? O5 Dy2 O3 135.1(4) . . ? O4 Dy2 O7 85.5(4) 2_765 . ? O6 Dy2 O7 77.5(4) 2_665 . ? O2 Dy2 O7 135.3(4) . . ? O5 Dy2 O7 58.5(4) . . ? O3 Dy2 O7 77.4(4) . . ? O4 Dy2 O10 130.7(4) 2_765 . ? O6 Dy2 O10 72.1(4) 2_665 . ? O2 Dy2 O10 87.7(4) . . ? O5 Dy2 O10 80.4(4) . . ? O3 Dy2 O10 137.4(4) . . ? O7 Dy2 O10 123.9(4) . . ? O4 Dy2 O9 76.3(4) 2_765 . ? O6 Dy2 O9 126.2(4) 2_665 . ? O2 Dy2 O9 79.4(4) . . ? O5 Dy2 O9 88.0(4) . . ? O3 Dy2 O9 130.1(4) . . ? O7 Dy2 O9 143.0(4) . . ? O10 Dy2 O9 56.3(4) . . ? O4 Dy2 S4 88.8(3) 2_765 . ? O6 Dy2 S4 81.7(3) 2_665 . ? O2 Dy2 S4 29.3(3) . . ? O5 Dy2 S4 164.5(3) . . ? O3 Dy2 S4 29.6(3) . . ? O7 Dy2 S4 106.7(3) . . ? O10 Dy2 S4 113.8(3) . . ? O9 Dy2 S4 104.8(3) . . ? O4 Dy2 S5 86.0(3) 2_765 . ? O6 Dy2 S5 86.5(3) 2_665 . ? O2 Dy2 S5 164.3(3) . . ? O5 Dy2 S5 29.2(3) . . ? O3 Dy2 S5 106.5(3) . . ? O7 Dy2 S5 29.3(3) . . ? O10 Dy2 S5 102.3(3) . . ? O9 Dy2 S5 116.3(3) . . ? S4 Dy2 S5 135.95(13) . . ? O4 Dy2 S1 103.5(3) 2_765 . ? O6 Dy2 S1 99.3(3) 2_665 . ? O2 Dy2 S1 82.5(3) . . ? O5 Dy2 S1 83.6(3) . . ? O3 Dy2 S1 141.3(3) . . ? O7 Dy2 S1 140.5(3) . . ? O10 Dy2 S1 28.3(3) . . ? O9 Dy2 S1 28.0(3) . . ? S4 Dy2 S1 111.77(12) . . ? S5 Dy2 S1 111.98(13) . . ? O9 S1 O10 104.1(7) . . ? O9 S1 O12 112.1(7) . . ? O10 S1 O12 111.7(7) . . ? O9 S1 O11 111.7(7) . . ? O10 S1 O11 112.8(7) . . ? O12 S1 O11 104.8(7) . . ? O9 S1 Dy1 130.0(5) . . ? O10 S1 Dy1 125.9(5) . . ? O12 S1 Dy1 52.1(5) . . ? O11 S1 Dy1 52.7(5) . . ? O9 S1 Dy2 52.8(5) . . ? O10 S1 Dy2 51.3(5) . . ? O12 S1 Dy2 126.9(5) . . ? O11 S1 Dy2 128.3(5) . . ? Dy1 S1 Dy2 177.04(15) . . ? O13 S2 O16 112.9(8) . . ? O13 S2 O14 108.0(7) . . ? O16 S2 O14 110.8(7) . . ? O13 S2 O15 113.4(7) . . ? O16 S2 O15 103.2(6) . . ? O14 S2 O15 108.4(7) . . ? O13 S2 Dy1 128.0(5) . . ? O16 S2 Dy1 52.4(5) . . ? O14 S2 Dy1 123.9(5) . . ? O15 S2 Dy1 50.9(4) . . ? O18 S3 O17 109.7(8) . . ? O18 S3 O20 112.5(8) . . ? O17 S3 O20 108.2(8) . . ? O18 S3 O19 112.7(8) . . ? O17 S3 O19 110.2(8) . . ? O20 S3 O19 103.3(7) . . ? O18 S3 Dy1 131.3(6) . . ? O17 S3 Dy1 118.9(5) . . ? O20 S3 Dy1 52.4(5) . . ? O19 S3 Dy1 51.0(5) . . ? O4 S4 O1 110.5(8) . . ? O4 S4 O2 108.0(8) . . ? O1 S4 O2 111.8(8) . . ? O4 S4 O3 110.0(7) . . ? O1 S4 O3 112.8(7) . . ? O2 S4 O3 103.5(7) . . ? O4 S4 Dy2 119.9(5) . . ? O1 S4 Dy2 129.6(6) . . ? O2 S4 Dy2 51.1(5) . . ? O3 S4 Dy2 52.5(5) . . ? O8 S5 O6 111.0(8) . . ? O8 S5 O5 112.1(8) . . ? O6 S5 O5 107.8(7) . . ? O8 S5 O7 110.7(9) . . ? O6 S5 O7 112.0(7) . . ? O5 S5 O7 103.0(7) . . ? O8 S5 Dy2 128.2(6) . . ? O6 S5 Dy2 120.8(5) . . ? O5 S5 Dy2 51.3(5) . . ? O7 S5 Dy2 51.8(5) . . ? S4 O2 Dy2 99.7(6) . . ? S4 O3 Dy2 98.0(6) . . ? S4 O4 Dy2 147.3(8) . 2_765 ? S5 O5 Dy2 99.5(6) . . ? S5 O6 Dy2 144.2(7) . 2_665 ? S5 O7 Dy2 98.9(6) . . ? S1 O9 Dy2 99.1(6) . . ? S1 O10 Dy2 100.5(6) . . ? S1 O11 Dy1 98.2(6) . . ? S1 O12 Dy1 99.3(6) . . ? S2 O14 Dy1 154.1(7) . 2_756 ? S2 O15 Dy1 99.9(6) . . ? S2 O16 Dy1 98.7(6) . . ? S3 O17 Dy1 149.3(8) . 2_656 ? S3 O19 Dy1 99.8(7) . . ? S3 O20 Dy1 98.3(6) . . ? C1 N1 C2 120(3) . . ? C1 N1 H1D 107.3 . . ? C2 N1 H1D 107.3 . . ? C1 N1 H1E 107.3 . . ? C2 N1 H1E 107.3 . . ? H1D N1 H1E 106.9 . . ? C3 N2 C4 116(2) . . ? C3 N2 H2D 108.4 . . ? C4 N2 H2D 108.4 . . ? C3 N2 H2E 108.4 . . ? C4 N2 H2E 108.4 . . ? H2D N2 H2E 107.5 . . ? C5 N3 C6 113.1(19) . . ? C5 N3 H3D 109.0 . . ? C6 N3 H3D 109.0 . . ? C5 N3 H3E 109.0 . . ? C6 N3 H3E 109.0 . . ? H3D N3 H3E 107.8 . . ? C8 N4 C7 116.4(19) . . ? C8 N4 H4D 108.2 . . ? C7 N4 H4D 108.2 . . ? C8 N4 H4E 108.2 . . ? C7 N4 H4E 108.2 . . ? H4D N4 H4E 107.3 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 5.790 _refine_diff_density_min -2.279 _refine_diff_density_rms 0.321 data_zd-49 _database_code_depnum_ccdc_archive 'CCDC 875285' #TrackingRef '5a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Dy2(SO4)8]' _chemical_formula_sum 'C10 H50 Dy2 N10 O32 S8' _chemical_formula_weight 1404.08 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' Dy Dy -0.1892 4.4098 '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 8.7260(18) _cell_length_b 9.828(2) _cell_length_c 13.475(3) _cell_angle_alpha 99.102(2) _cell_angle_beta 92.703(3) _cell_angle_gamma 115.764(2) _cell_volume 1018.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1848 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 23.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 4.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5554 _exptl_absorpt_correction_T_max 0.6348 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7183 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3546 _reflns_number_gt 3004 _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^)+(0.0536P)^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 3546 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy -0.85344(4) 0.18164(4) 0.20858(3) 0.01823(13) Uani 1 1 d . . . S1 S -0.9661(2) -0.0527(2) 0.34248(14) 0.0245(4) Uani 1 1 d . . . S2 S -0.5064(2) 0.3414(2) 0.34433(14) 0.0243(4) Uani 1 1 d . . . S3 S -0.7634(2) 0.0143(2) -0.02592(14) 0.0202(4) Uani 1 1 d . . . S4 S -0.8615(3) 0.4792(2) 0.19557(15) 0.0253(4) Uani 1 1 d . . . O1 O -0.5589(6) 0.2305(6) 0.2433(4) 0.0275(12) Uani 1 1 d . . . O2 O -0.8821(6) -0.0548(6) 0.2470(4) 0.0246(12) Uani 1 1 d . . . O3 O -0.7873(7) 0.1286(6) 0.0473(4) 0.0313(13) Uani 1 1 d . . . O4 O -0.5882(7) 0.0846(7) -0.0498(4) 0.0328(13) Uani 1 1 d . . . O5 O -0.9911(7) 0.0886(6) 0.3495(4) 0.0289(13) Uani 1 1 d . . . O6 O -0.7477(7) 0.4179(6) 0.1493(4) 0.0304(13) Uani 1 1 d . . . O7 O -0.9748(7) 0.3576(6) 0.2485(4) 0.0349(14) Uani 1 1 d . . . O8 O -0.6640(7) 0.3575(6) 0.3610(4) 0.0339(14) Uani 1 1 d . . . O9 O -0.8801(7) -0.0222(7) -0.1195(4) 0.0368(14) Uani 1 1 d . . . O10 O -1.1290(7) -0.1881(6) 0.3286(5) 0.0350(14) Uani 1 1 d . . . O11 O -0.7620(8) 0.6244(6) 0.2663(5) 0.0428(16) Uani 1 1 d . . . O12 O -0.8016(8) -0.1225(7) 0.0153(5) 0.0449(16) Uani 1 1 d . . . O13 O -0.4596(8) 0.2742(7) 0.4215(4) 0.0422(16) Uani 1 1 d . . . O14 O -0.9627(8) 0.4993(7) 0.1152(5) 0.0459(17) Uani 1 1 d . . . O15 O -0.3660(8) 0.4859(7) 0.3361(5) 0.0459(17) Uani 1 1 d . . . N5 N -0.5729(8) 0.9173(7) 0.2200(5) 0.0306(16) Uani 1 1 d . . . H5C H -0.5519 0.9422 0.1597 0.046 Uiso 1 1 calc R . . H5D H -0.6342 0.9616 0.2485 0.046 Uiso 1 1 calc R . . H5E H -0.6316 0.8154 0.2123 0.046 Uiso 1 1 calc R . . N2 N -0.1117(8) 0.6896(7) 0.0871(5) 0.0283(15) Uani 1 1 d . . . H2C H -0.0619 0.7833 0.1263 0.042 Uiso 1 1 calc R . . H2D H -0.1305 0.6973 0.0232 0.042 Uiso 1 1 calc R . . H2E H -0.0433 0.6443 0.0910 0.042 Uiso 1 1 calc R . . N1 N -0.3262(9) 0.3232(8) 0.0975(5) 0.0341(17) Uani 1 1 d . . . H1C H -0.3865 0.2301 0.0587 0.051 Uiso 1 1 calc R . . H1D H -0.3476 0.3197 0.1613 0.051 Uiso 1 1 calc R . . H1E H -0.2148 0.3529 0.0948 0.051 Uiso 1 1 calc R . . N3 N 0.9104(9) 0.6429(8) 0.4932(6) 0.0368(18) Uani 1 1 d . . . H3C H 0.9627 0.7424 0.4902 0.055 Uiso 1 1 calc R . . H3D H 0.8582 0.6315 0.5486 0.055 Uiso 1 1 calc R . . H3E H 0.8331 0.5910 0.4386 0.055 Uiso 1 1 calc R . . O16 O -0.8569(8) -0.0459(8) 0.4277(5) 0.0488(17) Uani 1 1 d . . . N4 N -0.4411(10) 0.7776(9) 0.3924(5) 0.0410(19) Uani 1 1 d . . . H4C H -0.4548 0.7605 0.4551 0.061 Uiso 1 1 calc R . . H4D H -0.3441 0.7761 0.3760 0.061 Uiso 1 1 calc R . . H4E H -0.5293 0.7046 0.3492 0.061 Uiso 1 1 calc R . . C2 C -0.2785(11) 0.5955(9) 0.1221(7) 0.034(2) Uani 1 1 d . . . H2A H -0.3500 0.6481 0.1202 0.041 Uiso 1 1 calc R . . H2B H -0.2566 0.5892 0.1921 0.041 Uiso 1 1 calc R . . C1 C -0.3758(11) 0.4349(9) 0.0606(6) 0.033(2) Uani 1 1 d . . . H1A H -0.4977 0.4011 0.0627 0.040 Uiso 1 1 calc R . . H1B H -0.3552 0.4361 -0.0094 0.040 Uiso 1 1 calc R . . C3 C 1.0396(11) 0.5821(9) 0.4967(7) 0.034(2) Uani 1 1 d . . . H3A H 1.0964 0.5949 0.4363 0.041 Uiso 1 1 calc R . . H3B H 1.1259 0.6412 0.5550 0.041 Uiso 1 1 calc R . . C5 C -0.4098(10) 0.9711(11) 0.2853(7) 0.040(2) Uani 1 1 d . . . H5A H -0.3478 1.0824 0.2943 0.048 Uiso 1 1 calc R . . H5B H -0.3406 0.9278 0.2516 0.048 Uiso 1 1 calc R . . C4 C -0.4327(12) 0.9280(11) 0.3875(7) 0.044(2) Uani 1 1 d . . . H4A H -0.3380 1.0061 0.4363 0.053 Uiso 1 1 calc R . . H4B H -0.5375 0.9291 0.4077 0.053 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 Dy1 0.0190(2) 0.0129(2) 0.0185(2) 0.00224(14) 0.00139(14) 0.00373(15) S1 0.0250(11) 0.0191(10) 0.0239(10) 0.0076(8) 0.0034(8) 0.0039(9) S2 0.0196(10) 0.0219(10) 0.0220(10) 0.0052(8) -0.0005(8) 0.0008(8) S3 0.0174(10) 0.0189(10) 0.0200(9) -0.0001(8) 0.0023(8) 0.0054(8) S4 0.0278(11) 0.0147(10) 0.0317(11) 0.0036(8) 0.0012(9) 0.0085(9) O1 0.022(3) 0.029(3) 0.029(3) -0.001(2) 0.000(2) 0.011(3) O2 0.023(3) 0.024(3) 0.029(3) 0.009(2) 0.010(2) 0.010(2) O3 0.028(3) 0.036(3) 0.025(3) -0.002(3) 0.007(2) 0.012(3) O4 0.021(3) 