Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Premyslaw Starynowicz' _publ_contact_author_address ; Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 Wroclaw 50-383 POLAND ; _publ_contact_author_email PSTA@WCHUWR.CHEM.UNI.WROC.PL _publ_section_title ; Two complexes of Sm(II) with crown ethers electrochemical synthesis, structure and spectroscopy ; _publ_author_name 'Premyslaw Starynowicz' data_sm45sc _database_code_depnum_ccdc_archive 'CCDC 226735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Cl2 O14 Sm' _chemical_formula_weight 613.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 'P 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.045(3) _cell_length_b 11.053(2) _cell_length_c 13.108(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.34(3) _cell_angle_gamma 90.00 _cell_volume 2056.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1657 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20 _exptl_crystal_description irregular _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 3.182 _exptl_absorpt_correction_type 'analytical, from the crystal shape' _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.600 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8636 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 22.55 _reflns_number_total 2695 _reflns_number_gt 2025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software (1999)' _computing_cell_refinement 'Kuma KM4 software (1999)' _computing_data_reduction 'Kuma KM4 software (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 2695 _refine_ls_number_parameters 255 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.1017 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.2121 _refine_ls_goodness_of_fit_ref 1.323 _refine_ls_restrained_S_all 1.312 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.5000 0.2214(2) 0.2500 0.097(2) Uani 1 d S . . Sm2 Sm 0.0000 0.72145(13) 0.2500 0.0348(19) Uani 1 d S . . Cl1A Cl 0.3127(6) 0.2468(13) 0.3454(15) 0.079(6) Uani 0.50 d PDU . . Cl1B Cl 0.3140(6) 0.2431(15) 0.3075(15) 0.094(8) Uani 0.50 d PDU . . Cl2 Cl 0.1876(3) 0.7465(3) 0.1739(3) 0.038(2) Uani 1 d . . . O1 O 0.3966(11) 0.1744(19) 0.3668(15) 0.123(8) Uani 1 d D . . O2A O 0.336(2) 0.334(3) 0.276(2) 0.079(10) Uiso 0.50 d PD . . O2B O 0.320(2) 0.266(3) 0.2012(18) 0.069(8) Uiso 0.50 d PD . . O3 O 0.2271(9) 0.1812(15) 0.2955(12) 0.088(6) Uani 1 d D . . O4A O 0.318(3) 0.298(3) 0.448(2) 0.095(10) Uiso 0.50 d PD . . O4B O 0.301(4) 0.364(3) 0.341(4) 0.155(19) Uiso 0.50 d PD . . O5 O 0.1719(11) 0.7998(18) 0.2637(12) 0.090(6) Uani 1 d . . . O6 O 0.2681(13) 0.682(2) 0.201(2) 0.133(9) Uani 1 d . . . O7 O 0.1112(14) 0.667(2) 0.1349(19) 0.157(12) Uani 1 d . . . O8 O 0.1910(13) 0.827(2) 0.0981(15) 0.112(7) Uani 1 d . . . O11 O 0.4663(18) -0.011(2) 0.1486(19) 0.055(7) Uiso 0.50 d PD A -1 O12 O 0.386(3) 0.175(3) 0.013(3) 0.056(15) Uiso 0.50 d PD A -1 O13 O 0.4413(15) 0.3998(19) 0.079(2) 0.039(6) Uiso 0.50 d PD A -1 O14 O 0.5079(14) 0.447(2) 0.2999(14) 0.038(6) Uiso 0.50 d PD A -1 O15 O 0.6139(18) 0.270(2) 0.429(2) 0.061(7) Uiso 0.50 d PD A -1 O16 O 0.5731(18) 0.032(2) 0.3528(18) 0.050(7) Uiso 0.50 d PD A -1 C1 C 0.376(2) -0.028(4) 0.051(2) 0.084(14) Uiso 0.50 d PD A -1 H1A H 0.3684 -0.1119 0.0271 0.101 Uiso 0.50 calc PR A -1 H1B H 0.3210 -0.0019 0.0666 0.101 Uiso 0.50 calc PR A -1 C2 C 0.394(3) 0.045(3) -0.026(3) 0.061(11) Uiso 0.50 d PD A -1 H2A H 0.3475 0.0315 -0.0969 0.074 Uiso 0.50 calc PR A -1 H2B H 0.4561 0.0305 -0.0299 0.074 Uiso 0.50 calc PR A -1 C3 C 0.407(3) 0.269(3) -0.062(3) 0.077(13) Uiso 0.50 d PD A -1 H3A H 0.4744 0.2799 -0.0470 0.093 Uiso 0.50 calc PR A -1 H3B H 0.3769 0.2501 -0.1377 0.093 Uiso 0.50 calc PR A -1 C4 C 0.367(3) 0.368(4) -0.030(3) 0.074(14) Uiso 0.50 d PD A -1 H4A H 0.3071 0.3470 -0.0211 0.089 Uiso 0.50 calc PR A -1 H4B H 0.3572 0.4343 -0.0808 0.089 Uiso 0.50 calc PR A -1 C5 C 0.4116(17) 0.514(2) 0.126(2) 0.023(7) Uiso 0.50 d PD A -1 H5A H 0.3951 0.5786 0.0728 0.027 Uiso 0.50 calc PR A -1 H5B H 0.3582 0.4978 0.1497 0.027 Uiso 0.50 calc PR A -1 C6 C 0.490(2) 0.545(3) 0.2125(18) 0.052(11) Uiso 0.50 d PD A -1 H6A H 0.4803 0.6222 0.2417 0.062 Uiso 0.50 calc PR A -1 H6B H 0.5445 0.5515 0.1888 0.062 Uiso 0.50 calc PR A -1 C7 C 0.584(2) 0.475(3) 0.4087(18) 0.042(9) Uiso 0.50 d PD A -1 H7A H 0.6452 0.4821 0.3989 0.051 Uiso 0.50 calc PR A -1 H7B H 0.5705 0.5517 0.4369 0.051 Uiso 0.50 calc PR A -1 C8 C 0.586(3) 0.383(2) 0.480(3) 0.036(8) Uiso 0.50 d PD A -1 H8A H 0.5246 0.3728 0.4882 0.044 Uiso 0.50 calc PR A -1 H8B H 0.6319 0.3998 0.5508 0.044 Uiso 0.50 calc PR A -1 C9 C 0.622(6) 0.156(4) 0.499(5) 0.07(3) Uiso 0.50 d PD A -1 H9A H 0.6626 0.1691 0.5730 0.087 Uiso 0.50 calc PR A -1 H9B H 0.5602 0.1297 0.5001 0.087 Uiso 0.50 calc PR A -1 C10 C 0.660(2) 0.072(4) 0.447(3) 0.075(13) Uiso 0.50 d PD A -1 H10A H 0.6881 0.0048 0.4940 0.089 Uiso 0.50 calc PR A -1 H10B H 0.7070 0.1092 0.4213 0.089 Uiso 0.50 calc PR A -1 C11 C 0.5761(18) -0.090(3) 0.299(3) 0.058(11) Uiso 0.50 d PD A -1 H11A H 0.6150 -0.0870 0.2528 0.070 Uiso 0.50 calc PR A -1 H11B H 0.5989 -0.1542 0.3518 0.070 Uiso 0.50 calc PR A -1 C12 C 0.4821(19) -0.106(3) 0.239(3) 0.052(10) Uiso 0.50 d PD A -1 H12A H 0.4421 -0.0910 0.2822 0.063 Uiso 0.50 calc PR A -1 H12B H 0.4703 -0.1875 0.2093 0.063 Uiso 0.50 calc PR A -1 O21 O 0.0068(18) 0.954(2) 0.3323(17) 0.053(7) Uiso 0.50 d PD B -1 O22 O 0.1089(14) 0.766(2) 0.4626(17) 0.037(5) Uiso 0.50 d PD B -1 O23 O 0.0776(16) 0.547(2) 0.3972(18) 0.048(6) Uiso 0.50 d PD B -1 O24 O -0.0231(15) 0.493(2) 0.1936(17) 0.053(7) Uiso 0.50 d PD B -1 O25 O -0.101(2) 0.672(2) 0.0604(19) 0.076(9) Uiso 0.50 d PD B -1 O26 O -0.0545(16) 0.911(2) 0.1185(17) 0.049(7) Uiso 0.50 d PD B -1 C21 C 0.078(3) 0.968(4) 0.447(2) 0.099(17) Uiso 0.50 d PD B -1 H21A H 0.1400 0.9800 0.4398 0.119 Uiso 0.50 calc PR B -1 H21B H 0.0629 1.0419 0.4774 0.119 Uiso 0.50 calc PR B -1 C22 C 0.086(4) 0.877(3) 0.521(3) 0.076(14) Uiso 0.50 d PD B -1 H22A H 0.0281 0.8655 0.5361 0.092 Uiso 0.50 calc PR B -1 H22B H 0.1370 0.8930 0.5881 