# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Xu, Yan' 'Zheng, Lei' 'Zhang, Deng' 'Fu, Jie' _publ_contact_author_name 'Dr Yan Xu ' _publ_contact_author_email yanxu@njut.edu.cn _publ_section_title ; Structural Systematic Design of Organic Templated Samarium Sulfates and Their Luminescence Property ; # Attachment '- 1.CIF' data_zl-19 _database_code_depnum_ccdc_archive 'CCDC 826954' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H72 N9 O48 S12 Sm5' _chemical_formula_weight 2319.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.6494(13) _cell_length_b 35.261(2) _cell_length_c 10.1318(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.0040(10) _cell_angle_gamma 90.00 _cell_volume 6685.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9615 _cell_measurement_theta_min 2.486 _cell_measurement_theta_max 26.685 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4516 _exptl_absorpt_coefficient_mu 4.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5961 _exptl_absorpt_correction_T_max 0.6449 _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 25302 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.18 _reflns_number_total 6822 _reflns_number_gt 5885 _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^)+(0.0489P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6822 _refine_ls_number_parameters 431 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.5000 0.219045(10) 0.7500 0.01534(9) Uani 1 2 d S . . Sm2 Sm 0.136982(13) 0.029916(7) 0.47797(3) 0.01630(8) Uani 1 1 d . . . Sm3 Sm 0.256985(12) 0.191965(6) 0.51053(3) 0.01392(8) Uani 1 1 d . . . S1 S 0.15520(6) 0.24702(3) 0.17933(13) 0.0147(2) Uani 1 1 d . . . S2 S 0.20721(6) 0.10966(3) 0.51998(14) 0.0193(3) Uani 1 1 d . . . S3 S 0.05788(6) 0.03541(3) 0.13945(13) 0.0155(2) Uani 1 1 d . . . S4 S 0.13268(6) 0.23292(3) 0.55673(13) 0.0160(2) Uani 1 1 d . . . S5 S 0.25400(7) -0.02691(4) 0.37347(15) 0.0254(3) Uani 1 1 d . . . S6 S 0.40358(6) 0.15562(3) 0.54316(14) 0.0197(3) Uani 1 1 d . . . O1 O 0.20029(17) 0.28064(9) 0.2482(4) 0.0180(7) Uani 1 1 d . . . O2 O 0.18455(18) 0.25314(9) 0.5131(4) 0.0182(7) Uani 1 1 d . . . O3 O 0.08507(19) 0.02804(9) 0.0285(4) 0.0227(8) Uani 1 1 d . . . O4 O 0.14993(18) 0.19246(9) 0.5553(4) 0.0218(8) Uani 1 1 d . . . O5 O 0.23954(19) 0.07328(10) 0.5044(4) 0.0253(8) Uani 1 1 d . . . O6 O 0.08288(18) 0.25368(10) 0.1702(4) 0.0233(8) Uani 1 1 d . . . O7 O 0.10020(19) 0.06533(10) 0.2417(4) 0.0244(8) Uani 1 1 d . . . O8 O 0.39329(18) 0.17553(10) 0.6648(4) 0.0216(8) Uani 1 1 d . . . O9 O 0.06001(18) 0.24002(10) 0.4453(4) 0.0255(8) Uani 1 1 d . . . O10 O 0.06511(18) 0.00128(9) 0.2291(4) 0.0207(7) Uani 1 1 d . . . O11 O 0.25821(18) 0.13152(9) 0.6452(4) 0.0235(8) Uani 1 1 d . . . O12 O 0.15199(19) 0.24236(10) 0.0340(4) 0.0256(8) Uani 1 1 d . . . O13 O 0.33658(18) 0.16180(10) 0.4120(4) 0.0260(8) Uani 1 1 d . . . O14 O 0.14192(19) 0.09874(10) 0.5370(4) 0.0264(8) Uani 1 1 d . . . O15 O -0.01703(18) 0.04809(10) 0.0633(4) 0.0232(8) Uani 1 1 d . . . O16 O 0.18551(18) 0.21259(9) 0.2664(4) 0.0216(8) Uani 1 1 d . . . O17 O 0.18986(18) 0.13441(9) 0.3924(4) 0.0226(8) Uani 1 1 d . . . O18 O 0.46550(19) 0.17477(11) 0.5369(4) 0.0291(9) Uani 1 1 d . . . O19 O 0.1397(2) 0.24493(10) 0.6982(4) 0.0285(9) Uani 1 1 d . . . O20 O 0.4164(2) 0.11535(10) 0.5737(4) 0.0354(10) Uani 1 1 d . . . O21 O 0.2141(2) -0.01496(11) 0.4575(4) 0.0323(9) Uani 1 1 d . . . O22 O 0.2099(2) -0.01898(13) 0.2199(4) 0.0454(11) Uani 1 1 d . . . O23 O 0.2716(3) -0.06646(12) 0.3950(5) 0.0516(13) Uani 1 1 d . . . O24 O 0.3190(3) -0.00421(16) 0.4219(6) 0.0666(15) Uani 1 1 d . . . N1 N 0.2311(3) 0.19288(12) -0.0641(5) 0.0285(11) Uani 1 1 d . . . H1D H 0.2475 0.2005 -0.1293 0.034 Uiso 1 1 calc R . . H1E H 0.2063 0.2122 -0.0501 0.034 Uiso 1 1 calc R . . N2 N 0.3811(3) -0.0847(2) 0.3021(7) 0.0637(19) Uani 1 1 d . . . H2D H 0.3749 -0.0988 0.2237 0.076 Uiso 1 1 calc R . . H2E H 0.3374 -0.0787 0.2954 0.076 Uiso 1 1 calc R . . N3 N 0.0000 -0.06589(17) 0.2500 0.0272(14) Uani 1 2 d S . . H3E H 0.0076 -0.0513 0.3279 0.033 Uiso 1 1 d R . . N4 N 0.0000 0.1298(3) 0.2500 0.106(5) Uani 1 2 d S . . H4E H -0.0380 0.1152 0.1980 0.127 Uiso 1 1 d R . . N5 N 0.5016(6) 0.2432(4) 0.3224(12) 0.051(3) Uani 0.50 1 d P . . H5D H 0.5412 0.2429 0.4069 0.061 Uiso 0.50 1 d PR . . H5E H 0.4639 0.2429 0.3452 0.061 Uiso 0.50 1 d PR . . N6 N 0.2783(9) 0.0617(4) 0.2531(15) 0.055(4) Uani 0.50 1 d P A 1 H6D H 0.2587 0.0397 0.2096 0.066 Uiso 0.50 1 calc PR A 1 H6E H 0.2779 0.0621 0.3416 0.066 Uiso 0.50 1 calc PR A 1 N6A N 0.3137(8) 0.0731(4) 0.3122(13) 0.046(3) Uani 0.50 1 d P A 2 H6AD H 0.3300 0.0908 0.3827 0.056 Uiso 0.50 1 calc PR A 2 H6AE H 0.3022 0.0524 0.3498 0.056 Uiso 0.50 1 calc PR A 2 C1 C 0.2926(4) 0.1839(2) 0.0753(7) 0.0474(17) Uani 1 1 d . . . H1A H 0.3223 0.2059 0.1101 0.071 Uiso 1 1 calc R . . H1B H 0.3199 0.1636 0.0605 0.071 Uiso 1 1 calc R . . H1C H 0.2754 0.1762 0.1458 0.071 Uiso 1 1 calc R . . C2 C 0.1829(4) 0.16000(18) -0.1241(7) 0.0442(16) Uani 1 1 d . . . H2A H 0.1437 0.1672 -0.2137 0.066 Uiso 1 1 calc R . . H2B H 0.1648 0.1520 -0.0554 0.066 Uiso 1 1 calc R . . H2C H 0.2088 0.1395 -0.1419 0.066 Uiso 1 1 calc R . . C3 C 0.4163(6) -0.0506(3) 0.2965(13) 0.109(4) Uani 1 1 d U . . H3A H 0.3888 -0.0376 0.2069 0.164 Uiso 1 1 calc R . . H3B H 0.4627 -0.0564 0.3015 0.164 Uiso 1 1 calc R . . H3C H 0.4214 -0.0347 0.3772 0.164 Uiso 1 1 calc R . . C4 C 0.4168(6) -0.1075(3) 0.4303(13) 0.113(4) Uani 1 1 d U . . H4A H 0.3893 -0.1300 0.4232 0.170 Uiso 1 1 calc R . . H4B H 0.4217 -0.0933 0.5148 0.170 Uiso 1 1 calc R . . H4C H 0.4633 -0.1145 0.4383 0.170 Uiso 1 1 calc R . . C5 C 0.0651(4) -0.08827(18) 0.2785(8) 0.0494(18) Uani 1 1 d . . . H5A H 0.1044 -0.0714 0.2956 0.074 Uiso 1 1 calc R . . H5B H 0.0573 -0.1040 0.1957 0.074 Uiso 1 1 calc R . . H5C H 0.0760 -0.1040 0.3627 0.074 Uiso 1 1 calc R . . C6 C 0.0198(5) 0.1510(2) 0.1503(11) 0.081(3) Uani 1 1 d . . . H6A H 0.0319 0.1337 0.0911 0.122 Uiso 1 1 calc R . . H6B H 0.0602 0.1668 0.2047 0.122 Uiso 1 1 calc R . . H6C H -0.0197 0.1666 0.0891 0.122 Uiso 1 1 calc R . . C7 C 0.5000 0.2099(4) 0.2500 0.076(4) Uani 1 2 d S . . H7A H 0.5011 0.1889 0.3110 0.114 Uiso 0.50 1 d PR . . H7B H 0.4571 0.2088 0.1612 0.114 Uiso 0.50 1 d PR . . H7C H 0.5409 0.2088 0.2281 0.114 Uiso 0.50 1 d PR . . C8 C 0.5000 0.2800(3) 0.2500 0.056(3) Uani 1 2 d S . . H8A H 0.5012 0.3004 0.3139 0.084 Uiso 0.50 1 d PR . . H8B H 0.5409 0.2817 0.2283 0.084 Uiso 0.50 1 d PR . . H8C H 0.4572 0.2817 0.1614 0.084 Uiso 0.50 1 d PR . . C9 C 0.3653(5) 0.0642(3) 0.2728(10) 0.086(3) Uani 1 1 d . . . C10 C 0.2413(4) 0.0893(2) 0.1774(9) 0.057(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.00995(17) 0.01803(18) 0.01610(19) 0.000 0.00364(14) 0.000 Sm2 0.01537(14) 0.01593(14) 0.01718(15) -0.00061(9) 0.00645(11) -0.00189(9) Sm3 0.01197(13) 0.01366(13) 0.01503(14) -0.00025(9) 0.00463(11) -0.00116(9) S1 0.0103(6) 0.0200(6) 0.0129(6) -0.0011(4) 0.0042(5) 0.0003(4) S2 0.0167(6) 0.0151(6) 0.0245(7) -0.0009(5) 0.0072(5) -0.0031(5) S3 0.0147(6) 0.0163(6) 0.0158(6) -0.0008(4) 0.0068(5) -0.0005(4) S4 0.0105(6) 0.0196(6) 0.0182(6) 0.0040(5) 0.0063(5) 0.0013(4) S5 0.0263(7) 0.0309(7) 0.0208(7) 0.0030(5) 0.0116(6) 0.0082(6) S6 0.0158(6) 0.0197(6) 0.0220(7) -0.0049(5) 0.0064(5) 0.0008(5) O1 0.0143(17) 0.0214(17) 0.0163(18) -0.0011(14) 0.0044(15) -0.0016(13) O2 0.0164(17) 0.0190(17) 0.0205(19) 0.0012(14) 0.0091(15) -0.0028(13) O3 0.024(2) 0.0287(19) 0.0187(19) -0.0013(15) 0.0122(16) 0.0016(15) O4 0.0163(18) 0.0174(18) 0.034(2) 0.0053(15) 0.0127(17) 0.0008(13) O5 0.026(2) 0.0165(17) 0.035(2) 0.0006(15) 