#------------------------------------------------------------------------------ #$Date: 2015-05-09 10:47:43 +0300 (Sat, 09 May 2015) $ #$Revision: 135958 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/48/7054807.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7054807 loop_ _publ_author_name 'Klementyeva, Svetlana V.' 'Arleth, Nicholas' 'Meyer, Karsten' 'Konchenko, Sergey N.' 'Roesky, Peter W.' _publ_section_title ; Dithionite and sulfinate complexes from the reaction of SO2with decamethylsamarocene ; _journal_name_full 'New J. Chem.' _journal_paper_doi 10.1039/C5NJ00318K _journal_year 2015 _chemical_formula_moiety 'C60 H90 O8 S4 Sm2, C7 H8' _chemical_formula_sum 'C67 H98 O8 S4 Sm2' _chemical_formula_weight 1460.39 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-01-20 _audit_creation_method ; ? ; _audit_update_record ; 2015-02-05 deposited with the CCDC. 2015-03-31 downloaded from the CCDC. ; _cell_angle_alpha 76.608(2) _cell_angle_beta 72.242(2) _cell_angle_gamma 74.217(2) _cell_formula_units_Z 1 _cell_length_a 11.8154(4) _cell_length_b 12.3472(4) _cell_length_c 12.4497(4) _cell_measurement_temperature 100 _cell_volume 1642.46(10) _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_collection 'STOE X-AREA' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100 _diffrn_detector Pilatus100K _diffrn_detector_area_resol_mean 5.81 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'STOE STADI VARI' _diffrn_measurement_method 'area detector' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17852 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.043 _diffrn_reflns_theta_min 1.741 _diffrn_source 'Mo LFF Sealed Tube' _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 1.949 _exptl_absorpt_correction_T_max 0.8300 _exptl_absorpt_correction_T_min 0.6834 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-Red, X-Shape' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.476 _exptl_crystal_description rod _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.104 _refine_diff_density_max 1.907 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.176 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 368 _refine_ls_number_reflns 6440 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0302 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+2.0957P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0825 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6131 _reflns_number_total 6440 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5nj00318k2.cif _cod_data_source_block 4 _cod_database_code 7054807 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C32-C34 1.4 with sigma of 0.02 C34-C31 2 with sigma of 0.02 C33-C34 \\sim C34-C31 with sigma of 0.02 C33-C32 \\sim C32-C31 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C33) = Uanis(C32) = Uanis(C34) = Uanis(C31) 4. Others Fixed Sof: C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) 5.a Aromatic/amide H refined with riding coordinates: C31(H31), C33(H33) 5.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B, H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A, H34B,H34C) ; _shelx_res_file ; TITL KS14-06B CELL 0.71073 11.8154 12.3472 12.4497 76.608 72.242 74.217 ZERR 1 0.0004 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H O S Sm UNIT 67 98 8 4 2 DFIX 1.4 C32 C34 DFIX 2 C34 C31 SADI C33 C34 C34 C31 SADI C33 C32 C32 C31 EADP C33 C32 C34 C31 L.S. 30 0 0 PLAN 10 TEMP -173.15 FREE C31 C34 MORE -1 BOND $H CONF fmap 2 53 acta 52 REM REM REM WGHT 0.052200 2.095700 FVAR 0.50435 SM1 5 1.034358 0.121006 0.553573 11.00000 0.01194 0.01206 = 0.01188 -0.00334 -0.00446 -0.00215 S1 4 