0.092 Uiso 0.50 calc PR B -1 C23 C 0.149(5) 0.664(4) 0.544(4) 0.14(2) Uiso 0.50 d PD B -1 H23A H 0.2053 0.6912 0.6002 0.162 Uiso 0.50 calc PR B -1 H23B H 0.1030 0.6404 0.5777 0.162 Uiso 0.50 calc PR B -1 C24 C 0.170(3) 0.566(6) 0.491(4) 0.107(19) Uiso 0.50 d PD B -1 H24A H 0.1858 0.4953 0.5376 0.129 Uiso 0.50 calc PR B -1 H24B H 0.2217 0.5838 0.4648 0.129 Uiso 0.50 calc PR B -1 C25 C 0.096(2) 0.428(3) 0.347(3) 0.051(10) Uiso 0.50 d PD B -1 H25A H 0.1436 0.4420 0.3125 0.061 Uiso 0.50 calc PR B -1 H25B H 0.1207 0.3682 0.4032 0.061 Uiso 0.50 calc PR B -1 C26 C 0.015(4) 0.387(3) 0.272(4) 0.099(17) Uiso 0.50 d PD B -1 H26A H -0.0307 0.3633 0.3063 0.118 Uiso 0.50 calc PR B -1 H26B H 0.0273 0.3171 0.2334 0.118 Uiso 0.50 calc PR B -1 C27 C -0.1114(19) 0.468(3) 0.0949(19) 0.044(9) Uiso 0.50 d PD B -1 H27A H -0.1116 0.3846 0.0723 0.052 Uiso 0.50 calc PR B -1 H27B H -0.1677 0.4821 0.1138 0.052 Uiso 0.50 calc PR B -1 C28 C -0.111(3) 0.544(2) 0.011(2) 0.036(8) Uiso 0.50 d PD B -1 H28A H -0.1689 0.5369 -0.0491 0.043 Uiso 0.50 calc PR B -1 H28B H -0.0582 0.5262 -0.0131 0.043 Uiso 0.50 calc PR B -1 C29 C -0.103(2) 0.7591(19) -0.031(2) 0.028(7) Uiso 0.50 d PD B -1 H29A H -0.0426 0.7631 -0.0424 0.034 Uiso 0.50 calc PR B -1 H29B H -0.1515 0.7373 -0.0988 0.034 Uiso 0.50 calc PR B -1 C30 C -0.124(2) 0.865(2) 0.011(2) 0.034(8) Uiso 0.50 d PD B -1 H30A H -0.1852 0.8554 0.0200 0.041 Uiso 0.50 calc PR B -1 H30B H -0.1312 0.9284 -0.0430 0.041 Uiso 0.50 calc PR B -1 C31 C -0.0669(19) 1.029(3) 0.176(3) 0.073(13) Uiso 0.50 d PD B -1 H31A H -0.0849 1.0952 0.1248 0.088 Uiso 0.50 calc PR B -1 H31B H -0.1144 1.0185 0.2101 0.088 Uiso 0.50 calc PR B -1 C32 C 0.0209(15) 1.048(2) 0.2517(19) 0.021(7) Uiso 0.50 d PD B -1 H32A H 0.0287 1.1301 0.2802 0.025 Uiso 0.50 calc PR B -1 H32B H 0.0722 1.0277 0.2254 0.025 Uiso 0.50 calc PR B -1 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 0.073(2) 0.066(2) 0.127(3) 0.000 0.0021(13) 0.000 Sm2 0.036(2) 0.035(2) 0.030(2) 0.000 0.0070(8) 0.000 Cl1A 0.043(8) 0.123(15) 0.064(11) -0.012(8) 0.009(6) -0.002(7) Cl1B 0.054(9) 0.135(16) 0.072(13) -0.016(10) -0.007(7) 0.007(9) Cl2 0.043(3) 0.037(3) 0.034(3) 0.0007(17) 0.0136(19) 0.0047(19) O1 0.073(12) 0.149(19) 0.108(14) -0.004(13) -0.021(10) 0.069(12) O3 0.065(10) 0.097(13) 0.078(10) 0.015(9) -0.008(8) -0.054(9) O5 0.080(10) 0.139(16) 0.065(9) -0.047(10) 0.044(8) -0.054(11) O6 0.083(13) 0.15(2) 0.19(2) 0.080(17) 0.077(14) 0.030(13) O7 0.106(14) 0.22(3) 0.19(2) -0.16(2) 0.104(15) -0.062(16) O8 0.092(12) 0.144(18) 0.116(14) 0.083(13) 0.056(11) 0.044(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 O15 2.47(3) . yes Sm1 O16 2.53(2) . yes Sm1 O1 2.57(2) . yes Sm1 O14 2.57(2) . yes Sm1 O2B 2.61(3) . yes Sm1 O11 2.86(3) . yes Sm1 O2A 2.88(3) . yes Sm1 O13 2.89(2) . yes Sm1 O12 3.06(5) . yes Sm1 Cl1B 3.139(14) 2_655 no Sm1 Cl1B 3.139(14) . no Sm2 O25 2.51(3) . yes Sm2 O24 2.62(3) . yes Sm2 O7 2.666(15) . yes Sm2 O26 2.67(2) . yes Sm2 O5 2.676(14) . yes Sm2 O23 2.70(2) . yes Sm2 O22 2.77(2) . yes Sm2 O22 2.77(2) 2 no Sm2 O21 2.78(2) . yes Sm2 O21 2.78(2) 2 no Cl1A Cl1B 0.51(3) . no Cl1A O4B 1.31(4) . no Cl1A O3 1.434(13) . no Cl1A O4A 1.439(14) . no Cl1A O1 1.441(13) . no Cl1A O2A 1.446(14) . no Cl1A O2B 1.94(3) . no Cl1B O2A 1.17(3) . no Cl1B O3 1.438(13) . no Cl1B O1 1.445(13) . no Cl1B O4B 1.445(14) . no Cl1B O2B 1.450(14) . no Cl1B O4A 1.92(3) . no Cl2 O8 1.350(16) . no Cl2 O6 1.350(19) . no Cl2 O7 1.401(19) . no Cl2 O5 1.404(14) . no O2A O2B 1.19(4) . no O2A O4B 1.19(5) . no O4A O4B 1.53(6) . no O11 C1 1.538(10) . no O11 C12 1.541(10) . no O12 C2 1.535(10) . no O12 C3 1.538(10) . no O13 C5 1.535(10) . no O13 C4 1.537(10) . no O14 C6 1.529(10) . no O14 C7 1.539(10) . no O15 C8 1.541(10) . no O15 C9 1.543(10) . no O16 C10 1.537(10) . no O16 C11 1.538(10) . no C1 C2 1.382(10) . no C3 C4 1.384(10) . no C5 C6 1.381(10) . no C7 C8 1.380(10) . no C9 C10 1.383(10) . no C11 C12 1.382(10) . no O21 C21 1.538(10) . no O21 C32 1.547(10) . no O22 C22 1.535(10) . no O22 C23 1.538(10) . no O23 C25 1.534(10) . no O23 C24 1.534(10) . no O24 C26 1.537(10) . no O24 C27 1.541(10) . no O25 C29 1.534(10) . no O25 C28 1.535(10) . no O26 C31 1.538(10) . no O26 C30 1.542(10) . no C21 C22 1.379(10) . no C23 C24 1.378(10) . no C25 C26 1.379(10) . no C27 C28 1.382(10) . no C29 C30 1.379(10) . no C31 C32 1.384(10) . no 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 O15 Sm1 O16 68.3(8) . . no O15 Sm1 O1 81.0(7) . . no O16 Sm1 O1 76.0(7) . . no O15 Sm1 O14 65.7(7) . . no O16 Sm1 O14 133.6(6) . . no O1 Sm1 O14 91.8(7) . . no O15 Sm1 O2B 121.9(8) . . no O16 Sm1 O2B 121.3(9) . . no O1 Sm1 O2B 53.3(6) . . no O14 Sm1 O2B 80.5(8) . . no O15 Sm1 O11 126.8(7) . . no O16 Sm1 O11 59.0(7) . . no O1 Sm1 O11 92.6(7) . . no O14 Sm1 O11 167.4(6) . . no O2B Sm1 O11 92.7(9) . . no O15 Sm1 O2A 98.5(9) . . no O16 Sm1 O2A 122.2(8) . . no O1 Sm1 O2A 46.1(6) . . no O14 Sm1 O2A 61.4(8) . . no O2B Sm1 O2A 24.3(8) . . no O11 Sm1 O2A 114.5(9) . . no O15 Sm1 O13 121.8(8) . . no O16 Sm1 O13 160.4(7) . . no O1 Sm1 O13 120.6(5) . . no O14 Sm1 O13 60.8(6) . . no O2B Sm1 O13 69.8(7) . . no O11 Sm1 O13 106.9(7) . . no O2A Sm1 O13 75.1(6) . . no O15 Sm1 O12 170.1(9) . . no O16 Sm1 O12 113.6(8) . . no O1 Sm1 O12 109.0(8) . . no O14 Sm1 O12 112.7(7) . . no O2B Sm1 O12 66.2(9) . . no O11 Sm1 O12 54.7(8) . . no O2A Sm1 O12 88.7(10) . . no O13 Sm1 O12 53.4(7) . . no O15 Sm1 Cl1B 79.6(6) . 2_655 no O16 Sm1 Cl1B 85.8(7) . 2_655 no O1 Sm1 Cl1B 157.2(4) . 2_655 no O14 Sm1 Cl1B 91.0(5) . 2_655 no O2B Sm1 Cl1B 149.3(4) . 2_655 no O11 Sm1 Cl1B 89.6(6) . 2_655 no O2A Sm1 Cl1B 149.5(7) . 2_655 no O13 Sm1 Cl1B 80.2(5) . 2_655 no O12 Sm1 Cl1B 90.8(8) . 