0.045(4) 0.029(3) 0.003(3) 0.007(2) 0.014(3) O5 0.036(3) 0.016(3) 0.030(3) 0.004(2) 0.009(3) 0.007(3) O6 0.035(3) 0.028(3) 0.035(3) 0.016(3) 0.017(3) 0.016(3) O7 0.030(3) 0.031(3) 0.049(4) 0.013(3) 0.018(3) 0.015(3) O8 0.028(3) 0.028(3) 0.030(3) -0.013(3) -0.005(3) 0.006(3) O9 0.024(3) 0.048(4) 0.024(3) -0.004(3) -0.001(2) 0.006(3) O10 0.029(3) 0.016(3) 0.048(4) 0.003(3) 0.013(3) 0.000(3) O11 0.053(4) 0.019(3) 0.044(4) 0.000(3) 0.003(3) 0.008(3) O12 0.061(4) 0.030(3) 0.052(4) 0.018(3) 0.020(3) 0.022(3) O13 0.036(4) 0.052(4) 0.032(3) 0.020(3) 0.001(3) 0.010(3) O14 0.049(4) 0.026(3) 0.062(4) 0.008(3) -0.012(3) 0.018(3) O15 0.036(4) 0.033(4) 0.047(4) 0.015(3) -0.004(3) -0.006(3) N5 0.034(4) 0.027(4) 0.034(4) 0.006(3) 0.006(3) 0.017(3) N2 0.025(4) 0.016(3) 0.036(4) 0.006(3) 0.003(3) 0.003(3) N1 0.030(4) 0.029(4) 0.036(4) 0.001(3) 0.007(3) 0.009(3) N3 0.034(4) 0.030(4) 0.043(5) 0.004(3) 0.001(3) 0.012(4) O16 0.054(4) 0.056(4) 0.035(4) 0.016(3) -0.005(3) 0.022(4) N4 0.046(5) 0.053(5) 0.031(4) 0.016(4) 0.009(4) 0.026(4) C2 0.038(5) 0.030(5) 0.037(5) 0.006(4) 0.008(4) 0.017(4) C1 0.035(5) 0.026(5) 0.032(5) 0.004(4) 0.001(4) 0.010(4) C3 0.030(5) 0.021(4) 0.043(5) 0.001(4) 0.000(4) 0.006(4) C5 0.021(5) 0.050(6) 0.044(6) 0.020(5) 0.003(4) 0.008(4) C4 0.037(5) 0.054(6) 0.038(5) 0.005(5) -0.005(4) 0.020(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 Dy1 O9 2.297(5) 2_355 ? Dy1 O3 2.313(5) . ? Dy1 O2 2.371(5) . ? Dy1 O6 2.382(5) . ? Dy1 O5 2.386(5) . ? Dy1 O7 2.398(5) . ? Dy1 O1 2.408(5) . ? Dy1 O8 2.452(5) . ? Dy1 S4 2.9876(19) . ? Dy1 S1 3.0065(18) . ? Dy1 S2 3.069(2) . ? S1 O16 1.431(6) . ? S1 O10 1.441(5) . ? S1 O5 1.486(5) . ? S1 O2 1.512(5) . ? S2 O15 1.443(6) . ? S2 O13 1.447(6) . ? S2 O8 1.475(6) . ? S2 O1 1.512(6) . ? S3 O12 1.446(6) . ? S3 O4 1.455(5) . ? S3 O3 1.467(5) . ? S3 O9 1.475(6) . ? S4 O11 1.454(6) . ? S4 O14 1.457(6) . ? S4 O6 1.482(5) . ? S4 O7 1.491(5) . ? O9 Dy1 2.297(5) 2_355 ? N5 C5 1.469(10) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N2 C2 1.493(9) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N1 C1 1.485(10) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N3 C3 1.490(10) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.460(11) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.501(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C3 1.473(15) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C4 1.502(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O9 Dy1 O3 78.00(19) 2_355 . ? O9 Dy1 O2 81.4(2) 2_355 . ? O3 Dy1 O2 93.42(18) . . ? O9 Dy1 O6 107.5(2) 2_355 . ? O3 Dy1 O6 73.86(19) . . ? O2 Dy1 O6 162.04(17) . . ? O9 Dy1 O5 83.27(19) 2_355 . ? O3 Dy1 O5 148.76(19) . . ? O2 Dy1 O5 58.93(17) . . ? O6 Dy1 O5 136.29(18) . . ? O9 Dy1 O7 83.8(2) 2_355 . ? O3 Dy1 O7 120.81(19) . . ? O2 Dy1 O7 138.67(17) . . ? O6 Dy1 O7 59.01(17) . . ? O5 Dy1 O7 81.17(17) . . ? O9 Dy1 O1 147.2(2) 2_355 . ? O3 Dy1 O1 78.26(18) . . ? O2 Dy1 O1 77.78(17) . . ? O6 Dy1 O1 87.08(18) . . ? O5 Dy1 O1 106.65(18) . . ? O7 Dy1 O1 128.07(19) . . ? O9 Dy1 O8 152.32(19) 2_355 . ? O3 Dy1 O8 129.31(18) . . ? O2 Dy1 O8 99.02(19) . . ? O6 Dy1 O8 80.40(19) . . ? O5 Dy1 O8 73.72(18) . . ? O7 Dy1 O8 77.74(19) . . ? O1 Dy1 O8 57.24(18) . . ? O9 Dy1 S4 96.78(16) 2_355 . ? O3 Dy1 S4 97.87(14) . . ? O2 Dy1 S4 167.96(12) . . ? O6 Dy1 S4 29.38(13) . . ? O5 Dy1 S4 109.07(13) . . ? O7 Dy1 S4 29.64(13) . . ? O1 Dy1 S4 108.57(13) . . ? O8 Dy1 S4 77.00(14) . . ? O9 Dy1 S1 82.64(15) 2_355 . ? O3 Dy1 S1 122.39(14) . . ? O2 Dy1 S1 29.79(12) . . ? O6 Dy1 S1 162.99(14) . . ? O5 Dy1 S1 29.20(13) . . ? O7 Dy1 S1 110.06(13) . . ? O1 Dy1 S1 91.38(13) . . ? O8 Dy1 S1 84.52(14) . . ? S4 Dy1 S1 138.25(6) . . ? O9 Dy1 S2 169.18(15) 2_355 . ? O3 Dy1 S2 104.70(14) . . ? O2 Dy1 S2 87.92(13) . . ? O6 Dy1 S2 83.29(14) . . ? O5 Dy1 S2 89.62(14) . . ? O7 Dy1 S2 103.21(15) . . ? O1 Dy1 S2 28.98(13) . . ? O8 Dy1 S2 28.27(13) . . ? S4 Dy1 S2 93.23(5) . . ? S1 Dy1 S2 87.17(5) . . ? O16 S1 O10 110.9(4) . . ? O16 S1 O5 112.7(4) . . ? O10 S1 O5 110.7(3) . . ? O16 S1 O2 110.4(3) . . ? O10 S1 O2 109.1(3) . . ? O5 S1 O2 102.6(3) . . ? O16 S1 Dy1 122.9(3) . . ? O10 S1 Dy1 126.1(3) . . ? O5 S1 Dy1 51.6(2) . . ? O2 S1 Dy1 51.14(19) . . ? O15 S2 O13 111.3(4) . . ? O15 S2 O8 111.7(4) . . ? O13 S2 O8 111.9(3) . . ? O15 S2 O1 109.6(3) . . ? O13 S2 O1 109.6(3) . . ? O8 S2 O1 102.4(3) . . ? O15 S2 Dy1 125.3(3) . . ? O13 S2 Dy1 123.3(3) . . ? O8 S2 Dy1 51.9(2) . . ? O1 S2 Dy1 50.5(2) . . ? O12 S3 O4 112.3(4) . . ? O12 S3 O3 109.8(3) . . ? O4 S3 O3 108.2(3) . . ? O12 S3 O9 110.8(4) . . ? O4 S3 O9 107.9(3) . . ? O3 S3 O9 107.7(3) . . ? O11 S4 O14 110.6(4) . . ? O11 S4 O6 110.8(4) . . ? O14 S4 O6 108.8(4) . . ? O11 S4 O7 111.3(4) . . ? O14 S4 O7 110.4(4) . . ? O6 S4 O7 104.7(3) . . ? O11 S4 Dy1 125.0(3) . . ? O14 S4 Dy1 124.3(3) . . ? O6 S4 Dy1 52.0(2) . . ? O7 S4 Dy1 52.7(2) . . ? S2 O1 Dy1 100.5(3) . . ? S1 O2 Dy1 99.1(2) . . ? S3 O3 Dy1 144.5(3) . . ? S1 O5 Dy1 99.2(3) . . ? S4 O6 Dy1 98.6(2) . . ? S4 O7 Dy1 97.7(3) . . ? S2 O8 Dy1 99.8(3) . . ? S3 O9 Dy1 146.1(3) . 2_355 ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N2 C2 C1 114.3(7) . . ? N2 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N1 C1 C2 112.7(7) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C3 C3 N3 111.9(9) 2_766 . ? C3 C3 H3A 109.2 2_766 . ? N3 C3 H3A 109.2 . . ? C3 C3 H3B 109.2 2_766 . ? N3 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N5 C5 C4 113.2(7) . . ? N5 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N4 C4 C5 114.8(8) . . ? N4 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N4 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.967 _refine_diff_density_min -1.708 _refine_diff_density_rms 0.202 data_zd-26 _database_code_depnum_ccdc_archive 'CCDC 875286' #TrackingRef '5b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Ho2(SO4)8]' _chemical_formula_sum 'C10 H50 Ho2 N10 O32 S8' _chemical_formula_weight 1408.94 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' Ho Ho -0.2175 4.6783 '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 8.734(2) _cell_length_b 9.824(3) _cell_length_c 13.466(4) _cell_angle_alpha 99.028(3) _cell_angle_beta 92.819(3) _cell_angle_gamma 115.737(3) _cell_volume 1019.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3027 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.85 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 4.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5997 _exptl_absorpt_correction_T_max 0.6685 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7485 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3695 _reflns_number_gt 3346 _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^)+(0.0300P)^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 3695 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.010 _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 Ho1 Ho 0.85384(2) 0.81834(2) -0.208667(15) 0.01423(8) Uani 1 1 d . . . S1 S 0.96577(14) 1.05156(13) -0.34239(9) 0.0203(3) Uani 1 1 d . . . S2 S 1.23580(13) 1.01296(12) -0.02571(8) 0.0163(2) Uani 1 1 d . . . S3 S 0.86143(14) 0.52154(13) -0.19559(9) 0.0218(3) Uani 1 1 d . . . S4 S 0.50818(13) 0.65965(13) -0.34371(8) 0.0211(3) Uani 1 1 d . . . O1 O 0.5601(4) 0.7701(4) -0.2429(2) 0.0243(7) Uani 1 1 d . . . O2 O 0.8829(4) 1.0540(3) -0.2468(2) 0.0229(7) Uani 1 1 d . . . O3 O 1.2113(4) 1.1279(4) 0.0485(2) 0.0272(8) Uani 1 1 d . . . O4 O 0.9914(4) 0.9097(3) -0.3491(2) 0.0253(7) Uani 1 1 d . . . O5 O 1.4112(4) 1.0849(4) -0.0486(2) 0.0295(8) Uani 1 1 d . . . O6 O 0.9728(4) 0.6419(4) -0.2490(3) 0.0308(8) Uani 1 1 d . . . O7 O 0.7484(4) 0.5841(4) -0.1487(2) 0.0268(8) Uani 1 1 d . . . O8 O 1.1198(4) 0.9762(4) -0.1201(2) 0.0318(8) Uani 1 1 d . . . O9 O 0.6652(4) 0.6410(4) -0.3612(2) 0.0314(8) Uani 1 1 d . . . O10 O 1.1298(4) 1.1883(4) -0.3287(3) 0.0329(8) Uani 1 1 d . . . O11 O 0.7614(4) 0.3766(4) -0.2654(3) 0.0367(9) Uani 1 1 d . . . O12 O 1.1993(5) 0.8766(4) 0.0160(3) 0.0401(9) Uani 1 1 d . . . O13 O 0.4596(4) 0.7251(4) -0.4214(3) 0.0378(9) Uani 1 1 d . . . O14 O 0.3658(4) 0.5146(4) -0.3347(3) 0.0408(10) Uani 1 1 d . . . O15 O 0.9624(5) 0.5009(4) -0.1154(3) 0.0437(10) Uani 1 1 d . . . O16 O 0.8561(5) 1.0446(5) -0.4280(3) 0.0475(11) Uani 1 1 d . . . N1 N 0.5749(5) 0.0842(4) -0.2190(3) 0.0248(9) Uani 1 1 d . . . H1C H 0.5551 0.0580 -0.1589 0.037 Uiso 1 1 calc R . . H1D H 0.6321 0.1863 -0.2106 0.037 Uiso 1 1 calc R . . H1E H 0.6369 0.0414 -0.2484 0.037 Uiso 1 1 calc R . . N2 N 0.4424(5) 0.2229(5) -0.3912(3) 0.0378(11) Uani 1 1 d . . . H2C H 0.4571 0.2416 -0.4535 0.057 Uiso 1 1 calc R . . H2D H 0.5294 0.2960 -0.3472 0.057 Uiso 1 1 calc R . . H2E H 0.3446 0.2227 -0.3754 0.057 Uiso 1 1 calc R . . N3 N 