#------------------------------------------------------------------------------ #$Date: 2018-01-25 05:48:15 +0200 (Thu, 25 Jan 2018) $ #$Revision: 205623 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045401.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_7045401 loop_ _publ_author_name 'Akhtar, Muhammad Nadeem' 'Lan, Yanhua' 'AlDamen, Murad A.' 'Zheng, Yan-Zhen' 'Anson, Christopher' 'Powell, Annie K.' _publ_section_title ; Effect of Ligand Substitution on the SMM Properties of Three Isostructural Families of Double-Cubane Mn4Ln2 ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04304J _journal_year 2018 _chemical_formula_moiety 'C59.96 H115.88 Mn4 N4 O26 Sm2, 2(C2 H3 N), C7 H8, H2 O' _chemical_formula_sum 'C71 H132 Mn4 N6 O27 Sm2' _chemical_formula_weight 2022.28 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2018-01-11 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-01-12 deposited with the CCDC. 2018-01-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.614(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 27.1856(10) _cell_length_b 14.5451(5) _cell_length_c 21.9395(8) _cell_measurement_reflns_used 9874 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.96 _cell_measurement_theta_min 2.33 _cell_volume 8666.2(5) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.920 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.920 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 27447 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.920 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.120 _diffrn_reflns_theta_min 1.823 _diffrn_source 'rotating anode' _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_T_max 0.798 _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0540 before and 0.0268 after correction. The Ratio of minimum to maximum transmission is 0.7306. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description block _exptl_crystal_F_000 4160 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.714 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 703 _refine_ls_number_reflns 9738 _refine_ls_number_restraints 445 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+10.3535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.0715 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8227 _reflns_number_total 9738 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04304j2.cif _cod_data_source_block 20-mn4sm2 _cod_database_code 7045401 _shelx_shelxl_version_number 2017/1 _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. ; _shelx_estimated_absorpt_t_max 0.798 _shelx_estimated_absorpt_t_min 0.498 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances C46-C47 1.5 with sigma of 0.02 O5B-H5B = O5A-H5A = O3B-H3B = O3A-H3A 0.88 with sigma of 0.04 H3B-O12 = H5A-O12 = H5B-O12 1.95 with sigma of 0.02 C12-C13A \\sim C12-C13B \\sim C12-C13C \\sim C12-C14A \\sim C12-C14B \\sim C12-C14C \\sim C12-C15A ~ C12-C15B \\sim C12-C15C with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C2A \\sim C13C \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C32A) = Uanis(C32B) 4. Rigid body (RIGU) restrains C41, C42, C43, C44, C45, C46, C47 