2_655 no O15 Sm1 Cl1B 98.5(6) . . no O16 Sm1 Cl1B 101.6(7) . . no O1 Sm1 Cl1B 27.0(3) . . no O14 Sm1 Cl1B 80.5(6) . . no O2B Sm1 Cl1B 27.3(3) . . no O11 Sm1 Cl1B 98.4(6) . . no O2A Sm1 Cl1B 21.9(6) . . no O13 Sm1 Cl1B 93.8(5) . . no O12 Sm1 Cl1B 90.7(8) . . no Cl1B Sm1 Cl1B 171.2(6) 2_655 . no O25 Sm2 O24 62.0(7) . . no O25 Sm2 O7 71.3(8) . . no O24 Sm2 O7 70.9(8) . . no O25 Sm2 O26 64.9(7) . . no O24 Sm2 O26 126.3(6) . . no O7 Sm2 O26 85.9(8) . . no O25 Sm2 O5 113.2(7) . . no O24 Sm2 O5 111.4(6) . . no O7 Sm2 O5 48.5(5) . . no O26 Sm2 O5 82.7(7) . . no O25 Sm2 O23 121.9(7) . . no O24 Sm2 O23 60.0(7) . . no O7 Sm2 O23 92.3(8) . . no O26 Sm2 O23 171.9(7) . . no O5 Sm2 O23 90.2(7) . . no O25 Sm2 O22 177.3(7) . . no O24 Sm2 O22 115.8(6) . . no O7 Sm2 O22 109.7(6) . . no O26 Sm2 O22 117.5(6) . . no O5 Sm2 O22 68.8(5) . . no O23 Sm2 O22 55.8(6) . . no O25 Sm2 O22 23.0(6) . 2 no O24 Sm2 O22 84.9(7) . 2 no O7 Sm2 O22 75.2(7) . 2 no O26 Sm2 O22 41.9(6) . 2 no O5 Sm2 O22 104.2(5) . 2 no O23 Sm2 O22 144.8(7) . 2 no O22 Sm2 O22 159.3(9) . 2 no O25 Sm2 O21 121.3(7) . . no O24 Sm2 O21 170.3(7) . . no O7 Sm2 O21 118.6(7) . . no O26 Sm2 O21 59.1(7) . . no O5 Sm2 O21 76.3(6) . . no O23 Sm2 O21 115.6(6) . . no O22 Sm2 O21 60.6(6) . . no O22 Sm2 O21 99.1(6) 2 . no O25 Sm2 O21 83.4(7) . 2 no O24 Sm2 O21 143.0(6) . 2 no O7 Sm2 O21 86.5(8) . 2 no O26 Sm2 O21 19.3(5) . 2 no O5 Sm2 O21 68.7(7) . 2 no O23 Sm2 O21 152.8(7) . 2 no O22 Sm2 O21 99.1(6) . 2 no O22 Sm2 O21 60.6(6) 2 2 no O21 Sm2 O21 44.4(8) . 2 no Cl1B Cl1A O4B 95(4) . . no Cl1B Cl1A O3 80.3(17) . . no O4B Cl1A O3 113(3) . . no Cl1B Cl1A O4A 161(3) . . no O4B Cl1A O4A 67(3) . . no O3 Cl1A O4A 113(2) . . no Cl1B Cl1A O1 80.3(17) . . no O4B Cl1A O1 131(3) . . no O3 Cl1A O1 113.8(15) . . no O4A Cl1A O1 105(2) . . no Cl1B Cl1A O2A 48(3) . . no O4B Cl1A O2A 51(2) . . no O3 Cl1A O2A 115(2) . . no O4A Cl1A O2A 112(2) . . no O1 Cl1A O2A 97(2) . . no Cl1B Cl1A O2B 11(2) . . no O4B Cl1A O2B 84(3) . . no O3 Cl1A O2B 86.9(13) . . no O4A Cl1A O2B 150(2) . . no O1 Cl1A O2B 85.5(14) . . no O2A Cl1A O2B 37.5(17) . . no Cl1A Cl1B O2A 113(4) . . no Cl1A Cl1B O3 79.5(17) . . no O2A Cl1B O3 136(2) . . no Cl1A Cl1B O1 79.6(17) . . no O2A Cl1B O1 110(2) . . no O3 Cl1B O1 113.4(15) . . no Cl1A Cl1B O4B 65(4) . . no O2A Cl1B O4B 53(2) . . no O3 Cl1B O4B 105(3) . . no O1 Cl1B O4B 120(3) . . no Cl1A Cl1B O2B 165(3) . . no O2A Cl1B O2B 52.5(19) . . no O3 Cl1B O2B 109.0(17) . . no O1 Cl1B O2B 107.0(18) . . no O4B Cl1B O2B 101(3) . . no Cl1A Cl1B O4A 14(3) . . no O2A Cl1B O4A 99(2) . . no O3 Cl1B O4A 89.6(15) . . no O1 Cl1B O4A 84.5(16) . . no O4B Cl1B O4A 52(3) . . no O2B Cl1B O4A 151(2) . . no Cl1A Cl1B Sm1 124.7(16) . . no O2A Cl1B Sm1 66.6(18) . . no O3 Cl1B Sm1 142.0(14) . . no O1 Cl1B Sm1 54.0(11) . . no O4B Cl1B Sm1 111(2) . . no O2B Cl1B Sm1 55.7(12) . . no O4A Cl1B Sm1 120.5(12) . . no O8 Cl2 O6 107.3(11) . . no O8 Cl2 O7 111.8(16) . . no O6 Cl2 O7 108.6(16) . . no O8 Cl2 O5 113.4(13) . . no O6 Cl2 O5 112.7(14) . . no O7 Cl2 O5 102.9(9) . . no Cl1A O1 Cl1B 20.2(11) . . no Cl1A O1 Sm1 115.8(14) . . no Cl1B O1 Sm1 99.0(13) . . no Cl1B O2A O2B 76(2) . . no Cl1B O2A O4B 75(2) . . no O2B O2A O4B 139(4) . . no Cl1B O2A Cl1A 18.8(13) . . no O2B O2A Cl1A 95(2) . . no O4B O2A Cl1A 59(2) . . no Cl1B O2A Sm1 91(2) . . no O2B O2A Sm1 65(2) . . no O4B O2A Sm1 143(3) . . no Cl1A O2A Sm1 100.5(18) . . no O2A O2B Cl1B 51.7(13) . . no O2A O2B Cl1A 47.9(11) . . no Cl1B O2B Cl1A 3.8(9) . . no O2A O2B Sm1 91(2) . . no Cl1B O2B Sm1 97.0(13) . . no Cl1A O2B Sm1 97.5(10) . . no Cl1A O3 Cl1B 20.3(11) . . no Cl1A O4A O4B 52.3(13) . . no Cl1A O4A Cl1B 5.0(9) . . no O4B O4A Cl1B 47.8(9) . . no O2A O4B Cl1A 70.4(16) . . no O2A O4B Cl1B 51.7(16) . . no Cl1A O4B Cl1B 20.4(12) . . no O2A O4B O4A 123(3) . . no Cl1A O4B O4A 60(2) . . no Cl1B O4B O4A 81(3) . . no Cl2 O5 Sm2 103.6(7) . . no Cl2 O7 Sm2 104.2(8) . . no C1 O11 C12 115(2) . . no C1 O11 Sm1 118(2) . . no C12 O11 Sm1 107.3(19) . . no C2 O12 C3 111(3) . . no C2 O12 Sm1 115(3) . . no C3 O12 Sm1 112(3) . . no C5 O13 C4 110(2) . . no C5 O13 Sm1 107.9(15) . . no C4 O13 Sm1 120(2) . . no C6 O14 C7 116.3(19) . . no C6 O14 Sm1 120.7(15) . . no C7 O14 Sm1 112.9(17) . . no C8 O15 C9 113(2) . . no C8 O15 Sm1 113(2) . . no C9 O15 Sm1 106(3) . . no C10 O16 C11 119(2) . . no C10 O16 Sm1 107(2) . . no C11 O16 Sm1 123.8(19) . . no C2 C1 O11 102(3) . . no C1 C2 O12 105(3) . . no C4 C3 O12 98(3) . . no C3 C4 O13 102(3) . . no C6 C5 O13 104(2) . . no C5 C6 O14 109(2) . . no C8 C7 O14 109(3) . . no C7 C8 O15 105(3) . . no C10 C9 O15 102(3) . . no C9 C10 O16 102(4) . . no C12 C11 O16 101(3) . . no C11 C12 O11 103(3) . . no C21 O21 C32 113(2) . . no C21 O21 Sm2 113(2) . . no C32 O21 Sm2 110.7(15) . . no C22 O22 C23 110(3) . . no C22 O22 Sm2 119(2) . . no C23 O22 Sm2 122(3) . . no C25 O23 C24 102(3) . . no C25 O23 Sm2 113.6(18) . . no C24 O23 Sm2 122(3) . . no C26 O24 C27 117(2) . . no C26 O24 Sm2 124(2) . . no C27 O24 Sm2 113.8(18) . . no C29 O25 C28 105.9(18) . . no C29 O25 Sm2 119.2(17) . . no C28 O25 Sm2 123.8(18) . . no C31 O26 C30 124.6(18) . . no C31 O26 Sm2 114(2) . . no C30 O26 Sm2 107.7(16) . . no C22 C21 O21 119(4) . . no C21 C22 O22 102(3) . . no C24 C23 O22 109(4) . . no C23 C24 O23 102(4) . . no C26 C25 O23 110(3) . . no C25 C26 O24 105(3) . . no C28 C27 O24 109(2) . . no C27 C28 O25 105(2) . . no C30 C29 O25 100(2) . . no C29 C30 O26 118(2) . . no C32 C31 O26 104(2) . . no C31 C32 O21 94(2) . . no _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.093 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.138 data_smc5nt _database_code_depnum_ccdc_archive 'CCDC 226736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Cl2 O18 Sm' _chemical_formula_weight 789.77 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, y+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 17.903(9) _cell_length_b 17.903(9) _cell_length_c 17.903(9) _cell_angle_alpha 108.35(6) _cell_angle_beta 108.35(6) _cell_angle_gamma 108.35(6) _cell_volume 4591(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5313 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 28 _exptl_crystal_description 'flat needle' _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type 'analytical, from the crystal shape' _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.849 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19321 