0.0149(18) 0.0007(15) O6 0.0108(17) 0.032(2) 0.026(2) -0.0049(15) 0.0067(16) 0.0006(14) O7 0.028(2) 0.0219(18) 0.023(2) -0.0028(15) 0.0102(17) -0.0058(15) O8 0.0198(18) 0.0251(18) 0.0203(19) -0.0058(15) 0.0090(16) 0.0002(15) O9 0.0120(18) 0.033(2) 0.027(2) 0.0072(16) 0.0039(16) 0.0000(15) O10 0.0204(18) 0.0175(17) 0.0215(19) 0.0020(14) 0.0062(15) -0.0013(14) O11 0.0210(19) 0.0165(17) 0.025(2) 0.0022(14) 0.0020(16) -0.0046(14) O12 0.028(2) 0.033(2) 0.0174(19) -0.0023(16) 0.0105(17) 0.0010(16) O13 0.0178(19) 0.034(2) 0.020(2) -0.0048(16) 0.0025(16) 0.0012(15) O14 0.023(2) 0.0230(19) 0.037(2) -0.0069(16) 0.0157(17) -0.0063(15) O15 0.0177(18) 0.0260(19) 0.025(2) 0.0023(15) 0.0081(16) 0.0026(15) O16 0.0238(19) 0.0188(17) 0.0175(19) 0.0015(14) 0.0041(16) 0.0007(14) O17 0.027(2) 0.0166(17) 0.0213(19) 0.0003(14) 0.0069(16) -0.0040(14) O18 0.0190(19) 0.038(2) 0.034(2) -0.0062(18) 0.0154(18) -0.0028(16) O19 0.030(2) 0.038(2) 0.021(2) -0.0012(16) 0.0144(18) 0.0013(17) O20 0.036(2) 0.0202(19) 0.045(3) -0.0023(18) 0.011(2) 0.0066(17) O21 0.033(2) 0.040(2) 0.027(2) -0.0038(18) 0.0156(19) 0.0100(18) O22 0.050(3) 0.059(3) 0.021(2) 0.001(2) 0.009(2) 0.022(2) O23 0.080(4) 0.041(3) 0.051(3) 0.017(2) 0.045(3) 0.031(2) O24 0.038(3) 0.089(4) 0.075(4) -0.012(3) 0.025(3) -0.018(3) N1 0.035(3) 0.025(2) 0.033(3) 0.004(2) 0.022(2) 0.000(2) N2 0.041(4) 0.084(5) 0.064(5) -0.037(4) 0.019(3) -0.008(3) N3 0.033(4) 0.022(3) 0.024(3) 0.000 0.009(3) 0.000 N4 0.096(9) 0.048(6) 0.184(14) 0.000 0.071(10) 0.000 N5 0.032(6) 0.089(9) 0.030(6) -0.014(6) 0.012(5) 0.006(6) N6 0.099(12) 0.036(7) 0.037(8) -0.005(6) 0.037(8) -0.022(8) N6A 0.074(10) 0.042(7) 0.029(7) -0.020(5) 0.027(7) -0.034(7) C1 0.047(4) 0.048(4) 0.034(4) 0.010(3) 0.005(3) -0.007(3) C2 0.047(4) 0.045(4) 0.034(4) 0.002(3) 0.010(3) -0.008(3) C3 0.093(6) 0.118(7) 0.147(8) -0.047(6) 0.079(6) -0.037(6) C4 0.088(6) 0.128(7) 0.115(7) -0.028(6) 0.034(6) 0.044(6) C5 0.048(4) 0.035(4) 0.065(5) 0.003(3) 0.025(4) 0.014(3) C6 0.057(6) 0.058(5) 0.112(8) 0.026(5) 0.020(5) 0.012(4) C7 0.032(6) 0.088(9) 0.092(10) 0.000 0.010(6) 0.000 C8 0.040(6) 0.064(7) 0.060(7) 0.000 0.017(5) 0.000 C9 0.077(7) 0.115(8) 0.057(6) -0.002(5) 0.019(5) 0.012(6) C10 0.068(5) 0.060(5) 0.059(5) -0.020(4) 0.042(4) -0.016(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 Sm1 O9 2.337(4) 8_556 ? Sm1 O9 2.337(4) 7_556 ? Sm1 O6 2.383(3) 8_556 ? Sm1 O6 2.383(3) 7_556 ? Sm1 O18 2.511(4) . ? Sm1 O18 2.511(4) 2_656 ? Sm1 O8 2.519(3) 2_656 ? Sm1 O8 2.519(3) . ? Sm1 S6 3.1354(12) . ? Sm1 S6 3.1354(12) 2_656 ? Sm2 O22 2.303(4) 6_556 ? Sm2 O21 2.315(4) . ? Sm2 O15 2.417(3) 2 ? Sm2 O3 2.460(3) 6_556 ? Sm2 O14 2.491(3) . ? Sm2 O7 2.516(4) . ? Sm2 O5 2.533(3) . ? Sm2 O10 2.533(3) . ? Sm2 S2 3.1095(12) . ? Sm2 S3 3.1198(12) . ? Sm3 O2 2.346(3) 7_556 ? Sm3 O16 2.396(3) . ? Sm3 O1 2.421(3) 7_556 ? Sm3 O4 2.437(3) . ? Sm3 O17 2.464(3) . ? Sm3 O13 2.493(3) . ? Sm3 O11 2.525(3) . ? Sm3 O2 2.631(3) . ? Sm3 O8 2.642(3) . ? Sm3 S2 3.0937(12) . ? Sm3 S4 3.1478(12) . ? Sm3 S6 3.1731(12) . ? S1 O12 1.455(4) . ? S1 O6 1.475(3) . ? S1 O16 1.475(3) . ? S1 O1 1.487(3) . ? S2 O17 1.473(3) . ? S2 O11 1.478(4) . ? S2 O14 1.480(3) . ? S2 O5 1.485(4) . ? S3 O15 1.476(3) . ? S3 O3 1.476(3) . ? S3 O10 1.477(3) . ? S3 O7 1.478(4) . ? S4 O19 1.442(4) . ? S4 O9 1.469(4) . ? S4 O4 1.472(3) . ? S4 O2 1.500(3) . ? S5 O23 1.434(4) . ? S5 O24 1.458(5) . ? S5 O22 1.460(4) . ? S5 O21 1.475(4) . ? S6 O20 1.453(4) . ? S6 O18 1.471(4) . ? S6 O13 1.474(4) . ? S6 O8 1.509(3) . ? O1 Sm3 2.421(3) 7_556 ? O2 Sm3 2.346(3) 7_556 ? O3 Sm2 2.460(3) 6 ? O6 Sm1 2.383(3) 7_556 ? O9 Sm1 2.337(4) 7_556 ? O15 Sm2 2.417(3) 2 ? O22 Sm2 2.303(4) 6 ? N1 C1 1.480(8) . ? N1 C2 1.482(7) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N2 C3 1.419(11) . ? N2 C4 1.438(12) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? N3 C5 1.479(7) 2 ? N3 C5 1.479(7) . ? N3 H3E 0.8996 . ? N4 C6 1.447(10) . ? N4 C6 1.447(10) 2 ? N4 H4E 0.8990 . ? N5 C7 1.377(14) . ? N5 N5 1.44(2) 2_655 ? N5 C8 1.484(14) . ? N5 H5D 0.9000 . ? N5 H5E 0.9000 . ? N6 C10 1.273(15) . ? N6 C9 1.725(18) . ? N6 H6D 0.9000 . ? N6 H6E 0.9000 . ? N6A C9 1.325(15) . ? N6A C10 1.643(16) . ? N6A H6AD 0.9000 . ? N6A H6AE 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 N5 1.377(14) 2_655 ? C7 H7A 0.9602 . ? C7 H7B 0.9601 . ? C7 H7C 0.9599 . ? C8 N5 1.484(14) 2_655 ? C8 H8A 0.9599 . ? C8 H8B 0.9600 . ? C8 H8C 0.9599 . ? 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 Sm1 O9 103.72(19) 8_556 7_556 ? O9 Sm1 O6 80.70(13) 8_556 8_556 ? O9 Sm1 O6 70.32(12) 7_556 8_556 ? O9 Sm1 O6 70.32(12) 8_556 7_556 ? O9 Sm1 O6 80.70(13) 7_556 7_556 ? O6 Sm1 O6 132.40(17) 8_556 7_556 ? O9 Sm1 O18 165.50(11) 8_556 . ? O9 Sm1 O18 78.45(13) 7_556 . ? O6 Sm1 O18 86.70(12) 8_556 . ? O6 Sm1 O18 124.01(12) 7_556 . ? O9 Sm1 O18 78.45(13) 8_556 2_656 ? O9 Sm1 O18 165.50(11) 7_556 2_656 ? O6 Sm1 O18 124.01(11) 8_556 2_656 ? O6 Sm1 O18 86.70(12) 7_556 2_656 ? O18 Sm1 O18 103.12(18) . 2_656 ? O9 Sm1 O8 90.70(12) 8_556 2_656 ? O9 Sm1 O8 137.74(11) 7_556 2_656 ? O6 Sm1 O8 73.29(11) 8_556 2_656 ? O6 Sm1 O8 141.19(12) 7_556 2_656 ? O18 Sm1 O8 78.76(12) . 2_656 ? O18 Sm1 O8 55.78(11) 2_656 2_656 ? O9 Sm1 O8 137.74(11) 8_556 . ? O9 Sm1 O8 90.70(12) 7_556 . ? O6 Sm1 O8 141.19(12) 8_556 . ? O6 Sm1 O8 73.29(11) 7_556 . ? O18 Sm1 O8 55.78(11) . . ? O18 Sm1 O8 78.76(12) 2_656 . ? O8 Sm1 O8 104.95(15) 2_656 . ? O9 Sm1 S6 165.04(9) 8_556 . ? O9 Sm1 S6 85.12(9) 7_556 . ? O6 Sm1 S6 113.91(9) 8_556 . ? O6 Sm1 S6 99.81(9) 7_556 . ? O18 Sm1 S6 27.46(8) . . ? O18 Sm1 S6 90.03(9) 2_656 . ? O8 Sm1 S6 90.62(8) 2_656 . ? O8 Sm1 S6 28.38(8) . . ? O9 Sm1 S6 85.12(9) 8_556 2_656 ? O9 Sm1 S6 165.04(9) 7_556 2_656 ? O6 Sm1 S6 99.81(8) 8_556 2_656 ? O6 Sm1 S6 113.91(9) 7_556 2_656 ? O18 Sm1 S6 90.03(9) . 2_656 ? O18 Sm1 S6 27.46(8) 2_656 2_656 ? O8 Sm1 S6 28.38(8) 2_656 2_656 ? O8 Sm1 S6 90.62(8) . 2_656 ? S6 Sm1 S6 88.99(5) . 2_656 ? O22 Sm2 O21 79.39(16) 6_556 . ? O22 Sm2 O15 112.96(15) 6_556 2 ? O21 Sm2 O15 149.15(13) . 2 ? O22 Sm2 O3 77.64(13) 6_556 6_556 ? O21 Sm2 O3 80.06(13) . 6_556 ? O15 Sm2 O3 75.61(12) 2 6_556 ? O22 Sm2 O14 88.04(14) 6_556 . ? O21 Sm2 O14 136.67(13) . . ? O15 Sm2 O14 73.64(11) 2 . ? O3 Sm2 O14 137.44(11) 6_556 . ? O22 Sm2 O7 153.43(13) 6_556 . ? O21 Sm2 O7 101.32(13) . . ? O15 Sm2 O7 80.13(12) 2 . ? O3 Sm2 O7 128.86(11) 6_556 . ? O14 Sm2 O7 73.15(12) . . ? O22 Sm2 O5 81.20(13) 6_556 . ? O21 Sm2 O5 81.17(13) . . ? O15 Sm2 O5 127.44(11) 2 . ? O3 Sm2 O5 153.89(12) 6_556 . ? O14 Sm2 O5 55.87(11) . . ? O7 Sm2 O5 72.77(11) . . ? O22 Sm2 O10 146.83(14) 6_556 . ? O21 Sm2 O10 76.93(12) . . ? O15 Sm2 O10 78.87(11) 2 . ? O3 Sm2 O10 75.68(11) 6_556 . ? O14 Sm2 O10 125.06(11) . . ? O7 Sm2 O10 55.69(11) . . ? O5 Sm2 O10 117.25(11) . . ? O22 Sm2 S2 87.04(11) 6_556 . ? O21 Sm2 S2 109.38(10) . . ? O15 Sm2 S2 99.70(8) 2 . ? O3 Sm2 S2 160.35(8) 6_556 . ? O14 Sm2 S2 27.97(8) . . ? O7 Sm2 S2 67.49(8) . . ? O5 Sm2 S2 28.22(8) . . ? O10 Sm2 S2 122.67(8) . . ? O22 Sm2 S3 169.54(13) 6_556 . ? O21 Sm2 S3 90.23(10) . . ? O15 Sm2 S3 76.77(9) 2 . ? O3 Sm2 S3 102.05(8) 6_556 . ? O14 Sm2 S3 98.78(9) . . ? O7 Sm2 S3 27.86(8) . . ? O5 Sm2 S3 96.01(8) . . ? O10 Sm2 S3 27.89(7) . . ? S2 Sm2 S3 95.25(3) . . ? O2 Sm3 O16 76.31(12) 7_556 . ? O2 Sm3 O1 77.89(11) 7_556 7_556 ? O16 Sm3 O1 136.37(11) . 