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N31B, C31B, C32B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N31A, C31A, C32A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C26, C27B, C30B, C29B, C28B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C30A, C27A, C29A, C28A, C26 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C21, C22A, C24A, C24B, C22B, C25B, C25A, C23 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C7, N2B, N2A, Mn2, C9B, C9A, C10B, C10A, O5B, O5A, C2B, C2A, C1B, C1A, N1B, N1A, C3, C5B, C6B, C5A, C6A, O3B, O3A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Same fragment restrains {C21, C22B, C23, C24B, C25B} sigma for 1-2: 0.02, 1-3: 0.04 as {C21, C22A, C23, C24A, C25A} {C26, C27B, C28B, C29B, C30B} sigma for 1-2: 0.02, 1-3: 0.04 as {C26, C27A, C28A, C29A, C30A} {N31B, C31B, C32B} sigma for 1-2: 0.02, 1-3: 0.04 as {N31A, C31A, C32A} 6. Others Fixed Sof: N1A(0.55) C1A(0.55) H1AA(0.55) H1AB(0.55) C2A(0.55) H2AA(0.55) H2AB(0.55) N2A(0.55) N1B(0.45) C1B(0.45) H1BA(0.45) H1BB(0.45) C2B(0.45) H2BA(0.45) H2BB(0.45) N2B(0.45) H3AA(0.55) H3AB(0.55) H3BC(0.45) H3BD(0.45) C5A(0.55) H5AA(0.55) H5AB(0.55) C6A(0.55) H6AA(0.55) H6AB(0.55) O3A(0.55) H3A(0.55) C5B(0.45) H5BA(0.45) H5BB(0.45) C6B(0.45) H6BA(0.45) H6BB(0.45) O3B(0.45) H3B(0.45) H7AA(0.55) H7AB(0.55) H7BC(0.45) H7BD(0.45) C9A(0.55) H9AA(0.55) H9AB(0.55) C10A(0.55) H10A(0.55) H10B(0.55) O5A(0.55) H5A(0.55) C9B(0.45) H9BA(0.45) H9BB(0.45) C10B(0.45) H10C(0.45) H10D(0.45) O5B(0.45) H5B(0.45) C13A(0.47) H13A(0.47) H13B(0.47) H13C(0.47) C14A(0.47) H14A(0.47) H14B(0.47) H14C(0.47) C15A(0.47) H15A(0.47) H15B(0.47) H15C(0.47) C14B(0.29) H14D(0.29) H14E(0.29) H14F(0.29) C13B(0.29) H13D(0.29) H13E(0.29) H13F(0.29) C15B(0.29) H15D(0.29) H15E(0.29) H15F(0.29) C13C(0.24) H13G(0.24) H13H(0.24) H13I(0.24) C14C(0.24) H14G(0.24) H14H(0.24) H14I(0.24) C15C(0.24) H15G(0.24) H15H(0.24) H15I(0.24) C22A(0.5) H23A(0.45) H23B(0.45) H23C(0.45) H23D(0.55) H23E(0.55) H23F(0.55) C24A(0.45) H24A(0.45) H24B(0.45) H24C(0.45) C25A(0.45) H25A(0.45) H25B(0.45) H25C(0.45) C22B(0.5) C24B(0.54) H24D(0.54) H24E(0.54) H24F(0.54) C25B(0.54) H25D(0.54) H25E(0.54) H25F(0.54) C27A(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C27B(0.5) C28B(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C29B(0.5) H29D(0.5) H29E(0.5) H29F(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5) N31A(0.5) C31A(0.5) C32A(0.5) H32A(0.5) H32B(0.5) H32C(0.5) N31B(0.5) C31B(0.5) C32B(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5) C46(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) O51B(0.5) 7.a Secondary CH2 refined with riding coordinates: C1A(H1AA,H1AB), C2A(H2AA,H2AB), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9A(H9AA,H9AB), C10A(H10A,H10B), C9B(H9BA,H9BB), C10B(H10C,H10D) 7.b Me refined with riding coordinates: C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D, H14E,H14F), C13B(H13D,H13E,H13F), C15B(H15D,H15E,H15F), C13C(H13G,H13H,H13I), C14C(H14G,H14H,H14I), C15C(H15G,H15H,H15I), C18(H18A,H18B,H18C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C23(H23D,H23E,H23F), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C24B(H24D,H24E,H24F), C25B(H25D, H25E,H25F), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F) 7.c Aromatic/amide H refined with riding coordinates: C41(H41), C42(H42), C43(H43), C44(H44), C45(H45) 7.d Fitted hexagon refined as free rotating group: C41(C42,C43,C44,C45,C46) 7.e Idealised Me refined as rotating group: C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C47(H47A,H47B,H47C) ; _shelx_res_file ; TITL p417r in C2/c p417r.res created by SHELXL-2017/1 at 11:49:48 on 11-Jan-2018 CELL 0.71073 27.1856 14.5451 21.9395 90 92.614 90 ZERR 4 0.001 0.0005 0.0008 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Mn Sm UNIT 284 528 24 108 16 8 DFIX 1.5 C46 C47 DFIX 0.88 0.04 O5B H5B O5A H5A O3B H3B O3A H3A DFIX 1.95 H3B O12 H5A O12 H5B O12 SADI C12 C13A C12 C13B C12 C13C C12 C14A C12 C14B C12 C14C C12 C15A C12 = C15B C12 C15C SIMU C2A C13C C15A RIGU C41 > C47 RIGU N31B C31B C32B RIGU N31A C31A C32A RIGU C26 C27B C30B C29B C28B RIGU C30A C27A C29A C28A C26 RIGU C21 C22A C24A C24B C22B C25B C25A C23 RIGU C7 N2B N2A Mn2 C9B C9A C10B C10A O5B O5A C2B C2A C1B C1A N1B N1A C3 = C5B C6B C5A C6A O3B O3A EADP C32A C32B L.S. 16 PLAN 20 SIZE 0.41 0.22 0.12 TEMP -173 HTAB O3A O12 HTAB O3B O12 HTAB O5A O12 HTAB O5B O12 HTAB OMIT-26 10 11 BOND $H fmap 2 acta OMIT 1 1 0 OMIT 0 1 2 OMIT 1 1 2 OMIT 2 0 0 OMIT 2 18 0 REM REM REM WGHT 0.031400 10.353500 FVAR 0.09681 SM1 6 0.180078 0.262757 0.605985 11.00000 0.01538 0.02187 = 0.01106 -0.00206 0.00079 -0.00124 MN1 5 0.254654 0.349023 0.499380 11.00000 0.01665 0.01298 = 0.01546 -0.00018 0.00283 -0.00033 MN2 5 0.180977 0.259516 0.400660 11.00000 0.01563 0.04379 = 0.01355 0.00385 -0.00228 -0.00148 O1 4 0.204512 0.257333 0.502320 11.00000 0.01382 0.01456 = 0.01318 0.00103 -0.00082 0.00058 PART 1 N1A 3 0.158951 0.377083 0.326957 10.55000 0.01984 0.02726 = 0.01559 -0.00125 -0.00183 0.00201 C1A 1 0.131938 0.332540 0.274766 10.55000 0.02839 0.02896 = 0.01871 0.00087 -0.00926 0.00295 AFIX 23 H1AA 2 0.132583 0.373508 0.238776 10.55000 -1.20000 H1AB 2 0.097116 0.323985 0.284882 10.55000 -1.20000 AFIX 0 C2A 1 0.153657 0.240125 0.258714 10.55000 0.03724 0.03037 = 0.01495 -0.00345 -0.00858 0.00395 AFIX 23 H2AA 2 0.132497 0.210935 0.226282 10.55000 -1.20000 H2AB 2 0.186624 0.249725 0.242399 10.55000 -1.20000 AFIX 0 N2A 3 0.158207 0.177265 0.312141 10.55000 0.01614 0.02421 = 0.01679 -0.00052 -0.00252 -0.00114 PART 0 PART 2 N1B 3 0.169151 0.339540 0.307596 10.45000 0.01975 0.03095 = 0.01904 0.00266 -0.00321 0.00096 C1B 1 0.160803 0.275550 0.255738 10.45000 0.03219 0.03969 = 0.01659 0.00288 -0.00878 0.00266 AFIX 23 H1BA 2 0.193082 0.255261 0.241477 10.45000 -1.20000 H1BB 2 0.143522 0.308804 0.221707 10.45000 -1.20000 AFIX 0 C2B 1 0.131057 0.191986 0.271278 10.45000 0.02979 0.03612 = 0.01734 0.00045 -0.00512 0.00320 AFIX 23 H2BA 2 0.096858 0.211135 0.278449 10.45000 -1.20000 H2BB 2 0.129988 0.149289 0.236101 10.45000 -1.20000 AFIX 0 N2B 3 0.151362 0.143289 0.325667 10.45000 0.01824 0.02761 = 0.01394 -0.00166 -0.00091 -0.00303 PART 0 C3 1 0.210349 0.405760 0.306018 11.00000 0.03272 0.04909 = 0.03148 0.02392 -0.01426 -0.01492 PART 1 AFIX 23 H3AA 2 0.225193 0.355692 0.282427 10.55000 -1.20000 H3AB 2 0.207868 0.461486 0.280151 10.55000 -1.20000 AFIX 23 PART 0 PART 2 H3BC 2 0.196600 0.465140 0.291213 10.45000 -1.20000 H3BD 2 0.232953 0.383846 0.275011 10.45000 -1.20000 AFIX 0 PART 0 C4 1 0.241124 0.424904 0.364185 11.00000 0.02190 