0.0876(5) 0.3566(5) -0.4925(3) 0.0327(10) Uani 1 1 d . . . H3C H 0.0354 0.2570 -0.4897 0.049 Uiso 1 1 calc R . . H3D H 0.1638 0.4084 -0.4373 0.049 Uiso 1 1 calc R . . H3E H 0.1411 0.3684 -0.5474 0.049 Uiso 1 1 calc R . . N4 N 0.3262(5) -0.3234(5) -0.0976(3) 0.0310(10) Uani 1 1 d . . . H4C H 0.3873 -0.2301 -0.0592 0.046 Uiso 1 1 calc R . . H4D H 0.2151 -0.3523 -0.0946 0.046 Uiso 1 1 calc R . . H4E H 0.3468 -0.3208 -0.1616 0.046 Uiso 1 1 calc R . . N5 N 0.1139(5) -0.6894(4) -0.0865(3) 0.0260(9) Uani 1 1 d . . . H5C H 0.0630 -0.7828 -0.1260 0.039 Uiso 1 1 calc R . . H5D H 0.0461 -0.6434 -0.0893 0.039 Uiso 1 1 calc R . . H5E H 0.1336 -0.6980 -0.0228 0.039 Uiso 1 1 calc R . . C1 C 0.4098(6) 0.0292(6) -0.2840(4) 0.0324(12) Uani 1 1 d . . . H1A H 0.3413 0.0738 -0.2510 0.039 Uiso 1 1 calc R . . H1B H 0.3474 -0.0820 -0.2925 0.039 Uiso 1 1 calc R . . C2 C 0.4361(7) 0.0722(6) -0.3873(4) 0.0369(14) Uani 1 1 d . . . H2A H 0.5423 0.0729 -0.4058 0.044 Uiso 1 1 calc R . . H2B H 0.3434 -0.0062 -0.4371 0.044 Uiso 1 1 calc R . . C3 C -0.0410(6) 0.4165(5) -0.4975(4) 0.0318(12) Uani 1 1 d . . . H3A H -0.1003 0.4021 -0.4381 0.038 Uiso 1 1 calc R . . H3B H -0.1251 0.3585 -0.5570 0.038 Uiso 1 1 calc R . . C4 C 0.3749(6) -0.4347(5) -0.0604(4) 0.0291(12) Uani 1 1 d . . . H4A H 0.3539 -0.4355 0.0097 0.035 Uiso 1 1 calc R . . H4B H 0.4968 -0.4007 -0.0620 0.035 Uiso 1 1 calc R . . C5 C 0.2781(6) -0.5965(5) -0.1218(4) 0.0310(12) Uani 1 1 d . . . H5A H 0.2555 -0.5911 -0.1919 0.037 Uiso 1 1 calc R . . H5B H 0.3501 -0.6486 -0.1195 0.037 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 Ho1 0.01465(11) 0.01357(11) 0.01374(12) 0.00265(8) 0.00139(8) 0.00573(8) S1 0.0203(6) 0.0198(6) 0.0193(6) 0.0084(5) 0.0034(5) 0.0060(5) S2 0.0142(5) 0.0182(6) 0.0147(6) 0.0017(4) 0.0022(4) 0.0061(4) S3 0.0226(6) 0.0161(6) 0.0279(7) 0.0042(5) 0.0016(5) 0.0099(5) S4 0.0157(5) 0.0235(6) 0.0181(6) 0.0062(5) -0.0003(4) 0.0029(5) O1 0.0196(16) 0.0285(18) 0.0233(18) 0.0016(14) 0.0011(13) 0.0106(14) O2 0.0253(17) 0.0220(17) 0.0261(18) 0.0101(14) 0.0109(14) 0.0122(14) O3 0.0312(18) 0.0277(18) 0.0206(18) -0.0021(14) 0.0055(14) 0.0133(15) O4 0.0368(19) 0.0192(17) 0.0216(18) 0.0054(14) 0.0110(15) 0.0129(15) O5 0.0136(16) 0.045(2) 0.0263(19) 0.0062(16) 0.0046(14) 0.0097(15) O6 0.0308(18) 0.0238(18) 0.041(2) 0.0095(16) 0.0169(16) 0.0134(15) O7 0.0359(19) 0.0257(18) 0.0272(19) 0.0135(15) 0.0151(15) 0.0175(16) O8 0.0192(17) 0.048(2) 0.0174(18) 0.0003(16) -0.0047(14) 0.0083(16) O9 0.0270(18) 0.040(2) 0.0259(19) -0.0011(16) -0.0009(15) 0.0165(16) O10 0.0293(19) 0.0197(18) 0.045(2) 0.0066(16) 0.0153(16) 0.0056(15) O11 0.043(2) 0.0205(18) 0.038(2) -0.0026(16) 0.0006(17) 0.0095(16) O12 0.053(2) 0.029(2) 0.049(2) 0.0199(18) 0.0230(19) 0.0225(18) O13 0.032(2) 0.059(3) 0.030(2) 0.0276(19) 0.0044(16) 0.0206(19) O14 0.0264(19) 0.035(2) 0.038(2) 0.0148(17) -0.0057(16) -0.0086(16) O15 0.047(2) 0.038(2) 0.053(3) 0.0117(19) -0.0127(19) 0.0260(19) O16 0.046(2) 0.061(3) 0.034(2) 0.024(2) -0.0086(18) 0.020(2) N1 0.029(2) 0.029(2) 0.021(2) 0.0086(18) 0.0021(17) 0.0160(18) N2 0.037(3) 0.059(3) 0.032(3) 0.024(2) 0.012(2) 0.029(2) N3 0.032(2) 0.033(2) 0.031(2) 0.000(2) -0.0028(19) 0.015(2) N4 0.030(2) 0.031(2) 0.032(2) 0.0030(19) 0.0073(19) 0.0141(19) N5 0.028(2) 0.020(2) 0.031(2) 0.0075(18) 0.0003(18) 0.0110(18) C1 0.026(3) 0.036(3) 0.036(3) 0.013(2) -0.002(2) 0.013(2) C2 0.033(3) 0.056(4) 0.022(3) 0.001(3) 0.001(2) 0.023(3) C3 0.024(3) 0.027(3) 0.043(3) 0.005(2) 0.001(2) 0.012(2) C4 0.024(3) 0.027(3) 0.031(3) 0.009(2) 0.001(2) 0.006(2) C5 0.034(3) 0.025(3) 0.032(3) 0.007(2) 0.011(2) 0.011(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 Ho1 O8 2.289(3) . ? Ho1 O3 2.297(3) 2_775 ? Ho1 O2 2.358(3) . ? Ho1 O7 2.369(3) . ? Ho1 O4 2.376(3) . ? Ho1 O6 2.388(3) . ? Ho1 O1 2.404(3) . ? Ho1 O9 2.453(3) . ? Ho1 S3 2.9775(14) . ? Ho1 S1 2.9950(13) . ? Ho1 S4 3.0553(12) . ? S1 O16 1.435(4) . ? S1 O10 1.455(3) . ? S1 O4 1.495(3) . ? S1 O2 1.510(3) . ? S2 O12 1.448(3) . ? S2 O5 1.455(3) . ? S2 O8 1.478(3) . ? S2 O3 1.482(3) . ? S3 O11 1.447(3) . ? S3 O15 1.455(3) . ? S3 O6 1.483(3) . ? S3 O7 1.490(3) . ? S4 O13 1.446(3) . ? S4 O14 1.457(3) . ? S4 O9 1.485(3) . ? S4 O1 1.509(3) . ? O3 Ho1 2.297(3) 2_775 ? N1 C1 1.480(6) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N2 C2 1.467(7) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N3 C3 1.480(6) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.478(6) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? N5 C5 1.477(6) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? C1 C2 1.515(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.493(9) 2_564 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.509(6) . ? C4 H4A 0.9700 . ? C4 H4B 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 O8 Ho1 O3 78.14(11) . 2_775 ? O8 Ho1 O2 81.52(12) . . ? O3 Ho1 O2 93.14(11) 2_775 . ? O8 Ho1 O7 107.24(12) . . ? O3 Ho1 O7 73.71(11) 2_775 . ? O2 Ho1 O7 161.80(11) . . ? O8 Ho1 O4 83.12(11) . . ? O3 Ho1 O4 148.81(11) 2_775 . ? O2 Ho1 O4 59.32(10) . . ? O7 Ho1 O4 136.32(10) . . ? O8 Ho1 O6 83.86(12) . . ? O3 Ho1 O6 121.17(11) 2_775 . ? O2 Ho1 O6 138.73(11) . . ? O7 Ho1 O6 59.23(11) . . ? O4 Ho1 O6 80.76(11) . . ? O8 Ho1 O1 147.38(12) . . ? O3 Ho1 O1 78.04(11) 2_775 . ? O2 Ho1 O1 77.88(10) . . ? O7 Ho1 O1 86.96(11) . . ? O4 Ho1 O1 107.06(11) . . ? O6 Ho1 O1 127.84(11) . . ? O8 Ho1 O9 151.89(11) . . ? O3 Ho1 O9 129.51(11) 2_775 . ? O2 Ho1 O9 99.55(11) . . ? O7 Ho1 O9 80.33(11) . . ? O4 Ho1 O9 73.75(11) . . ? O6 Ho1 O9 76.94(11) . . ? O1 Ho1 O9 57.77(11) . . ? O8 Ho1 S3 96.58(10) . . ? O3 Ho1 S3 98.10(8) 2_775 . ? O2 Ho1 S3 167.98(8) . . ? O7 Ho1 S3 29.67(8) . . ? O4 Ho1 S3 108.71(8) . . ? O6 Ho1 S3 29.56(8) . . ? O1 Ho1 S3 108.57(8) . . ? O9 Ho1 S3 76.52(8) . . ? O8 Ho1 S1 82.75(9) . . ? O3 Ho1 S1 122.21(9) 2_775 . ? O2 Ho1 S1 29.85(8) . . ? O7 Ho1 S1 163.29(8) . . ? O4 Ho1 S1 29.55(8) . . ? O6 Ho1 S1 110.04(8) . . ? O1 Ho1 S1 91.45(8) . . ? O9 Ho1 S1 84.75(9) . . ? S3 Ho1 S1 138.23(3) . . ? O8 Ho1 S4 169.36(9) . . ? O3 Ho1 S4 104.62(8) 2_775 . ? O2 Ho1 S4 88.04(8) . . ? O7 Ho1 S4 83.36(8) . . ? O4 Ho1 S4 89.82(8) . . ? O6 Ho1 S4 102.91(9) . . ? O1 Ho1 S4 29.08(8) . . ? O9 Ho1 S4 28.71(8) . . ? S3 Ho1 S4 93.21(3) . . ? S1 Ho1 S4 87.18(3) . . ? O16 S1 O10 110.7(2) . . ? O16 S1 O4 112.8(2) . . ? O10 S1 O4 110.70(19) . . ? O16 S1 O2 110.7(2) . . ? O10 S1 O2 109.05(19) . . ? O4 S1 O2 102.47(18) . . ? O16 S1 Ho1 122.83(16) . . ? O10 S1 Ho1 126.36(16) . . ? O4 S1 Ho1 51.61(12) . . ? O2 S1 Ho1 51.03(12) . . ? O12 S2 O5 112.2(2) . . ? O12 S2 O8 111.2(2) . . ? O5 S2 O8 107.88(19) . . ? O12 S2 O3 109.6(2) . . ? O5 S2 O3 107.76(19) . . ? O8 S2 O3 108.1(2) . . ? O11 S3 O15 110.3(2) . . ? O11 S3 O6 111.3(2) . . ? O15 S3 O6 110.9(2) . . ? O11 S3 O7 111.0(2) . . ? O15 S3 O7 108.7(2) . . ? O6 S3 O7 104.52(18) . . ? O11 S3 Ho1 125.19(16) . . ? O15 S3 Ho1 124.48(15) . . ? O6 S3 Ho1 52.62(13) . . ? O7 S3 Ho1 51.90(12) . . ? O13 S4 O14 110.5(2) . . ? O13 S4 O9 112.2(2) . . ? O14 S4 O9 111.5(2) . . ? O13 S4 O1 110.1(2) . . ? O14 S4 O1 109.0(2) . . ? O9 S4 O1 103.24(18) . . ? O13 S4 Ho1 124.00(15) . . ? O14 S4 Ho1 125.35(15) . . ? O9 S4 Ho1 52.52(13) . . ? O1 S4 Ho1 50.75(12) . . ? S4 O1 Ho1 100.17(15) . . ? S1 O2 Ho1 99.12(15) . . ? S2 O3 Ho1 145.0(2) . 2_775 ? S1 O4 Ho1 98.84(15) . . ? S3 O6 Ho1 97.81(16) . . ? S3 O7 Ho1 98.43(15) . . ? S2 O8 Ho1 145.9(2) . . ? S4 O9 Ho1 98.77(16) . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? N1 C1 C2 111.7(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 113.5(4) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N3 C3 C3 111.4(5) . 2_564 ? N3 C3 H3A 109.4 . . ? C3 C3 H3A 109.4 2_564 . ? N3 C3 H3B 109.4 . . ? C3 C3 H3B 109.4 2_564 . ? H3A C3 H3B 108.0 . . ? N4 C4 C5 113.2(4) . . ? N4 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N4 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? N5 C5 C4 114.0(4) . . ? N5 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? N5 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.556 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.138 data_zd-15 _database_code_depnum_ccdc_archive 'CCDC 875287' #TrackingRef '5c.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Er2(SO4)8]' _chemical_formula_sum 'C10 H50 Er2 N10 O32 S8' _chemical_formula_weight 1413.60 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' Er Er -0.2586 4.9576 '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 8.7375(18) _cell_length_b 9.817(2) _cell_length_c 13.443(3) _cell_angle_alpha 98.975(2) _cell_angle_beta 92.892(2) _cell_angle_gamma 115.750(2) _cell_volume 1016.