7_556 ? O2 Sm3 O4 124.01(11) 7_556 . ? O16 Sm3 O4 88.77(12) . . ? O1 Sm3 O4 77.38(11) 7_556 . ? O2 Sm3 O17 146.92(12) 7_556 . ? O16 Sm3 O17 76.92(11) . . ? O1 Sm3 O17 135.18(11) 7_556 . ? O4 Sm3 O17 74.23(11) . . ? O2 Sm3 O13 81.74(12) 7_556 . ? O16 Sm3 O13 86.48(12) . . ? O1 Sm3 O13 123.63(11) 7_556 . ? O4 Sm3 O13 151.74(11) . . ? O17 Sm3 O13 77.56(12) . . ? O2 Sm3 O11 149.69(11) 7_556 . ? O16 Sm3 O11 132.48(11) . . ? O1 Sm3 O11 82.82(11) 7_556 . ? O4 Sm3 O11 73.03(11) . . ? O17 Sm3 O11 56.12(11) . . ? O13 Sm3 O11 89.93(12) . . ? O2 Sm3 O2 69.14(12) 7_556 . ? O16 Sm3 O2 69.92(11) . . ? O1 Sm3 O2 68.23(11) 7_556 . ? O4 Sm3 O2 55.12(10) . . ? O17 Sm3 O2 118.34(11) . . ? O13 Sm3 O2 145.82(11) . . ? O11 Sm3 O2 124.22(11) . . ? O2 Sm3 O8 77.06(11) 7_556 . ? O16 Sm3 O8 135.62(11) . . ? O1 Sm3 O8 69.38(10) 7_556 . ? O4 Sm3 O8 135.61(11) . . ? O17 Sm3 O8 110.28(11) . . ? O13 Sm3 O8 54.95(11) . . ? O11 Sm3 O8 74.35(11) . . ? O2 Sm3 O8 129.93(10) . . ? O2 Sm3 S2 165.69(8) 7_556 . ? O16 Sm3 S2 104.41(8) . . ? O1 Sm3 S2 109.09(8) 7_556 . ? O4 Sm3 S2 70.22(8) . . ? O17 Sm3 S2 27.91(8) . . ? O13 Sm3 S2 84.04(9) . . ? O11 Sm3 S2 28.25(8) . . ? O2 Sm3 S2 124.82(7) . . ? O8 Sm3 S2 93.48(8) . . ? O2 Sm3 S4 97.11(8) 7_556 . ? O16 Sm3 S4 80.16(9) . . ? O1 Sm3 S4 68.84(8) 7_556 . ? O4 Sm3 S4 26.91(8) . . ? O17 Sm3 S4 97.10(8) . . ? O13 Sm3 S4 166.46(8) . . ? O11 Sm3 S4 97.43(8) . . ? O2 Sm3 S4 28.33(7) . . ? O8 Sm3 S4 138.10(7) . . ? S2 Sm3 S4 97.08(3) . . ? O2 Sm3 S6 80.48(8) 7_556 . ? O16 Sm3 S6 111.99(9) . . ? O1 Sm3 S6 97.55(8) 7_556 . ? O4 Sm3 S6 152.11(8) . . ? O17 Sm3 S6 91.94(8) . . ? O13 Sm3 S6 26.90(8) . . ? O11 Sm3 S6 79.14(8) . . ? O2 Sm3 S6 148.35(7) . . ? O8 Sm3 S6 28.25(7) . . ? S2 Sm3 S6 86.14(3) . . ? S4 Sm3 S6 166.34(3) . . ? O12 S1 O6 110.0(2) . . ? O12 S1 O16 109.8(2) . . ? O6 S1 O16 109.3(2) . . ? O12 S1 O1 108.5(2) . . ? O6 S1 O1 108.60(19) . . ? O16 S1 O1 110.6(2) . . ? O17 S2 O11 105.4(2) . . ? O17 S2 O14 111.1(2) . . ? O11 S2 O14 112.9(2) . . ? O17 S2 O5 111.8(2) . . ? O11 S2 O5 110.6(2) . . ? O14 S2 O5 105.1(2) . . ? O17 S2 Sm3 51.53(13) . . ? O11 S2 Sm3 53.97(13) . . ? O14 S2 Sm3 125.33(15) . . ? O5 S2 Sm3 129.56(14) . . ? O17 S2 Sm2 119.29(14) . . ? O11 S2 Sm2 135.32(14) . . ? O14 S2 Sm2 52.11(14) . . ? O5 S2 Sm2 53.77(14) . . ? Sm3 S2 Sm2 170.36(5) . . ? O15 S3 O3 107.9(2) . . ? O15 S3 O10 112.3(2) . . ? O3 S3 O10 110.6(2) . . ? O15 S3 O7 109.2(2) . . ? O3 S3 O7 110.9(2) . . ? O10 S3 O7 105.9(2) . . ? O15 S3 Sm2 122.62(15) . . ? O3 S3 Sm2 129.44(15) . . ? O10 S3 Sm2 53.38(14) . . ? O7 S3 Sm2 52.71(14) . . ? O19 S4 O9 110.8(2) . . ? O19 S4 O4 111.8(2) . . ? O9 S4 O4 109.3(2) . . ? O19 S4 O2 111.7(2) . . ? O9 S4 O2 108.5(2) . . ? O4 S4 O2 104.58(19) . . ? O19 S4 Sm3 122.47(16) . . ? O9 S4 Sm3 126.61(16) . . ? O4 S4 Sm3 48.54(13) . . ? O2 S4 Sm3 56.33(13) . . ? O23 S5 O24 110.2(3) . . ? O23 S5 O22 110.6(3) . . ? O24 S5 O22 108.9(3) . . ? O23 S5 O21 110.9(2) . . ? O24 S5 O21 108.0(3) . . ? O22 S5 O21 108.2(2) . . ? O20 S6 O18 112.0(2) . . ? O20 S6 O13 110.7(2) . . ? O18 S6 O13 113.2(2) . . ? O20 S6 O8 110.8(2) . . ? O18 S6 O8 104.3(2) . . ? O13 S6 O8 105.4(2) . . ? O20 S6 Sm1 123.20(17) . . ? O18 S6 Sm1 51.93(15) . . ? O13 S6 Sm1 125.86(15) . . ? O8 S6 Sm1 52.50(13) . . ? O20 S6 Sm3 119.75(17) . . ? O18 S6 Sm3 128.21(16) . . ? O13 S6 Sm3 49.91(14) . . ? O8 S6 Sm3 55.94(13) . . ? Sm1 S6 Sm3 95.16(3) . . ? S1 O1 Sm3 132.90(19) . 7_556 ? S4 O2 Sm3 152.1(2) . 7_556 ? S4 O2 Sm3 95.33(15) . . ? Sm3 O2 Sm3 110.86(12) 7_556 . ? S3 O3 Sm2 130.1(2) . 6 ? S4 O4 Sm3 104.54(16) . . ? S2 O5 Sm2 98.01(17) . . ? S1 O6 Sm1 153.6(2) . 7_556 ? S3 O7 Sm2 99.43(17) . . ? S6 O8 Sm1 99.11(16) . . ? S6 O8 Sm3 95.81(16) . . ? Sm1 O8 Sm3 128.88(14) . . ? S4 O9 Sm1 139.5(2) . 7_556 ? S3 O10 Sm2 98.73(16) . . ? S2 O11 Sm3 97.78(17) . . ? S6 O13 Sm3 103.20(18) . . ? S2 O14 Sm2 99.92(17) . . ? S3 O15 Sm2 141.4(2) . 2 ? S1 O16 Sm3 142.0(2) . . ? S2 O17 Sm3 100.56(17) . . ? S6 O18 Sm1 100.61(18) . . ? S5 O21 Sm2 145.1(2) . . ? S5 O22 Sm2 159.2(3) . 6 ? C1 N1 C2 112.3(5) . . ? C1 N1 H1D 109.1 . . ? C2 N1 H1D 109.1 . . ? C1 N1 H1E 109.1 . . ? C2 N1 H1E 109.1 . . ? H1D N1 H1E 107.9 . . ? C3 N2 C4 115.7(8) . . ? C3 N2 H2D 108.3 . . ? C4 N2 H2D 108.3 . . ? C3 N2 H2E 108.3 . . ? C4 N2 H2E 108.3 . . ? H2D N2 H2E 107.4 . . ? C5 N3 C5 115.5(7) 2 . ? C5 N3 H3E 106.5 2 . ? C5 N3 H3E 109.1 . . ? C6 N4 C6 117.8(11) . 2 ? C6 N4 H4E 108.7 . . ? C6 N4 H4E 105.7 2 . ? C7 N5 N5 58.5(6) . 2_655 ? C7 N5 C8 119.4(9) . . ? N5 N5 C8 61.0(5) 2_655 . ? C7 N5 H5D 107.7 . . ? N5 N5 H5D 126.9 2_655 . ? C8 N5 H5D 107.6 . . ? C7 N5 H5E 107.4 . . ? N5 N5 H5E 126.1 2_655 . ? C8 N5 H5E 107.2 . . ? H5D N5 H5E 106.9 . . ? C10 N6 C9 111.2(9) . . ? C10 N6 H6D 109.4 . . ? C9 N6 H6D 109.4 . . ? C10 N6 H6E 109.4 . . ? C9 N6 H6E 109.4 . . ? H6D N6 H6E 108.0 . . ? C9 N6A C10 113.4(9) . . ? C9 N6A H6AD 108.9 . . ? C10 N6A H6AD 108.9 . . ? C9 N6A H6AE 108.9 . . ? C10 N6A H6AE 108.9 . . ? H6AD N6A H6AE 107.7 . . ? 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 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 N5 63.1(11) . 2_655 ? N5 C7 H7A 109.1 . . ? N5 C7 H7A 172.2 2_655 . ? N5 C7 H7B 109.8 . . ? N5 C7 H7B 74.4 2_655 . ? H7A C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? N5 C7 H7C 74.7 2_655 . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C8 N5 58.1(9) 2_655 . ? N5 C8 H8A 167.4 2_655 . ? N5 C8 H8A 109.3 . . ? N5 C8 H8B 77.3 2_655 . ? N5 C8 H8B 109.4 . . ? H8A C8 H8B 109.5 . . ? N5 C8 H8C 77.0 2_655 . ? N5 C8 H8C 109.7 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6A C9 N6 27.7(6) . . ? N6 C10 N6A 29.6(7) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.850 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.201 # Attachment '- 2.CIF' data_zd-7 _database_code_depnum_ccdc_archive 'CCDC 826955' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H40 N8 O28 S7 Sm2' _chemical_formula_weight 1221.60 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.761(4) _cell_length_b 14.877(2) _cell_length_c 10.4238(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3374.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4830 _cell_measurement_theta_min 2.563 _cell_measurement_theta_max 26.172 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 3.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6907 _exptl_absorpt_correction_T_max 0.7150 _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 23746 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6240 _reflns_number_gt 5430 _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^)+(0.0305P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.113(11) _refine_ls_number_reflns 6240 _refine_ls_number_parameters 478 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Sm1 Sm -0.564003(14) -0.57731(2) -2.40219(3) 0.01584(8) Uani 1 1 d . . . Sm2 Sm -0.550680(15) -0.89070(2) -2.41572(3) 0.01837(9) Uani 1 1 d . . . S1 S -0.43918(7) -0.74707(10) -2.4187(3) 0.0185(4) Uani 1 1 d . . . S2 S -0.64511(11) -0.74442(14) -2.6010(2) 0.0176(5) Uani 1 1 d . . . S3 S -0.63660(11) -0.74342(14) -2.2015(2) 0.0178(5) Uani 1 1 d . . . S4 S -0.53269(8) -1.02601(12) -2.70871(16) 0.0176(4) Uani 1 1 d . . . S5 S -0.65898(9) -1.06512(13) -2.33041(18) 0.0221(4) Uani 1 1 d . . . S6 S -0.67149(8) -0.44305(13) -2.46886(17) 0.0185(4) Uani 1 1 d . . . S7 S -0.51561(9) -0.48012(13) -2.14747(16) 0.0191(4) Uani 1 1 d . . . O1 O -0.7125(2) -1.0290(4) -2.2591(5) 0.0309(13) Uani 1 1 d . . . O2 O -0.5969(2) -1.0483(4) -2.7046(6) 0.0338(14) Uani 1 1 d . . . O3 O -0.4463(2) -0.8421(3) -2.4598(5) 0.0279(13) Uani 1 1 d . . . O4 O -0.5164(2) -0.9646(4) -2.6025(5) 0.0266(13) Uani 1 1 d . . . O5 O -0.7006(2) -0.7190(4) -2.2034(6) 0.0397(16) Uani 1 1 d . . . O6 O -0.6064(2) -0.4458(3) -2.5141(5) 0.0250(12) Uani 1 1 d . . . O7 O -0.4925(2) -1.1059(3) -2.7008(5) 0.0240(12) Uani 1 1 d . . . O8 O -0.5732(2) -0.4549(4) -2.2120(5) 0.0296(13) Uani 1 1 d . . . O9 O -0.7120(2) -0.4623(4) -2.5769(5) 0.0305(13) Uani 1 1 d . . . O10 O -0.6759(2) -0.5151(3) -2.3706(4) 0.0218(12) Uani 1 1 d . . . O11 O -0.5171(2) -0.9838(3) -2.8335(4) 0.0206(11) Uani 1 1 d . . . O12 O -0.5245(2) -0.5168(4) -2.0166(5) 0.0256(13) Uani 1 1 d . . . O13 O -0.6368(2) -0.6658(3) -2.5159(5) 0.0219(12) Uani 1 1 d . . . O14 O -0.4729(2) -0.4041(3) -2.1332(5) 0.0249(13) Uani 1 1 d . . . O15 O -0.6240(2) -0.8136(3) -2.2987(5) 0.0230(12) Uani 1 1 d . . . O16 O -0.6173(3) -0.7754(4) -2.0761(5) 0.0423(17) Uani 1 1 d . . . O17 O -0.4024(3) -0.7406(4) -2.3038(5) 0.0299(15) Uani 1 1 d . . . O18 O -0.4143(3) -0.6942(4) -2.5234(5) 0.0305(14) Uani 1 1 d . . . O19 O -0.6491(2) -0.7129(3) -2.7350(5) 0.0242(12) Uani 1 1 d . . . O20 O -0.5911(2) -0.8048(4) -2.5896(5) 0.0234(12) Uani 1 1 d . . . O21 O -0.6315(2) -0.9940(3) -2.4096(7) 0.0440(14) Uani 1 1 d . . . O22 O -0.5041(2) -0.7183(3) -2.3923(6) 0.0261(12) Uani 1 1 d . . . O23 O -0.5992(2) -0.6630(3) -2.2303(5) 0.0253(12) Uani 1 1 d . . . O24 O -0.6783(2) -1.1394(3) -2.4103(7) 0.0411(13) Uani 1 1 d . . . O25 O -0.6863(2) -0.3558(3) -2.4162(7) 0.0284(11) Uani 1 1 d . . . O26 O -0.4873(2) -0.5492(3) -2.2319(4) 0.0223(12) Uani 1 1 d . . . O27 O -0.6998(2) -0.7932(4) -2.5648(5) 0.0271(13) Uani 1 1 d . . . O28 O -0.6148(3) -1.0971(4) -2.2335(6) 0.0489(18) Uani 1 1 d . . . N1 N -0.4819(3) -0.7772(5) -0.7364(6) 0.0329(18) Uani 1 1 d . . . H1C H -0.5112 -0.7643 -0.6798 0.049 Uiso 1 1 calc R . . H1D H -0.4469 -0.7510 -0.7127 0.049 Uiso 1 1 calc R . . H1E H -0.4765 -0.8365 -0.7396 0.049 Uiso 1 1 calc R . . N2 N -0.4778(3) -0.7143(5) -1.0851(6) 0.0303(17) Uani 1 1 d . . . H2C H -0.4502 -0.7255 -1.1460 0.046 Uiso 1 1 calc R . . H2D H -0.4808 -0.6552 -1.0732 0.046 Uiso 1 1 calc R . . H2E H -0.5142 -0.7361 -1.1089 0.046 Uiso 1 1 calc R . . N3 N -0.7245(3) -0.6391(4) -1.9443(6) 0.0314(17) Uani 1 1 d . . . H3C H -0.7272 -0.6836 -2.0011 0.047 Uiso 1 1 calc R . . H3D H -0.7599 -0.6092 -1.9420 0.047 Uiso 1 1 calc R . . H3E H -0.7165 -0.6616 -1.8671 0.047 Uiso 1 1 calc R . . N4 N -0.6317(3) -0.5246(4) -1.7763(6) 0.0302(16) Uani 1 1 d . . . H4C H -0.6277 -0.4763 -1.7266 0.045 Uiso 1 1 calc R . . H4D H -0.5946 -0.5452 -1.7975 0.045 Uiso 1 1 calc R . . H4E H -0.6522 -0.5670 -1.7341 0.045 Uiso 1 1 calc R . . N5 N -0.6972(3) -0.1536(4) -1.6709(6) 0.0286(16) Uani 1 1 d . . . H5C H -0.6630 -0.1477 -1.7170 0.043 Uiso 1 1 calc R . . H5D H -0.6883 -0.1477 -1.5880 0.043 Uiso 1 1 calc R . . H5E H -0.7240 -0.1114 -1.6939 0.043 Uiso 1 1 calc R . . N6 N -0.8080(3) -0.3459(4) -1.6504(6) 0.0293(16) Uani 1 1 d . . . H6C H -0.8424 -0.3539 -1.6056 0.044 Uiso 1 1 calc R . . H6D H -0.7812 -0.3889 -1.6306 0.044 Uiso 1 1 calc R . . H6E H -0.8165 -0.3484 -1.7339 0.044 Uiso 1 1 calc R . . C1 C -0.5000(5) -0.7442(7) -0.8635(8) 0.057(3) Uani 1 1 d . . . H1A H -0.5385 -0.7729 -0.8862 0.068 Uiso 1 1 calc R . . H1B H -0.5081 -0.6803 -0.8562 0.068 Uiso 1 1 calc R . . C2 C -0.4587(4) -0.7569(6) -0.9665(8) 0.038(2) Uani 1 1 d . . . H2A H -0.4539 -0.8209 -0.9815 0.046 Uiso 1 1 calc R . . H2B H -0.4188 -0.7332 -0.9421 0.046 Uiso 1 1 calc R . . C3 C -0.6746(3) -0.5772(5) -1.9823(7) 0.0273(19) Uani 1 1 d . . . H3A H -0.6836 -0.5537 -2.0670 0.033 Uiso 1 1 calc R . . H3B H -0.6366 -0.6110 -1.9881 0.033 Uiso 1 1 calc R . . C4 C -0.6653(3) -0.5004(5) -1.8927(8) 0.0317(19) Uani 1 1 d . . . H4A H -0.6430 -0.4533 -1.9370 0.038 Uiso 1 1 calc R . . H4B H -0.7051 -0.4764 -1.8686 0.038 Uiso 1 1 calc R . . C5 C -0.7236(5) -0.2417(6) -1.6936(10) 0.033(3) Uani 1 1 d . . . H5A H -0.6938 -0.2874 -1.6703 0.039 Uiso 1 1 calc R . . H5B H -0.7325 -0.2482 -1.7843 0.039 Uiso 1 1 calc R . . C6 C -0.7812(5) -0.2564(5) -1.6190(9) 0.022(2) Uani 1 1 d . . . H6A H -0.8106 -0.2095 -1.6392 0.027 Uiso 1 1 calc R . . H6B H -0.7722 -0.2534 -1.5279 0.027 Uiso 1 1 calc R . . N8 N -0.7570(3) -0.8675(4) -2.3378(6) 0.0254(15) Uani 1 1 d . . . H8C H -0.7569 -0.8278 -2.2740 0.038 Uiso 1 1 calc R . . H8D H -0.7407 -0.8427 -2.4076 0.038 Uiso 1 1 calc R . . H8E H -0.7351 -0.9155 -2.3153 0.038 Uiso 1 1 calc R . . N7 N -0.8864(3) -0.9710(4) -2.5236(6) 0.0271(16) Uani 1 1 d . . . H7C H -0.8867 -1.0111 -2.5870 0.041 Uiso 1 1 calc R . . H7D H -0.8982 -0.9177 -2.5535 0.041 Uiso 1 1 calc R . . H7E H -0.9120 -0.9886 -2.4620 0.041 Uiso 1 1 calc R . . C8 C -0.8206(3) -0.8950(5) -2.3651(7) 0.0279(19) Uani 1 1 d . . . H8A H -0.8444 -0.8425 -2.3890 0.034 Uiso 1 1 calc R . . H8B H -0.8387 -0.9201 -2.2879 0.034 Uiso 1 1 calc R . . C7 C -0.8243(3) -0.9638(6) -2.4716(7) 0.031(2) Uani 1 1 d . . . H7A H -0.7962 -0.9470 -2.5397 0.037 Uiso 1 1 calc R . . H7B H -0.8116 -1.0219 -2.4388 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 Sm1 0.01577(17) 0.01652(18) 0.01523(16) 0.0009(2) -0.0003(2) -0.00046(13) Sm2 0.01964(17) 0.02214(19) 0.01333(16) -0.0024(2) -0.0017(2) 0.00713(14) S1 0.0153(8) 0.0208(9) 0.0195(9) 0.0017(9) -0.0005(10) -0.0013(6) S2 0.0212(13) 0.0166(13) 0.0150(10) 0.0009(8) -0.0025(9) 0.0009(9) S3 0.0155(12) 0.0205(13) 0.0175(10) -0.0018(8) 0.0063(8) -0.0032(9) S4 0.0187(10) 0.0170(10) 0.0171(8) -0.0046(7) 0.0014(7) 0.0019(8) S5 0.0198(10) 0.0210(11) 0.0254(10) -0.0041(8) 0.0016(8) -0.0019(8) S6 0.0143(10) 0.0197(11) 0.0216(9) 0.0009(8) 0.0006(7) 0.0053(8) S7 0.0184(11) 0.0191(12) 0.0198(9) -0.0028(8) -0.0056(8) 0.0003(8) O1 0.023(3) 0.031(3) 0.039(3) 0.002(3) 0.010(2) 0.007(3) O2 0.018(3) 0.034(4) 0.050(3) -0.012(3) 0.005(3) -0.003(3) O3 0.037(3) 0.018(3) 0.029(3) -0.003(2) 0.004(2) -0.003(2) O4 0.032(3) 0.030(3) 0.018(3) -0.011(2) 0.003(2) 0.004(3) O5 0.015(3) 0.041(4) 0.063(4) -0.029(3) 0.006(3) -0.003(3) O6 0.023(3) 0.024(3) 0.028(3) 0.004(2) 0.005(2) 0.003(2) O7 0.030(3) 0.022(3) 0.020(3) 0.002(2) 0.001(2) 0.006(2) O8 0.028(3) 0.023(3) 0.038(3) -0.007(3) -0.014(3) 0.004(2) O9 0.030(3) 0.034(3) 0.027(3) 0.001(2) -0.006(2) 0.007(3) O10 0.025(3) 0.022(3) 0.018(3) 0.003(2) 0.0009(19) 0.002(2) O11 0.025(3) 0.019(3) 0.017(2) 0.000(2) -0.001(2) 0.005(2) O12 0.017(3) 0.037(4) 0.023(3) 0.000(2) 0.004(2) -0.003(2) O13 0.022(3) 0.018(3) 0.026(3) -0.005(2) -0.001(2) 0.004(2) O14 0.024(3) 0.019(3) 0.032(3) -0.004(2) -0.006(2) -0.002(2) O15 0.023(3) 0.021(3) 0.025(3) -0.010(2) -0.002(2) 0.005(2) O16 0.084(5) 0.023(4) 0.020(3) 0.002(3) 0.000(3) -0.003(3) O17 0.018(3) 0.039(4) 0.032(3) -0.006(3) -0.012(2) 0.005(3) O18 0.023(3) 0.031(4) 0.038(3) 0.020(3) 0.012(3) 0.003(3) O19 0.032(3) 0.023(3) 0.018(3) 0.002(2) -0.005(2) 0.006(3) O20 0.025(3) 0.025(3) 0.020(3) 0.001(2) -0.003(2) 0.008(2) O21 0.060(4) 0.028(3) 0.044(3) 0.001(4) 0.024(4) -0.010(3) O22 0.020(3) 0.027(3) 0.031(3) 0.002(3) 0.004(3) 0.006(2) O23 0.031(3) 0.025(3) 0.020(3) 0.001(2) 0.006(2) -0.010(2) O24 0.060(3) 0.025(3) 0.038(3) -0.007(4) 0.000(4) -0.018(2) O25 0.037(3) 0.015(2) 0.034(3) -0.006(3) -0.002(3) 0.009(2) O26 0.028(3) 0.019(3) 0.019(3) -0.002(2) -0.002(2) -0.002(2) O27 0.023(3) 0.029(3) 0.029(3) 0.003(2) -0.001(2) -0.009(3) O28 0.040(4) 0.065(5) 0.042(4) -0.009(3) -0.012(3) 0.019(3) N1 0.030(4) 0.049(5) 0.020(4) 0.006(3) 0.008(3) 0.012(4) N2 0.040(4) 0.029(4) 0.022(4) 0.000(3) -0.004(3) 0.000(4) N3 0.031(4) 0.025(4) 0.038(4) -0.004(3) -0.004(3) -0.003(3) N4 0.037(4) 0.027(4) 0.027(3) -0.005(3) -0.014(3) 0.002(3) N5 0.023(4) 0.030(4) 0.033(4) 0.004(3) 0.001(3) 0.000(3) N6 0.021(4) 0.032(4) 0.035(4) 0.007(3) 0.007(3) -0.001(3) C1 0.056(7) 0.087(8) 0.027(5) 0.007(5) 0.004(4) 0.020(6) C2 0.036(5) 0.057(7) 0.021(4) 0.011(4) -0.007(4) 0.008(4) C3 0.030(5) 0.032(5) 0.020(4) -0.004(3) -0.004(3) -0.003(4) C4 0.033(4) 0.024(4) 0.038(5) -0.001(4) -0.009(5) 