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1672 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 28.46 _reflns_number_total 3978 _reflns_number_gt 2899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software (1999)' _computing_cell_refinement 'Kuma KM4 software (1999)' _computing_data_reduction 'Kuma KM4 software (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 -0.04(2) _refine_ls_number_reflns 3978 _refine_ls_number_parameters 356 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.021 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.03975(8) 0.89473(8) 0.29155(8) 0.02616(14) Uani 1 d . . . Cl1 Cl -0.0196(2) 1.1773(2) 0.6713(2) 0.0419(9) Uani 1 d . . . Cl2 Cl 0.3771(3) 1.0817(3) 0.2859(3) 0.0593(12) Uani 1 d . . . O1 O 0.0355(6) 0.8755(7) 0.4368(6) 0.055(3) Uani 1 d . . . O2 O -0.0448(6) 0.7284(6) 0.2755(7) 0.052(3) Uani 1 d . . . O3 O -0.1288(6) 0.7834(8) 0.1667(6) 0.056(3) Uani 1 d D . . O4A O -0.0487(12) 0.9885(13) 0.2451(12) 0.047(5) Uiso 0.50 d PD A 1 O4B O -0.0691(11) 0.9491(11) 0.2056(11) 0.035(5) Uiso 0.50 d PD A 2 O5 O -0.0295(6) 0.9775(6) 0.3863(7) 0.061(3) Uani 1 d D . . O11A O 0.0315(10) 0.8980(10) 0.1367(10) 0.028(5) Uiso 0.50 d PD A 1 O11B O 0.0327(12) 0.8577(13) 0.1257(13) 0.053(6) Uiso 0.50 d PD A 2 O12 O 0.1485(6) 1.0341(6) 0.2857(6) 0.062(3) Uani 1 d D . . O13 O 0.1842(7) 1.0336(7) 0.4450(8) 0.067(4) Uani 1 d . . . O14 O 0.1854(6) 0.8767(6) 0.3677(6) 0.050(3) Uani 1 d D . . O15A O 0.0609(11) 0.7716(12) 0.1810(11) 0.032(5) Uiso 0.50 d PD A 1 O15B O 0.0743(15) 0.7576(15) 0.2064(15) 0.053(6) Uiso 0.50 d PD A 2 O21A O -0.0860(11) 1.2107(11) 0.6793(10) 0.032(4) Uiso 0.50 d P . . O21B O -0.0251(13) 1.2580(13) 0.7074(13) 0.057(6) Uiso 0.50 d P . . O22 O -0.0571(6) 1.1021(6) 0.6841(6) 0.066(3) Uani 1 d . . . O23A O -0.0186(12) 1.1584(10) 0.5941(11) 0.025(4) Uiso 0.50 d P . . O23B O -0.0676(15) 1.1469(13) 0.5706(13) 0.058(6) Uiso 0.50 d P . . O24A O 0.0672(9) 1.2321(9) 0.7468(10) 0.029(4) Uiso 0.50 d P . . O24B O 0.066(2) 1.190(2) 0.678(2) 0.146(11) Uiso 0.50 d P . . O31 O 0.3223(8) 1.1094(11) 0.2421(11) 0.154(7) Uani 1 d . . . O32 O 0.4017(7) 1.1079(7) 0.3759(7) 0.077(3) Uani 1 d . . . O33 O 0.4552(6) 1.1030(7) 0.2747(6) 0.066(3) Uani 1 d . . . O34 O 0.3233(7) 0.9803(9) 0.2407(9) 0.115(5) Uani 1 d . . . C1 C 0.0239(9) 0.7886(11) 0.4308(10) 0.059(5) Uani 1 d . . . H1A H 0.0173 0.7836 0.4811 0.071 Uiso 1 calc R . . H1B H 0.0747 0.7803 0.4302 0.071 Uiso 1 calc R . . C2 C -0.0603(9) 0.7191(9) 0.3440(9) 0.053(4) Uani 1 d . . . H2A H -0.0728 0.6600 0.3374 0.064 Uiso 1 calc R . . H2B H -0.1107 0.7288 0.3439 0.064 Uiso 1 calc R . . C3 C -0.1173(12) 0.6674(11) 0.1898(11) 0.094(8) Uani 1 d . . . H3A H -0.1483 0.6120 0.1896 0.113 Uiso 1 calc R . . H3B H -0.0953 0.6553 0.1466 0.113 Uiso 1 calc R . . C4 C -0.1791(10) 0.7038(11) 0.1651(11) 0.062(5) Uani 1 d U . . H4A H -0.2281 0.6627 0.1065 0.074 Uiso 1 calc R . . H4B H -0.2026 0.7154 0.2071 0.074 Uiso 1 calc R . . C5A C -0.1699(19) 0.8369(18) 0.147(2) 0.075(13) Uiso 0.50 d PD A 1 H5A H -0.2021 0.8417 0.1816 0.090 Uiso 0.50 calc PR A 1 H5B H -0.2141 0.8021 0.0855 0.090 Uiso 0.50 calc PR A 1 C5B C -0.1953(12) 0.7984(17) 0.1162(17) 0.024(6) Uiso 0.50 d PD A 2 H5C H -0.2329 0.8071 0.1434 0.029 Uiso 0.50 calc PR A 2 H5D H -0.2314 0.7509 0.0560 0.029 Uiso 0.50 calc PR A 2 C6A C -0.1213(16) 0.9283(16) 0.1594(15) 0.060(9) Uiso 0.50 d PD A 1 H6A H -0.0996 0.9243 0.1158 0.072 Uiso 0.50 calc PR A 1 H6B H -0.1629 0.9523 0.1478 0.072 Uiso 0.50 calc PR A 1 C6B C -0.1373(14) 0.8815(14) 0.1202(13) 0.041(7) Uiso 0.50 d PD A 2 H6C H -0.1100 0.8666 0.0826 0.049 Uiso 0.50 calc PR A 2 H6D H -0.1745 0.9056 0.0953 0.049 Uiso 0.50 calc PR A 2 C7A C -0.0719(12) 1.0421(12) 0.3019(11) 0.013(5) Uiso 0.50 d PD A 1 H7A H -0.1342 1.0106 0.2855 0.016 Uiso 0.50 calc PR A 1 H7B H -0.0615 1.0962 0.2965 0.016 Uiso 0.50 calc PR A 1 C7B C -0.1007(15) 0.9958(16) 0.2576(12) 0.036(7) Uiso 0.50 d PD A 2 H7C H -0.1592 0.9547 0.2443 0.043 Uiso 0.50 calc PR A 2 H7D H -0.1067 1.0407 0.2406 0.043 Uiso 0.50 calc PR A 2 C8A C -0.016(2) 1.0634(10) 0.3949(14) 0.051(9) Uiso 0.50 d PD A 1 H8A H 0.0456 1.1022 0.4155 0.062 Uiso 0.50 calc PR A 1 H8B H -0.0366 1.0906 0.4348 0.062 Uiso 0.50 calc PR A 1 C8B C -0.043(2) 1.0391(13) 0.3549(15) 0.047(8) Uiso 0.50 d PD A 2 H8C H 0.0141 1.0839 0.3693 0.057 Uiso 0.50 calc PR A 2 H8D H -0.0695 1.0685 0.3853 0.057 Uiso 0.50 calc PR A 2 C9 C 0.0037(10) 0.9944(11) 0.4775(10) 0.066(5) Uani 1 d U . . H9A H -0.0287 1.0179 0.5040 0.079 Uiso 1 calc R . . H9B H 0.0659 1.0375 0.5107 0.079 Uiso 1 calc R . . C10 C -0.0078(10) 0.9080(10) 0.4801(9) 0.057(4) Uani 1 d . . . H10A H 0.0176 0.9179 0.5410 0.069 Uiso 1 calc R . . H10B H -0.0702 0.8662 0.4507 0.069 Uiso 1 calc R . . C11B C 0.098(2) 0.9341(12) 0.1336(15) 0.092(15) Uiso 0.50 d PD A 2 H11C H 0.0761 0.9328 0.0761 0.110 Uiso 0.50 calc PR A 2 H11D H 0.1501 0.9256 0.1431 0.110 Uiso 0.50 calc PR A 2 C11A C 0.0942(13) 0.9692(10) 0.1348(10) 0.027(6) Uiso 0.50 d PD A 1 H11A H 0.0674 0.9728 0.0806 0.032 Uiso 0.50 calc PR A 1 H11B H 0.1448 0.9593 0.1366 0.032 Uiso 0.50 calc PR A 1 C12A C 0.123(2) 1.0533(13) 0.2132(9) 0.036(8) Uiso 0.50 d PD A 1 H12A H 0.1728 1.1018 0.2197 0.043 Uiso 0.50 calc PR A 1 H12B H 0.0751 1.0687 0.2080 0.043 Uiso 0.50 calc PR A 1 C12B C 0.128(3) 1.0269(17) 0.2009(11) 0.11(2) Uiso 0.50 d PD A 2 H12C H 0.1804 1.0670 0.2022 0.137 Uiso 0.50 calc PR A 2 H12D H 0.0822 1.0445 0.1833 0.137 Uiso 0.50 calc PR A 2 C13 C 0.1969(10) 1.1163(10) 0.3660(9) 0.065(5) Uani 1 d DU . . H13A H 0.2387 1.1608 0.3597 0.078 Uiso 1 calc R . . H13B H 0.1565 1.1374 0.3788 0.078 Uiso 1 calc R . . C14 C 0.2426(15) 1.1009(12) 0.4356(13) 0.114(8) Uani 1 d . . . H14A H 0.2746 1.1554 0.4907 0.137 Uiso 1 calc R . . H14B H 0.2855 1.0837 0.4238 0.137 Uiso 1 calc R . . C15 C 0.2339(13) 0.9969(15) 0.4950(12) 0.105(8) Uani 1 d . . . H15A H 0.2855 1.0455 0.5487 0.126 Uiso 1 calc R . . H15B H 0.1962 0.9611 0.5121 0.126 Uiso 1 calc R . . C16 C 0.2614(11) 0.9444(14) 0.4430(11) 