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5022 _cell_measurement_theta_min 2.348 _cell_measurement_theta_max 26.539 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 4.626 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.5437 _exptl_absorpt_correction_T_max 0.6548 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7208 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3542 _reflns_number_gt 3367 _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^)+(0.0280P)^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 3542 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 Er1 Er -0.85417(2) 0.181461(17) 0.208554(12) 0.01305(7) Uani 1 1 d . . . S1 S -0.96573(12) -0.05083(11) 0.34228(7) 0.0191(2) Uani 1 1 d . . . S2 S -0.50895(12) 0.34018(11) 0.34340(7) 0.0195(2) Uani 1 1 d . . . S3 S -0.76468(11) 0.01216(10) -0.02528(7) 0.0148(2) Uani 1 1 d . . . S4 S -0.86163(12) 0.47766(11) 0.19553(8) 0.0201(2) Uani 1 1 d . . . O1 O -0.5615(3) 0.2295(3) 0.2420(2) 0.0233(6) Uani 1 1 d . . . O2 O -0.8828(3) -0.0535(3) 0.2464(2) 0.0210(6) Uani 1 1 d . . . O3 O -0.7910(4) 0.1264(3) 0.0488(2) 0.0256(7) Uani 1 1 d . . . O4 O -0.5886(3) 0.0853(4) -0.0481(2) 0.0283(7) Uani 1 1 d . . . O5 O -0.9913(4) 0.0900(3) 0.3487(2) 0.0238(6) Uani 1 1 d . . . O6 O -0.7486(4) 0.4138(3) 0.1482(2) 0.0270(7) Uani 1 1 d . . . O7 O -0.9720(4) 0.3576(3) 0.2500(2) 0.0285(7) Uani 1 1 d . . . O8 O -0.6653(4) 0.3583(4) 0.3605(2) 0.0309(7) Uani 1 1 d . . . O9 O -0.8817(3) -0.0253(4) -0.1201(2) 0.0288(7) Uani 1 1 d . . . O10 O -1.1298(4) -0.1881(3) 0.3292(2) 0.0309(7) Uani 1 1 d . . . O11 O -0.7598(4) 0.6234(3) 0.2659(2) 0.0342(8) Uani 1 1 d . . . O12 O -0.8001(4) -0.1246(4) 0.0161(3) 0.0384(8) Uani 1 1 d . . . O13 O -0.4593(4) 0.2739(4) 0.4209(2) 0.0377(8) Uani 1 1 d . . . O14 O -0.9636(4) 0.4981(4) 0.1152(3) 0.0406(8) Uani 1 1 d . . . O15 O -0.3673(4) 0.4855(4) 0.3340(2) 0.0394(9) Uani 1 1 d . . . N5 N -0.5758(4) 0.9156(4) 0.2181(2) 0.0245(8) Uani 1 1 d . . . H5C H -0.5561 0.9400 0.1574 0.037 Uiso 1 1 calc R . . H5D H -0.6369 0.9598 0.2468 0.037 Uiso 1 1 calc R . . H5E H -0.6338 0.8136 0.2108 0.037 Uiso 1 1 calc R . . N2 N -0.1133(4) 0.6893(4) 0.0855(3) 0.0265(8) Uani 1 1 d . . . H2C H -0.0627 0.7833 0.1245 0.040 Uiso 1 1 calc R . . H2D H -0.1328 0.6966 0.0214 0.040 Uiso 1 1 calc R . . H2E H -0.0452 0.6437 0.0894 0.040 Uiso 1 1 calc R . . N1 N -0.3263(5) 0.3240(4) 0.0981(3) 0.0313(9) Uani 1 1 d . . . H1C H -0.3867 0.2309 0.0592 0.047 Uiso 1 1 calc R . . H1D H -0.3476 0.3206 0.1619 0.047 Uiso 1 1 calc R . . H1E H -0.2150 0.3536 0.0955 0.047 Uiso 1 1 calc R . . N3 N 0.9101(5) 0.6419(4) 0.4931(3) 0.0301(9) Uani 1 1 d . . . H3C H 0.9613 0.7415 0.4902 0.045 Uiso 1 1 calc R . . H3D H 0.8577 0.6299 0.5485 0.045 Uiso 1 1 calc R . . H3E H 0.8334 0.5895 0.4382 0.045 Uiso 1 1 calc R . . O16 O -0.8555(4) -0.0442(4) 0.4279(2) 0.0450(9) Uani 1 1 d . . . N4 N -0.4413(5) 0.7780(5) 0.3920(3) 0.0370(10) Uani 1 1 d . . . H4C H -0.4551 0.7605 0.4547 0.056 Uiso 1 1 calc R . . H4D H -0.3443 0.7770 0.3757 0.056 Uiso 1 1 calc R . . H4E H -0.5293 0.7049 0.3485 0.056 Uiso 1 1 calc R . . C2 C -0.2774(5) 0.5971(5) 0.1210(3) 0.0277(10) Uani 1 1 d . . . H2A H -0.3489 0.6498 0.1185 0.033 Uiso 1 1 calc R . . H2B H -0.2546 0.5924 0.1914 0.033 Uiso 1 1 calc R . . C1 C -0.3755(5) 0.4356(5) 0.0608(3) 0.0278(10) Uani 1 1 d . . . H1A H -0.4970 0.4022 0.0635 0.033 Uiso 1 1 calc R . . H1B H -0.3564 0.4354 -0.0096 0.033 Uiso 1 1 calc R . . C3 C 1.0394(6) 0.5835(5) 0.4974(4) 0.0312(10) Uani 1 1 d . . . H3A H 1.1241 0.6422 0.5567 0.037 Uiso 1 1 calc R . . H3B H 1.0978 0.5985 0.4376 0.037 Uiso 1 1 calc R . . C5 C -0.4111(5) 0.9707(5) 0.2831(3) 0.0313(11) Uani 1 1 d . . . H5A H -0.3485 1.0819 0.2907 0.038 Uiso 1 1 calc R . . H5B H -0.3431 0.9257 0.2499 0.038 Uiso 1 1 calc R . . C4 C -0.4335(6) 0.9305(5) 0.3872(3) 0.0351(12) Uani 1 1 d . . . H4A H -0.3387 1.0091 0.4358 0.042 Uiso 1 1 calc R . . H4B H -0.5382 0.9316 0.4071 0.042 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 Er1 0.01431(10) 0.01363(10) 0.01096(11) 0.00181(7) 0.00073(7) 0.00635(7) S1 0.0200(5) 0.0196(5) 0.0160(5) 0.0075(4) 0.0029(4) 0.0062(4) S2 0.0156(5) 0.0221(5) 0.0150(5) 0.0056(4) -0.0019(4) 0.0030(4) S3 0.0137(5) 0.0176(5) 0.0121(5) 0.0010(4) 0.0010(4) 0.0069(4) S4 0.0211(5) 0.0161(5) 0.0246(6) 0.0035(4) 0.0005(4) 0.0102(4) O1 0.0199(14) 0.0296(16) 0.0203(15) -0.0006(12) -0.0013(12) 0.0131(12) O2 0.0246(15) 0.0245(15) 0.0208(15) 0.0096(12) 0.0115(12) 0.0146(12) O3 0.0333(16) 0.0288(16) 0.0160(15) -0.0027(12) 0.0039(12) 0.0174(13) O4 0.0144(14) 0.0440(18) 0.0226(16) 0.0041(14) 0.0057(12) 0.0100(13) O5 0.0373(17) 0.0177(14) 0.0181(15) 0.0053(11) 0.0105(13) 0.0125(13) O6 0.0348(17) 0.0253(15) 0.0299(17) 0.0123(13) 0.0126(14) 0.0185(14) O7 0.0275(16) 0.0211(15) 0.0421(19) 0.0119(13) 0.0177(14) 0.0124(13) O8 0.0267(16) 0.0425(18) 0.0203(16) -0.0059(14) -0.0035(13) 0.0173(14) O9 0.0161(14) 0.0451(18) 0.0164(15) -0.0020(13) -0.0027(12) 0.0088(13) O10 0.0277(16) 0.0184(15) 0.0392(19) 0.0066(13) 0.0104(14) 0.0027(13) O11 0.0418(19) 0.0182(15) 0.0345(19) -0.0022(13) 0.0018(15) 0.0088(14) O12 0.052(2) 0.0301(17) 0.042(2) 0.0169(15) 0.0184(17) 0.0219(16) O13 0.0301(17) 0.060(2) 0.0281(18) 0.0251(16) 0.0021(14) 0.0194(16) O14 0.0396(19) 0.0360(18) 0.052(2) 0.0125(16) -0.0111(16) 0.0224(16) O15 0.0287(17) 0.0357(18) 0.0326(19) 0.0132(15) -0.0006(14) -0.0064(14) N5 0.0282(19) 0.0277(19) 0.0218(19) 0.0068(15) 0.0026(15) 0.0157(16) N2 0.0282(19) 0.0212(18) 0.027(2) 0.0036(15) -0.0005(16) 0.0092(15) N1 0.033(2) 0.029(2) 0.029(2) 0.0001(16) 0.0067(17) 0.0124(17) N3 0.033(2) 0.033(2) 0.023(2) -0.0019(16) -0.0052(16) 0.0160(17) O16 0.043(2) 0.062(2) 0.0296(19) 0.0212(17) -0.0070(16) 0.0205(18) N4 0.036(2) 0.060(3) 0.027(2) 0.019(2) 0.0081(18) 0.028(2) C2 0.032(2) 0.030(2) 0.021(2) 0.0068(18) 0.0098(19) 0.012(2) C1 0.027(2) 0.027(2) 0.023(2) 0.0081(18) -0.0003(19) 0.0061(19) C3 0.026(2) 0.029(2) 0.038(3) 0.007(2) 0.001(2) 0.0110(19) C5 0.022(2) 0.036(3) 0.033(3) 0.011(2) -0.0015(19) 0.010(2) C4 0.034(3) 0.050(3) 0.022(3) -0.005(2) -0.003(2) 0.024(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 Er1 O9 2.274(3) 2_355 ? Er1 O3 2.287(3) . ? Er1 O2 2.350(3) . ? Er1 O6 2.353(3) . ? Er1 O5 2.369(3) . ? Er1 O7 2.380(3) . ? Er1 O1 2.394(3) . ? Er1 O8 2.444(3) . ? Er1 S4 2.9687(11) . ? Er1 S1 2.9845(10) . ? Er1 S2 3.0489(11) . ? S1 O16 1.438(3) . ? S1 O10 1.458(3) . ? S1 O5 1.484(3) . ? S1 O2 1.513(3) . ? S2 O13 1.452(3) . ? S2 O15 1.456(3) . ? S2 O8 1.477(3) . ? S2 O1 1.514(3) . ? S3 O12 1.448(3) . ? S3 O4 1.460(3) . ? S3 O3 1.483(3) . ? S3 O9 1.484(3) . ? S4 O11 1.456(3) . ? S4 O14 1.458(3) . ? S4 O7 1.486(3) . ? S4 O6 1.500(3) . ? O9 Er1 2.274(3) 2_355 ? N5 C5 1.475(5) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N2 C2 1.476(5) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N1 C1 1.481(6) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N3 C3 1.474(6) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.480(6) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.501(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C3 1.493(8) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C4 1.512(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O9 Er1 O3 77.76(10) 2_355 . ? O9 Er1 O2 81.75(10) 2_355 . ? O3 Er1 O2 92.76(10) . . ? O9 Er1 O6 107.05(11) 2_355 . ? O3 Er1 O6 73.75(10) . . ? O2 Er1 O6 161.40(10) . . ? O9 Er1 O5 83.23(10) 2_355 . ? O3 Er1 O5 148.40(10) . . ? O2 Er1 O5 59.41(9) . . ? O6 Er1 O5 136.66(10) . . ? O9 Er1 O7 83.96(11) 2_355 . ? O3 Er1 O7 121.67(10) . . ? O2 Er1 O7 138.63(9) . . ? O6 Er1 O7 59.72(10) . . ? O5 Er1 O7 80.50(10) . . ? O9 Er1 O1 147.32(10) 2_355 . ? O3 Er1 O1 77.98(10) . . ? O2 Er1 O1 77.90(9) . . ? O6 Er1 O1 86.64(10) . . ? O5 Er1 O1 107.33(10) . . ? O7 Er1 O1 127.73(10) . . ? O9 Er1 O8 152.08(10) 2_355 . ? O3 Er1 O8 129.68(10) . . ? O2 Er1 O8 99.59(10) . . ? O6 Er1 O8 80.39(11) . . ? O5 Er1 O8 73.93(10) . . ? O7 Er1 O8 76.72(10) . . ? O1 Er1 O8 57.84(9) . . ? O9 Er1 S4 96.40(8) 2_355 . ? O3 Er1 S4 98.37(8) . . ? O2 Er1 S4 168.08(7) . . ? O6 Er1 S4 29.98(7) . . ? O5 Er1 S4 108.72(7) . . ? O7 Er1 S4 29.74(7) . . ? O1 Er1 S4 108.52(7) . . ? O8 Er1 S4 76.52(8) . . ? O9 Er1 S1 82.98(8) 2_355 . ? O3 Er1 S1 122.01(8) . . ? O2 Er1 S1 30.06(7) . . ? O6 Er1 S1 163.44(8) . . ? O5 Er1 S1 29.43(7) . . ? O7 Er1 S1 109.69(7) . . ? O1 Er1 S1 91.68(7) . . ? O8 Er1 S1 84.77(8) . . ? S4 Er1 S1 138.12(3) . . ? O9 Er1 S2 169.65(8) 2_355 . ? O3 Er1 S2 104.83(8) . . ? O2 Er1 S2 88.08(7) . . ? O6 Er1 S2 83.25(8) . . ? O5 Er1 S2 89.93(7) . . ? O7 Er1 S2 102.62(8) . . ? O1 Er1 S2 29.26(7) . . ? O8 Er1 S2 28.59(7) . . ? S4 Er1 S2 93.14(3) . . ? S1 Er1 S2 87.25(3) . . ? O16 S1 O10 110.4(2) . . ? O16 S1 O5 113.1(2) . . ? O10 S1 O5 110.79(17) . . ? O16 S1 O2 110.42(19) . . ? O10 S1 O2 109.27(17) . . ? O5 S1 O2 102.55(15) . . ? O16 S1 Er1 122.79(14) . . ? O10 S1 Er1 126.73(14) . . ? O5 S1 Er1 51.66(11) . . ? O2 S1 Er1 51.06(10) . . ? O13 S2 O15 110.73(19) . . ? O13 S2 O8 112.72(19) . . ? O15 S2 O8 111.4(2) . . ? O13 S2 O1 109.82(19) . . ? O15 S2 O1 108.87(18) . . ? O8 S2 O1 102.94(16) . . ? O13 S2 Er1 124.00(14) . . ? O15 S2 Er1 125.11(14) . . ? O8 S2 Er1 52.34(11) . . ? O1 S2 Er1 50.63(10) . . ? O12 S3 O4 111.98(19) . . ? O12 S3 O3 109.91(18) . . ? O4 S3 O3 107.99(17) . . ? O12 S3 O9 111.00(19) . . ? O4 S3 O9 108.10(17) . . ? O3 S3 O9 107.70(17) . . ? O11 S4 O14 110.64(19) . . ? O11 S4 O7 110.94(18) . . ? O14 S4 O7 111.14(19) . . ? O11 S4 O6 110.80(18) . . ? O14 S4 O6 108.88(19) . . ? O7 S4 O6 104.26(16) . . ? O11 S4 Er1 124.91(14) . . ? O14 S4 Er1 124.42(14) . . ? O7 S4 Er1 52.60(11) . . ? O6 S4 Er1 51.66(11) . . ? S2 O1 Er1 100.10(14) . . ? S1 O2 Er1 98.88(13) . . ? S3 O3 Er1 145.28(18) . . ? S1 O5 Er1 98.92(14) . . ? S4 O6 Er1 98.36(14) . . ? S4 O7 Er1 97.66(14) . . ? S2 O8 Er1 99.07(14) . . ? S3 O9 Er1 146.30(18) . 