0.005(3) C5 0.016(5) 0.050(7) 0.032(5) 0.004(4) -0.004(4) -0.002(5) C6 0.024(6) 0.017(5) 0.026(5) 0.005(3) 0.011(4) 0.002(4) N8 0.023(4) 0.018(4) 0.036(4) -0.003(3) -0.002(3) -0.003(3) N7 0.027(4) 0.030(4) 0.024(3) -0.007(3) 0.004(3) 0.002(3) C8 0.029(5) 0.034(5) 0.021(4) -0.005(3) 0.003(3) -0.001(4) C7 0.021(4) 0.043(6) 0.029(4) -0.009(4) -0.004(3) 0.004(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 Sm1 O23 2.328(5) . ? Sm1 O13 2.376(5) . ? Sm1 O6 2.457(5) . ? Sm1 O22 2.471(4) . ? Sm1 O26 2.472(5) . ? Sm1 O14 2.554(5) 2_444 ? Sm1 O10 2.627(5) . ? Sm1 O12 2.663(5) 2_444 ? Sm1 O8 2.699(5) . ? Sm1 S6 3.1532(19) . ? Sm1 S7 3.2015(19) . ? Sm1 S7 3.2044(19) 2_444 ? Sm2 O15 2.313(5) . ? Sm2 O21 2.337(5) . ? Sm2 O4 2.357(5) . ? Sm2 O20 2.385(5) . ? Sm2 O3 2.428(5) . ? Sm2 O7 2.429(5) 2_435 ? Sm2 O11 2.529(5) 2_435 ? Sm2 O22 2.769(4) . ? Sm2 S4 3.0794(18) 2_435 ? Sm2 S1 3.2332(16) . ? S1 O17 1.444(6) . ? S1 O18 1.450(5) . ? S1 O3 1.485(5) . ? S1 O22 1.502(5) . ? S2 O27 1.443(5) . ? S2 O19 1.475(5) . ? S2 O13 1.480(5) . ? S2 O20 1.485(5) . ? S3 O5 1.439(6) . ? S3 O16 1.453(6) . ? S3 O23 1.478(5) . ? S3 O15 1.480(5) . ? S4 O2 1.437(5) . ? S4 O7 1.478(5) . ? S4 O4 1.478(5) . ? S4 O11 1.484(5) . ? S4 Sm2 3.0794(18) 2_434 ? S5 O24 1.446(6) . ? S5 O21 1.469(6) . ? S5 O28 1.473(6) . ? S5 O1 1.482(5) . ? S6 O25 1.445(5) . ? S6 O9 1.459(5) . ? S6 O10 1.485(5) . ? S6 O6 1.493(5) . ? S7 O14 1.470(5) . ? S7 O8 1.472(5) . ? S7 O12 1.482(5) . ? S7 O26 1.487(5) . ? S7 Sm1 3.2044(19) 2_445 ? O7 Sm2 2.429(5) 2_434 ? O11 Sm2 2.529(5) 2_434 ? O12 Sm1 2.663(5) 2_445 ? O14 Sm1 2.554(5) 2_445 ? N1 C1 1.467(11) . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N2 C2 1.450(10) . ? N2 H2C 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N3 C3 1.477(9) . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 C4 1.461(9) . ? N4 H4C 0.8900 . ? N4 H4D 0.8900 . ? N4 H4E 0.8900 . ? N5 C5 1.451(10) . ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N6 C6 1.491(10) . ? N6 H6C 0.8900 . ? N6 H6D 0.8900 . ? N6 H6E 0.8900 . ? C1 C2 1.413(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.490(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.490(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N8 C8 1.470(9) . ? N8 H8C 0.8900 . ? N8 H8D 0.8900 . ? N8 H8E 0.8900 . ? N7 C7 1.459(9) . ? N7 H7C 0.8900 . ? N7 H7D 0.8900 . ? N7 H7E 0.8900 . ? C8 C7 1.512(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 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 O23 Sm1 O13 82.03(18) . . ? O23 Sm1 O6 132.65(17) . . ? O13 Sm1 O6 87.35(16) . . ? O23 Sm1 O22 71.15(18) . . ? O13 Sm1 O22 84.41(16) . . ? O6 Sm1 O22 153.30(18) . . ? O23 Sm1 O26 76.24(17) . . ? O13 Sm1 O26 154.41(16) . . ? O6 Sm1 O26 117.37(17) . . ? O22 Sm1 O26 75.95(17) . . ? O23 Sm1 O14 140.35(17) . 2_444 ? O13 Sm1 O14 71.32(16) . 2_444 ? O6 Sm1 O14 75.92(16) . 2_444 ? O22 Sm1 O14 77.38(18) . 2_444 ? O26 Sm1 O14 118.86(16) . 2_444 ? O23 Sm1 O10 77.96(16) . . ? O13 Sm1 O10 68.87(15) . . ? O6 Sm1 O10 55.30(15) . . ? O22 Sm1 O10 141.55(15) . . ? O26 Sm1 O10 118.46(15) . . ? O14 Sm1 O10 116.64(14) 2_444 . ? O23 Sm1 O12 150.49(16) . 2_444 ? O13 Sm1 O12 123.37(16) . 2_444 ? O6 Sm1 O12 68.93(16) . 2_444 ? O22 Sm1 O12 94.77(16) . 2_444 ? O26 Sm1 O12 75.18(16) . 2_444 ? O14 Sm1 O12 53.62(16) 2_444 2_444 ? O10 Sm1 O12 122.79(15) . 2_444 ? O23 Sm1 O8 77.28(17) . . ? O13 Sm1 O8 133.66(16) . . ? O6 Sm1 O8 77.50(16) . . ? O22 Sm1 O8 125.53(17) . . ? O26 Sm1 O8 53.77(15) . . ? O14 Sm1 O8 142.08(16) 2_444 . ? O10 Sm1 O8 66.49(14) . . ? O12 Sm1 O8 91.60(16) 2_444 . ? O23 Sm1 S6 105.80(14) . . ? O13 Sm1 S6 75.30(12) . . ? O6 Sm1 S6 27.45(12) . . ? O22 Sm1 S6 159.71(12) . . ? O26 Sm1 S6 123.51(12) . . ? O14 Sm1 S6 95.40(12) 2_444 . ? O10 Sm1 S6 27.93(10) . . ? O12 Sm1 S6 96.02(12) 2_444 . ? O8 Sm1 S6 71.30(11) . . ? O23 Sm1 S7 73.58(13) . . ? O13 Sm1 S7 152.02(13) . . ? O6 Sm1 S7 99.07(12) . . ? O22 Sm1 S7 100.09(13) . . ? O26 Sm1 S7 26.63(12) . . ? O14 Sm1 S7 136.66(12) 2_444 . ? O10 Sm1 S7 92.39(10) . . ? O12 Sm1 S7 84.04(11) 2_444 . ? O8 Sm1 S7 27.22(11) . . ? S6 Sm1 S7 98.09(5) . . ? O23 Sm1 S7 159.68(13) . 2_444 ? O13 Sm1 S7 96.32(13) . 2_444 ? O6 Sm1 S7 67.18(12) . 2_444 ? O22 Sm1 S7 88.52(13) . 2_444 ? O26 Sm1 S7 99.36(12) . 2_444 ? O14 Sm1 S7 26.65(12) 2_444 2_444 ? O10 Sm1 S7 120.50(10) . 2_444 ? O12 Sm1 S7 27.31(11) 2_444 2_444 ? O8 Sm1 S7 116.51(12) . 2_444 ? S6 Sm1 S7 93.23(5) . 2_444 ? S7 Sm1 S7 111.313(15) . 2_444 ? O15 Sm2 O21 77.99(18) . . ? O15 Sm2 O4 152.28(18) . . ? O21 Sm2 O4 87.4(2) . . ? O15 Sm2 O20 83.16(18) . . ? O21 Sm2 O20 95.5(2) . . ? O4 Sm2 O20 74.85(18) . . ? O15 Sm2 O3 126.72(17) . . ? O21 Sm2 O3 154.89(17) . . ? O4 Sm2 O3 71.71(17) . . ? O20 Sm2 O3 92.37(17) . . ? O15 Sm2 O7 77.93(17) . 2_435 ? O21 Sm2 O7 104.6(2) . 2_435 ? O4 Sm2 O7 129.01(18) . 2_435 ? O20 Sm2 O7 148.68(17) . 2_435 ? O3 Sm2 O7 79.58(17) . 2_435 ? O15 Sm2 O11 126.15(17) . 2_435 ? O21 Sm2 O11 86.84(18) . 2_435 ? O4 Sm2 O11 75.59(17) . 2_435 ? O20 Sm2 O11 150.20(16) . 2_435 ? O3 Sm2 O11 74.80(16) . 2_435 ? O7 Sm2 O11 56.40(16) 2_435 2_435 ? O15 Sm2 O22 75.34(16) . . ? O21 Sm2 O22 151.92(15) . . ? O4 Sm2 O22 112.88(18) . . ? O20 Sm2 O22 72.87(17) . . ? O3 Sm2 O22 53.02(15) . . ? O7 Sm2 O22 78.28(17) 2_435 . ? O11 Sm2 O22 116.13(15) 2_435 . ? O15 Sm2 S4 103.67(13) . 2_435 ? O21 Sm2 S4 99.20(17) . 2_435 ? O4 Sm2 S4 101.82(14) . 2_435 ? O20 Sm2 S4 164.79(13) . 2_435 ? O3 Sm2 S4 72.61(12) . 2_435 ? O7 Sm2 S4 28.08(12) 2_435 2_435 ? O11 Sm2 S4 28.59(11) 2_435 2_435 ? O22 Sm2 S4 95.47(12) . 2_435 ? O15 Sm2 S1 101.26(13) . . ? O21 Sm2 S1 178.96(18) . . ? O4 Sm2 S1 93.58(14) . . ? O20 Sm2 S1 85.12(13) . . ? O3 Sm2 S1 25.75(12) . . ? O7 Sm2 S1 74.50(13) 2_435 . ? O11 Sm2 S1 93.05(12) 2_435 . ? O22 Sm2 S1 27.61(9) . . ? S4 Sm2 S1 80.25(6) 2_435 . ? O17 S1 O18 112.4(3) . . ? O17 S1 O3 111.1(3) . . ? O18 S1 O3 109.8(3) . . ? O17 S1 O22 110.5(4) . . ? O18 S1 O22 109.5(3) . . ? O3 S1 O22 103.1(3) . . ? O17 S1 Sm2 116.9(3) . . ? O18 S1 Sm2 130.2(3) . . ? O3 S1 Sm2 45.2(2) . . ? O22 S1 Sm2 58.73(18) . . ? O27 S2 O19 111.0(3) . . ? O27 S2 O13 109.9(3) . . ? O19 S2 O13 108.9(3) . . ? O27 S2 O20 109.1(3) . . ? O19 S2 O20 108.4(3) . . ? O13 S2 O20 109.5(3) . . ? O5 S3 O16 111.9(4) . . ? O5 S3 O23 109.0(3) . . ? O16 S3 O23 106.8(3) . . ? O5 S3 O15 110.4(3) . . ? O16 S3 O15 109.3(3) . . ? O23 S3 O15 109.3(3) . . ? O2 S4 O7 112.9(3) . . ? O2 S4 O4 110.7(3) . . ? O7 S4 O4 108.3(3) . . ? O2 S4 O11 110.2(3) . . ? O7 S4 O11 104.7(3) . . ? O4 S4 O11 109.9(3) . . ? O2 S4 Sm2 120.1(2) . 2_434 ? O7 S4 Sm2 50.7(2) . 2_434 ? O4 S4 Sm2 129.2(2) . 2_434 ? O11 S4 Sm2 54.65(19) . 2_434 ? O24 S5 O21 110.2(4) . . ? O24 S5 O28 109.7(4) . . ? O21 S5 O28 110.7(4) . . ? O24 S5 O1 109.7(3) . . ? O21 S5 O1 109.9(3) . . ? O28 S5 O1 106.6(3) . . ? O25 S6 O9 109.6(3) . . ? O25 S6 O10 111.8(3) . . ? O9 S6 O10 110.6(3) . . ? O25 S6 O6 110.9(3) . . ? O9 S6 O6 108.9(3) . . ? O10 S6 O6 105.0(3) . . ? O25 S6 Sm1 130.6(2) . . ? O9 S6 Sm1 119.6(2) . . ? O10 S6 Sm1 55.91(19) . . ? O6 S6 Sm1 49.3(2) . . ? O14 S7 O8 112.9(3) . . ? O14 S7 O12 105.8(3) . . ? O8 S7 O12 113.8(3) . . ? O14 S7 O26 109.3(3) . . ? O8 S7 O26 105.0(3) . . ? O12 S7 O26 110.2(3) . . ? O14 S7 Sm1 129.7(2) . . ? O8 S7 Sm1 57.0(2) . . ? O12 S7 Sm1 123.7(2) . . ? O26 S7 Sm1 48.2(2) . . ? O14 S7 Sm1 51.2(2) . 2_445 ? O8 S7 Sm1 139.2(2) . 2_445 ? O12 S7 Sm1 55.5(2) . 2_445 ? O26 S7 Sm1 115.6(2) . 2_445 ? Sm1 S7 Sm1 163.73(6) . 2_445 ? S1 O3 Sm2 109.0(3) . . ? S4 O4 Sm2 146.2(3) . . ? S6 O6 Sm1 103.2(3) . . ? S4 O7 Sm2 101.2(2) . 