0.03006 = 0.02276 0.01261 0.00033 -0.00064 AFIX 23 H4A 2 0.273698 0.449242 0.353776 11.00000 -1.20000 H4B 2 0.224583 0.471909 0.388664 11.00000 -1.20000 AFIX 0 O2 4 0.247504 0.342336 0.399134 11.00000 0.01904 0.02455 = 0.01536 0.00733 -0.00043 0.00113 PART 1 C5A 1 0.127162 0.450003 0.350820 10.55000 0.02213 AFIX 23 H5AA 2 0.106350 0.476314 0.316959 10.55000 -1.20000 H5AB 2 0.147924 0.499910 0.368755 10.55000 -1.20000 AFIX 0 C6A 1 0.094819 0.411569 0.398720 10.55000 0.02056 0.03011 = 0.02007 0.00337 -0.00156 0.00632 AFIX 23 H6AA 2 0.073782 0.460280 0.415286 10.55000 -1.20000 H6AB 2 0.073483 0.361909 0.381554 10.55000 -1.20000 AFIX 0 O3A 4 0.128499 0.376541 0.445086 10.55000 0.02470 0.02821 = 0.01281 0.00711 -0.00384 0.00514 H3A 2 0.112190 0.355167 0.474327 10.55000 -1.20000 PART 0 PART 2 C5B 1 0.124714 0.395471 0.314330 10.45000 0.02948 0.03050 = 0.03077 0.00505 -0.00201 0.00966 AFIX 23 H5BA 2 0.095566 0.358694 0.300850 10.45000 -1.20000 H5BB 2 0.126236 0.449490 0.287028 10.45000 -1.20000 AFIX 0 C6B 1 0.117986 0.428280 0.377798 10.45000 0.03029 0.03769 = 0.02901 0.00200 0.00344 0.01073 AFIX 23 H6BA 2 0.144030 0.472972 0.390179 10.45000 -1.20000 H6BB 2 0.085527 0.458419 0.380715 10.45000 -1.20000 AFIX 0 O3B 4 0.121055 0.348859 0.415799 10.45000 0.03316 0.04714 = 0.01954 0.00435 0.00314 0.01273 H3B 2 0.114615 0.325623 0.453106 10.45000 -1.20000 PART 0 C7 1 0.197373 0.101262 0.307474 11.00000 0.02232 0.04771 = 0.02238 -0.01785 -0.00390 0.00546 PART 1 AFIX 23 H7AA 2 0.180957 0.045267 0.290889 10.55000 -1.20000 H7AB 2 0.221450 0.121211 0.277641 10.55000 -1.20000 AFIX 23 PART 0 PART 2 H7BC 2 0.216563 0.145261 0.283638 10.45000 -1.20000 H7BD 2 0.190550 0.045859 0.282274 10.45000 -1.20000 AFIX 0 PART 0 C8 1 0.225458 0.075780 0.366470 11.00000 0.02231 0.03199 = 0.02132 -0.00968 0.00168 -0.00554 AFIX 23 H8A 2 0.204693 0.035787 0.391229 11.00000 -1.20000 H8B 2 0.255476 0.040992 0.357049 11.00000 -1.20000 AFIX 0 O4 4 0.238928 0.156210 0.400487 11.00000 0.01945 0.02583 = 0.01496 -0.00627 -0.00019 -0.00305 PART 1 C9A 1 0.110344 0.132935 0.322425 10.55000 0.02235 0.03756 = 0.03007 -0.01019 -0.00212 -0.01018 AFIX 23 H9AA 2 0.083714 0.173466 0.305834 10.55000 -1.20000 H9AB 2 0.108523 0.074668 0.299108 10.55000 -1.20000 AFIX 0 C10A 1 0.101172 0.112734 0.386936 10.55000 0.03605 0.03871 = 0.02402 -0.00432 -0.00133 -0.01498 AFIX 23 H10A 2 0.066264 0.095340 0.390977 10.55000 -1.20000 H10B 2 0.122076 0.060735 0.401468 10.55000 -1.20000 AFIX 0 O5A 4 0.112346 0.192403 0.422473 10.55000 0.02974 0.03291 = 0.02468 -0.00677 0.00452 -0.00851 H5A 2 0.109858 0.197033 0.462315 10.55000 -1.20000 PART 0 PART 2 C9B 1 0.113493 0.082788 0.350584 10.45000 0.02204 0.03237 = 0.01330 -0.00241 -0.00107 -0.00505 AFIX 23 H9BA 2 0.129473 0.030108 0.372108 10.45000 -1.20000 H9BB 2 0.091737 0.058477 0.316933 10.45000 -1.20000 AFIX 0 C10B 1 0.082764 0.138427 0.395423 10.45000 0.00802 0.05556 = 0.02427 -0.02114 0.00183 -0.00063 AFIX 23 H10C 2 0.068742 0.194604 0.375980 10.45000 -1.20000 H10D 2 0.055820 0.100917 0.411377 10.45000 -1.20000 AFIX 0 O5B 4 0.119330 0.160485 0.442672 10.45000 0.02238 H5B 2 0.099426 0.184874 0.467716 10.45000 -1.20000 PART 0 O6 4 0.211463 0.457829 0.504119 11.00000 0.04145 0.01841 = 0.03635 0.00622 0.02220 