2_355 ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N2 C2 C1 114.5(4) . . ? N2 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N1 C1 C2 113.2(4) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N3 C3 C3 111.8(5) . 2_766 ? N3 C3 H3A 109.3 . . ? C3 C3 H3A 109.3 2_766 . ? N3 C3 H3B 109.3 . . ? C3 C3 H3B 109.3 2_766 . ? H3A C3 H3B 107.9 . . ? N5 C5 C4 112.8(4) . . ? N5 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C4 C5 113.5(4) . . ? N4 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N4 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.501 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.147 data_zd-14 _database_code_depnum_ccdc_archive 'CCDC 875288' #TrackingRef '5d.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Tm2(SO4)8]' _chemical_formula_sum 'C10 H50 N10 O32 S8 Tm2' _chemical_formula_weight 1416.94 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' Tm Tm -0.3139 5.2483 '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 8.727(4) _cell_length_b 9.793(4) _cell_length_c 13.407(9) _cell_angle_alpha 99.014(7) _cell_angle_beta 93.045(7) _cell_angle_gamma 115.736(4) _cell_volume 1010.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2237 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 23.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 4.895 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.5686 _exptl_absorpt_correction_T_max 0.6403 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7394 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3671 _reflns_number_gt 3262 _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^)+(0.0280P)^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 3671 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Tm1 Tm -0.85448(3) 0.18113(3) 0.208350(17) 0.01457(9) Uani 1 1 d . . . S1 S -0.96540(18) -0.05030(16) 0.34188(11) 0.0205(3) Uani 1 1 d . . . S2 S -0.50988(17) 0.33945(16) 0.34263(11) 0.0210(3) Uani 1 1 d . . . S3 S -0.76519(16) 0.01152(15) -0.02504(10) 0.0163(3) Uani 1 1 d . . . S4 S -0.86107(18) 0.47708(16) 0.19549(11) 0.0224(3) Uani 1 1 d . . . O1 O -0.5624(5) 0.2293(4) 0.2416(3) 0.0251(9) Uani 1 1 d . . . O2 O -0.8830(5) -0.0526(4) 0.2460(3) 0.0222(9) Uani 1 1 d . . . O3 O -0.7921(5) 0.1245(4) 0.0495(3) 0.0268(9) Uani 1 1 d . . . O4 O -0.5897(5) 0.0860(5) -0.0478(3) 0.0303(10) Uani 1 1 d . . . O5 O -0.9905(5) 0.0908(4) 0.3474(3) 0.0252(9) Uani 1 1 d . . . O6 O -0.7500(5) 0.4117(4) 0.1478(3) 0.0250(9) Uani 1 1 d . . . O7 O -0.9719(5) 0.3567(4) 0.2496(3) 0.0309(10) Uani 1 1 d . . . O8 O -0.6659(5) 0.3576(5) 0.3601(3) 0.0301(10) Uani 1 1 d . . . O9 O -0.8822(5) -0.0260(5) -0.1204(3) 0.0293(10) Uani 1 1 d . . . O10 O -1.1285(5) -0.1869(4) 0.3286(3) 0.0315(10) Uani 1 1 d . . . O11 O -0.7592(5) 0.6221(4) 0.2657(3) 0.0369(11) Uani 1 1 d . . . O12 O -0.7995(6) -0.1255(5) 0.0153(3) 0.0379(11) Uani 1 1 d . . . O13 O -0.4607(5) 0.2723(5) 0.4208(3) 0.0381(11) Uani 1 1 d . . . O14 O -0.9625(6) 0.4989(5) 0.1152(3) 0.0430(12) Uani 1 1 d . . . O15 O -0.3685(5) 0.4842(5) 0.3338(3) 0.0413(12) Uani 1 1 d . . . N5 N -0.5774(6) 0.9151(5) 0.2177(3) 0.0262(11) Uani 1 1 d . . . H5C H -0.5576 0.9396 0.1569 0.039 Uiso 1 1 calc R . . H5D H -0.6383 0.9596 0.2465 0.039 Uiso 1 1 calc R . . H5E H -0.6358 0.8128 0.2103 0.039 Uiso 1 1 calc R . . N2 N -0.1131(6) 0.6883(5) 0.0860(3) 0.0244(11) Uani 1 1 d . . . H2C H -0.0620 0.7828 0.1249 0.037 Uiso 1 1 calc R . . H2D H -0.1327 0.6952 0.0216 0.037 Uiso 1 1 calc R . . H2E H -0.0455 0.6422 0.0902 0.037 Uiso 1 1 calc R . . N1 N -0.3267(6) 0.3229(5) 0.0984(4) 0.0294(12) Uani 1 1 d . . . H1C H -0.3876 0.2297 0.0591 0.044 Uiso 1 1 calc R . . H1D H -0.3481 0.3194 0.1624 0.044 Uiso 1 1 calc R . . H1E H -0.2153 0.3520 0.0961 0.044 Uiso 1 1 calc R . . N3 N 0.9091(6) 0.6412(6) 0.4932(4) 0.0309(12) Uani 1 1 d . . . H3C H 0.9591 0.7411 0.4902 0.046 Uiso 1 1 calc R . . H3D H 0.8571 0.6288 0.5488 0.046 Uiso 1 1 calc R . . H3E H 0.8319 0.5880 0.4381 0.046 Uiso 1 1 calc R . . O16 O -0.8536(6) -0.0418(6) 0.4282(3) 0.0487(13) Uani 1 1 d . . . N4 N -0.4408(6) 0.7791(6) 0.3920(4) 0.0340(13) Uani 1 1 d . . . H4C H -0.4547 0.7618 0.4549 0.051 Uiso 1 1 calc R . . H4D H -0.3435 0.7784 0.3760 0.051 Uiso 1 1 calc R . . H4E H -0.5287 0.7055 0.3482 0.051 Uiso 1 1 calc R . . C2 C -0.2777(8) 0.5969(7) 0.1214(5) 0.0316(15) Uani 1 1 d . . . H2A H -0.3490 0.6498 0.1185 0.038 Uiso 1 1 calc R . . H2B H -0.2552 0.5922 0.1921 0.038 Uiso 1 1 calc R . . C1 C -0.3749(7) 0.4361(7) 0.0612(4) 0.0309(15) Uani 1 1 d . . . H1A H -0.4967 0.4028 0.0632 0.037 Uiso 1 1 calc R . . H1B H -0.3553 0.4361 -0.0094 0.037 Uiso 1 1 calc R . . C3 C 1.0411(8) 0.5840(6) 0.4973(5) 0.0318(15) Uani 1 1 d . . . H3A H 1.1264 0.6430 0.5567 0.038 Uiso 1 1 calc R . . H3B H 1.0987 0.5983 0.4371 0.038 Uiso 1 1 calc R . . C5 C -0.4113(7) 0.9704(7) 0.2835(5) 0.0318(15) Uani 1 1 d . . . H5A H -0.3483 1.0818 0.2913 0.038 Uiso 1 1 calc R . . H5B H -0.3435 0.9250 0.2503 0.038 Uiso 1 1 calc R . . C4 C -0.4336(8) 0.9305(8) 0.3869(5) 0.0367(16) Uani 1 1 d . . . H4A H -0.3389 1.0096 0.4359 0.044 Uiso 1 1 calc R . . H4B H -0.5386 0.9313 0.4065 0.044 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 Tm1 0.01488(14) 0.01454(13) 0.01372(14) 0.00224(9) 0.00088(9) 0.00638(10) S1 0.0196(7) 0.0206(7) 0.0194(7) 0.0071(6) 0.0015(6) 0.0064(6) S2 0.0153(7) 0.0245(8) 0.0183(7) 0.0061(6) -0.0012(6) 0.0041(6) S3 0.0147(7) 0.0189(7) 0.0139(7) 0.0004(6) 0.0005(5) 0.0073(6) S4 0.0222(8) 0.0170(7) 0.0283(8) 0.0033(6) -0.0007(6) 0.0100(6) O1 0.024(2) 0.031(2) 0.022(2) -0.0003(18) -0.0001(17) 0.0150(19) O2 0.025(2) 0.022(2) 0.024(2) 0.0086(17) 0.0107(17) 0.0130(18) O3 0.031(2) 0.027(2) 0.021(2) -0.0022(18) 0.0031(18) 0.0144(19) O4 0.014(2) 0.042(3) 0.027(2) 0.002(2) 0.0026(18) 0.0062(19) O5 0.035(2) 0.019(2) 0.020(2) 0.0028(17) 0.0101(18) 0.0100(19) O6 0.032(2) 0.027(2) 0.027(2) 0.0120(18) 0.0126(19) 0.0192(19) O7 0.030(2) 0.022(2) 0.046(3) 0.0075(19) 0.013(2) 0.0154(19) O8 0.029(2) 0.039(3) 0.022(2) -0.0038(19) -0.0009(18) 0.018(2) O9 0.018(2) 0.046(3) 0.016(2) -0.0046(19) -0.0042(17) 0.010(2) O10 0.030(2) 0.019(2) 0.040(3) 0.0085(19) 0.014(2) 0.0041(19) O11 0.042(3) 0.018(2) 0.036(3) -0.0048(19) -0.004(2) 0.005(2) O12 0.050(3) 0.027(2) 0.042(3) 0.013(2) 0.010(2) 0.020(2) O13 0.033(3) 0.057(3) 0.032(3) 0.026(2) 0.005(2) 0.021(2) O14 0.048(3) 0.040(3) 0.052(3) 0.012(2) -0.010(2) 0.031(2) O15 0.032(3) 0.034(3) 0.036(3) 0.010(2) -0.004(2) -0.006(2) N5 0.030(3) 0.028(3) 0.028(3) 0.006(2) 0.003(2) 0.021(2) N2 0.028(3) 0.021(3) 0.025(3) 0.006(2) 0.001(2) 0.011(2) N1 0.026(3) 0.028(3) 0.030(3) 0.004(2) 0.009(2) 0.009(2) N3 0.031(3) 0.029(3) 0.030(3) -0.004(2) -0.003(2) 0.016(2) O16 0.044(3) 0.067(3) 0.035(3) 0.025(2) -0.008(2) 0.021(3) N4 0.031(3) 0.056(4) 0.027(3) 0.018(3) 0.010(2) 0.026(3) C2 0.031(4) 0.035(4) 0.031(4) 0.004(3) 0.011(3) 0.016(3) C1 0.024(3) 0.028(3) 0.029(4) 0.007(3) -0.004(3) 0.002(3) C3 0.026(3) 0.029(4) 0.036(4) 0.004(3) 0.002(3) 0.009(3) C5 0.025(3) 0.038(4) 0.038(4) 0.016(3) 0.003(3) 0.017(3) C4 0.038(4) 0.048(4) 0.025(4) 0.000(3) 0.000(3) 0.023(3) _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 Tm1 O9 2.258(4) 2_355 ? Tm1 O3 2.271(4) . ? Tm1 O2 2.332(4) . ? Tm1 O6 2.336(4) . ? Tm1 O5 2.347(4) . ? Tm1 O7 2.367(4) . ? Tm1 O1 2.385(4) . ? Tm1 O8 2.431(4) . ? Tm1 S4 2.9553(19) . ? Tm1 S1 2.9715(17) . ? Tm1 S2 3.0315(18) . ? S1 O16 1.441(4) . ? S1 O10 1.446(4) . ? S1 O5 1.482(4) . ? S1 O2 1.507(4) . ? S2 O15 1.447(4) . ? S2 O13 1.458(4) . ? S2 O8 1.474(4) . ? S2 O1 1.501(4) . ? S3 O12 1.442(4) . ? S3 O4 1.456(4) . ? S3 O3 1.477(4) . ? S3 O9 1.483(4) . ? S4 O11 1.446(4) . ? S4 O14 1.457(4) . ? S4 