2_434 ? S7 O8 Sm1 95.8(2) . . ? S6 O10 Sm1 96.2(2) . . ? S4 O11 Sm2 96.8(2) . 2_434 ? S7 O12 Sm1 97.1(2) . 2_445 ? S2 O13 Sm1 144.9(3) . . ? S7 O14 Sm1 102.2(3) . 2_445 ? S3 O15 Sm2 147.0(3) . . ? S2 O20 Sm2 132.6(3) . . ? S5 O21 Sm2 142.7(4) . . ? S1 O22 Sm1 137.0(3) . . ? S1 O22 Sm2 93.7(2) . . ? Sm1 O22 Sm2 126.10(17) . . ? S3 O23 Sm1 141.3(3) . . ? S7 O26 Sm1 105.2(3) . . ? 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 . . ? C6 N6 H6C 109.5 . . ? C6 N6 H6D 109.5 . . ? H6C N6 H6D 109.5 . . ? C6 N6 H6E 109.5 . . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? C2 C1 N1 118.0(8) . . ? C2 C1 H1A 107.8 . . ? N1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? N1 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? C1 C2 N2 114.0(7) . . ? C1 C2 H2A 108.8 . . ? N2 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? N2 C2 H2B 108.8 . . ? H2A C2 H2B 107.6 . . ? N3 C3 C4 114.2(6) . . ? N3 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N3 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N4 C4 C3 113.5(6) . . ? N4 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N4 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N5 C5 C6 112.4(8) . . ? N5 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N5 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 N6 110.2(7) . . ? C5 C6 H6A 109.6 . . ? N6 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? N6 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 N8 H8C 109.5 . . ? C8 N8 H8D 109.5 . . ? H8C N8 H8D 109.5 . . ? C8 N8 H8E 109.5 . . ? H8C N8 H8E 109.5 . . ? H8D N8 H8E 109.5 . . ? C7 N7 H7C 109.5 . . ? C7 N7 H7D 109.5 . . ? H7C N7 H7D 109.5 . . ? C7 N7 H7E 109.5 . . ? H7C N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? N8 C8 C7 112.4(6) . . ? N8 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N8 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N7 C7 C8 111.9(6) . . ? N7 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N7 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.849 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.126 # Attachment '- 3.CIF' data_zl-21 _database_code_depnum_ccdc_archive 'CCDC 826956' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H14 N O14 S3 Sm' _chemical_formula_weight 522.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.237(3) _cell_length_b 9.364(3) _cell_length_c 9.557(3) _cell_angle_alpha 70.491(2) _cell_angle_beta 78.215(3) _cell_angle_gamma 79.378(3) _cell_volume 756.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3838 _cell_measurement_theta_min 2.272 _cell_measurement_theta_max 27.037 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 510 _exptl_absorpt_coefficient_mu 4.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5803 _exptl_absorpt_correction_T_max 0.6226 _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 5648 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2859 _reflns_number_gt 2698 _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^)+(0.0318P)^2^+0.8831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2859 _refine_ls_number_parameters 208 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Sm1 Sm 0.050430(13) -1.103912(13) 0.251289(13) 0.01820(3) Uani 1 1 d . . . S1 S 0.12181(8) -0.80693(7) -0.05216(7) 0.02429(15) Uani 1 1 d . . . S2 S -0.20230(7) -0.97921(7) 0.45737(7) 0.01895(14) Uani 1 1 d . . . S3 S 0.25894(8) -1.40509(8) 0.32078(9) 0.03068(18) Uani 1 1 d . . . O1 O -0.1121(2) -0.8912(2) 0.3157(2) 0.0239(4) Uani 1 1 d . . . O2 O -0.3577(2) -0.9572(2) 0.4364(2) 0.0314(5) Uani 1 1 d . . . O3 O -0.1357(2) -1.1397(2) 0.4814(2) 0.0260(5) Uani 1 1 d . . . O4 O -0.1906(2) -0.9258(2) 0.5818(2) 0.0318(5) Uani 1 1 d . . . O5 O 0.1825(2) -0.8501(3) -0.1912(2) 0.0381(6) Uani 1 1 d . . . O6 O -0.0393(2) -0.8293(3) -0.0242(2) 0.0388(5) Uani 1 1 d . . . O7 O 0.1906(2) -0.9156(2) 0.0740(2) 0.0341(5) Uani 1 1 d . . . O8 O 0.1438(3) -0.6543(3) -0.0696(3) 0.0594(7) Uani 1 1 d . . . O9 O 0.0968(2) -1.3702(2) 0.3792(2) 0.0292(5) Uani 1 1 d . . . O10 O 0.2977(2) -1.2565(2) 0.2095(2) 0.0286(5) Uani 1 1 d . . . O11 O 0.2784(3) -1.5229(2) 0.2494(3) 0.0573(7) Uani 1 1 d . . . O12 O 0.3458(3) -1.4488(3) 0.4423(3) 0.0635(8) Uani 1 1 d . . . O1W O -0.4425(3) -1.2425(3) 0.4094(3) 0.0655(9) Uani 1 1 d D . . H1WA H -0.3722(13) -1.214(2) 0.3387(16) 0.098 Uiso 1 1 d D . . H1WB H -0.493(2) -1.1752(12) 0.4467(19) 0.098 Uiso 1 1 d D . . H1WC H -0.430(3) -1.3320(10) 0.468(2) 0.098 Uiso 1 1 d D . . O2W O -0.0130(3) -0.6062(3) 0.2942(3) 0.0565(8) Uani 1 1 d D . . H2WA H -0.052(2) -0.5353(15) 0.2254(14) 0.085 Uiso 1 1 d D . . H2WB H -0.019(3) -0.6956(9) 0.295(2) 0.085 Uiso 1 1 d D . . H2WC H -0.020(3) -0.5907(17) 0.3774(10) 0.085 Uiso 1 1 d D . . C2 C -0.3546(5) -0.6334(4) 0.1325(5) 0.0595(12) Uani 1 1 d . . . H2A H -0.2527 -0.6143 0.1134 0.089 Uiso 1 1 calc R . . H2B H -0.3963 -0.6385 0.2344 0.089 Uiso 1 1 calc R . . H2C H -0.4105 -0.5521 0.0654 0.089 Uiso 1 1 calc R . . C1 C -0.5122(4) -0.8222(5) 0.1322(5) 0.0622(12) Uani 1 1 d . . . H1A H -0.5059 -0.9174 0.1125 0.093 Uiso 1 1 calc R . . H1B H -0.5711 -0.7442 0.0653 0.093 Uiso 1 1 calc R . . H1C H -0.5579 -0.8329 0.2342 0.093 Uiso 1 1 calc R . . N1 N -0.3614(3) -0.7795(3) 0.1084(3) 0.0423(8) Uani 1 1 d . . . H1D H -0.3183 -0.7745 0.0138 0.051 Uiso 1 1 calc R . . H1E H -0.3071 -0.8542 0.1708 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01747(6) 0.02021(6) 0.01804(6) -0.00802(5) -0.00083(5) -0.00319(5) S1 0.0300(3) 0.0237(3) 0.0207(3) -0.0028(2) -0.0073(2) -0.0109(3) S2 0.0164(3) 0.0237(3) 0.0183(3) -0.0088(2) -0.0020(2) -0.0028(2) S3 0.0241(3) 0.0208(3) 0.0450(4) -0.0065(3) -0.0074(3) -0.0021(3) O1 0.0244(9) 0.0225(8) 0.0230(8) -0.0074(7) 0.0010(7) -0.0030(7) O2 0.0195(8) 0.0430(10) 0.0367(10) -0.0186(8) -0.0046(8) -0.0045(8) O3 0.0285(9) 0.0231(9) 0.0212(9) -0.0038(7) 0.0007(8) -0.0008(8) O4 0.0308(10) 0.0458(11) 0.0258(9) -0.0206(8) -0.0055(8) -0.0023(9) O5 0.0287(10) 0.0667(13) 0.0217(9) -0.0144(9) 0.0038(8) -0.0202(10) O6 0.0252(10) 0.0657(12) 0.0366(10) -0.0317(9) -0.0011(8) -0.0069(9) O7 0.0411(10) 0.0329(10) 0.0274(10) 0.0025(8) -0.0137(8) -0.0155(9) O8 0.0991(17) 0.0261(11) 0.0627(14) 0.0019(10) -0.0483(13) -0.0212(12) O9 0.0262(9) 0.0236(9) 0.0351(10) -0.0076(8) 0.0017(8) -0.0067(8) O10 0.0246(9) 0.0250(9) 0.0343(10) -0.0097(8) 0.0018(8) -0.0047(8) O11 0.0368(12) 0.0360(10) 0.1067(18) -0.0426(11) 0.0065(12) -0.0042(10) O12 0.0562(13) 0.0502(15) 0.0760(17) 0.0130(13) -0.0419(13) -0.0129(12) O1W 0.0573(16) 0.0454(13) 0.0819(18) -0.0226(13) 0.0233(14) -0.0098(12) O2W 0.0733(16) 0.0439(13) 0.0534(14) -0.0056(11) -0.0210(13) -0.0152(12) C2 0.055(2) 0.051(2) 0.066(2) -0.0043(19) -0.0210(19) -0.0028(18) C1 0.045(2) 0.079(3) 0.063(2) -0.018(2) -0.0065(18) -0.018(2) N1 0.0283(12) 0.0571(17) 0.0356(13) -0.0108(12) -0.0056(11) 0.0029(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 Sm1 O4 2.360(2) 2_536 ? Sm1 O7 2.368(2) . ? Sm1 O9 2.3832(19) . ? Sm1 O1 2.4372(19) . ? Sm1 O3 2.4657(18) . ? Sm1 O6 2.476(2) 2_535 ? Sm1 O5 2.481(2) 2_535 ? Sm1 O10 2.4946(19) . ? Sm1 S2 3.0570(9) . ? Sm1 S3 3.0615(10) . ? Sm1 S1 3.1044(10) 2_535 ? Sm1 S1 3.3297(10) . ? S1 O8 1.430(3) . ? S1 O7 1.466(2) . ? S1 O5 1.488(2) . ? S1 O6 1.499(2) . ? S1 Sm1 3.1044(10) 2_535 ? S2 O2 1.457(2) . ? S2 O4 1.465(2) . ? S2 O3 1.4752(19) . ? S2 O1 1.5015(18) . ? S3 O11 1.447(3) . ? S3 O12 1.450(3) . ? S3 O10 1.4949(19) . ? S3 O9 1.504(2) . ? O4 Sm1 2.360(2) 2_536 ? O5 Sm1 2.481(2) 2_535 ? O6 Sm1 2.476(2) 2_535 ? O1W H1WA 0.844(8) . ? O1W H1WB 0.845(8) . ? O1W H1WC 0.842(8) . ? O2W H2WA 0.847(8) . ? O2W H2WB 0.846(8) . ? O2W H2WC 0.843(8) . ? C2 N1 1.476(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C1 N1 1.472(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N1 H1D 0.9000 . ? N1 H1E 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 O4 Sm1 O7 82.73(7) 2_536 . ? O4 Sm1 O9 85.05(7) 2_536 . ? O7 Sm1 O9 136.06(7) . . ? O4 Sm1 O1 82.17(7) 2_536 . ? O7 Sm1 O1 85.71(7) . . ? O9 Sm1 O1 133.96(6) . . ? O4 Sm1 O3 79.41(7) 2_536 . ? O7 Sm1 O3 140.73(7) . . ? O9 Sm1 O3 76.76(6) . . ? O1 Sm1 O3 57.47(6) . . ? O4 Sm1 O6 150.07(7) 2_536 2_535 ? O7 Sm1 O6 82.21(8) . 