0.00915 O7 4 0.163602 0.422217 0.580526 11.00000 0.01854 0.03134 = 0.01785 0.00267 0.00121 0.00273 C11 1 0.180920 0.477578 0.544081 11.00000 0.01939 0.02269 = 0.01710 -0.00278 -0.00268 0.00163 C12 1 0.166202 0.579754 0.547170 11.00000 0.04180 0.02612 = 0.02766 -0.00572 -0.00132 0.01614 PART 1 C13A 1 0.131921 0.606019 0.492564 10.47000 0.03205 AFIX 33 H13A 2 0.146178 0.584942 0.454787 10.47000 -1.50000 H13B 2 0.099728 0.576950 0.496735 10.47000 -1.50000 H13C 2 0.127932 0.672962 0.491245 10.47000 -1.50000 AFIX 0 C14A 1 0.149425 0.607256 0.607702 10.47000 0.04858 AFIX 33 H14A 2 0.173693 0.587500 0.639429 10.47000 -1.50000 H14B 2 0.145835 0.674252 0.609151 10.47000 -1.50000 H14C 2 0.117631 0.578240 0.614641 10.47000 -1.50000 AFIX 0 C15A 1 0.215001 0.640913 0.533153 10.47000 0.02601 AFIX 33 H15A 2 0.226858 0.623914 0.493168 10.47000 -1.50000 H15B 2 0.206451 0.706367 0.533179 10.47000 -1.50000 H15C 2 0.240888 0.629050 0.564725 10.47000 -1.50000 AFIX 0 PART 0 PART 2 C14B 1 0.113333 0.577528 0.579581 10.29000 0.04283 AFIX 33 H14D 2 0.089364 0.543299 0.553731 10.29000 -1.50000 H14E 2 0.117342 0.547401 0.619452 10.29000 -1.50000 H14F 2 0.101558 0.640550 0.585014 10.29000 -1.50000 AFIX 0 C13B 1 0.154219 0.616977 0.484324 10.29000 0.03097 AFIX 33 H13D 2 0.131150 0.575437 0.462493 10.29000 -1.50000 H13E 2 0.139191 0.677925 0.487543 10.29000 -1.50000 H13F 2 0.184504 0.621838 0.461962 10.29000 -1.50000 AFIX 0 C15B 1 0.200255 0.631538 0.587744 10.29000 0.05095 AFIX 33 H15D 2 0.204562 0.599307 0.626849 10.29000 -1.50000 H15E 2 0.232159 0.636950 0.568986 10.29000 -1.50000 H15F 2 0.186846 0.693037 0.594568 10.29000 -1.50000 AFIX 0 PART 0 PART 3 C13C 1 0.205418 0.638873 0.516954 10.24000 0.09258 AFIX 33 H13G 2 0.237568 0.628701 0.537904 10.24000 -1.50000 H13H 2 0.207084 0.621506 0.473939 10.24000 -1.50000 H13I 2 0.196514 0.703968 0.519826 10.24000 -1.50000 AFIX 0 C14C 1 0.116288 0.590302 0.518734 10.24000 0.04605 AFIX 33 H14G 2 0.116383 0.571189 0.475907 10.24000 -1.50000 H14H 2 0.093171 0.551896 0.540409 10.24000 -1.50000 H14I 2 0.106157 0.654826 0.521000 10.24000 -1.50000 AFIX 0 C15C 1 0.169213 0.608487 0.614847 10.24000 0.02903 AFIX 33 H15G 2 0.202989 0.600193 0.631491 10.24000 -1.50000 H15H 2 0.159776 0.673234 0.618339 10.24000 -1.50000 H15I 2 0.146791 0.570304 0.637748 10.24000 -1.50000 AFIX 0 PART 0 O8 4 0.308017 0.441500 0.494677 11.00000 0.03435 0.02151 = 0.02851 -0.00645 0.01560 -0.00931 O9 4 0.352037 0.388222 0.419069 11.00000 0.01968 0.02884 = 0.02017 -0.00721 0.00186 -0.00396 C16 1 0.341817 0.448140 0.457057 11.00000 0.01870 0.02059 = 0.01639 0.00259 -0.00207 0.00092 C17 1 0.371142 0.538421 0.457078 11.00000 0.02671 0.01902 = 0.02970 0.00130 0.00803 -0.00398 C18 1 0.359396 0.600535 0.510293 11.00000 0.04303 0.02416 = 0.04248 -0.00852 0.01051 -0.01167 AFIX 33 H18A 2 0.378885 0.657064 0.508428 11.00000 -1.50000 H18B 2 0.324268 0.615942 0.507933 11.00000 -1.50000 H18C 2 0.367471 0.568605 0.548792 11.00000 -1.50000 AFIX 0 C19 1 0.426542 0.515796 0.459860 11.00000 0.02423 0.03454 = 0.05364 0.00303 0.00354 -0.00704 AFIX 33 H19A 2 0.434026 0.475793 0.425554 11.00000 -1.50000 H19B 2 0.445526 0.572856 0.457465 11.00000 -1.50000 H19C 2 0.435326 0.484340 0.498332 11.00000 -1.50000 AFIX 0 C20 1 0.356885 