O7 1.484(4) . ? S4 O6 1.495(4) . ? O9 Tm1 2.258(4) 2_355 ? N5 C5 1.485(7) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N2 C2 1.476(7) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N1 C1 1.487(7) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N3 C3 1.486(7) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.468(7) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.490(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C3 1.499(11) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C4 1.498(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O9 Tm1 O3 77.91(14) 2_355 . ? O9 Tm1 O2 81.82(14) 2_355 . ? O3 Tm1 O2 92.43(13) . . ? O9 Tm1 O6 106.88(14) 2_355 . ? O3 Tm1 O6 73.92(13) . . ? O2 Tm1 O6 161.38(13) . . ? O9 Tm1 O5 83.06(14) 2_355 . ? O3 Tm1 O5 148.12(13) . . ? O2 Tm1 O5 59.45(13) . . ? O6 Tm1 O5 136.76(13) . . ? O9 Tm1 O7 83.74(15) 2_355 . ? O3 Tm1 O7 122.05(14) . . ? O2 Tm1 O7 138.54(13) . . ? O6 Tm1 O7 59.86(13) . . ? O5 Tm1 O7 80.37(13) . . ? O9 Tm1 O1 147.48(14) 2_355 . ? O3 Tm1 O1 77.74(13) . . ? O2 Tm1 O1 78.01(13) . . ? O6 Tm1 O1 86.59(13) . . ? O5 Tm1 O1 107.57(13) . . ? O7 Tm1 O1 127.78(13) . . ? O9 Tm1 O8 151.90(13) 2_355 . ? O3 Tm1 O8 129.74(14) . . ? O2 Tm1 O8 99.53(14) . . ? O6 Tm1 O8 80.64(14) . . ? O5 Tm1 O8 73.94(13) . . ? O7 Tm1 O8 76.79(14) . . ? O1 Tm1 O8 57.88(13) . . ? O9 Tm1 S4 96.40(11) 2_355 . ? O3 Tm1 S4 98.74(10) . . ? O2 Tm1 S4 168.08(9) . . ? O6 Tm1 S4 30.01(9) . . ? O5 Tm1 S4 108.67(10) . . ? O7 Tm1 S4 29.86(10) . . ? O1 Tm1 S4 108.34(9) . . ? O8 Tm1 S4 76.49(10) . . ? O9 Tm1 S1 82.97(11) 2_355 . ? O3 Tm1 S1 121.67(10) . . ? O2 Tm1 S1 30.05(9) . . ? O6 Tm1 S1 163.61(10) . . ? O5 Tm1 S1 29.49(9) . . ? O7 Tm1 S1 109.62(10) . . ? O1 Tm1 S1 91.81(9) . . ? O8 Tm1 S1 84.71(11) . . ? S4 Tm1 S1 138.12(4) . . ? O9 Tm1 S2 169.73(11) 2_355 . ? O3 Tm1 S2 104.62(11) . . ? O2 Tm1 S2 88.10(10) . . ? O6 Tm1 S2 83.34(10) . . ? O5 Tm1 S2 90.15(10) . . ? O7 Tm1 S2 102.76(11) . . ? O1 Tm1 S2 29.19(9) . . ? O8 Tm1 S2 28.71(9) . . ? S4 Tm1 S2 93.06(4) . . ? S1 Tm1 S2 87.32(5) . . ? O16 S1 O10 111.0(3) . . ? O16 S1 O5 112.9(3) . . ? O10 S1 O5 110.9(2) . . ? O16 S1 O2 110.5(3) . . ? O10 S1 O2 109.3(2) . . ? O5 S1 O2 101.8(2) . . ? O16 S1 Tm1 122.29(19) . . ? O10 S1 Tm1 126.66(18) . . ? O5 S1 Tm1 51.22(14) . . ? O2 S1 Tm1 50.78(14) . . ? O15 S2 O13 110.8(3) . . ? O15 S2 O8 111.6(3) . . ? O13 S2 O8 112.2(2) . . ? O15 S2 O1 109.0(2) . . ? O13 S2 O1 109.8(3) . . ? O8 S2 O1 103.1(2) . . ? O15 S2 Tm1 125.42(19) . . ? O13 S2 Tm1 123.65(18) . . ? O8 S2 Tm1 52.38(15) . . ? O1 S2 Tm1 50.79(15) . . ? O12 S3 O4 112.1(3) . . ? O12 S3 O3 110.0(2) . . ? O4 S3 O3 108.0(2) . . ? O12 S3 O9 110.9(3) . . ? O4 S3 O9 107.7(2) . . ? O3 S3 O9 107.9(2) . . ? O11 S4 O14 110.3(3) . . ? O11 S4 O7 111.1(3) . . ? O14 S4 O7 111.3(3) . . ? O11 S4 O6 111.2(3) . . ? O14 S4 O6 108.8(3) . . ? O7 S4 O6 103.9(2) . . ? O11 S4 Tm1 124.87(19) . . ? O14 S4 Tm1 124.82(19) . . ? O7 S4 Tm1 52.55(16) . . ? O6 S4 Tm1 51.40(14) . . ? S2 O1 Tm1 100.02(19) . . ? S1 O2 Tm1 99.18(18) . . ? S3 O3 Tm1 146.2(2) . . ? S1 O5 Tm1 99.29(18) . . ? S4 O6 Tm1 98.59(18) . . ? S4 O7 Tm1 97.6(2) . . ? S2 O8 Tm1 98.91(19) . . ? S3 O9 Tm1 146.1(2) . 2_355 ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N2 C2 C1 114.0(5) . . ? N2 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N1 C1 C2 113.6(5) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N3 C3 C3 110.1(6) . 2_766 ? N3 C3 H3A 109.6 . . ? C3 C3 H3A 109.6 2_766 . ? N3 C3 H3B 109.6 . . ? C3 C3 H3B 109.6 2_766 . ? H3A C3 H3B 108.2 . . ? N5 C5 C4 112.8(5) . . ? N5 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C4 C5 113.6(5) . . ? N4 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N4 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.646 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.158 data_zd-17 _database_code_depnum_ccdc_archive 'CCDC 875289' #TrackingRef '5e.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Yb2(SO4)8]' _chemical_formula_sum 'C10 H50 N10 O32 S8 Yb2' _chemical_formula_weight 1425.16 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' Yb Yb -0.3850 5.5486 '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 8.744(10) _cell_length_b 9.802(12) _cell_length_c 13.444(16) _cell_angle_alpha 99.049(13) _cell_angle_beta 93.013(13) _cell_angle_gamma 115.786(13) _cell_volume 1015(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3027 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.85 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 5.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5350 _exptl_absorpt_correction_T_max 0.6292 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7189 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3538 _reflns_number_gt 3184 _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^)+(0.0280P)^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 3538 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb -0.85505(3) 0.18094(3) 0.208238(19) 0.01519(10) Uani 1 1 d . . . S1 S -0.9651(2) -0.04935(18) 0.34192(12) 0.0212(4) Uani 1 1 d . . . S2 S -0.51044(19) 0.33935(19) 0.34260(12) 0.0217(4) Uani 1 1 d . . . S3 S -0.76559(18) 0.01124(17) -0.02484(11) 0.0175(3) Uani 1 1 d . . . S4 S -0.8613(2) 0.47582(18) 0.19581(12) 0.0223(4) Uani 1 1 d . . . O1 O -0.5645(5) 0.2288(5) 0.2417(3) 0.0262(10) Uani 1 1 d . . . O2 O -0.8829(5) -0.0521(5) 0.2451(3) 0.0204(10) Uani 1 1 d . . . O3 O -0.7944(5) 0.1235(5) 0.0492(3) 0.0257(10) Uani 1 1 d . . . O4 O -0.5903(5) 0.0864(5) -0.0465(3) 0.0306(11) Uani 1 1 d . . . O5 O -0.9917(5) 0.0922(5) 0.3472(3) 0.0244(10) Uani 1 1 d . . . O6 O -0.7519(6) 0.4107(5) 0.1474(3) 0.0280(11) Uani 1 1 d . . . O7 O -0.9722(5) 0.3559(5) 0.2497(3) 0.0293(11) Uani 1 1 d . . . O8 O -0.6669(6) 0.3569(6) 0.3597(3) 0.0327(12) Uani 1 1 d . . . O9 O -0.8821(5) -0.0269(5) -0.1204(3) 0.0309(12) Uani 1 1 d . . . O10 O -1.1280(6) -0.1873(5) 0.3293(4) 0.0339(12) Uani 1 1 d . . . O11 O -0.7579(6) 0.6222(5) 0.2659(4) 0.0354(12) Uani 1 1 d . . . O12 O -0.7986(6) -0.1262(5) 0.0156(4) 0.0370(12) Uani 1 1 d . . . O13 O -0.4612(6) 0.2729(6) 0.4209(4) 0.0380(13) Uani 1 1 d . . . O14 O -0.9637(6) 0.4981(6) 0.1146(4) 0.0449(14) Uani 1 1 d . . . O15 O -0.3698(6) 0.4841(6) 0.3324(4) 0.0401(13) Uani 1 1 d . . . N5 N -0.5770(6) 0.9143(6) 0.2172(4) 0.0245(13) Uani 1 1 d . . . H5C H -0.5578 0.9385 0.1565 0.037 Uiso 1 1 calc R . . H5D H -0.6379 0.9586 0.2460 0.037 Uiso 1 1 calc R . . H5E H -0.6349 0.8121 0.2100 0.037 Uiso 1 1 calc R . . N2 N -0.1133(6) 0.6892(6) 0.0852(4) 0.0266(13) Uani 1 1 d . . . H2C H -0.0616 0.7837 0.1238 0.040 Uiso 1 1 calc R . . H2D H -0.1327 0.6958 0.0209 0.040 Uiso 1 1 calc R . . H2E H -0.0464 0.6426 0.0894 0.040 Uiso 1 1 calc R . . N1 N -0.3258(7) 0.3240(6) 0.0995(4) 0.0279(13) Uani 1 1 d . . . H1C H -0.3863 0.2305 0.0606 0.042 Uiso 1 1 calc R . . H1D H -0.3477 0.3210 0.1633 0.042 Uiso 1 1 calc R . . H1E H -0.2145 0.3533 0.0975 0.042 Uiso 1 1 calc R . . N3 N 0.9088(7) 0.6427(7) 0.4923(4) 0.0341(15) Uani 1 1 d . . . H3C H 0.9598 0.7425 0.4893 0.051 Uiso 1 1 calc R . . H3D H 0.8566 0.6308 0.5476 0.051 Uiso 1 1 calc R . . H3E H 0.8319 0.5898 0.4373 0.051 Uiso 1 1 calc R . . O16 O -0.8540(7) -0.0412(7) 0.4282(4) 0.0491(15) Uani 1 1 d . . . N4 N -0.4403(7) 0.7787(7) 0.3926(4) 0.0358(15) Uani 1 1 d . . . H4C H -0.4541 0.7617 0.4554 0.054 Uiso 1 1 calc R . . H4D H -0.3434 0.7773 0.3766 0.054 Uiso 1 1 calc R . . H4E H -0.5284 0.7052 0.3491 0.054 Uiso 1 1 calc R . . C2 C -0.2776(8) 0.5989(7) 0.1207(5) 0.0299(16) Uani 1 1 d . . . H2A H -0.3490 0.6512 0.1165 0.036 Uiso 1 1 calc R . . H2B H -0.2554 0.5961 0.1917 0.036 Uiso 1 1 calc R . . C1 C -0.3741(8) 0.4361(8) 0.0615(5) 0.0312(17) Uani 1 1 d . . . H1A H -0.4957 0.4024 0.0633 0.037 Uiso 1 1 calc R . . H1B H -0.3544 0.4351 -0.0089 0.037 Uiso 1 1 calc R . . C3 C 1.0392(9) 0.5843(7) 0.4967(6) 0.0338(17) Uani 1 1 d . . . H3A H 1.1249 0.6445 0.5555 0.041 Uiso 1 1 calc R . . H3B H 1.0963 0.5981 0.4365 0.041 Uiso 1 1 calc R . . C5 C -0.4115(8) 0.9702(8) 0.2823(5) 0.0309(17) Uani 1 1 d . . . H5A H -0.3485 1.0814 0.2890 0.037 Uiso 1 1 calc R . . H5B H -0.3444 0.9240 0.2494 0.037 Uiso 1 1 calc R . . C4 C -0.4318(10) 0.9327(9) 0.3873(5) 0.041(2) Uani 1 1 d . . . H4A H -0.3358 1.0121 0.4352 0.049 Uiso 1 1 calc R . . H4B H -0.5356 0.9348 0.4076 0.049 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 Yb1 0.01702(15) 0.01498(15) 0.01248(16) 0.00119(10) 0.00103(10) 0.00684(11) S1 0.0207(8) 0.0206(8) 0.0181(9) 0.0055(7) 0.0032(7) 0.0049(7) S2 0.0167(8) 0.0243(9) 0.0165(8) 0.0036(7) 0.0000(6) 0.0027(7) S3 0.0152(8) 0.0190(8) 0.0144(8) -0.0008(6) 0.0016(6) 0.0058(6) S4 0.0248(9) 0.0175(8) 0.0251(9) 0.0025(7) 0.0002(7) 0.0109(7) O1 