2_535 ? O9 Sm1 O6 88.08(8) . 2_535 ? O1 Sm1 O6 122.15(7) . 2_535 ? O3 Sm1 O6 127.10(7) . 2_535 ? O4 Sm1 O5 151.98(6) 2_536 2_535 ? O7 Sm1 O5 119.32(7) . 2_535 ? O9 Sm1 O5 88.83(7) . 2_535 ? O1 Sm1 O5 82.57(7) . 2_535 ? O3 Sm1 O5 72.57(7) . 2_535 ? O6 Sm1 O5 56.51(7) 2_535 2_535 ? O4 Sm1 O10 74.86(7) 2_536 . ? O7 Sm1 O10 78.35(7) . . ? O9 Sm1 O10 57.72(6) . . ? O1 Sm1 O10 153.41(7) . . ? O3 Sm1 O10 128.78(6) . . ? O6 Sm1 O10 76.86(7) 2_535 . ? O5 Sm1 O10 123.82(8) 2_535 . ? O4 Sm1 S2 80.67(5) 2_536 . ? O7 Sm1 S2 114.07(6) . . ? O9 Sm1 S2 105.23(5) . . ? O1 Sm1 S2 29.02(4) . . ? O3 Sm1 S2 28.50(4) . . ? O6 Sm1 S2 129.18(5) 2_535 . ? O5 Sm1 S2 74.62(6) 2_535 . ? O10 Sm1 S2 150.95(5) . . ? O4 Sm1 S3 77.56(5) 2_536 . ? O7 Sm1 S3 107.30(6) . . ? O9 Sm1 S3 28.76(5) . . ? O1 Sm1 S3 154.11(5) . . ? O3 Sm1 S3 102.58(4) . . ? O6 Sm1 S3 82.47(5) 2_535 . ? O5 Sm1 S3 108.55(6) 2_535 . ? O10 Sm1 S3 28.99(4) . . ? S2 Sm1 S3 129.80(2) . . ? O4 Sm1 S1 171.76(5) 2_536 2_535 ? O7 Sm1 S1 102.78(6) . 2_535 ? O9 Sm1 S1 86.74(6) . 2_535 ? O1 Sm1 S1 104.18(5) . 2_535 ? O3 Sm1 S1 99.43(6) . 2_535 ? O6 Sm1 S1 28.41(5) 2_535 2_535 ? O5 Sm1 S1 28.17(5) 2_535 2_535 ? O10 Sm1 S1 100.05(6) . 2_535 ? S2 Sm1 S1 102.27(3) . 2_535 ? S3 Sm1 S1 94.83(3) . 2_535 ? O4 Sm1 S1 102.06(5) 2_536 . ? O7 Sm1 S1 22.72(5) . . ? O9 Sm1 S1 149.23(5) . . ? O1 Sm1 S1 76.81(5) . . ? O3 Sm1 S1 133.81(4) . . ? O6 Sm1 S1 70.76(6) 2_535 . ? O5 Sm1 S1 97.13(5) 2_535 . ? O10 Sm1 S1 94.87(5) . . ? S2 Sm1 S1 105.45(3) . . ? S3 Sm1 S1 123.04(2) . . ? S1 Sm1 S1 84.68(3) 2_535 . ? O8 S1 O7 110.54(15) . . ? O8 S1 O5 111.94(15) . . ? O7 S1 O5 109.64(13) . . ? O8 S1 O6 113.24(15) . . ? O7 S1 O6 107.58(12) . . ? O5 S1 O6 103.60(13) . . ? O8 S1 Sm1 124.84(11) . 2_535 ? O7 S1 Sm1 124.62(10) . 2_535 ? O5 S1 Sm1 51.95(9) . 2_535 ? O6 S1 Sm1 51.83(9) . 2_535 ? O8 S1 Sm1 132.02(11) . . ? O7 S1 Sm1 38.61(8) . . ? O5 S1 Sm1 113.61(10) . . ? O6 S1 Sm1 69.37(8) . . ? Sm1 S1 Sm1 95.32(3) 2_535 . ? O2 S2 O4 109.80(12) . . ? O2 S2 O3 111.69(12) . . ? O4 S2 O3 111.42(12) . . ? O2 S2 O1 109.40(11) . . ? O4 S2 O1 109.68(12) . . ? O3 S2 O1 104.72(10) . . ? O2 S2 Sm1 122.23(9) . . ? O4 S2 Sm1 127.89(8) . . ? O3 S2 Sm1 52.89(7) . . ? O1 S2 Sm1 51.94(7) . . ? O11 S3 O12 111.75(17) . . ? O11 S3 O10 111.30(14) . . ? O12 S3 O10 110.03(14) . . ? O11 S3 O9 110.04(14) . . ? O12 S3 O9 109.83(15) . . ? O10 S3 O9 103.59(11) . . ? O11 S3 Sm1 127.11(12) . . ? O12 S3 Sm1 121.04(13) . . ? O10 S3 Sm1 53.97(8) . . ? O9 S3 Sm1 49.71(7) . . ? S2 O1 Sm1 99.05(9) . . ? S2 O3 Sm1 98.61(8) . . ? S2 O4 Sm1 151.15(12) . 2_536 ? S1 O5 Sm1 99.88(10) . 2_535 ? S1 O6 Sm1 99.77(10) . 2_535 ? S1 O7 Sm1 118.67(12) . . ? S3 O9 Sm1 101.53(9) . . ? S3 O10 Sm1 97.05(9) . . ? H1WA O1W H1WB 116.7(16) . . ? H1WA O1W H1WC 117.1(18) . . ? H1WB O1W H1WC 116.9(16) . . ? H2WA O2W H2WB 114.8(17) . . ? H2WA O2W H2WC 117.1(16) . . ? H2WB O2W H2WC 118.1(15) . . ? 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 . . ? 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 . . ? C1 N1 C2 115.3(3) . . ? C1 N1 H1D 108.5 . . ? C2 N1 H1D 108.5 . . ? C1 N1 H1E 108.5 . . ? C2 N1 H1E 108.5 . . ? H1D N1 H1E 107.5 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.683 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.127 # Attachment '- 4.CIF' data_zl-4-2 _database_code_depnum_ccdc_archive 'CCDC 826957' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 N3 O12 S3 Sm' _chemical_formula_weight 576.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.618(3) _cell_length_b 10.496(4) _cell_length_c 10.535(4) _cell_angle_alpha 71.826(4) _cell_angle_beta 73.584(4) _cell_angle_gamma 76.454(4) _cell_volume 956.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3280 _cell_measurement_theta_min 2.684 _cell_measurement_theta_max 27.026 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 3.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6252 _exptl_absorpt_correction_T_max 0.7024 _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 6592 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0547 _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 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3317 _reflns_number_gt 2903 _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^)+(0.0767P)^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 Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3317 _refine_ls_number_parameters 235 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.23322(3) 0.05548(3) -0.08535(3) 0.02684(15) Uani 1 1 d . . . S1 S 0.02370(19) -0.05262(18) -0.18927(17) 0.0325(4) Uani 1 1 d . . . S2 S 0.46489(18) -0.18288(16) 0.01918(18) 0.0322(4) Uani 1 1 d . . . S3 S 0.2561(2) 0.28755(18) -0.34522(18) 0.0382(4) Uani 1 1 d . . . O1 O 0.1681(5) 0.2944(5) -0.2069(5) 0.0366(11) Uani 1 1 d . . . O2 O 0.4591(5) -0.1056(5) -0.1226(5) 0.0405(12) Uani 1 1 d . . . O3 O -0.0145(5) 0.0706(5) -0.1342(5) 0.0402(12) Uani 1 1 d . . . O4 O 0.1743(5) -0.1104(5) -0.1771(5) 0.0404(12) Uani 1 1 d . . . O5 O 0.3316(5) -0.1197(5) 0.1050(5) 0.0389(12) Uani 1 1 d . . . O6 O 0.3287(6) 0.1440(5) -0.3278(5) 0.0434(12) Uani 1 1 d . . . O7 O 0.5963(5) -0.1686(5) 0.0510(5) 0.0406(12) Uani 1 1 d . . . O8 O -0.0787(5) -0.1459(5) -0.0989(5) 0.0361(11) Uani 1 1 d . . . O9 O 0.4625(6) -0.3269(5) 0.0388(6) 0.0508(14) Uani 1 1 d . . . O10 O 0.0076(7) -0.0155(7) -0.3283(5) 0.0605(17) Uani 1 1 d . . . O11 O 0.1616(7) 0.3214(6) -0.4399(5) 0.0607(16) Uani 1 1 d . . . O12 O 0.3638(7) 0.3794(6) -0.3933(6) 0.0581(16) Uani 1 1 d . . . C1 C -0.2144(14) 0.3230(11) -0.4185(12) 0.096(4) Uani 1 1 d . . . H1C H -0.1847 0.2416 -0.4492 0.143 Uiso 1 1 calc R . . H1D H -0.1924 0.3998 -0.4950 0.143 Uiso 1 1 calc R . . H1E H -0.3181 0.3339 -0.3793 0.143 Uiso 1 1 calc R . . C2 C -0.1709(12) 0.4310(10) -0.2601(11) 0.076(3) Uani 1 1 d . . . H2C H -0.1146 0.4177 -0.1935 0.115 Uiso 1 1 calc R . . H2D H -0.2737 0.4436 -0.2174 0.115 Uiso 1 1 calc R . . H2E H -0.1487 0.5100 -0.3337 0.115 Uiso 1 1 calc R . . C3 C 0.7927(12) -0.5397(11) 0.1006(13) 0.093(4) Uani 1 1 d . . . H3C H 0.8291 -0.4570 0.0466 0.140 Uiso 1 1 calc R . . H3D H 0.7813 -0.5878 0.0411 0.140 Uiso 1 1 calc R . . H3E H 0.8611 -0.5954 0.1547 0.140 Uiso 1 1 calc R . . C4 C 0.5894(12) -0.6278(10) 0.2759(11) 0.073(3) Uani 1 1 d . . . H4A H 0.4967 -0.5999 0.3324 0.110 Uiso 1 1 calc R . . H4B H 0.6542 -0.6847 0.3332 0.110 Uiso 1 1 calc R . . H4C H 0.5748 -0.6776 0.2195 0.110 Uiso 1 1 calc R . . C5 C -0.3400(11) 0.0196(12) -0.4351(11) 0.085(3) Uani 1 1 d D . . H5A H -0.3038 0.1044 -0.4640 0.127 Uiso 1 1 d R A . H5B H -0.3437 -0.0055 -0.5141 0.127 Uiso 1 1 d R . . H5C H -0.4368 0.0291 -0.3772 0.127 Uiso 1 1 d R . . C6 C -0.2349(12) -0.2100(11) -0.3008(12) 0.081(3) Uani 1 1 d D . . H6A H -0.1479 -0.2335 -0.2654 0.122 Uiso 1 1 d R A . H6B H -0.3186 -0.2283 -0.2264 0.122 Uiso 1 1 d R . . H6C H -0.2256 -0.2630 -0.3633 0.122 Uiso 1 1 d R . . N1 N -0.1342(9) 0.3131(8) -0.3138(8) 0.069(2) Uani 1 1 d . . . H1A H -0.1535 0.2395 -0.2438 0.083 Uiso 1 1 calc R . . H1B H -0.0371 0.3007 -0.3510 