0.083(7) Uani 1 d . . . H16A H 0.3009 0.9799 0.4271 0.099 Uiso 1 calc R . . H16B H 0.2923 0.9203 0.4758 0.099 Uiso 1 calc R . . C17A C 0.1997(19) 0.814(3) 0.309(3) 0.08(3) Uiso 0.50 d PD A 1 H17A H 0.2282 0.7877 0.3403 0.094 Uiso 0.50 calc PR A 1 H17B H 0.2394 0.8449 0.2902 0.094 Uiso 0.50 calc PR A 1 C17B C 0.210(2) 0.824(2) 0.312(3) 0.06(3) Uiso 0.50 d PD A 2 H17C H 0.2619 0.8210 0.3476 0.071 Uiso 0.50 calc PR A 2 H17D H 0.2251 0.8497 0.2751 0.071 Uiso 0.50 calc PR A 2 C18B C 0.134(3) 0.7336(18) 0.256(2) 0.13(2) Uiso 0.50 d PD A 2 H18C H 0.1469 0.6927 0.2182 0.159 Uiso 0.50 calc PR A 2 H18D H 0.1121 0.7091 0.2903 0.159 Uiso 0.50 calc PR A 2 C18A C 0.116(2) 0.7428(15) 0.2292(14) 0.053(9) Uiso 0.50 d PD A 1 H18A H 0.1310 0.7066 0.1893 0.064 Uiso 0.50 calc PR A 1 H18B H 0.0819 0.7053 0.2477 0.064 Uiso 0.50 calc PR A 1 C19A C 0.0652(15) 0.7738(15) 0.1037(13) 0.014(5) Uiso 0.50 d PD A 1 H19A H 0.0446 0.7144 0.0587 0.017 Uiso 0.50 calc PR A 1 H19B H 0.1256 0.8101 0.1175 0.017 Uiso 0.50 calc PR A 1 C19B C 0.080(2) 0.745(2) 0.1257(17) 0.075(11) Uiso 0.50 d PD A 2 H19C H 0.0624 0.6835 0.0905 0.090 Uiso 0.50 calc PR A 2 H19D H 0.1403 0.7802 0.1390 0.090 Uiso 0.50 calc PR A 2 C20B C 0.0206(16) 0.7730(12) 0.0748(15) 0.039(7) Uiso 0.50 d PD A 2 H20C H 0.0315 0.7726 0.0249 0.047 Uiso 0.50 calc PR A 2 H20D H -0.0405 0.7303 0.0514 0.047 Uiso 0.50 calc PR A 2 C20A C 0.0069(13) 0.8124(10) 0.0718(12) 0.025(5) Uiso 0.50 d PD A 1 H20A H 0.0090 0.8162 0.0196 0.029 Uiso 0.50 calc PR A 1 H20B H -0.0538 0.7730 0.0546 0.029 Uiso 0.50 calc PR A 1 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 Sm 0.0248(4) 0.0343(4) 0.0259(4) 0.0142(3) 0.0147(3) 0.0176(3) Cl1 0.044(2) 0.040(2) 0.050(2) 0.0214(18) 0.0190(19) 0.0302(19) Cl2 0.041(2) 0.099(4) 0.052(3) 0.049(3) 0.025(2) 0.032(2) O1 0.036(6) 0.095(9) 0.044(6) 0.037(6) 0.026(5) 0.029(6) O2 0.050(7) 0.042(6) 0.065(7) 0.016(6) 0.037(6) 0.021(5) O3 0.040(6) 0.102(9) 0.032(6) 0.035(6) 0.020(5) 0.032(6) O5 0.070(7) 0.026(6) 0.101(9) 0.022(6) 0.058(7) 0.029(5) O12 0.052(6) 0.071(8) 0.078(8) 0.049(6) 0.034(6) 0.026(6) O13 0.047(7) 0.044(7) 0.079(8) -0.006(6) 0.051(7) -0.004(5) O14 0.032(6) 0.073(7) 0.054(7) 0.041(6) 0.019(5) 0.022(5) O22 0.044(6) 0.063(7) 0.096(8) 0.054(6) 0.032(5) 0.013(5) O31 0.097(10) 0.29(2) 0.30(2) 0.271(18) 0.141(13) 0.146(13) O32 0.079(8) 0.105(9) 0.051(7) 0.037(6) 0.033(6) 0.044(7) O33 0.032(6) 0.112(9) 0.068(7) 0.042(6) 0.036(5) 0.036(6) O34 0.061(9) 0.108(12) 0.126(12) 0.037(9) 0.031(8) 0.010(8) C1 0.052(11) 0.108(14) 0.083(12) 0.092(12) 0.039(9) 0.054(10) C2 0.041(9) 0.063(10) 0.054(10) 0.042(9) 0.018(8) 0.011(8) C3 0.079(14) 0.056(12) 0.061(12) -0.038(10) 0.049(11) -0.018(11) C4 0.033(7) 0.069(9) 0.054(8) 0.009(6) 0.031(7) -0.001(6) C9 0.070(8) 0.066(9) 0.048(8) -0.008(6) 0.046(7) 0.032(6) C10 0.054(10) 0.068(11) 0.042(9) 0.012(8) 0.038(8) 0.014(9) C13 0.056(8) 0.036(8) 0.102(10) 0.024(7) 0.043(7) 0.020(6) C14 0.14(2) 0.045(13) 0.094(16) -0.024(11) 0.075(16) 0.004(13) C15 0.051(14) 0.114(19) 0.056(14) 0.000(13) 0.000(11) -0.005(13) C16 0.046(12) 0.16(2) 0.040(11) 0.037(13) 0.025(10) 0.044(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm O15A 2.678(16) . yes Sm O3 2.689(12) . yes Sm O12 2.694(10) . yes Sm O14 2.707(9) . yes Sm O4B 2.714(18) . yes Sm O5 2.740(9) . yes Sm O1 2.749(9) . yes Sm O11A 2.750(15) . yes Sm O2 2.754(9) . yes Sm O13 2.755(13) . yes Sm O4A 2.781(18) . yes Sm O11B 2.783(19) . yes Sm O15B 2.82(2) . yes Cl1 O23A 1.323(16) . no Cl1 O22 1.428(9) . no Cl1 O21B 1.434(19) . no Cl1 O24B 1.44(3) . no Cl1 O24A 1.445(15) . no Cl1 O21A 1.513(16) . no Cl1 O23B 1.55(2) . no Cl2 O31 1.375(11) . no Cl2 O32 1.399(10) . no Cl2 O33 1.424(9) . no Cl2 O34 1.537(14) . no O1 C10 1.386(15) . no O1 C1 1.466(16) . no O2 C2 1.387(14) . no O2 C3 1.425(17) . no O3 C5B 1.409(11) . no O3 C4 1.412(17) . no O3 C5A 1.440(11) . no O4A C6A 1.424(12) . no O4A C7A 1.424(11) . no O4B C6B 1.421(12) . no O4B C7B 1.423(11) . no O5 C8A 1.429(11) . no O5 C8B 1.436(11) . no O5 C9 1.441(16) . no O11A C20A 1.424(11) . no O11A C11A 1.427(10) . no O11B C20B 1.405(11) . no O11B C11B 1.418(11) . no O12 C12B 1.398(11) . no O12 C12A 1.422(11) . no O12 C13 1.436(14) . no O13 C14 1.42(2) . no O13 C15 1.50(2) . no O14 C16 1.384(18) . no O14 C17A 1.426(11) . no O14 C17B 1.429(11) . no O15A C19A 1.422(11) . no O15A C18A 1.431(11) . no O15B C18B 1.423(12) . no O15B C19B 1.431(11) . no O21A O21B 0.98(2) . no O23A O23B 0.77(2) . no O23A O24B 1.54(3) . no O24A O24B 1.22(3) . no C1 C2 1.537(18) . no C3 C4 1.47(2) . no C5A C6A 1.496(15) . no C5B C6B 1.487(15) . no C7A C8A 1.493(15) . no C7B C8B 1.487(15) . no C9 C10 1.51(2) . no C11B C12B 1.504(15) . no C11A C12A 1.491(15) . no C13 C14 1.42(2) . no C15 C16 1.42(2) . no C17A C18A 1.487(16) . no C17B C18B 1.492(16) . no C19A C20A 1.490(15) . no C19B C20B 1.484(15) . no 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 O15A Sm O3 78.7(5) . . no O15A Sm O12 96.3(4) . . no O3 Sm O12 124.1(3) . . no O15A Sm O14 65.1(4) . . no O3 Sm O14 135.4(3) . . no O12 Sm O14 86.5(3) . . no O15A Sm O4B 112.7(5) . . no O3 Sm O4B 57.1(4) . . no O12 Sm O4B 75.4(4) . . no O14 Sm O4B 161.5(4) . . no O15A Sm O5 162.7(4) . . no O3 Sm O5 86.3(3) . . no O12 Sm O5 99.3(3) . . no O14 Sm O5 123.2(3) . . no O4B Sm O5 64.7(4) . . no O15A Sm O1 115.7(4) . . no O3 Sm O1 101.4(3) . . no O12 Sm O1 129.0(3) . . no O14 Sm O1 74.1(3) . . no O4B Sm O1 120.5(4) . . no O5 Sm O1 58.6(3) . . no O15A Sm O11A 61.3(5) . . no O3 Sm O11A 73.9(4) . . no O12 Sm O11A 56.4(4) . . no O14 Sm O11A 107.3(4) . . no O4B Sm O11A 59.4(5) . . no O5 Sm O11A 122.8(4) . . no O1 Sm O11A 174.6(4) . . no O15A Sm O2 66.9(4) . . no O3 Sm O2 59.6(3) . . no O12 Sm O2 162.5(3) . . no O14 Sm O2 81.9(3) . . no O4B Sm O2 114.8(4) . . no O5 Sm O2 98.0(3) . . no O1 Sm O2 59.9(3) . . no O11A Sm O2 114.9(4) . . no O15A Sm O13 120.1(4) . . no O3 Sm O13 161.1(3) . . no O12 Sm O13 59.9(3) . . no O14 Sm O13 59.8(3) . . no O4B Sm O13 112.1(5) . . no O5 Sm O13 74.7(3) . . no O1 Sm O13 69.6(3) . . no