0.587830 0.396929 11.00000 0.05175 0.02862 = 0.04034 0.01166 0.00600 -0.00547 AFIX 33 H20A 2 0.364377 0.548108 0.362485 11.00000 -1.50000 H20B 2 0.321575 0.601706 0.395435 11.00000 -1.50000 H20C 2 0.375612 0.645185 0.394509 11.00000 -1.50000 AFIX 0 O10 4 0.189587 0.333382 0.709206 11.00000 0.03438 0.02603 = 0.01667 -0.00202 -0.00123 -0.00077 O11 4 0.178303 0.183623 0.706263 11.00000 0.04631 0.02658 = 0.01711 -0.00040 0.00512 -0.01056 SAME 0.02 0.04 C21 C22B C23 C24B C25B C21 1 0.182165 0.257703 0.735664 11.00000 0.01984 0.03206 = 0.01384 -0.00261 0.00148 -0.00690 PART 1 C22A 1 0.173242 0.267958 0.804323 10.50000 0.04511 0.03506 = 0.01131 -0.00262 0.00666 -0.01592 PART 0 C23 1 0.218880 0.313972 0.835482 11.00000 0.05225 0.05166 = 0.01663 -0.00472 0.00346 -0.02043 PART 1 AFIX 33 H23A 2 0.223205 0.375450 0.818252 10.45000 -1.50000 H23B 2 0.214317 0.319049 0.879406 10.45000 -1.50000 H23C 2 0.248125 0.276662 0.828594 10.45000 -1.50000 AFIX 33 PART 0 PART 2 H23D 2 0.212884 0.376169 0.819656 10.55000 -1.50000 H23E 2 0.215741 0.313799 0.879804 10.55000 -1.50000 H23F 2 0.252159 0.294378 0.825980 10.55000 -1.50000 AFIX 0 PART 0 PART 1 C24A 1 0.125727 0.324022 0.810633 10.45000 0.05473 0.04075 = 0.02564 -0.00781 0.02251 -0.00704 AFIX 33 H24A 2 0.129687 0.384878 0.792323 10.45000 -1.50000 H24B 2 0.098131 0.291967 0.789661 10.45000 -1.50000 H24C 2 0.119109 0.330918 0.853931 10.45000 -1.50000 AFIX 0 C25A 1 0.168045 0.173374 0.832346 10.45000 0.06242 0.04526 = 0.01697 0.00235 0.00280 -0.01768 AFIX 33 H25A 2 0.198560 0.138614 0.827955 10.45000 -1.50000 H25B 2 0.161596 0.179660 0.875732 10.45000 -1.50000 H25C 2 0.140618 0.140709 0.811463 10.45000 -1.50000 AFIX 0 PART 0 PART 2 C22B 1 0.180841 0.247124 0.805561 10.50000 0.03055 0.03640 = 0.01518 -0.00600 0.00507 -0.00350 C24B 1 0.129555 0.282527 0.822664 10.54000 0.03550 0.03628 = 0.03239 -0.00456 0.01465 -0.00768 AFIX 33 H24D 2 0.125223 0.346047 0.808524 10.54000 -1.50000 H24E 2 0.103908 0.243657 0.803233 10.54000 -1.50000 H24F 2 0.127074 0.280283 0.867062 10.54000 -1.50000 AFIX 0 C25B 1 0.187414 0.148829 0.827510 10.54000 0.03576 0.04030 = 0.01290 0.00328 0.00393 -0.00955 AFIX 33 H25D 2 0.186208 0.147013 0.872069 10.54000 -1.50000 H25E 2 0.160970 0.110508 0.809331 10.54000 -1.50000 H25F 2 0.219312 0.125449 0.815312 10.54000 -1.50000 AFIX 0 PART 0 O12 4 0.100824 0.275959 0.533957 11.00000 0.02121 0.05763 = 0.02128 -0.01006 -0.00080 0.00548 O13 4 0.091594 0.281530 0.632859 11.00000 0.02018 0.05909 = 0.02278 -0.00655 0.00336 0.00166 SAME 0.02 0.04 C26 C27B > C30B C26 1 0.073739 0.285573 0.579217 11.00000 0.01977 0.06858 = 0.02732 -0.01259 -0.00045 0.00564 PART 1 C27A 1 0.016641 0.281559 0.568647 10.50000 0.01645 0.04933 = 0.03820 -0.00731 0.00258 0.00209 C28A 1 0.001916 0.375721 0.592713 10.50000 0.03303 0.04964 = 0.13372 -0.01773 -0.01590 0.01486 AFIX 33 H28A 2 0.011515 0.380163 0.636214 10.50000 -1.50000 H28B 2 0.018601 0.423939 0.570271 10.50000 -1.50000 H28C 2 -0.033813 0.383463 0.587092 10.50000 -1.50000 AFIX 0 C29A 1 0.003216 0.269033 0.502127 10.50000 0.01692 0.24277 = 0.05423 -0.03105 -0.01246 0.01919 AFIX 33 H29A 2 0.019876 0.315880 0.478463 10.50000 -1.50000 H29B 2 0.013501 0.207776 0.489147 10.50000 -1.50000 H29C 2 -0.032504 0.275255 0.495288 