0.022(2) 0.026(3) 0.026(3) -0.001(2) 0.000(2) 0.009(2) O2 0.022(2) 0.022(2) 0.022(2) 0.0086(19) 0.0095(19) 0.0125(19) O3 0.036(3) 0.026(2) 0.015(2) -0.0016(19) 0.003(2) 0.016(2) O4 0.017(2) 0.042(3) 0.024(3) -0.002(2) 0.005(2) 0.008(2) O5 0.034(3) 0.019(2) 0.020(2) 0.0051(19) 0.011(2) 0.011(2) O6 0.035(3) 0.029(3) 0.025(3) 0.010(2) 0.012(2) 0.016(2) O7 0.026(3) 0.025(3) 0.039(3) 0.007(2) 0.016(2) 0.013(2) O8 0.031(3) 0.046(3) 0.020(3) 0.000(2) 0.001(2) 0.019(2) O9 0.018(2) 0.042(3) 0.018(3) -0.009(2) -0.0042(19) 0.007(2) O10 0.031(3) 0.022(3) 0.039(3) 0.003(2) 0.016(2) 0.003(2) O11 0.039(3) 0.021(2) 0.034(3) -0.005(2) -0.001(2) 0.006(2) O12 0.051(3) 0.031(3) 0.032(3) 0.012(2) 0.015(2) 0.018(2) O13 0.036(3) 0.056(3) 0.032(3) 0.026(3) 0.000(2) 0.023(3) O14 0.047(3) 0.037(3) 0.054(4) 0.007(3) -0.006(3) 0.025(3) O15 0.031(3) 0.038(3) 0.033(3) 0.012(2) -0.003(2) -0.002(2) N5 0.025(3) 0.025(3) 0.026(3) 0.005(2) -0.003(2) 0.014(3) N2 0.028(3) 0.021(3) 0.030(3) 0.005(3) -0.001(3) 0.010(3) N1 0.034(3) 0.025(3) 0.027(3) 0.007(3) 0.010(3) 0.014(3) N3 0.029(3) 0.034(3) 0.037(4) -0.002(3) -0.002(3) 0.016(3) O16 0.047(3) 0.066(4) 0.028(3) 0.016(3) -0.009(2) 0.019(3) N4 0.036(4) 0.054(4) 0.027(3) 0.018(3) 0.008(3) 0.024(3) C2 0.037(4) 0.027(4) 0.029(4) 0.005(3) 0.008(3) 0.016(3) C1 0.027(4) 0.027(4) 0.027(4) 0.001(3) 0.005(3) 0.002(3) C3 0.027(4) 0.030(4) 0.035(4) -0.001(3) 0.002(3) 0.007(3) C5 0.021(4) 0.030(4) 0.032(4) 0.004(3) 0.000(3) 0.004(3) C4 0.039(4) 0.048(5) 0.028(4) -0.006(4) 0.000(4) 0.018(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 Yb1 O9 2.257(4) 2_355 ? Yb1 O3 2.274(5) . ? Yb1 O2 2.325(5) . ? Yb1 O6 2.334(5) . ? Yb1 O5 2.348(5) . ? Yb1 O7 2.364(5) . ? Yb1 O1 2.378(5) . ? Yb1 O8 2.429(5) . ? Yb1 S4 2.945(4) . ? Yb1 S1 2.970(3) . ? Yb1 S2 3.038(3) . ? S1 O16 1.442(5) . ? S1 O10 1.454(5) . ? S1 O5 1.496(5) . ? S1 O2 1.522(4) . ? S2 O15 1.451(5) . ? S2 O13 1.459(5) . ? S2 O8 1.476(5) . ? S2 O1 1.504(5) . ? S3 O12 1.450(5) . ? S3 O4 1.452(5) . ? S3 O3 1.479(4) . ? S3 O9 1.485(4) . ? S4 O11 1.456(5) . ? S4 O14 1.477(5) . ? S4 O7 1.482(5) . ? S4 O6 1.487(5) . ? O9 Yb1 2.257(4) 2_355 ? N5 C5 1.479(8) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N2 C2 1.475(8) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N1 C1 1.486(8) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N3 C3 1.484(8) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.493(9) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.500(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C3 1.509(13) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C4 1.513(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O9 Yb1 O3 77.57(17) 2_355 . ? O9 Yb1 O2 82.14(17) 2_355 . ? O3 Yb1 O2 92.17(15) . . ? O9 Yb1 O6 106.33(17) 2_355 . ? O3 Yb1 O6 73.92(16) . . ? O2 Yb1 O6 161.25(15) . . ? O9 Yb1 O5 83.15(17) 2_355 . ? O3 Yb1 O5 148.30(16) . . ? O2 Yb1 O5 60.16(14) . . ? O6 Yb1 O5 136.37(15) . . ? O9 Yb1 O7 83.50(18) 2_355 . ? O3 Yb1 O7 122.04(15) . . ? O2 Yb1 O7 138.66(15) . . ? O6 Yb1 O7 59.91(16) . . ? O5 Yb1 O7 79.77(16) . . ? O9 Yb1 O1 147.70(16) 2_355 . ? O3 Yb1 O1 78.18(15) . . ? O2 Yb1 O1 77.78(14) . . ? O6 Yb1 O1 86.94(15) . . ? O5 Yb1 O1 107.70(16) . . ? O7 Yb1 O1 127.82(15) . . ? O9 Yb1 O8 151.85(15) 2_355 . ? O3 Yb1 O8 130.10(16) . . ? O2 Yb1 O8 99.52(17) . . ? O6 Yb1 O8 80.98(17) . . ? O5 Yb1 O8 73.78(17) . . ? O7 Yb1 O8 76.82(17) . . ? O1 Yb1 O8 57.78(15) . . ? O9 Yb1 S4 96.15(14) 2_355 . ? O3 Yb1 S4 98.80(12) . . ? O2 Yb1 S4 168.29(10) . . ? O6 Yb1 S4 29.97(12) . . ? O5 Yb1 S4 108.16(11) . . ? O7 Yb1 S4 29.95(11) . . ? O1 Yb1 S4 108.39(11) . . ? O8 Yb1 S4 76.52(13) . . ? O9 Yb1 S1 83.39(14) 2_355 . ? O3 Yb1 S1 121.76(13) . . ? O2 Yb1 S1 30.41(10) . . ? O6 Yb1 S1 163.59(11) . . ? O5 Yb1 S1 29.85(11) . . ? O7 Yb1 S1 109.42(13) . . ? O1 Yb1 S1 91.58(11) . . ? O8 Yb1 S1 84.41(14) . . ? S4 Yb1 S1 137.96(6) . . ? O9 Yb1 S2 169.94(13) 2_355 . ? O3 Yb1 S2 105.00(13) . . ? O2 Yb1 S2 88.02(11) . . ? O6 Yb1 S2 83.69(12) . . ? O5 Yb1 S2 90.18(13) . . ? O7 Yb1 S2 102.77(14) . . ? O1 Yb1 S2 29.13(11) . . ? O8 Yb1 S2 28.66(11) . . ? S4 Yb1 S2 93.07(7) . . ? S1 Yb1 S2 87.08(7) . . ? O16 S1 O10 110.2(3) . . ? O16 S1 O5 113.4(3) . . ? O10 S1 O5 111.0(3) . . ? O16 S1 O2 110.9(3) . . ? O10 S1 O2 109.3(3) . . ? O5 S1 O2 101.8(2) . . ? O16 S1 Yb1 122.7(2) . . ? O10 S1 Yb1 127.1(2) . . ? O5 S1 Yb1 51.41(17) . . ? O2 S1 Yb1 50.66(17) . . ? O15 S2 O13 111.3(3) . . ? O15 S2 O8 111.7(3) . . ? O13 S2 O8 112.2(3) . . ? O15 S2 O1 108.6(3) . . ? O13 S2 O1 110.2(3) . . ? O8 S2 O1 102.4(3) . . ? O15 S2 Yb1 124.6(2) . . ? O13 S2 Yb1 123.9(2) . . ? O8 S2 Yb1 52.12(19) . . ? O1 S2 Yb1 50.31(17) . . ? O12 S3 O4 111.6(3) . . ? O12 S3 O3 110.2(3) . . ? O4 S3 O3 108.1(3) . . ? O12 S3 O9 111.1(3) . . ? O4 S3 O9 108.0(3) . . ? O3 S3 O9 107.7(3) . . ? O11 S4 O14 110.2(3) . . ? O11 S4 O7 111.4(3) . . ? O14 S4 O7 111.2(3) . . ? O11 S4 O6 111.3(3) . . ? O14 S4 O6 108.2(3) . . ? O7 S4 O6 104.4(3) . . ? O11 S4 Yb1 124.9(2) . . ? O14 S4 Yb1 124.8(2) . . ? O7 S4 Yb1 52.79(18) . . ? O6 S4 Yb1 51.61(18) . . ? S2 O1 Yb1 100.6(2) . . ? S1 O2 Yb1 98.9(2) . . ? S3 O3 Yb1 146.2(3) . . ? S1 O5 Yb1 98.7(2) . . ? S4 O6 Yb1 98.4(2) . . ? S4 O7 Yb1 97.3(2) . . ? S2 O8 Yb1 99.2(2) . . ? S3 O9 Yb1 146.2(3) . 2_355 ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N2 C2 C1 113.8(5) . . ? N2 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N2 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N1 C1 C2 114.1(6) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N3 C3 C3 112.0(7) . 2_766 ? N3 C3 H3A 109.2 . . ? C3 C3 H3A 109.2 2_766 . ? N3 C3 H3B 109.2 . . ? C3 C3 H3B 109.2 2_766 . ? H3A C3 H3B 107.9 . . ? N5 C5 C4 113.2(5) . . ? N5 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? N4 C4 C5 113.1(6) . . ? N4 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N4 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.219 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.164 data_1 _database_code_depnum_ccdc_archive 'CCDC 875290' #TrackingRef '5f.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[H3N(CH2)2NH3]5[Lu2(SO4)8]' _chemical_formula_sum 'C10 H50 Lu2 N10 O32 S8' _chemical_formula_weight 1429.02 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' Lu Lu -0.4720 5.8584 '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 8.7343(6) _cell_length_b 9.7850(7) _cell_length_c 13.3866(14) _cell_angle_alpha 98.9500(10) _cell_angle_beta 93.1600(10) _cell_angle_gamma 115.7150(10) _cell_volume 1008.52(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3122 _cell_measurement_theta_min 2.353 _cell_measurement_theta_max 25.926 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 5.398 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.4788 _exptl_absorpt_correction_T_max 0.6144 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7198 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3516 _reflns_number_gt 3233 _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^)+(0.0280P)^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 3516 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Lu1 Lu -0.85556(2) 0.18078(2) 0.208194(15) 0.01371(8) Uani 1 1 d . . . S1 S -0.96447(16) -0.04845(14) 0.34197(9) 0.0196(3) Uani 1 1 d . . . S2 S -0.51144(15) 0.33921(15) 0.34244(9) 0.0203(3) Uani 1 1 d . . . S3 S -0.76610(14) 0.01033(14) -0.02482(9) 0.0157(3) Uani 1 1 d . . . S4 S -0.86123(16) 0.47589(14) 0.19546(10) 0.0201(3) Uani 1 1 d . . . O1 O -0.5664(4) 0.2278(4) 0.2414(3) 0.0245(8) Uani 1 1 d . . . O2 O -0.8831(4) -0.0519(4) 0.2449(3) 0.0214(8) Uani 1 1 d . . . O3 O -0.7971(4) 0.1221(4) 0.0497(2) 0.0242(8) Uani 1 1 d . . . O4 O -0.5902(4) 0.0879(4) -0.0469(3) 0.0271(9) Uani 1 1 d . . . O5 O -0.9911(4) 0.0922(4) 0.3469(2) 0.0244(8) Uani 1 1 d . . . O6 O -0.7508(4) 0.4099(4) 0.1473(3) 0.0246(8) Uani 1 1 d . . . O7 O -0.9709(4) 0.3558(4) 0.2496(3) 0.0287(9) Uani 1 1 d . . . O8 O -0.6673(4) 0.3578(4) 0.3602(3) 0.0317(9) Uani 1 1 d . . . O9 O -0.8823(4) -0.0290(4) -0.1205(3) 0.0296(9) Uani 1 1 d . . . O10 O -1.1273(4) -0.1858(4) 0.3292(3) 0.0314(9) Uani 1 1 d . . . O11 O -0.7573(5) 0.6216(4) 0.2653(3) 0.0336(9) Uani 1 1 d . . . O12 O -0.7983(5) -0.1263(4) 0.0163(3) 0.0351(10) Uani 1 1 d . . . O13 O -0.4610(5) 0.2734(5) 0.4202(3) 0.0371(10) Uani 1 1 d . . . O14 O -0.9639(5) 0.4974(4) 0.1154(3) 0.0394(10) Uani 1 1 d . . . O15 O -0.3694(5) 0.4844(5) 0.3328(3) 0.0402(10) Uani 1 1 d . . . N5 N -0.5767(5) 0.9144(5) 0.2163(3) 0.0249(10) Uani 1 1 d . . . H5C H -0.5576 0.9386 0.1553 0.037 Uiso 1 1 calc R . . H5D H -0.6382 0.9583 0.2450 0.037 Uiso 1 1 calc R . . H5E H -0.6340 0.8121 0.2092 0.037 Uiso 1 1 calc R . . N2 N -0.1122(5) 0.6903(5) 0.0850(3) 0.0234(10) Uani 1 