O11A Sm O13 115.7(4) . . no O2 Sm O13 123.2(4) . . no O15A Sm O4A 125.9(5) . . no O3 Sm O4A 69.3(5) . . no O12 Sm O4A 69.9(4) . . no O14 Sm O4A 154.3(4) . . no O4B Sm O4A 14.6(4) . . no O5 Sm O4A 54.3(4) . . no O1 Sm O4A 112.6(4) . . no O11A Sm O4A 68.5(5) . . no O2 Sm O4A 123.3(5) . . no O13 Sm O4A 98.2(5) . . no O15A Sm O11B 47.0(6) . . no O3 Sm O11B 71.4(4) . . no O12 Sm O11B 66.1(5) . . no O14 Sm O11B 98.8(4) . . no O4B Sm O11B 70.6(5) . . no O5 Sm O11B 135.3(4) . . no O1 Sm O11B 161.6(5) . . no O11A Sm O11B 14.4(4) . . no O2 Sm O11B 102.7(5) . . no O13 Sm O11B 122.1(5) . . no O4A Sm O11B 81.3(5) . . no O23A Cl1 O22 114.7(8) . . no O23A Cl1 O21B 113.3(10) . . no O22 Cl1 O21B 124.4(10) . . no O23A Cl1 O24B 67.7(14) . . no O22 Cl1 O24B 108.6(13) . . no O21B Cl1 O24B 114.3(16) . . no O23A Cl1 O24A 113.9(10) . . no O22 Cl1 O24A 104.4(7) . . no O21B Cl1 O24A 79.7(10) . . no O24B Cl1 O24A 49.8(12) . . no O23A Cl1 O21A 113.3(9) . . no O22 Cl1 O21A 95.8(8) . . no O21B Cl1 O21A 38.8(8) . . no O24B Cl1 O21A 152.7(14) . . no O24A Cl1 O21A 113.1(9) . . no O23A Cl1 O23B 29.6(8) . . no O22 Cl1 O23B 106.4(8) . . no O21B Cl1 O23B 101.5(11) . . no O24B Cl1 O23B 97.4(16) . . no O24A Cl1 O23B 141.0(10) . . no O21A Cl1 O23B 86.9(10) . . no O31 Cl2 O32 118.4(9) . . no O31 Cl2 O33 111.5(7) . . no O32 Cl2 O33 108.5(6) . . no O31 Cl2 O34 104.8(10) . . no O32 Cl2 O34 104.7(7) . . no O33 Cl2 O34 108.2(7) . . no C10 O1 C1 111.5(10) . . no C10 O1 Sm 122.8(9) . . no C1 O1 Sm 114.1(8) . . no C2 O2 C3 113.7(11) . . no C2 O2 Sm 120.2(8) . . no C3 O2 Sm 113.0(10) . . no C5B O3 C4 101.9(13) . . no C5B O3 C5A 25.4(16) . . no C4 O3 C5A 119.6(16) . . no C5B O3 Sm 131.5(12) . . no C4 O3 Sm 122.2(9) . . no C5A O3 Sm 107.2(15) . . no C6A O4A C7A 112.5(19) . . no C6A O4A Sm 106.1(15) . . no C7A O4A Sm 124.3(12) . . no C6B O4B C7B 113.2(19) . . no C6B O4B Sm 113.5(14) . . no C7B O4B Sm 114.2(11) . . no C8A O5 C8B 25.1(10) . . no C8A O5 C9 101.5(12) . . no C8B O5 C9 125.4(14) . . no C8A O5 Sm 116.9(14) . . no C8B O5 Sm 106.2(13) . . no C9 O5 Sm 115.8(8) . . no C20A O11A C11A 114.3(12) . . no C20A O11A Sm 110.6(11) . . no C11A O11A Sm 122.9(10) . . no C20B O11B C11B 120.2(15) . . no C20B O11B Sm 117.2(14) . . no C11B O11B Sm 108.0(13) . . no C12B O12 C12A 20.6(17) . . no C12B O12 C13 124.7(13) . . no C12A O12 C13 108.0(11) . . no C12B O12 Sm 115.2(16) . . no C12A O12 Sm 122.7(12) . . no C13 O12 Sm 116.0(8) . . no C14 O13 C15 110.7(16) . . no C14 O13 Sm 116.7(11) . . no C15 O13 Sm 108.8(9) . . no C16 O14 C17A 114.8(16) . . no C16 O14 C17B 108.5(19) . . no C17A O14 C17B 8(3) . . no C16 O14 Sm 123.4(10) . . no C17A O14 Sm 116(2) . . no C17B O14 Sm 119(2) . . no C19A O15A C18A 118.3(19) . . no C19A O15A Sm 121.8(12) . . no C18A O15A Sm 110.4(13) . . no C18B O15B C19B 109(3) . . no C18B O15B Sm 121.4(16) . . no C19B O15B Sm 120.2(19) . . no O21B O21A Cl1 66.2(15) . . no O21A O21B Cl1 75.0(16) . . no O23B O23A Cl1 92(2) . . no O23B O23A O24B 152(3) . . no Cl1 O23A O24B 59.8(15) . . no O23A O23B Cl1 58.6(19) . . no O24B O24A Cl1 65.0(17) . . no O24A O24B Cl1 65.2(18) . . no O24A O24B O23A 114(3) . . no Cl1 O24B O23A 52.5(13) . . no O1 C1 C2 106.5(10) . . no O2 C2 C1 107.0(11) . . no O2 C3 C4 110.5(14) . . no O3 C4 C3 105.5(13) . . no O3 C5A C6A 125(2) . . no O3 C5B C6B 98.4(16) . . no O4A C6A C5A 115(2) . . no O4B C6B C5B 116(2) . . no O4A C7A C8A 108.2(15) . . no O4B C7B C8B 114.3(19) . . no O5 C8A C7A 101.7(13) . . no O5 C8B C7B 112.8(15) . . no O5 C9 C10 108.3(11) . . no O1 C10 C9 107.0(11) . . no O11B C11B C12B 124(2) . . no O11A C11A C12A 108.6(15) . . no O12 C12A C11A 103.8(13) . . no O12 C12B C11B 112.0(16) . . no C14 C13 O12 107.9(13) . . no C13 C14 O13 112.1(19) . . no C16 C15 O13 111.4(16) . . no O14 C16 C15 106.8(14) . . no O14 C17A C18A 112.6(17) . . no O14 C17B C18B 107.5(16) . . no O15B C18B C17B 97(3) . . no O15A C18A C17A 116(3) . . no O15A C19A C20A 106.5(16) . . no O15B C19B C20B 110(2) . . no O11B C20B C19B 113(2) . . no O11A C20A C19A 113.0(16) . . no _diffrn_measured_fraction_theta_max 0.747 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.747 _refine_diff_density_max 0.836 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.117 data_test _database_code_depnum_ccdc_archive 'CCDC 226737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Cl2 O18 Sm' _chemical_formula_weight 789.77 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, y+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 18.053(11) _cell_length_b 18.053(11) _cell_length_c 18.053(11) _cell_angle_alpha 108.30(6) _cell_angle_beta 108.30(6) _cell_angle_gamma 108.30(6) _cell_volume 4715(5) _cell_formula_units_Z 6 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 2931 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 28 _exptl_crystal_description 'flat needle' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 2.112 _exptl_absorpt_correction_type 'analytical, from the crystal shape' _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.849 _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(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 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16128 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.2135 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 28.34 _reflns_number_total 3499 _reflns_number_gt 2079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software (1999)' _computing_cell_refinement 'Kuma KM4 software (1999)' _computing_data_reduction 'Kuma KM4 software (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 -0.02(2) _refine_ls_number_reflns 3499 _refine_ls_number_parameters 367 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1464 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.03844(8) 0.89348(7) 0.29023(7) 0.04029(19) Uani 1 d . . . Cl1 Cl -0.0221(3) 1.1748(3) 0.6684(3) 0.0663(13) Uani 1 d . . . Cl2 Cl 0.3802(4) 1.0835(4) 0.2839(4) 0.0876(17) Uani 1 d . . . O1 O 0.0306(7) 0.8717(9) 0.4310(7) 0.068(4) Uani 1 d . . . O2 O -0.0468(8) 0.7287(7) 0.2729(9) 0.064(3) Uani 1 d . . . O3 O -0.1308(7) 0.7848(9) 0.1656(6) 0.075(4) Uani 1 d . . . O4 O -0.0612(9) 0.9669(10) 0.2263(11) 0.092(4) Uani 1 d . . . O5 O -0.0265(8) 0.9775(8) 0.3846(9) 0.076(4) Uani 1 d . . . O11 O 0.0328(10) 0.8851(12) 0.1334(9) 0.089(5) Uani 1 d . . . O12 O 0.1461(8) 1.0325(8) 0.2873(10) 0.087(4) Uani 1 d . . . O13 O 0.1811(8) 1.0273(9) 0.4384(9) 0.079(4) Uani 1 d . . . O14 O 0.1832(7) 0.8715(9) 0.3613(9) 0.072(3) Uani 1 d . . . O15 O 0.0639(8) 0.7662(8) 0.1876(8) 0.084(4) Uani 1 d . . . O21A O -0.0864(17) 1.2048(16) 0.6780(14) 0.080(7) Uiso 0.50 d P . . O21B O -0.0268(15) 1.2562(14) 0.7058(14) 0.062(6) Uiso 0.50 d P . . O22 O -0.0566(9) 1.1034(8) 0.6847(8) 0.107(4) Uani 1 d . . . O23A O -0.0186(19) 1.1609(15) 0.5933(18) 0.076(8) Uiso 0.50 d P . . O23B O -0.0691(18) 1.1426(15) 0.5730(16) 0.078(9) Uiso 0.50 d P . . O24A O 0.0655(13) 1.2278(12) 0.7395(13) 0.057(6) Uiso 0.50 d P . . O24B O 0.0635(18) 1.1841(17) 0.675(2) 0.120(9) Uiso 0.50 d P . . O31 O 0.3266(12) 1.1082(14) 0.2419(14) 0.207(10) Uani 1 d . . . O32 O 0.4019(9) 1.1091(10) 0.3708(10) 0.143(6) Uani 1 d . . . O33 O 0.4546(9) 1.0998(10) 0.2726(9) 0.134(6) Uani 1 d . . . O34 O 0.3262(11) 0.9879(17) 0.2491(12) 0.200(8) Uani 1 d . . . C1 C 0.0151(13) 0.7840(14) 0.4234(12) 0.085(7) Uani 1 d . . . H1A H 0.0050 0.7785 0.4715 0.102 Uiso 1 calc R . . H1B H 0.0660 0.7753 0.4259 0.102 Uiso 1 calc R . . C2 C -0.0623(10) 0.7179(10) 0.3390(13) 0.073(6) Uani 1 d . . . H2A H -0.0730 0.6593 0.3319 0.088 Uiso 1 calc R . . H2B H -0.1138 0.7250 0.3375 0.088 Uiso 1 calc R . . C3 C -0.1186(16) 0.6711(12) 0.1879(15) 0.101(9) Uani 1 d . . . H3A H -0.1494 0.6151 0.1858 0.121 Uiso 1 calc R . . H3B H -0.0965 0.6608 0.1451 0.121 Uiso 1 calc R . . C4 C -0.1792(12) 0.7062(14) 0.1649(12) 0.077(7) Uani 1 d . . . H4A H -0.2282 0.6654 0.1072 0.092 Uiso 1 calc R . . H4B H -0.2016 0.7176 0.2073 0.092 Uiso 1 calc R . . C5 C -0.1872(12) 0.8181(18) 0.1305(15) 0.118(10) Uani 1 d . . . H5A H -0.2216 0.8247 0.1616 0.142 Uiso 1 calc R . . H5B H -0.2269 0.7783 0.0689 0.142 Uiso 1 calc R . . C6 C -0.1292(14) 0.9065(19) 0.1416(14) 0.124(10) Uani 1 d . . . H6A H -0.1034 0.8966 0.1020 0.149 Uiso 1 calc R . . H6B H -0.1662 0.9329 0.1234 0.149 Uiso 1 calc R . . C8 C -0.0297(14) 1.0460(15) 0.3722(18) 0.111(9) Uani 1 d . . . H8A H 0.0288 1.0876 0.3879 0.133 Uiso 1 calc R . . H8B H -0.0502 1.0752 0.4102 0.133 Uiso 1 calc R . . C7 C -0.0862(18) 1.0191(19) 0.284(2) 0.111(9) Uani 1 d . . . H7A H -0.0824 1.0701 0.2751 0.133 Uiso 1 calc R . . H7B H -0.1463 0.9845 0.2706 0.133 Uiso 1 calc R . . C9 C 0.0037(11) 0.9963(14) 0.4738(15) 0.087(7) Uani 1 d . . . H9A H -0.0305 1.0183 0.4978 0.104 Uiso 1 calc R . . H9B H 0.0649 1.0396 0.5081 0.104 Uiso 1 calc R . . C10 C -0.0083(13) 0.9095(16) 0.4744(12) 0.102(8) Uani 1 d . . . H10A H 0.0171 0.9191 0.5346 0.123 Uiso 1 calc R . . H10B H -0.0704 0.8698 0.4467 0.123 Uiso 1 calc R . . C11 C 0.0979(14) 0.962(2) 0.1404(16) 0.137(12) Uani 1 d . . . H11A H 0.0744 0.9668 0.0869 0.165 Uiso 1 calc R . . H11B H 0.1491 0.9532 0.1445 0.165 Uiso 1 calc R . . C12 C 0.1260(14) 1.0457(15) 0.2161(18) 0.115(10) Uani 1 d . . . H12A H 0.1768 1.0921 0.2228 0.138 Uiso 1 calc R . . H12B H 0.0791 1.0624 0.2075 0.138 Uiso 1 calc R . . C13 C 0.1999(12) 1.1113(11) 0.3686(16) 0.090(8) Uani 1 d . . . H13A H 0.2432 1.1537 0.3625 0.108 Uiso 1 calc R . . H13B H 0.1640 1.1368 0.3850 0.108 Uiso 1 calc R . . C14 C 0.2425(16) 1.0905(17) 0.4345(16) 0.119(9) Uani 1 d . . . H14A H 0.2823 1.0699 0.4206 0.143 Uiso 1 calc R . . H14B H 0.2764 1.1425 0.4910 0.143 Uiso 1 calc R . . C15 C 0.2292(16) 0.9915(17) 0.4888(13) 0.113(9) Uani 1 d . . . H15A H 0.2798 1.0400 0.5419 0.135 Uiso 1 calc R . . H15B H 0.1911 0.9573 0.5061 0.135 Uiso 1 calc R . . C16 C 0.2583(12) 0.9375(15) 0.4408(14) 0.085(7) Uani 1 d . . . H16A H 0.3020 0.9722 0.4289 0.102 Uiso 1 calc R . . H16B H 0.2840 0.9114 0.4741 0.102 Uiso 1 calc R . . C17 C 0.2051(13) 0.8174(14) 0.3039(18) 0.111(9) Uani 1 d . . . H17A H 0.2441 0.7992 0.3356 0.133 Uiso 1 calc R . . H17B H 0.2338 0.8488 0.2781 0.133 Uiso 1 calc R . . C18 C 0.1218(19) 0.7413(16) 0.2360(19) 0.125(11) Uani 1 d . . . H18A H 0.1330 0.7010 0.1963 0.150 Uiso 1 calc R . . H18B H 0.0941 0.7110 0.2632 0.150 Uiso 1 calc R . . C19 C 0.0635(18) 0.7674(16) 0.1037(16) 0.118(10) Uani 1 d . . . H19A H 0.1231 0.7991 0.1142 0.142 Uiso 1 calc R . . H19B H 0.0390 0.7077 0.0586 0.142 Uiso 1 calc R . . C20 C 0.0144(16) 0.807(2) 0.0752(17) 0.122(10) Uani 1 d . . . H20A H 0.0213 0.8127 0.0258 0.146 Uiso 1 calc R . . H20B H -0.0469 0.7677 0.0535 0.146 Uiso 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 Sm 0.0346(5) 0.0452(6) 0.0414(5) 0.0180(4) 0.0184(4) 0.0194(3) Cl1 0.070(4) 0.071(3) 0.066(4) 0.034(3) 0.029(3) 0.040(3) Cl2 0.068(4) 0.125(5) 0.079(5) 0.055(4) 0.035(3) 0.045(4) O1 0.049(8) 0.090(10) 0.056(8) 0.027(7) 0.027(7) 0.026(8) O2 0.075(9) 0.064(9) 0.077(9) 0.040(8) 0.053(8) 0.033(8) O3 0.040(8) 0.109(11) 0.034(7) 0.021(7) 0.011(6) 0.005(8) O4 0.073(11) 0.128(13) 0.147(14) 0.101(12) 0.072(11) 0.069(10) O5 0.090(9) 0.056(9) 0.081(10) 0.024(8) 0.039(8) 0.042(7) O11 0.073(11) 0.106(13) 0.066(10) 0.039(9) 0.029(9) 0.017(9) O12 0.069(9) 0.082(11) 0.111(12) 0.071(10) 0.028(8) 0.021(8) O13 0.057(9) 0.078(10) 0.097(11) 0.030(8) 0.054(8) 0.015(8) O14 0.044(8) 0.095(10) 0.097(10) 0.054(9) 0.036(8) 0.041(8) O15 0.079(9) 0.071(9) 0.095(10) 0.010(7) 0.063(8) 0.031(7) O22 0.106(11) 0.101(10) 0.134(12) 0.091(9) 0.056(8) 0.032(8) O31 0.166(16) 0.37(3) 0.37(3) 0.33(3) 0.193(18) 0.217(19) O32 0.127(13) 0.184(16) 0.075(11) 0.041(10) 0.030(10) 0.057(11) O33 0.083(10) 0.202(15) 0.154(13) 0.097(11) 0.082(10) 0.065(11) O34 0.127(16) 0.26(2) 0.177(19) 0.094(18) 0.032(14) 0.089(17) C1 0.095(18) 0.118(19) 0.109(18) 0.087(16) 0.071(15) 0.066(15) C2 0.032(11) 0.054(12) 0.097(17) 0.042(12) 0.004(11) -0.002(9) C3 0.103(19) 0.032(12) 0.097(19) -0.035(12) 0.069(16) -0.009(13) C4 0.030(12) 0.075(16) 0.052(13) -0.001(12) 0.016(10) -0.026(11) C5 0.023(13) 