10.50000 -1.50000 AFIX 0 C30A 1 -0.009642 0.208179 0.604186 10.50000 0.01624 0.05635 = 0.10516 0.00611 0.00159 -0.00492 AFIX 33 H30A 2 -0.001274 0.215340 0.647849 10.50000 -1.50000 H30B 2 -0.045306 0.214673 0.596886 10.50000 -1.50000 H30C 2 0.000700 0.147194 0.590745 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C27B 1 0.020480 0.324870 0.565509 10.50000 0.01266 0.04460 = 0.04904 -0.01453 0.00037 -0.00038 C28B 1 -0.005320 0.339611 0.625179 10.50000 0.03165 0.07862 = 0.08103 0.00268 0.02739 0.00923 AFIX 33 H28D 2 0.011709 0.387989 0.648993 10.50000 -1.50000 H28E 2 -0.039556 0.358000 0.616121 10.50000 -1.50000 H28F 2 -0.004659 0.282297 0.648686 10.50000 -1.50000 AFIX 0 C29B 1 -0.004140 0.250383 0.526136 10.50000 0.01792 0.06808 = 0.15070 -0.05974 -0.01458 -0.00415 AFIX 33 H29D 2 -0.003859 0.192281 0.548766 10.50000 -1.50000 H29E 2 -0.038234 0.268178 0.515544 10.50000 -1.50000 H29F 2 0.013815 0.242715 0.488739 10.50000 -1.50000 AFIX 0 C30B 1 0.019487 0.414113 0.529214 10.50000 0.02753 0.06517 = 0.07229 0.00577 0.00341 0.01771 AFIX 33 H30D 2 0.035215 0.463022 0.553870 10.50000 -1.50000 H30E 2 0.037327 0.405651 0.491802 10.50000 -1.50000 H30F 2 -0.014721 0.431114 0.518607 10.50000 -1.50000 AFIX 0 SAME 0.02 0.04 N31B > C32B PART 0 PART 1 N31A 3 0.007774 -0.029845 0.683204 10.50000 0.05910 0.08786 = 0.06334 0.00602 -0.01107 -0.03571 C31A 1 0.038660 0.019623 0.696150 10.50000 0.03800 0.06037 = 0.03060 0.00885 0.00023 -0.01222 C32A 1 0.076771 0.088859 0.717357 10.50000 0.09638 0.09359 = 0.00819 0.00364 -0.00708 -0.06074 AFIX 137 H32A 2 0.097889 0.103688 0.683690 10.50000 -1.50000 H32B 2 0.096883 0.063166 0.751437 10.50000 -1.50000 H32C 2 0.060383 0.144857 0.730767 10.50000 -1.50000 AFIX 0 PART 0 PART 2 N31B 3 -0.022707 0.057196 0.654812 10.50000 0.09322 0.14260 = 0.07418 -0.04851 0.02284 -0.06502 C31B 1 0.014755 0.079645 0.677440 10.50000 0.07584 0.08733 = 0.04602 -0.01651 0.02465 -0.04329 C32B 1 0.066362 0.102524 0.702057 10.50000 0.09638 0.09359 = 0.00819 0.00364 -0.00708 -0.06074 AFIX 137 H32D 2 0.068737 0.091381 0.746146 10.50000 -1.50000 H32E 2 0.073476 0.167322 0.693959 10.50000 -1.50000 H32F 2 0.090210 0.063647 0.681968 10.50000 -1.50000 AFIX 66 PART 0 PART -1 C41 1 -0.003127 0.247991 0.266783 10.50000 0.03401 0.09374 = 0.10168 -0.01590 -0.03552 0.02886 AFIX 43 H41 2 -0.004232 0.182873 0.269784 10.50000 -1.20000 AFIX 65 C42 1 -0.016794 0.302019 0.315455 10.50000 0.03818 0.10421 = 0.08203 -0.00086 -0.03860 0.01514 AFIX 43 H42 2 -0.027240 0.273827 0.351722 10.50000 -1.20000 AFIX 65 C43 1 -0.015178 0.397296 0.311063 10.50000 0.04854 0.10236 = 0.07447 -0.03538 -0.03928 0.02515 AFIX 43 H43 2 -0.024519 0.434222 0.344329 10.50000 -1.20000 AFIX 65 C44 1 0.000106 0.438546 0.257999 10.50000 0.03621 0.09298 = 0.08382 -0.02536 -0.03364 0.02580 AFIX 43 H44 2 0.001210 0.503663 0.254998 10.50000 -1.20000 AFIX 65 C45 1 0.013773 0.384519 0.209327 10.50000 0.03418 0.11910 = 0.07564 -0.02620 -0.02697 0.02241 AFIX 43 H45 2 0.024218 0.412711 0.173060 10.50000 -1.20000 AFIX 65 C46 1 0.012157 0.289241 0.213717 10.50000 0.03312 0.11396 = 0.07647 -0.04748 -0.03840 0.02731 AFIX 0 C47 1 0.026012 0.234006 0.160130 10.50000 0.05895 0.17006 = 0.11172 -0.07143 -0.02215 0.03449 AFIX 137 H47A 2 -0.001433 