0.734710 0.086305 0.587124 11.00000 0.01247 0.01546 = 0.01439 -0.00276 -0.00385 -0.00211 S2 4 0.990766 0.109553 0.265935 11.00000 0.01600 0.01395 = 0.01183 -0.00096 -0.00600 -0.00260 O1 3 0.833717 0.101086 0.633371 11.00000 0.01555 0.02130 = 0.01709 -0.00484 -0.00429 -0.00501 O2 3 1.223088 0.027515 0.457186 11.00000 0.01653 0.01757 = 0.01836 -0.00641 -0.00258 -0.00272 O3 3 0.966281 0.125285 0.390458 11.00000 0.01772 0.02354 = 0.01286 -0.00336 -0.00775 -0.00161 O4 3 1.049669 -0.000394 0.725922 11.00000 0.02613 0.01456 = 0.02140 -0.00023 -0.01282 -0.00495 C1 1 0.971629 0.284548 0.680736 11.00000 0.01920 0.01379 = 0.01609 -0.00572 -0.00631 -0.00288 C2 1 0.949520 0.338949 0.573434 11.00000 0.01931 0.01270 = 0.01765 -0.00539 -0.00763 -0.00059 C3 1 1.063585 0.336607 0.490880 11.00000 0.01833 0.01044 = 0.01874 -0.00319 -0.00778 -0.00339 C4 1 1.156182 0.280289 0.548073 11.00000 0.01845 0.01252 = 0.02020 -0.00420 -0.00854 -0.00435 C5 1 1.099680 0.247383 0.665094 11.00000 0.02035 0.01382 = 0.01869 -0.00469 -0.00996 -0.00323 C6 1 0.877530 0.267421 0.792005 11.00000 0.02634 0.02408 = 0.01650 -0.00712 -0.00245 -0.00387 AFIX 137 H6A 2 0.798568 0.275904 0.777000 11.00000 -1.50000 H6B 2 0.871274 0.324390 0.837987 11.00000 -1.50000 H6C 2 0.901306 0.190784 0.833683 11.00000 -1.50000 AFIX 0 C7 1 0.827939 0.392498 0.548597 11.00000 0.01866 0.01961 = 0.02421 -0.00508 -0.00955 0.00034 AFIX 137 H7A 2 0.818731 0.356580 0.490224 11.00000 -1.50000 H7B 2 0.822702 0.474264 0.520709 11.00000 -1.50000 H7C 2 0.763057 0.381587 0.618651 11.00000 -1.50000 AFIX 0 C8 1 1.079643 0.390626 0.367422 11.00000 0.02350 0.01791 = 0.01740 -0.00189 -0.00790 -0.00468 AFIX 137 H8A 2 1.166368 0.375432 0.327458 11.00000 -1.50000 H8B 2 1.047706 0.473163 0.362290 11.00000 -1.50000 H8C 2 1.035325 0.358501 0.332028 11.00000 -1.50000 AFIX 0 C9 1 1.291813 0.262700 0.496403 11.00000 0.01691 0.02318 = 0.02304 -0.00362 -0.00734 -0.00642 AFIX 137 H9A 2 1.328137 0.180825 0.502276 11.00000 -1.50000 H9B 2 1.327473 0.297696 0.537578 11.00000 -1.50000 H9C 2 1.307940 0.298152 0.415789 11.00000 -1.50000 AFIX 0 C10 1 1.163454 0.188493 0.757171 11.00000 0.02509 0.02221 = 0.02061 -0.00179 -0.01346 -0.00517 AFIX 137 H10A 2 1.113988 0.139178 0.814582 11.00000 -1.50000 H10B 2 1.175207 0.245630 0.793465 11.00000 -1.50000 H10C 2 1.242803 0.142223 0.723579 11.00000 -1.50000 AFIX 0 C11 1 0.612695 0.055496 0.719094 11.00000 0.01212 0.01733 = 0.01441 -0.00350 -0.00201 -0.00224 C12 1 0.578218 0.157165 0.779727 11.00000 0.01270 0.01880 = 0.02075 -0.00744 -0.00274 -0.00110 C13 1 0.608311 0.122740 0.879985 11.00000 0.01188 0.02499 = 0.01766 -0.00632 -0.00097 -0.00465 C14 1 0.660832 -0.000913 0.893365 11.00000 0.01306 0.02736 = 0.01679 -0.00116 -0.00259 -0.00511 C15 1 0.661353 -0.042106 0.802070 11.00000 0.01339 0.01936 = 0.01614 -0.00175 -0.00150 -0.00222 C16 1 0.512145 0.038259 0.675281 11.00000 0.01604 0.02507 = 0.02166 -0.00707 -0.00528 -0.00477 AFIX 137 H16A 2 0.486396 0.106539 0.622537 11.00000 -1.50000 H16B 2 0.442535 0.024922 0.739972 11.00000 -1.50000 H16C 2 0.543100 -0.027724 0.635270 11.00000 -1.50000 AFIX 0 C17 1 0.521456 0.273806 0.729169 11.00000 0.02609 0.01813 = 0.02982 -0.00715 -0.01010 0.00125 AFIX 137 H17A 2 0.575101 0.297369 0.654848 11.00000 -1.50000 H17B 2 0.509348 0.327714 0.780448 11.00000 -1.50000 H17C 2 0.442689 0.272841 0.719050 11.00000 -1.50000 AFIX 0 C18 1 0.590838 0.192938 0.969105 11.00000 0.02490 0.03508 = 0.02279 -0.01200 -0.00299 -0.00875 AFIX 137 H18A 2 0.669725 0.188250 0.982451 11.00000 -1.50000 H18B 2 0.536198 0.164039 1.040360 11.00000 -1.50000 H18C 2 0.555132 0.272558 0.942946 11.00000 -1.50000 AFIX 0 C19 1 0.704021 -0.066471 0.996234 11.00000 0.02626 0.03807 = 0.01777 -0.00184 -0.00769 -0.00183 AFIX 137 H19A 2 0.771218 -0.037512 1.001587 11.00000 -1.50000 H19B 2 0.732195 -0.147451 0.989117 11.00000 -1.50000 H19C 2 0.636870 -0.057286 1.065213 11.00000 -1.50000 AFIX 0 C20 1 0.698209 -0.163015 0.782963 11.00000 0.02228 0.01864 = 0.02294 -0.00163 -0.00213 -0.00238 AFIX 137 H20A 2 0.636687 -0.180035 0.755306 11.00000 -1.50000 H20B 2 0.705260 -0.213717 0.855005 11.00000 -1.50000 H20C 2 0.776906 -0.174771 0.726019 11.00000 -1.50000 AFIX 0 C21 1 0.872574 0.219413 0.205914 11.00000 0.02018 0.01703 = 0.01319 -0.00074 -0.00923 -0.00300 C22 1 0.907976 0.332815 0.184708 11.00000 0.01931 0.01651 = 0.01569 0.00141 -0.00911 -0.00339 C23 1 0.817715 0.403783 0.246152 11.00000 0.01998 0.01617 = 0.01816 0.00038 -0.01183 -0.00229 C24 1 0.718204 0.343956 0.311050 11.00000 0.01675 0.02183 = 0.01609 -0.00050 -0.00907 -0.00202 C25 1 0.747649 0.237602 0.287553 11.00000 0.01743 0.02094 = 0.01656 -0.00031 -0.01083 -0.00260 C26 1 0.877894 0.180868 0.096036 11.00000 0.03139 0.02491 = 0.01702 -0.00402 -0.01325 -0.00351 AFIX 137 H26A 2 0.961957 0.168641 0.048549 11.00000 -1.50000 H26B 2 0.825643 0.239723 0.053969 11.00000 -1.50000 H26C 2 0.849496 0.109516 0.115115 11.00000 -1.50000 AFIX 0 C27 1 1.023873 0.355829 0.101638 11.00000 0.02287 0.02332 = 0.02141 0.00346 -0.00587 -0.00612 AFIX 137 H27A 2 1.022490 0.351523 0.024445 11.00000 -1.50000 H27B 2 1.093008 0.298881 0.122374 11.00000 -1.50000 H27C 2 1.032059 0.432161 0.103667 11.00000 -1.50000 AFIX 0 C28 1 0.810452 0.526579 0.246502 11.00000 0.02723 0.01503 = 0.03120 -0.00514 -0.01267 0.00029 AFIX 137 H28A 2 0.890232 0.544915 0.207826 11.00000 -1.50000 H28B 2 0.786263 0.540584 0.325547 11.00000 -1.50000 H28C 2 0.750102 0.574674 0.206361 11.00000 -1.50000 AFIX 0 C29 1 0.601758 0.401448 0.385106 11.00000 0.01898 0.02968 = 0.02823 -0.00767 -0.00788 0.00242 AFIX 137 H29A 2 0.619963 0.432357 0.442184 11.00000 -1.50000 H29B 2 0.550701 0.345956 0.423877 11.00000 -1.50000 H29C 2 0.558448 0.463633 0.337693 11.00000 -1.50000 AFIX 0 C30 1 0.669741 0.151727 0.320430 11.00000 0.02140 0.02661 = 0.02680 0.00112 -0.01223 -0.00877 AFIX 137 H30A 2 0.595497 0.176854 0.378726 11.00000 -1.50000 H30B 2 0.714741 0.077794 0.351126 11.00000 -1.50000 H30C 2 0.647961 0.144295 0.252969 11.00000 -1.50000 AFIX 0 C31 1 0.447162 0.448200 1.111134 11.00000 0.26844 0.04437 = 0.12904 -0.04863 -0.16299 0.05818 AFIX 43 H31 2 0.409349 0.413376 1.185095 11.00000 -1.20000 AFIX 0 C32 1 0.389694 0.489296 1.027310 11.00000 0.26844 0.04437 = 0.12904 -0.04863 -0.16299 0.05818 C33 1 0.438571 0.539463 0.918489 11.00000 0.26844 0.04437 = 0.12904 -0.04863 -0.16299 0.05818 AFIX 43 H33 2 0.390940 0.565252 0.864579 11.00000 -1.20000 AFIX 0 C34 1 0.287621 0.475944 1.044460 10.50000 0.26844 0.04437 = 0.12904 -0.04863 -0.16299 0.05818 AFIX 137 H34A 2 0.239851 0.542918 1.005895 10.50000 -1.50000 H34B 2 0.249191 0.466089 1.126811 10.50000 -1.50000 H34C 2 0.291092 0.408003 1.014573 10.50000 -1.50000 AFIX 0 HKLF 4 REM KS14-06B REM R1 = 0.0302 for 6131 Fo > 4sig(Fo) and 0.0319 for all 6440 data REM 368 parameters refined using 4 restraints END WGHT 0.0522 2.0956 REM Highest difference peak 1.907, deepest hole -1.312, 1-sigma level 0.176 Q1 1 0.4836 0.5426 0.9047 11.00000 0.05 1.91 Q2 1 0.3411 0.4650 1.0764 11.00000 0.05 1.72 Q3 1 0.4039 0.5079 0.9768 11.00000 0.05 1.56 Q4 1 0.9802 0.0754 0.5991 11.00000 0.05 1.37 Q5 1 1.0863 0.1671 0.5062 11.00000 0.05 1.20 Q6 1 0.4221 0.4218 1.1489 11.00000 0.05 0.97 Q7 1 0.8902 0.2707 0.1922 11.00000 0.05 0.55 Q8 1 0.6237 0.0579 0.9051 11.00000 0.05 0.54 Q9 1 0.2460 0.4986 1.1177 11.00000 