0.25(3) 0.121(19) 0.13(2) 0.030(13) 0.064(18) C6 0.046(15) 0.26(3) 0.090(18) 0.11(2) 0.032(14) 0.075(19) C8 0.11(2) 0.11(2) 0.19(3) 0.08(2) 0.09(2) 0.088(18) C7 0.11(2) 0.14(2) 0.22(3) 0.16(2) 0.116(19) 0.106(16) C9 0.050(13) 0.077(16) 0.11(2) 0.007(15) 0.031(13) 0.037(12) C10 0.070(15) 0.14(2) 0.060(14) 0.009(15) 0.038(12) 0.041(15) C11 0.053(16) 0.23(3) 0.13(2) 0.14(2) 0.037(16) 0.019(19) C12 0.051(16) 0.11(2) 0.13(2) 0.08(2) -0.007(16) 0.007(14) C13 0.039(13) 0.026(12) 0.16(3) 0.013(15) 0.038(15) 0.003(10) C14 0.09(2) 0.11(2) 0.12(2) 0.017(17) 0.038(18) 0.036(17) C15 0.082(19) 0.13(2) 0.051(16) -0.001(15) 0.027(14) 0.002(16) C16 0.048(14) 0.13(2) 0.076(17) 0.054(15) 0.023(13) 0.038(15) C17 0.070(17) 0.088(18) 0.20(3) 0.066(19) 0.066(18) 0.061(14) C18 0.19(3) 0.11(2) 0.24(3) 0.12(2) 0.17(3) 0.13(2) C19 0.16(3) 0.10(2) 0.10(2) 0.018(16) 0.10(2) 0.044(19) C20 0.09(2) 0.16(3) 0.09(2) 0.05(2) 0.052(18) 0.03(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 Sm O12 2.677(12) . yes Sm O5 2.706(12) . yes Sm O13 2.708(15) . yes Sm O3 2.719(13) . yes Sm O4 2.735(12) . yes Sm O14 2.739(11) . yes Sm O15 2.730(11) . yes Sm O1 2.730(11) . yes Sm O2 2.748(11) . yes Sm O11 2.755(13) . yes Cl1 O23A 1.32(2) . no Cl1 O22 1.409(11) . no Cl1 O24A 1.438(19) . no Cl1 O21B 1.45(2) . no Cl1 O21A 1.46(2) . no Cl1 O23B 1.47(2) . no Cl1 O24B 1.46(3) . no Cl2 O31 1.316(14) . no Cl2 O32 1.368(14) . no Cl2 O33 1.378(13) . no Cl2 O34 1.48(2) . no O1 C10 1.372(19) . no O1 C1 1.469(19) . no O2 C2 1.365(18) . no O2 C3 1.42(2) . no O3 C5 1.42(2) . no O3 C4 1.41(2) . no O4 C6 1.40(2) . no O4 C7 1.46(2) . no O5 C8 1.34(2) . no O5 C9 1.41(2) . no O11 C20 1.33(3) . no O11 C11 1.45(2) . no O12 C12 1.34(2) . no O12 C13 1.430(19) . no O13 C14 1.36(2) . no O13 C15 1.49(3) . no O14 C16 1.42(2) . no O14 C17 1.43(2) . no O15 C18 1.42(2) . no O15 C19 1.52(2) . no O21A O21B 1.01(2) . no O23A O23B 0.77(3) . no O23A O24B 1.55(3) . no O24A O24B 1.16(3) . no C1 C2 1.47(2) . no C3 C4 1.45(2) . no C5 C6 1.52(3) . no C8 C7 1.41(3) . no C9 C10 1.52(2) . no C11 C12 1.48(3) . no C13 C14 1.43(3) . no C15 C16 1.43(2) . no C17 C18 1.46(3) . no C19 C20 1.38(3) . no 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 O12 Sm O5 97.4(4) . . no O12 Sm O13 58.7(5) . . no O5 Sm O13 74.9(4) . . no O12 Sm O3 124.1(4) . . no O5 Sm O3 86.6(4) . . no O13 Sm O3 161.5(4) . . no O12 Sm O4 73.3(4) . . no O5 Sm O4 58.4(5) . . no O13 Sm O4 105.8(5) . . no O3 Sm O4 61.9(5) . . no O12 Sm O14 86.6(4) . . no O5 Sm O14 124.5(4) . . no O13 Sm O14 60.3(4) . . no O3 Sm O14 135.1(5) . . no O4 Sm O14 159.8(4) . . no O12 Sm O15 99.3(4) . . no O5 Sm O15 162.9(4) . . no O13 Sm O15 117.1(4) . . no O3 Sm O15 81.2(4) . . no O4 Sm O15 123.9(5) . . no O14 Sm O15 60.2(4) . . no O12 Sm O1 129.1(4) . . no O5 Sm O1 58.8(4) . . no O13 Sm O1 71.2(4) . . no O3 Sm O1 100.5(3) . . no O4 Sm O1 115.2(4) . . no O14 Sm O1 76.1(4) . . no O15 Sm O1 111.7(4) . . no O12 Sm O2 163.4(4) . . no O5 Sm O2 98.9(4) . . no O13 Sm O2 123.7(5) . . no O3 Sm O2 59.8(4) . . no O4 Sm O2 118.1(4) . . no O14 Sm O2 82.0(4) . . no O15 Sm O2 64.6(4) . . no O1 Sm O2 59.4(4) . . no O12 Sm O11 59.9(5) . . no O5 Sm O11 127.1(5) . . no O13 Sm O11 116.7(5) . . no O3 Sm O11 73.5(4) . . no O4 Sm O11 69.1(5) . . no O14 Sm O11 102.6(4) . . no O15 Sm O11 60.4(5) . . no O1 Sm O11 170.3(5) . . no O2 Sm O11 111.0(5) . . no O23A Cl1 O22 120.0(12) . . no O23A Cl1 O24A 109.0(15) . . no O22 Cl1 O24A 103.6(9) . . no O23A Cl1 O21B 111.3(13) . . no O22 Cl1 O21B 122.8(11) . . no O24A Cl1 O21B 80.7(12) . . no O23A Cl1 O21A 114.5(15) . . no O22 Cl1 O21A 93.4(12) . . no O24A Cl1 O21A 115.5(13) . . no O21B Cl1 O21A 40.4(10) . . no O23A Cl1 O23B 31.6(12) . . no O22 Cl1 O23B 106.5(11) . . no O24A Cl1 O23B 139.8(13) . . no O21B Cl1 O23B 104.0(13) . . no O21A Cl1 O23B 88.8(14) . . no O23A Cl1 O24B 67.5(15) . . no O22 Cl1 O24B 106.0(13) . . no O24A Cl1 O24B 47.2(11) . . no O21B Cl1 O24B 115.9(15) . . no O21A Cl1 O24B 156.2(15) . . no O23B Cl1 O24B 98.4(16) . . no O31 Cl2 O32 117.0(11) . . no O31 Cl2 O33 114.6(10) . . no O32 Cl2 O33 109.9(9) . . no O31 Cl2 O34 104.4(12) . . no O32 Cl2 O34 98.9(10) . . no O33 Cl2 O34 110.6(11) . . no C10 O1 C1 114.1(15) . . no C10 O1 Sm 120.6(12) . . no C1 O1 Sm 114.6(9) . . no C2 O2 C3 114.0(14) . . no C2 O2 Sm 121.0(10) . . no C3 O2 Sm 111.8(11) . . no C5 O3 C4 110.6(16) . . no C5 O3 Sm 121.4(13) . . no C4 O3 Sm 120.5(11) . . no C6 O4 C7 115.1(18) . . no C6 O4 Sm 110.6(13) . . no C7 O4 Sm 118.6(12) . . no C8 O5 C9 112.1(17) . . no C8 O5 Sm 113.4(13) . . no C9 O5 Sm 118.7(11) . . no C20 O11 C11 118.0(19) . . no C20 O11 Sm 114.7(15) . . no C11 O11 Sm 115.2(12) . . no C12 O12 C13 114.3(18) . . no C12 O12 Sm 121.9(12) . . no C13 O12 Sm 116.9(12) . . no C14 O13 C15 106.2(19) . . no C14 O13 Sm 120.8(14) . . no C15 O13 Sm 109.7(11) . . no C16 O14 C17 112.0(15) . . no C16 O14 Sm 122.3(11) . . no C17 O14 Sm 119.0(12) . . no C18 O15 C19 119.7(16) . . no C18 O15 Sm 113.7(12) . . no C19 O15 Sm 116.9(12) . . no O21B O21A Cl1 69(2) . . no O21A O21B Cl1 70(2) . . no O23B O23A Cl1 85(3) . . no O23B O23A O24B 143(4) . . no Cl1 O23A O24B 60.5(16) . . no O23A O23B Cl1 64(3) . . no O24B O24A Cl1 67.4(17) . . no O24A O24B Cl1 65.4(18) . . no O24A O24B O23A 111(3) . . no Cl1 O24B O23A 52.1(13) . . no O1 C1 C2 108.6(13) . . no O2 C2 C1 108.5(14) . . no O2 C3 C4 111.9(15) . . no O3 C4 C3 105.8(16) . . no O3 C5 C6 107.1(15) . . no O4 C6 C5 116.3(18) . . no O5 C8 C7 111(2) . . no C8 C7 O4 109.5(18) . . no O5 C9 C10 105.1(16) . . no O1 C10 C9 111.8(17) . . no O11 C11 C12 115.1(19) . . no O12 C12 C11 107(2) . . no C14 C13 O12 108.7(18) . . no O13 C14 C13 109(2) . . no C16 C15 O13 113.7(17) . . no O14 C16 C15 106.6(16) . . no O14 C17 C18 105.7(18) . . no O15 C18 C17 111.7(19) . . no C20 C19 O15 110(2) . . no O11 C20 C19 117(3) . . no _diffrn_measured_fraction_theta_max 0.674 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.674 _refine_diff_density_max 0.832 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.082