1 d . . . H2C H -0.0612 0.7848 0.1240 0.035 Uiso 1 1 calc R . . H2D H -0.1315 0.6972 0.0204 0.035 Uiso 1 1 calc R . . H2E H -0.0447 0.6441 0.0893 0.035 Uiso 1 1 calc R . . N1 N -0.3262(6) 0.3251(5) 0.1003(3) 0.0309(11) Uani 1 1 d . . . H1C H -0.3861 0.2310 0.0618 0.046 Uiso 1 1 calc R . . H1D H -0.3479 0.3229 0.1644 0.046 Uiso 1 1 calc R . . H1E H -0.2147 0.3549 0.0985 0.046 Uiso 1 1 calc R . . N3 N 0.9094(5) 0.6424(5) 0.4927(3) 0.0305(11) Uani 1 1 d . . . H3C H 0.9600 0.7423 0.4897 0.046 Uiso 1 1 calc R . . H3D H 0.8578 0.6303 0.5484 0.046 Uiso 1 1 calc R . . H3E H 0.8319 0.5895 0.4376 0.046 Uiso 1 1 calc R . . O16 O -0.8527(5) -0.0388(5) 0.4283(3) 0.0459(11) Uani 1 1 d . . . N4 N -0.4387(6) 0.7819(6) 0.3924(3) 0.0351(12) Uani 1 1 d . . . H4C H -0.4526 0.7640 0.4553 0.053 Uiso 1 1 calc R . . H4D H -0.3411 0.7820 0.3766 0.053 Uiso 1 1 calc R . . H4E H -0.5262 0.7081 0.3483 0.053 Uiso 1 1 calc R . . C2 C -0.2780(7) 0.5981(6) 0.1205(4) 0.0310(13) Uani 1 1 d . . . H2A H -0.3492 0.6511 0.1170 0.037 Uiso 1 1 calc R . . H2B H -0.2555 0.5943 0.1915 0.037 Uiso 1 1 calc R . . C1 C -0.3760(7) 0.4361(6) 0.0607(4) 0.0282(13) Uani 1 1 d . . . H1A H -0.4976 0.4027 0.0628 0.034 Uiso 1 1 calc R . . H1B H -0.3566 0.4346 -0.0100 0.034 Uiso 1 1 calc R . . C3 C 1.0403(7) 0.5840(6) 0.4966(5) 0.0327(14) Uani 1 1 d . . . H3A H 1.1267 0.6439 0.5555 0.039 Uiso 1 1 calc R . . H3B H 1.0965 0.5971 0.4358 0.039 Uiso 1 1 calc R . . C5 C -0.4107(7) 0.9713(6) 0.2821(4) 0.0303(13) Uani 1 1 d . . . H5A H -0.3479 1.0825 0.2886 0.036 Uiso 1 1 calc R . . H5B H -0.3430 0.9251 0.2496 0.036 Uiso 1 1 calc R . . C4 C -0.4328(7) 0.9335(7) 0.3877(4) 0.0339(14) Uani 1 1 d . . . H4A H -0.3383 1.0133 0.4365 0.041 Uiso 1 1 calc R . . H4B H -0.5381 0.9338 0.4069 0.041 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 Lu1 0.01449(12) 0.01298(12) 0.01312(12) 0.00237(8) 0.00211(8) 0.00573(9) S1 0.0203(6) 0.0182(7) 0.0188(7) 0.0078(5) 0.0037(5) 0.0060(6) S2 0.0158(6) 0.0224(7) 0.0174(6) 0.0057(5) -0.0005(5) 0.0034(6) S3 0.0137(6) 0.0165(6) 0.0152(6) 0.0012(5) 0.0021(5) 0.0059(5) S4 0.0216(7) 0.0148(7) 0.0243(7) 0.0030(5) 0.0015(5) 0.0089(6) O1 0.0221(19) 0.028(2) 0.0226(19) 0.0009(16) -0.0003(15) 0.0121(17) O2 0.0247(19) 0.0212(19) 0.0248(19) 0.0105(16) 0.0129(16) 0.0132(16) O3 0.029(2) 0.025(2) 0.0202(19) 0.0017(16) 0.0089(16) 0.0147(17) O4 0.0139(18) 0.039(2) 0.0208(19) 0.0031(17) 0.0047(15) 0.0062(17) O5 0.035(2) 0.0174(19) 0.0190(19) 0.0038(15) 0.0091(16) 0.0098(17) O6 0.034(2) 0.0211(19) 0.027(2) 0.0122(16) 0.0158(17) 0.0152(17) O7 0.026(2) 0.024(2) 0.040(2) 0.0091(18) 0.0159(17) 0.0124(17) O8 0.029(2) 0.041(2) 0.027(2) 0.0014(18) 0.0046(17) 0.020(2) O9 0.0203(19) 0.041(2) 0.018(2) -0.0007(17) -0.0024(16) 0.0082(18) O10 0.026(2) 0.0133(19) 0.043(2) 0.0021(17) 0.0126(18) -0.0022(17) O11 0.035(2) 0.017(2) 0.037(2) -0.0028(17) -0.0037(18) 0.0050(18) O12 0.051(3) 0.025(2) 0.039(2) 0.0156(18) 0.015(2) 0.021(2) O13 0.030(2) 0.055(3) 0.032(2) 0.025(2) 0.0046(18) 0.019(2) O14 0.042(2) 0.031(2) 0.047(3) 0.0091(19) -0.011(2) 0.019(2) O15 0.027(2) 0.034(2) 0.038(2) 0.014(2) 0.0010(19) -0.0075(19) N5 0.029(2) 0.028(3) 0.022(2) 0.005(2) 0.0027(19) 0.016(2) N2 0.023(2) 0.022(2) 0.023(2) 0.0043(19) 0.0019(19) 0.008(2) N1 0.033(3) 0.027(3) 0.033(3) 0.004(2) 0.013(2) 0.014(2) N3 0.029(3) 0.028(3) 0.032(3) -0.002(2) -0.006(2) 0.014(2) O16 0.044(3) 0.063(3) 0.031(2) 0.022(2) -0.006(2) 0.022(2) N4 0.034(3) 0.054(3) 0.024(3) 0.019(2) 0.013(2) 0.022(3) C2 0.030(3) 0.028(3) 0.032(3) 0.004(3) 0.010(3) 0.010(3) C1 0.030(3) 0.025(3) 0.023(3) 0.007(2) 0.003(2) 0.005(3) C3 0.021(3) 0.029(3) 0.045(4) 0.007(3) 0.001(3) 0.008(3) C5 0.024(3) 0.029(3) 0.029(3) 0.006(3) -0.007(2) 0.004(3) C4 0.036(3) 0.044(4) 0.020(3) -0.002(3) -0.003(3) 0.020(3) _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 Lu1 O9 2.244(3) 2_355 ? Lu1 O3 2.255(3) . ? Lu1 O2 2.317(3) . ? Lu1 O6 2.324(3) . ? Lu1 O5 2.335(3) . ? Lu1 O7 2.349(3) . ? Lu1 O1 2.365(3) . ? Lu1 O8 2.430(4) . ? Lu1 S4 2.9404(12) . ? Lu1 S1 2.9545(12) . ? Lu1 S2 3.0267(12) . ? S1 O16 1.435(4) . ? S1 O10 1.449(3) . ? S1 O5 1.485(3) . ? S1 O2 1.518(3) . ? S2 O13 1.448(4) . ? S2 O15 1.456(4) . ? S2 O8 1.477(4) . ? S2 O1 1.505(4) . ? S3 O12 1.445(4) . ? S3 O4 1.460(3) . ? S3 O9 1.478(3) . ? S3 O3 1.487(3) . ? S4 O11 1.449(4) . ? S4 O14 1.457(4) . ? S4 O7 1.480(4) . ? S4 O6 1.497(3) . ? O9 Lu1 2.244(3) 2_355 ? N5 C5 1.481(6) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N2 C2 1.487(6) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N1 C1 1.488(6) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N3 C3 1.485(6) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.473(7) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? C2 C1 1.496(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C3 1.502(10) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C4 1.517(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 O9 Lu1 O3 77.44(12) 2_355 . ? O9 Lu1 O2 82.47(13) 2_355 . ? O3 Lu1 O2 91.80(12) . . ? O9 Lu1 O6 106.42(13) 2_355 . ? O3 Lu1 O6 74.08(12) . . ? O2 Lu1 O6 160.75(12) . . ? O9 Lu1 O5 83.16(12) 2_355 . ? O3 Lu1 O5 147.88(12) . . ? O2 Lu1 O5 60.17(11) . . ? O6 Lu1 O5 136.69(12) . . ? O9 Lu1 O7 83.34(13) 2_355 . ? O3 Lu1 O7 122.21(12) . . ? O2 Lu1 O7 138.88(11) . . ? O6 Lu1 O7 60.16(12) . . ? O5 Lu1 O7 79.93(12) . . ? O9 Lu1 O1 147.95(13) 2_355 . ? O3 Lu1 O1 78.27(12) . . ? O2 Lu1 O1 77.71(11) . . ? O6 Lu1 O1 86.50(12) . . ? O5 Lu1 O1 107.71(12) . . ? O7 Lu1 O1 127.69(12) . . ? O9 Lu1 O8 151.53(12) 2_355 . ? O3 Lu1 O8 130.46(12) . . ? O2 Lu1 O8 99.86(12) . . ? O6 Lu1 O8 80.57(12) . . ? O5 Lu1 O8 73.87(12) . . ? O7 Lu1 O8 76.36(12) . . ? O1 Lu1 O8 58.09(11) . . ? O9 Lu1 S4 95.86(10) 2_355 . ? O3 Lu1 S4 98.99(9) . . ? O2 Lu1 S4 168.47(8) . . ? O6 Lu1 S4 30.26(8) . . ? O5 Lu1 S4 108.33(8) . . ? O7 Lu1 S4 29.91(9) . . ? O1 Lu1 S4 108.35(9) . . ? O8 Lu1 S4 76.20(9) . . ? O9 Lu1 S1 83.64(10) 2_355 . ? O3 Lu1 S1 121.48(9) . . ? O2 Lu1 S1 30.52(8) . . ? O6 Lu1 S1 163.58(9) . . ? O5 Lu1 S1 29.77(8) . . ? O7 Lu1 S1 109.51(9) . . ? O1 Lu1 S1 91.55(9) . . ? O8 Lu1 S1 84.56(9) . . ? S4 Lu1 S1 138.03(4) . . ? O9 Lu1 S2 170.39(10) 2_355 . ? O3 Lu1 S2 105.19(9) . . ? O2 Lu1 S2 88.18(9) . . ? O6 Lu1 S2 83.17(9) . . ? O5 Lu1 S2 90.28(9) . . ? O7 Lu1 S2 102.48(9) . . ? O1 Lu1 S2 29.25(8) . . ? O8 Lu1 S2 28.85(8) . . ? S4 Lu1 S2 92.86(3) . . ? S1 Lu1 S2 87.18(3) . . ? O16 S1 O10 110.9(2) . . ? O16 S1 O5 113.0(2) . . ? O10 S1 O5 110.8(2) . . ? O16 S1 O2 110.9(2) . . ? O10 S1 O2 109.0(2) . . ? O5 S1 O2 101.93(19) . . ? O16 S1 Lu1 122.21(18) . . ? O10 S1 Lu1 126.86(17) . . ? O5 S1 Lu1 51.33(13) . . ? O2 S1 Lu1 50.85(12) . . ? O13 S2 O15 110.5(2) . . ? O13 S2 O8 112.5(2) . . ? O15 S2 O8 111.7(2) . . ? O13 S2 O1 109.9(2) . . ? O15 S2 O1 109.2(2) . . ? O8 S2 O1 102.7(2) . . ? O13 S2 Lu1 124.04(17) . . ? O15 S2 Lu1 125.28(16) . . ? O8 S2 Lu1 52.56(14) . . ? O1 S2 Lu1 50.18(13) . . ? O12 S3 O4 112.4(2) . . ? O12 S3 O9 110.9(2) . . ? O4 S3 O9 107.7(2) . . ? O12 S3 O3 109.6(2) . . ? O4 S3 O3 108.1(2) . . ? O9 S3 O3 107.9(2) . . ? O11 S4 O14 110.4(2) . . ? O11 S4 O7 111.6(2) . . ? O14 S4 O7 111.0(2) . . ? O11 S4 O6 110.8(2) . . ? O14 S4 O6 109.0(2) . . ? O7 S4 O6 103.78(19) . . ? O11 S4 Lu1 124.86(16) . . ? O14 S4 Lu1 124.67(17) . . ? O7 S4 Lu1 52.35(13) . . ? O6 S4 Lu1 51.44(13) . . ? S2 O1 Lu1 100.57(17) . . ? S1 O2 Lu1 98.63(16) . . ? S3 O3 Lu1 146.6(2) . . ? S1 O5 Lu1 98.91(17) . . ? S4 O6 Lu1 98.30(17) . . ? S4 O7 Lu1 97.74(17) . . ? S2 O8 Lu1 98.59(18) . . ? S3 O9 Lu1 146.6(2) . 2_355 ? C5 N5 H5C 109.5 . . ? C5 N5 H5D 109.5 . . ? H5C N5 H5D 109.5 . . ? C5 N5 H5E 109.5 . . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? C2 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? C2 N2 H2E 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N3 H3C 109.5 . . ? C3 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C3 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C4 N4 H4C 109.5 . . ? C4 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C4 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? N2 C2 C1 114.5(5) . . ? N2 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N1 C1 C2 112.8(4) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N3 C3 C3 111.0(5) . 2_766 ? N3 C3 H3A 109.4 . . ? C3 C3 H3A 109.4 2_766 . ? N3 C3 H3B 109.4 . . ? C3 C3 H3B 109.4 2_766 . ? H3A C3 H3B 108.0 . . ? N5 C5 C4 112.6(4) . . ? N5 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N5 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C4 C5 112.3(4) . . ? N4 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N4 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.563 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.135