0.05 0.54 Q10 1 1.0516 0.1331 0.2208 11.00000 0.05 0.49 ; _shelx_res_checksum 4672 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy Sm1 Sm 1.03436(2) 0.12101(2) 0.55357(2) 0.01149(7) Uani 1 1 d . . S1 S 0.73471(6) 0.08631(6) 0.58712(6) 0.01415(15) Uani 1 1 d . . S2 S 0.99077(7) 0.10955(6) 0.26593(6) 0.01370(15) Uani 1 1 d . . O1 O 0.83372(19) 0.10109(19) 0.63337(18) 0.0175(4) Uani 1 1 d . . O2 O 1.2231(2) 0.02752(19) 0.45719(19) 0.0175(4) Uani 1 1 d . . O3 O 0.9663(2) 0.1253(2) 0.39046(18) 0.0177(4) Uani 1 1 d . . O4 O 1.0497(2) -0.00039(19) 0.7259(2) 0.0195(5) Uani 1 1 d . . C1 C 0.9716(3) 0.2845(3) 0.6807(3) 0.0155(6) Uani 1 1 d . . C2 C 0.9495(3) 0.3389(3) 0.5734(3) 0.0160(6) Uani 1 1 d . . C3 C 1.0636(3) 0.3366(2) 0.4909(3) 0.0149(6) Uani 1 1 d . . C4 C 1.1562(3) 0.2803(3) 0.5481(3) 0.0158(6) Uani 1 1 d . . C5 C 1.0997(3) 0.2474(3) 0.6651(3) 0.0162(6) Uani 1 1 d . . C6 C 0.8775(3) 0.2674(3) 0.7920(3) 0.0227(7) Uani 1 1 d . . H6A H 0.7986 0.2759 0.7770 0.034 Uiso 1 1 calc GR . H6B H 0.8713 0.3244 0.8380 0.034 Uiso 1 1 calc GR . H6C H 0.9013 0.1908 0.8337 0.034 Uiso 1 1 calc GR . C7 C 0.8279(3) 0.3925(3) 0.5486(3) 0.0206(6) Uani 1 1 d . . H7A H 0.8187 0.3566 0.4902 0.031 Uiso 1 1 calc GR . H7B H 0.8227 0.4743 0.5207 0.031 Uiso 1 1 calc GR . H7C H 0.7631 0.3816 0.6187 0.031 Uiso 1 1 calc GR . C8 C 1.0796(3) 0.3906(3) 0.3674(3) 0.0191(6) Uani 1 1 d . . H8A H 1.1664 0.3754 0.3275 0.029 Uiso 1 1 calc GR . H8B H 1.0477 0.4732 0.3623 0.029 Uiso 1 1 calc GR . H8C H 1.0353 0.3585 0.3320 0.029 Uiso 1 1 calc GR . C9 C 1.2918(3) 0.2627(3) 0.4964(3) 0.0201(6) Uani 1 1 d . . H9A H 1.3281 0.1808 0.5023 0.030 Uiso 1 1 calc GR . H9B H 1.3275 0.2977 0.5376 0.030 Uiso 1 1 calc GR . H9C H 1.3079 0.2982 0.4158 0.030 Uiso 1 1 calc GR . C10 C 1.1635(3) 0.1885(3) 0.7572(3) 0.0212(7) Uani 1 1 d . . H10A H 1.1140 0.1392 0.8146 0.032 Uiso 1 1 calc GR . H10B H 1.1752 0.2456 0.7935 0.032 Uiso 1 1 calc GR . H10C H 1.2428 0.1422 0.7236 0.032 Uiso 1 1 calc GR . C11 C 0.6127(3) 0.0555(3) 0.7191(3) 0.0150(6) Uani 1 1 d . . C12 C 0.5782(3) 0.1572(3) 0.7797(3) 0.0175(6) Uani 1 1 d . . C13 C 0.6083(3) 0.1227(3) 0.8800(3) 0.0182(6) Uani 1 1 d . . C14 C 0.6608(3) -0.0009(3) 0.8934(3) 0.0196(6) Uani 1 1 d . . C15 C 0.6614(3) -0.0421(3) 0.8021(3) 0.0173(6) Uani 1 1 d . . C16 C 0.5121(3) 0.0383(3) 0.6753(3) 0.0202(6) Uani 1 1 d . . H16A H 0.4864 0.1065 0.6225 0.030 Uiso 1 1 calc GR . H16B H 0.4425 0.0249 0.7400 0.030 Uiso 1 1 calc GR . H16C H 0.5431 -0.0277 0.6353 0.030 Uiso 1 1 calc GR . C17 C 0.5215(3) 0.2738(3) 0.7292(3) 0.0247(7) Uani 1 1 d . . H17A H 0.5751 0.2974 0.6548 0.037 Uiso 1 1 calc GR . H17B H 0.5093 0.3277 0.7804 0.037 Uiso 1 1 calc GR . H17C H 0.4427 0.2728 0.7190 0.037 Uiso 1 1 calc GR . C18 C 0.5908(3) 0.1929(3) 0.9691(3) 0.0266(7) Uani 1 1 d . . H18A H 0.6697 0.1882 0.9825 0.040 Uiso 1 1 calc GR . H18B H 0.5362 0.1640 1.0404 0.040 Uiso 1 1 calc GR . H18C H 0.5551 0.2726 0.9429 0.040 Uiso 1 1 calc GR . C19 C 0.7040(3) -0.0665(4) 0.9962(3) 0.0284(8) Uani 1 1 d . . H19A H 0.7712 -0.0375 1.0016 0.043 Uiso 1 1 calc GR . H19B H 0.7322 -0.1475 0.9891 0.043 Uiso 1 1 calc GR . H19C H 0.6369 -0.0573 1.0652 0.043 Uiso 1 1 calc GR . C20 C 0.6982(3) -0.1630(3) 0.7830(3) 0.0229(7) Uani 1 1 d . . H20A H 0.6367 -0.1800 0.7553 0.034 Uiso 1 1 calc GR . H20B H 0.7053 -0.2137 0.8550 0.034 Uiso 1 1 calc GR . H20C H 0.7769 -0.1748 0.7260 0.034 Uiso 1 1 calc GR . C21 C 0.8726(3) 0.2194(3) 0.2059(3) 0.0162(6) Uani 1 1 d . . C22 C 0.9080(3) 0.3328(3) 0.1847(3) 0.0169(6) Uani 1 1 d . . C23 C 0.8177(3) 0.4038(3) 0.2462(3) 0.0174(6) Uani 1 1 d . . C24 C 0.7182(3) 0.3440(3) 0.3111(3) 0.0180(6) Uani 1 1 d . . C25 C 