0.083 Uiso 1 1 calc R . . N2 N 0.6539(8) -0.5086(7) 0.1893(7) 0.0555(19) Uani 1 1 d . . . H2A H 0.5912 -0.4548 0.1378 0.067 Uiso 1 1 calc R . . H2B H 0.6652 -0.4616 0.2430 0.067 Uiso 1 1 calc R . . N3 N -0.2813(12) -0.0580(11) -0.3170(10) 0.033(3) Uani 0.50 1 d PDU A 1 H3A H -0.3494 -0.0457 -0.2414 0.040 Uiso 0.50 1 calc PR A 1 H3B H -0.2029 -0.0234 -0.3201 0.040 Uiso 0.50 1 calc PR A 1 N3A N -0.222(2) -0.0942(18) -0.414(2) 0.108(7) Uani 0.50 1 d PDU A 2 H3AA H -0.1959 -0.1245 -0.4894 0.130 Uiso 0.50 1 calc PR A 2 H3AB H -0.1455 -0.0597 -0.4123 0.130 Uiso 0.50 1 calc PR A 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 Sm1 0.0244(2) 0.0207(2) 0.0353(2) -0.00445(15) -0.01095(14) -0.00238(14) S1 0.0288(9) 0.0354(9) 0.0366(9) -0.0093(7) -0.0088(7) -0.0098(7) S2 0.0265(9) 0.0195(8) 0.0510(10) -0.0021(7) -0.0166(8) -0.0047(7) S3 0.0481(11) 0.0291(9) 0.0344(9) -0.0013(7) -0.0106(8) -0.0085(8) O1 0.047(3) 0.023(2) 0.038(3) -0.005(2) -0.014(2) -0.002(2) O2 0.036(3) 0.035(3) 0.043(3) -0.005(2) -0.012(2) 0.004(2) O3 0.037(3) 0.025(3) 0.061(3) -0.011(2) -0.021(2) 0.003(2) O4 0.028(3) 0.037(3) 0.064(3) -0.027(3) -0.010(2) -0.002(2) O5 0.031(3) 0.031(3) 0.043(3) 0.006(2) -0.011(2) -0.001(2) O6 0.044(3) 0.036(3) 0.041(3) -0.010(2) -0.001(2) 0.001(2) O7 0.026(3) 0.033(3) 0.065(3) -0.008(2) -0.020(2) -0.005(2) O8 0.035(3) 0.033(3) 0.044(3) -0.013(2) -0.004(2) -0.014(2) O9 0.051(3) 0.016(2) 0.092(4) -0.003(3) -0.039(3) -0.004(2) O10 0.058(4) 0.091(5) 0.038(3) -0.006(3) -0.009(3) -0.040(4) O11 0.087(5) 0.054(4) 0.041(3) 0.000(3) -0.029(3) -0.011(3) O12 0.066(4) 0.042(3) 0.059(4) -0.001(3) -0.002(3) -0.027(3) C1 0.123(11) 0.060(7) 0.108(9) 0.017(6) -0.065(8) -0.027(7) C2 0.078(7) 0.058(6) 0.082(7) -0.008(5) -0.007(6) -0.016(6) C3 0.090(9) 0.067(8) 0.120(10) -0.040(7) 0.005(8) -0.024(7) C4 0.088(8) 0.046(6) 0.078(7) -0.012(5) -0.017(6) -0.003(5) C5 0.052(6) 0.114(10) 0.096(8) -0.034(7) -0.022(6) -0.011(6) C6 0.072(7) 0.091(8) 0.100(8) -0.052(7) -0.018(6) -0.016(6) N1 0.066(5) 0.049(5) 0.071(5) 0.016(4) -0.022(4) -0.004(4) N2 0.066(5) 0.041(4) 0.070(5) -0.022(4) -0.038(4) 0.010(4) N3 0.026(5) 0.054(6) 0.031(5) -0.024(5) 0.001(4) -0.017(5) N3A 0.109(11) 0.120(11) 0.109(11) -0.028(8) -0.030(8) -0.039(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 Sm1 O8 2.395(5) 2 ? Sm1 O7 2.397(5) 2_655 ? Sm1 O6 2.413(5) . ? Sm1 O2 2.437(5) . ? Sm1 O1 2.457(4) . ? Sm1 O4 2.471(5) . ? Sm1 O5 2.501(4) . ? Sm1 O3 2.536(5) . ? Sm1 O3 2.858(5) 2 ? Sm1 S3 3.0377(19) . ? Sm1 S2 3.0812(18) . ? Sm1 S1 3.1047(18) . ? S1 O10 1.437(6) . ? S1 O4 1.459(5) . ? S1 O8 1.474(5) . ? S1 O3 1.506(5) . ? S1 Sm1 3.2276(19) 2 ? S2 O7 1.446(5) . ? S2 O9 1.465(5) . ? S2 O2 1.470(5) . ? S2 O5 1.491(5) . ? S3 O11 1.445(6) . ? S3 O12 1.458(6) . ? S3 O1 1.478(5) . ? S3 O6 1.483(5) . ? O3 Sm1 2.858(5) 2 ? O7 Sm1 2.397(5) 2_655 ? O8 Sm1 2.395(5) 2 ? C1 N1 1.482(13) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 N1 1.448(12) . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 N2 1.430(11) . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C3 H3E 0.9600 . ? C4 N2 1.454(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N3 1.442(13) . ? C5 N3A 1.450(16) . ? C5 H5A 0.9600 . ? C5 H5B 0.9601 . ? C5 H5C 0.9600 . ? C6 N3A 1.411(15) . ? C6 N3 1.521(12) . ? C6 H6A 0.9599 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N3A H3AA 0.9000 . ? N3A H3AB 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 O8 Sm1 O7 80.81(16) 2 2_655 ? O8 Sm1 O6 136.30(16) 2 . ? O7 Sm1 O6 86.38(18) 2_655 . ? O8 Sm1 O2 137.52(17) 2 . ? O7 Sm1 O2 79.44(17) 2_655 . ? O6 Sm1 O2 79.24(16) . . ? O8 Sm1 O1 78.78(16) 2 . ? O7 Sm1 O1 75.97(16) 2_655 . ? O6 Sm1 O1 57.57(16) . . ? O2 Sm1 O1 130.92(16) . . ? O8 Sm1 O4 125.67(16) 2 . ? O7 Sm1 O4 152.05(17) 2_655 . ? O6 Sm1 O4 79.37(18) . . ? O2 Sm1 O4 74.37(16) . . ? O1 Sm1 O4 114.67(17) . . ? O8 Sm1 O5 82.80(16) 2 . ? O7 Sm1 O5 78.33(17) 2_655 . ? O6 Sm1 O5 135.00(16) . . ? O2 Sm1 O5 56.55(16) . . ? O1 Sm1 O5 150.37(17) . . ? O4 Sm1 O5 94.92(17) . . ? O8 Sm1 O3 80.91(16) 2 . ? O7 Sm1 O3 148.11(16) 2_655 . ? O6 Sm1 O3 89.05(17) . . ? O2 Sm1 O3 130.52(16) . . ? O1 Sm1 O3 74.99(16) . . ? O4 Sm1 O3 56.20(15) . . ? O5 Sm1 O3 124.69(16) . . ? O8 Sm1 O3 53.07(15) 2 2 ? O7 Sm1 O3 122.80(16) 2_655 2 ? O6 Sm1 O3 149.90(17) . 2 ? O2 Sm1 O3 110.89(15) . 2 ? O1 Sm1 O3 118.16(15) . 2 ? O4 Sm1 O3 76.59(16) . 2 ? O5 Sm1 O3 65.48(14) . 2 ? O3 Sm1 O3 62.51(18) . 2 ? O8 Sm1 S3 107.56(12) 2 . ? O7 Sm1 S3 79.92(13) 2_655 . ? O6 Sm1 S3 28.77(12) . . ? O2 Sm1 S3 105.46(12) . . ? O1 Sm1 S3 28.80(11) . . ? O4 Sm1 S3 97.66(13) . . ? O5 Sm1 S3 154.02(12) . . ? O3 Sm1 S3 81.00(12) . . ? O3 Sm1 S3 139.76(10) 2 . ? O8 Sm1 S2 110.72(13) 2 . ? O7 Sm1 S2 77.46(12) 2_655 . ? O6 Sm1 S2 106.84(12) . . ? O2 Sm1 S2 27.91(12) . . ? O1 Sm1 S2 149.84(12) . . ? O4 Sm1 S2 83.79(12) . . ? O5 Sm1 S2 28.64(11) . . ? O3 Sm1 S2 133.73(11) . . ? O3 Sm1 S2 88.34(10) 2 . ? S3 Sm1 S2 131.15(5) . . ? O8 Sm1 S1 104.93(12) 2 . ? O7 Sm1 S1 168.44(13) 2_655 . ? O6 Sm1 S1 82.58(14) . . ? O2 Sm1 S1 101.75(13) . . ? O1 Sm1 S1 95.10(12) . . ? O4 Sm1 S1 27.44(11) . . ? O5 Sm1 S1 112.06(12) . . ? O3 Sm1 S1 28.78(11) . . ? O3 Sm1 S1 67.77(11) 2 . ? S3 Sm1 S1 88.72(5) . . ? S2 Sm1 S1 109.03(5) . . ? O10 S1 O4 112.6(3) . . ? O10 S1 O8 110.7(3) . . ? O4 S1 O8 110.9(3) . . ? O10 S1 O3 110.7(4) . . ? O4 S1 O3 105.4(3) . . ? O8 S1 O3 106.2(3) . . ? O10 S1 Sm1 125.6(2) . . ? O4 S1 Sm1 51.33(19) . . ? O8 S1 Sm1 123.6(2) . . ? O3 S1 Sm1 54.16(19) . . ? O10 S1 Sm1 127.6(3) . 2 ? O4 S1 Sm1 119.3(2) . 2 ? O8 S1 Sm1 43.92(18) . 2 ? O3 S1 Sm1 62.3(2) . 2 ? Sm1 S1 Sm1 93.55(5) . 2 ? O7 S2 O9 109.6(3) . . ? O7 S2 O2 110.2(3) . . ? O9 S2 O2 110.5(3) . . ? O7 S2 O5 110.4(3) . . ? O9 S2 O5 111.5(3) . . ? O2 S2 O5 104.4(3) . . ? O7 S2 Sm1 124.8(2) . . ? O9 S2 Sm1 125.6(2) . . ? O2 S2 Sm1 50.90(19) . . ? O5 S2 Sm1 53.54(18) . . ? O11 S3 O12 110.3(4) . . ? O11 S3 O1 110.3(3) . . ? O12 S3 O1 110.2(3) . . ? O11 S3 O6 109.9(3) . . ? O12 S3 O6 111.2(3) . . ? O1 S3 O6 104.8(3) . . ? O11 S3 Sm1 124.3(3) . . ? O12 S3 Sm1 125.4(3) . . ? O1 S3 Sm1 53.21(18) . . ? O6 S3 Sm1 51.55(19) . . ? S3 O1 Sm1 98.0(2) . . ? S2 O2 Sm1 101.2(2) . . ? S1 O3 Sm1 97.1(2) . . ? S1 O3 Sm1 89.9(2) . 2 ? Sm1 O3 Sm1 117.49(18) . 2 ? S1 O4 Sm1 101.2(2) . . ? S2 O5 Sm1 97.8(2) . . ? S3 O6 Sm1 99.7(2) . . ? S2 O7 Sm1 157.6(3) . 2_655 ? S1 O8 Sm1 110.8(2) . 2 ? 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 . . ? N3 C5 N3A 46.7(9) . . ? N3 C5 H5A 105.0 . . ? N3A C5 H5A 110.9 . . ? N3 C5 H5B 130.8 . . ? N3A C5 H5B 88.0 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 90.2 . . ? N3A C5 H5C 126.7 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3A C6 N3 45.9(9) . . ? N3A C6 H6A 109.2 . . ? N3 C6 H6A 105.1 . . ? N3A C6 H6B 127.9 . . ? N3 C6 H6B 90.8 . . ? H6A C6 H6B 109.5 . . ? N3A C6 H6C 88.7 . . ? N3 C6 H6C 130.2 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 N1 C1 114.1(8) . . ? C2 N1 H1A 108.7 . . ? C1 N1 H1A 108.7 . . ? C2 N1 H1B 108.7 . . ? C1 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? C3 N2 C4 113.7(8) . . ? C3 N2 H2A 108.8 . . ? C4 N2 H2A 108.8 . . ? C3 N2 H2B 108.8 . . ? C4 N2 H2B 108.8 . . ? H2A N2 H2B 107.7 . . ? C5 N3 C6 116.8(9) . . ? C5 N3 H3A 108.1 . . ? C6 N3 H3A 108.1 . . ? C5 N3 H3B 108.1 . . ? C6 N3 H3B 108.1 . . ? H3A N3 H3B 107.3 . . ? C6 N3A C5 123.8(16) . . ? C6 N3A H3AA 106.4 . . ? C5 N3A H3AA 106.4 . . ? C6 N3A H3AB 106.4 . . ? C5 N3A H3AB 106.4 . . ? H3AA N3A H3AB 106.4 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.052 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.174