0.7476(3) 0.2376(3) 0.2876(3) 0.0176(6) Uani 1 1 d . . C26 C 0.8779(3) 0.1809(3) 0.0960(3) 0.0232(7) Uani 1 1 d . . H26A H 0.9620 0.1686 0.0485 0.035 Uiso 1 1 calc GR . H26B H 0.8256 0.2397 0.0540 0.035 Uiso 1 1 calc GR . H26C H 0.8495 0.1095 0.1151 0.035 Uiso 1 1 calc GR . C27 C 1.0239(3) 0.3558(3) 0.1016(3) 0.0235(7) Uani 1 1 d . . H27A H 1.0225 0.3515 0.0244 0.035 Uiso 1 1 calc GR . H27B H 1.0930 0.2989 0.1224 0.035 Uiso 1 1 calc GR . H27C H 1.0321 0.4322 0.1037 0.035 Uiso 1 1 calc GR . C28 C 0.8105(3) 0.5266(3) 0.2465(3) 0.0241(7) Uani 1 1 d . . H28A H 0.8902 0.5449 0.2078 0.036 Uiso 1 1 calc GR . H28B H 0.7863 0.5406 0.3255 0.036 Uiso 1 1 calc GR . H28C H 0.7501 0.5747 0.2064 0.036 Uiso 1 1 calc GR . C29 C 0.6018(3) 0.4014(3) 0.3851(3) 0.0263(7) Uani 1 1 d . . H29A H 0.6200 0.4324 0.4422 0.039 Uiso 1 1 calc GR . H29B H 0.5507 0.3460 0.4239 0.039 Uiso 1 1 calc GR . H29C H 0.5584 0.4636 0.3377 0.039 Uiso 1 1 calc GR . C30 C 0.6697(3) 0.1517(3) 0.3204(3) 0.0237(7) Uani 1 1 d . . H30A H 0.5955 0.1769 0.3787 0.036 Uiso 1 1 calc GR . H30B H 0.7147 0.0778 0.3511 0.036 Uiso 1 1 calc GR . H30C H 0.6480 0.1443 0.2530 0.036 Uiso 1 1 calc GR . C31 C 0.4472(11) 0.4482(6) 1.1111(8) 0.134(3) Uani 1 1 d D . H31 H 0.4093 0.4134 1.1851 0.161 Uiso 1 1 calc R . C32 C 0.3897(11) 0.4893(5) 1.0273(7) 0.134(3) Uani 1 1 d D . C33 C 0.4386(10) 0.5395(6) 0.9185(7) 0.134(3) Uani 1 1 d D . H33 H 0.3909 0.5653 0.8646 0.161 Uiso 1 1 calc R . C34 C 0.2876(14) 0.4759(11) 1.0445(12) 0.134(3) Uani 0.5 1 d D P H34A H 0.2399 0.5429 1.0059 0.201 Uiso 0.5 1 calc GR P H34B H 0.2492 0.4661 1.1268 0.201 Uiso 0.5 1 calc GR P H34C H 0.2911 0.4080 1.0146 0.201 Uiso 0.5 1 calc GR P 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 0.01194(9) 0.01206(10) 0.01188(9) -0.00334(6) -0.00446(6) -0.00215(6) S1 0.0125(3) 0.0155(3) 0.0144(3) -0.0028(3) -0.0038(3) -0.0021(3) S2 0.0160(3) 0.0139(3) 0.0118(3) -0.0010(3) -0.0060(3) -0.0026(3) O1 0.0155(10) 0.0213(11) 0.0171(10) -0.0048(9) -0.0043(8) -0.0050(9) O2 0.0165(10) 0.0176(11) 0.0184(11) -0.0064(9) -0.0026(8) -0.0027(9) O3 0.0177(10) 0.0235(11) 0.0129(10) -0.0034(9) -0.0077(8) -0.0016(9) O4 0.0261(12) 0.0146(10) 0.0214(11) -0.0002(9) -0.0128(9) -0.0049(9) C1 0.0192(15) 0.0138(14) 0.0161(14) -0.0057(11) -0.0063(12) -0.0029(11) C2 0.0193(15) 0.0127(14) 0.0176(14) -0.0054(11) -0.0076(12) -0.0006(11) C3 0.0183(14) 0.0104(14) 0.0187(15) -0.0032(11) -0.0078(12) -0.0034(11) C4 0.0185(15) 0.0125(14) 0.0202(15) -0.0042(12) -0.0085(12) -0.0043(11) C5 0.0203(15) 0.0138(14) 0.0187(15) -0.0047(12) -0.0100(12) -0.0032(12) C6 0.0263(17) 0.0241(17) 0.0165(15) -0.0071(13) -0.0025(13) -0.0039(14) C7 0.0187(15) 0.0196(16) 0.0242(16) -0.0051(13) -0.0095(13) 0.0003(12) C8 0.0235(16) 0.0179(15) 0.0174(15) -0.0019(12) -0.0079(12) -0.0047(13) C9 0.0169(15) 0.0232(16) 0.0230(16) -0.0036(13) -0.0073(12) -0.0064(12) C10 0.0251(16) 0.0222(16) 0.0206(15) -0.0018(13) -0.0135(13) -0.0052(13) C11 0.0121(13) 0.0173(15) 0.0144(14) -0.0035(12) -0.0020(11) -0.0022(11) C12 0.0127(13) 0.0188(15) 0.0207(15) -0.0074(12) -0.0027(11) -0.0011(12) C13 0.0119(13) 0.0250(16) 0.0177(14) -0.0063(13) -0.0010(11) -0.0047(12) C14 0.0131(14) 0.0274(17) 0.0168(15) -0.0012(13) -0.0026(11) -0.0051(12) C15 0.0134(14) 0.0194(15) 0.0161(14) -0.0017(12) -0.0015(11) -0.0022(12) C16 0.0160(14) 0.0251(16) 0.0217(15) -0.0071(13) -0.0053(12) -0.0048(13) C17 0.0261(17) 0.0181(16) 0.0298(18) -0.0072(14) -0.0101(14) 0.0013(13) C18 0.0249(17) 0.035(2) 0.0228(17) -0.0120(15) -0.0030(13) -0.0087(15) C19 0.0263(17) 0.038(2) 0.0178(16) -0.0018(15) -0.0077(13) -0.0018(15) C20 0.0223(16) 0.0186(16) 0.0229(16) -0.0016(13) -0.0021(13) -0.0024(13) C21 0.0202(15) 0.0170(15) 0.0132(14) -0.0007(11) -0.0092(11) -0.0030(12) C22 0.0193(15) 0.0165(15) 0.0157(14) 0.0014(12) -0.0091(12) -0.0034(12) C23 0.0200(15) 0.0162(15) 0.0182(14) 0.0004(12) -0.0118(12) -0.0023(12) C24 0.0168(14) 0.0218(16) 0.0161(14) -0.0005(12) -0.0091(12) -0.0020(12) C25 0.0174(15) 0.0209(15) 0.0166(14) -0.0003(12) -0.0108(12) -0.0026(12) C26 0.0314(18) 0.0249(17) 0.0170(15) -0.0040(13) -0.0132(13) -0.0035(14) C27 0.0229(16) 0.0233(17) 0.0214(16) 0.0035(13) -0.0059(13) -0.0061(13) C28 0.0272(17) 0.0150(15) 0.0312(18) -0.0051(13) -0.0127(14) 0.0003(13) C29 0.0190(16) 0.0297(18) 0.0282(18) -0.0077(15) -0.0079(14) 0.0024(14) C30 0.0214(16) 0.0266(17) 0.0268(17) 0.0011(14) -0.0122(13) -0.0088(14) C31 0.268(9) 0.044(2) 0.129(4) -0.049(2) -0.163(6) 0.058(4) C32 0.268(9) 0.044(2) 0.129(4) -0.049(2) -0.163(6) 0.058(4) C33 0.268(9) 0.044(2) 0.129(4) -0.049(2) -0.163(6) 0.058(4) C34 0.268(9) 0.044(2) 0.129(4) -0.049(2) -0.163(6) 0.058(4) 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' 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' 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 S2 Sm1 Sm1 63.917(13) 2_756 2_756 O1 Sm1 Sm1 67.88(6) . 2_756 O1 Sm1 S2 66.45(6) . 2_756 O1 Sm1 O3 77.03(8) . . O1 Sm1 O4 78.78(8) . . O1 Sm1 C1 84.58(9) . . O1 Sm1 C2 86.15(9) . . O1 Sm1 C3 115.21(9) . . O1 Sm1 C4 133.90(9) . . O1 Sm1 C5 112.27(9) . . O2 Sm1 Sm1 75.49(5) . 2_756 O2 Sm1 S2 89.06(6) . 2_756 O2 Sm1 O1 142.04(8) . . O2 Sm1 O3 86.80(8) . . O2 Sm1 O4 91.81(8) . . O2 Sm1 C1 131.27(9) . . O2 Sm1 C2 130.44(9) . . O2 Sm1 C3 99.73(9) . . O2 Sm1 C4 83.96(9) . . O2 Sm1 C5 100.95(9) . . O3 Sm1 Sm1 49.31(6) . 2_756 O3 Sm1 S2 111.87(6) . 2_756 O3 Sm1 C1 127.01(9) . . O3 Sm1 C2 97.82(9) . . O3 Sm1 C3 93.71(9) . . O3 Sm1 C4 118.85(9) . . O3 Sm1 C5 144.26(9) . . O4 Sm1 Sm1 89.83(5) . 2_756 O4 Sm1 S2 26.24(6) . 2_756 O4 Sm1 O3 138.08(8) . . O4 Sm1 C1 83.61(9) . . O4 Sm1 C2 114.15(9) . . O4 Sm1 C3 127.66(9) . . O4 Sm1 C4 102.59(8) . . O4 Sm1 C5 77.03(9) . . C1 Sm1 Sm1 152.44(7) . 2_756 C1 Sm1 S2 104.93(7) . 2_756 C1 Sm1 C3 51.00(9) . . C1 Sm1 C4 50.54(9) . . C1 Sm1 C5 30.77(9) . . C2 Sm1 Sm1 140.82(7) . 2_756 C2 Sm1 S2 132.29(7) . 2_756 C2 Sm1 C1 30.95(9) . . C2 Sm1 C3 30.95(10) . . C2 Sm1 C4 50.66(9) . . C2 Sm1 C5 50.92(9) . . C3 Sm1 Sm1 142.51(7) . 2_756 C3 Sm1 S2 153.46(7) . 2_756 C3 Sm1 C4 30.54(9) . . C3 Sm1 C5 50.70(9) . . C4 Sm1 Sm1 156.34(7) . 2_756 C4 Sm1 S2 128.19(7) . 2_756 C5 Sm1 Sm1 166.36(7) . 2_756 C5 Sm1 S2 103.17(7) . 2_756 C5 Sm1 C4 30.41(9) . . O1 S1 O2 108.39(13) . 2_756 O1 S1 C11 103.26(13) . . O2 S1 C11 101.82(13) 2_756 . O3 S2 Sm1 66.55(9) . 2_756 O3 S2 C21 106.46(13) . . O4 S2 Sm1 42.90(8) 2_756 2_756 O4 S2 O3 104.88(13) 2_756 . O4 S2 C21 101.59(13) 2_756 . C21 S2 Sm1 129.85(10) . 2_756 S1 O1 Sm1 134.77(13) . . S1 O2 Sm1 132.00(13) 2_756 . S2 O3 Sm1 151.59(13) . . S2 O4 Sm1 110.86(12) 2_756 . C2 C1 Sm1 73.88(17) . . C2 C1 C5 108.0(3) . . C2 C1 C6 126.6(3) . . C5 C1 Sm1 75.97(17) . . C5 C1 C6 125.4(3) . . C6 C1 Sm1 115.9(2) . . C1 C2 Sm1 75.16(17) . . C1 C2 C3 108.3(3) . . C1 C2 C7 127.0(3) . . C3 C2 Sm1 75.92(17) . . C3 C2 C7 124.7(3) . . C7 C2 Sm1 116.0(2) . . C2 C3 Sm1 73.13(17) . . C2 C3 C8 124.8(3) . . C4 C3 Sm1 75.98(17) . . C4 C3 C2 107.6(3) . . C4 C3 C8 127.6(3) . . C8 C3 Sm1 119.2(2) . . C3 C4 Sm1 73.48(17) . . C3 C4 C9 126.7(3) . . C5 C4 Sm1 74.14(17) . . C5 C4 C3 108.3(3) . . C5 C4 C9 124.9(3) . . C9 C4 Sm1 120.7(2) . . C1 C5 Sm1 73.26(17) . . C1 C5 C10 125.9(3) . . C4 C5 Sm1 75.45(17) . . C4 C5 C1 107.8(3) . . C4 C5 C10 126.2(3) . . C10 C5 Sm1 119.2(2) . . C1 C6 H6A 109.5 . . C1 C6 H6B 109.5 . . C1 C6 H6C 109.5 . . H6A C6 H6B 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C2 C7 H7A 109.5 . . C2 C7 H7B 109.5 . . C2 C7 H7C 109.5 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C3 C8 H8A 109.5 . . C3 C8 H8B 109.5 . . C3 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C4 C9 H9A 109.5 . . C4 C9 H9B 109.5 . . C4 C9 H9C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C5 C10 H10A 109.5 . . C5 C10 H10B 109.5 . . C5 C10 H10C 109.5 . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C12 C11 S1 105.9(2) . . C12 C11 C16 115.0(3) . . C15 C11 S1 111.4(2) . . C15 C11 C12 103.8(2) . . C15 C11 C16 115.8(3) . . C16 C11 S1 104.5(2) . . C13 C12 C11 108.6(3) . . C13 C12 C17 129.0(3) . . C17 C12 C11 122.4(3) . . C12 C13 C14 109.3(3) . . C12 C13 C18 127.9(3) . . C14 C13 C18 122.8(3) . . C13 C14 C19 122.9(3) . . C15 C14 C13 109.7(3) . . C15 C14 C19 127.4(3) . . C14 C15 C11 108.5(3) . . C14 C15 C20 128.1(3) . . C20 C15 C11 123.4(3) . . C11 C16 H16A 109.5 . . C11 C16 H16B 109.5 . . C11 C16 H16C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C12 C17 H17A 109.5 . . C12 C17 H17B 109.5 . . C12 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . C13 C18 H18A 109.5 . . C13 C18 H18B 109.5 . . C13 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C14 C19 H19A 109.5 . . C14 C19 H19B 109.5 . . C14 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C15 C20 H20A 109.5 . . C15 C20 H20B 109.5 . . C15 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C22 C21 S2 107.0(2) . . C22 C21 C26 113.0(3) . . C25 C21 S2 114.4(2) . . C25 C21 C22 103.8(3) . . C25 C21 C26 114.2(3) . . C26 C21 S2 104.5(2) . . C23 C22 C21 108.7(3) . . C23 C22 C27 129.0(3) . . C27 C22 C21 122.1(3) . . C22 C23 C24 109.2(3) . . C22 C23 C28 127.2(3) . . C24 C23 C28 123.5(3) . . C23 C24 C29 122.5(3) . . C25 C24 C23 109.7(3) . . C25 C24 C29 127.7(3) . . C24 C25 C21 108.5(3) . . C24 C25 C30 128.7(3) . . C30 C25 C21 122.4(3) . . C21 C26 H26A 109.5 . . C21 C26 H26B 109.5 . . C21 C26 H26C 109.5 . . H26A C26 H26B 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C22 C27 H27A 109.5 . . C22 C27 H27B 109.5 . . C22 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C23 C28 H28A 109.5 . . C23 C28 H28B 109.5 . . C23 C28 H28C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C24 C29 H29A 109.5 . . C24 C29 H29B 109.5 . . C24 C29 H29C 109.5 . . H29A C29 H29B 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C25 C30 H30A 109.5 . . C25 C30 H30B 109.5 . . C25 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C32 C31 H31 122.9 . . C33 C31 H31 122.9 2_667 . C33 C31 C32 114.1(11) 2_667 . C31 C32 C33 126.2(11) . . C34 C32 C31 118.7(11) . . C34 C32 C33 114.9(7) . . C31 C33 C32 119.7(7) 2_667 . C31 C33 H33 120.2 2_667 . C32 C33 H33 120.2 . . C32 C34 H34A 109.5 . . C32 C34 H34B 109.5 . . C32 C34 H34C 109.5 . . H34A C34 H34B 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sm1 Sm1 3.8981(3) 2_756 Sm1 S2 3.2142(7) 2_756 Sm1 O1 2.331(2) . Sm1 O2 2.314(2) . Sm1 O3 2.387(2) . Sm1 O4 2.342(2) . Sm1 C1 2.662(3) . Sm1 C2 2.645(3) . Sm1 C3 2.681(3) . Sm1 C4 2.713(3) . Sm1 C5 2.696(3) . S1 O1 1.520(2) . S1 O2 1.529(2) 2_756 S1 C11 1.867(3) . S2 Sm1 3.2142(7) 2_756 S2 O3 1.536(2) . S2 O4 1.521(2) 2_756 S2 C21 1.867(3) . O2 S1 1.529(2) 2_756 O4 S2 1.521(2) 2_756 C1 C2 1.416(4) . C1 C5 1.422(4) . C1 C6 1.501(4) . C2 C3 1.422(4) . C2 C7 1.502(4) . C3 C4 1.421(4) . C3 C8 1.503(4) . C4 C5 1.419(4) . C4 C9 1.509(4) . C5 C10 1.501(4) . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 C12 1.512(4) . C11 C15 1.503(4) . C11 C16 1.530(4) . C12 C13 1.345(5) . C12 C17 1.494(5) . C13 C14 1.474(5) . C13 C18 1.494(5) . C14 C15 1.346(5) . C14 C19 1.500(5) . C15 C20 1.491(5) . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C21 C22 1.512(4) . C21 C25 1.507(4) . C21 C26 1.528(4) . C22 C23 1.340(5) . C22 C27 1.496(4) . C23 C24 1.482(4) . C23 C28 1.496(5) . C24 C25 1.341(5) . C24 C29 1.498(5) . C25 C30 1.496(4) . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31 0.9500 . C31 C32 1.344(8) . C31 C33 1.328(17) 2_667 C32 C33 1.372(12) . C32 C34 1.209(15) . C33 C31 1.328(17) 2_667 C33 H33 0.9500 . C34 H34A 0.9800 . C34 H34B 0.9800 . C34 H34C 0.9800 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Sm1 S2 O3 Sm1 87.1(3) 2_756 . Sm1 S2 C21 C22 147.71(16) 2_756 . Sm1 S2 C21 C25 33.3(3) 2_756 . Sm1 S2 C21 C26 -92.2(2) 2_756 . Sm1 C1 C2 C3 -69.4(2) . . Sm1 C1 C2 C7 111.6(3) . . Sm1 C1 C5 C4 68.2(2) . . Sm1 C1 C5 C10 -114.3(3) . . Sm1 C2 C3 C4 -68.8(2) . . Sm1 C2 C3 C8 114.2(3) . . Sm1 C3 C4 C5 -66.5(2) . . Sm1 C3 C4 C9 116.3(3) . . Sm1 C4 C5 C1 -66.7(2) . . Sm1 C4 C5 C10 115.8(3) . . S1 C11 C12 C13 -115.0(2) . . S1 C11 C12 C17 64.5(3) . . S1 C11 C15 C14 110.7(3) . . S1 C11 C15 C20 -71.3(3) . . S2 C21 C22 C23 -120.5(2) . . S2 C21 C22 C27 62.7(3) . . S2 C21 C25 C24 115.0(3) . . S2 C21 C25 C30 -72.0(3) . . O1 S1 C11 C12 59.0(2) . . O1 S1 C11 C15 -53.3(2) . . O1 S1 C11 C16 -179.1(2) . . O2 S1 O1 Sm1 64.2(2) 2_756 . O2 S1 C11 C12 171.34(19) 2_756 . O2 S1 C11 C15 59.0(2) 2_756 . O2 S1 C11 C16 -66.8(2) 2_756 . O3 S2 C21 C22 74.8(2) . . O3 S2 C21 C25 -39.6(3) . . O3 S2 C21 C26 -165.1(2) . . O4 S2 O3 Sm1 106.8(3) 2_756 . O4 S2 C21 C22 -175.7(2) 2_756 . O4 S2 C21 C25 69.9(2) 2_756 . O4 S2 C21 C26 -55.6(2) 2_756 . C1 C2 C3 Sm1 68.8(2) . . C1 C2 C3 C4 0.0(3) . . C1 C2 C3 C8 -177.0(3) . . C2 C1 C5 Sm1 -67.5(2) . . C2 C1 C5 C4 0.7(3) . . C2 C1 C5 C10 178.2(3) . . C2 C3 C4 Sm1 66.9(2) . . C2 C3 C4 C5 0.4(3) . . C2 C3 C4 C9 -176.8(3) . . C3 C4 C5 Sm1 66.1(2) . . C3 C4 C5 C1 -0.6(3) . . C3 C4 C5 C10 -178.2(3) . . C5 C1 C2 Sm1 68.9(2) . . C5 C1 C2 C3 -0.4(3) . . C5 C1 C2 C7 -179.5(3) . . C6 C1 C2 Sm1 -110.5(3) . . C6 C1 C2 C3 -179.9(3) . . C6 C1 C2 C7 1.1(5) . . C6 C1 C5 Sm1 112.0(3) . . C6 C1 C5 C4 -179.9(3) . . C6 C1 C5 C10 -2.3(5) . . C7 C2 C3 Sm1 -112.1(3) . . C7 C2 C3 C4 179.1(3) . . C7 C2 C3 C8 2.1(5) . . C8 C3 C4 Sm1 -116.2(3) . . C8 C3 C4 C5 177.3(3) . . C8 C3 C4 C9 0.1(5) . . C9 C4 C5 Sm1 -116.7(3) . . C9 C4 C5 C1 176.6(3) . . C9 C4 C5 C10 -0.9(5) . . C11 S1 O1 Sm1 171.65(17) . . C11 C12 C13 C14 -1.2(3) . . C11 C12 C13 C18 -179.6(3) . . C12 C11 C15 C14 -2.9(3) . . C12 C11 C15 C20 175.1(3) . . C12 C13 C14 C15 -0.8(4) . . C12 C13 C14 C19 180.0(3) . . C13 C14 C15 C11 2.4(3) . . C13 C14 C15 C20 -175.5(3) . . C15 C11 C12 C13 2.5(3) . . C15 C11 C12 C17 -178.1(3) . . C16 C11 C12 C13 130.1(3) . . C16 C11 C12 C17 -50.4(4) . . C16 C11 C15 C14 -130.1(3) . . C16 C11 C15 C20 47.9(4) . . C17 C12 C13 C14 179.4(3) . . C17 C12 C13 C18 1.0(6) . . C18 C13 C14 C15 177.7(3) . . C18 C13 C14 C19 -1.5(5) . . C19 C14 C15 C11 -178.5(3) . . C19 C14 C15 C20 3.7(5) . . C21 S2 O3 Sm1 -146.1(3) . . C21 C22 C23 C24 0.0(3) . . C21 C22 C23 C28 -176.3(3) . . C22 C21 C25 C24 -1.3(3) . . C22 C21 C25 C30 171.8(3) . . C22 C23 C24 C25 -0.9(3) . . C22 C23 C24 C29 -177.8(3) . . C23 C24 C25 C21 1.3(3) . . C23 C24 C25 C30 -171.2(3) . . C25 C21 C22 C23 0.8(3) . . C25 C21 C22 C27 -176.0(3) . . C26 C21 C22 C23 125.0(3) . . C26 C21 C22 C27 -51.8(4) . . C26 C21 C25 C24 -124.8(3) . . C26 C21 C25 C30 48.3(4) . . C27 C22 C23 C24 176.5(3) . . C27 C22 C23 C28 0.2(5) . . C28 C23 C24 C25 175.6(3) . . C28 C23 C24 C29 -1.3(5) . . C29 C24 C25 C21 178.0(3) . . C29 C24 C25 C30 5.5(5) . . C31 C32 C33 C31 -0.7(12) . 2_667 C33 C31 C32 C33 0.7(12) 2_667 . C33 C31 C32 C34 175.8(9) 2_667 . C34 C32 C33 C31 -176.0(9) . 2_667