0.233394 0.129580 10.50000 -1.50000 H47B 2 0.033565 0.170908 0.173124 10.50000 -1.50000 H47C 2 0.055039 0.261305 0.142359 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O51B 4 0.101084 0.445112 0.709653 10.50000 0.06489 HKLF 4 REM p417r in C2/c REM R1 = 0.0322 for 8227 Fo > 4sig(Fo) and 0.0430 for all 9738 data REM 703 parameters refined using 445 restraints END WGHT 0.0314 10.3604 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, -y+1/2, -z+1 HTAB C3 O11_$1 HTAB C4 O6 HTAB O3A^a O12 EQIV $2 x, -y+1, z-1/2 HTAB C5B^b O51B^b_$2 HTAB O3B^b O12 HTAB C7 O10_$1 HTAB C8 O8_$1 HTAB C8 O7_$1 HTAB O5A^a O12 EQIV $3 -x, -y, -z+1 HTAB C9B^b N31B^b_$3 HTAB O5B^b O12 HTAB C32A^a O11 EQIV $4 -x, y, -z+3/2 HTAB C32B^b N31B^b_$4 HTAB C32B^b O13 REM Highest difference peak 0.714, deepest hole -0.553, 1-sigma level 0.093 Q1 1 0.1890 0.6188 0.6007 11.00000 0.05 0.71 Q2 1 0.1825 0.2605 0.6433 11.00000 0.05 0.71 Q3 1 0.1873 0.2173 0.5803 11.00000 0.05 0.69 Q4 1 0.2100 0.6367 0.5654 11.00000 0.05 0.66 Q5 1 0.1054 0.5643 0.5532 11.00000 0.05 0.65 Q6 1 0.1776 0.2022 0.6286 11.00000 0.05 0.64 Q7 1 0.1253 0.5958 0.5952 11.00000 0.05 0.63 Q8 1 0.1741 0.3187 0.6116 11.00000 0.05 0.61 Q9 1 0.2103 0.2608 0.6127 11.00000 0.05 0.61 Q10 1 0.1492 0.2583 0.5927 11.00000 0.05 0.60 Q11 1 0.1771 0.6256 0.4957 11.00000 0.05 0.60 Q12 1 0.1730 0.2622 0.5661 11.00000 0.05 0.58 Q13 1 0.1386 0.6046 0.4705 11.00000 0.05 0.55 Q14 1 0.1558 0.2264 0.6063 11.00000 0.05 0.52 Q15 1 0.0967 0.3073 0.5114 11.00000 0.05 0.44 Q16 1 0.1814 0.2210 0.3877 11.00000 0.05 0.44 Q17 1 0.0979 0.2435 0.5289 11.00000 0.05 0.43 Q18 1 0.2224 0.6404 0.5187 11.00000 0.05 0.43 Q19 1 0.0261 0.3587 0.1472 11.00000 0.05 0.42 Q20 1 0.2175 0.3207 0.5025 11.00000 0.05 0.41 ; _shelx_res_checksum 78602 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.18008(2) 0.26276(2) 0.60598(2) 0.01610(5) Uani 1 1 d . . . . . Mn1 Mn 0.25465(2) 0.34902(3) 0.49938(2) 0.01497(9) Uani 1 1 d . . . . . Mn2 Mn 0.18098(2) 0.25952(3) 0.40066(2) 0.02441(11) Uani 1 1 d . U . . . O1 O 0.20451(6) 0.25733(11) 0.50232(8) 0.0139(4) Uani 1 1 d . . . . . N1A N 0.15895(19) 0.3771(4) 0.3270(2) 0.0210(10) Uani 0.55 1 d . U P A 1 C1A C 0.1319(2) 0.3325(4) 0.2748(2) 0.0257(11) Uani 0.55 1 d . U P A 1 H1AA H 0.132583 0.373508 0.238776 0.031 Uiso 0.55 1 calc R . P A 1 H1AB H 0.097116 0.323985 0.284882 0.031 Uiso 0.55 1 calc R . P A 1 C2A C 0.1537(4) 0.2401(5) 0.2587(4) 0.0278(17) Uani 0.55 1 d . U P A 1 H2AA H 0.132497 0.210935 0.226282 0.033 Uiso 0.55 1 calc R . P A 1 H2AB H 0.186624 0.249725 0.242399 0.033 Uiso 0.55 1 calc R . P A 1 N2A N 0.1582(2) 0.1773(4) 0.3121(3) 0.0191(12) Uani 0.55 1 d . U P A 1 N1B N 0.1692(2) 0.3395(5) 0.3076(3) 0.0234(13) Uani 0.45 1 d . U P A 2 C1B C 0.1608(5) 0.2756(6) 0.2557(5) 0.030(2) Uani 0.45 1 d . U P A 2 H1BA H 0.193082 0.255261 0.241477 0.036 Uiso 0.45 1 calc R . P A 2 H1BB H 0.143522 0.308804 0.221707 0.036 Uiso 0.45 1 calc R . P A 2 C2B C 0.1311(3) 0.1920(5) 0.2713(3) 0.0279(15) Uani 0.45 1 d . U P A 2 H2BA H 0.096858 0.211135 0.278449 0.034 Uiso 0.45 1 calc R . P A 2 H2BB H 0.129988 0.149289 0.236101 0.034 Uiso 0.45 1 calc R . P A 2 N2B N 0.1514(3) 0.1433(5) 0.3257(3) 0.0200(15) Uani 0.45 1 d . U P A 2 C3 C 0.21035(12) 0.4058(3) 0.30602(15) 0.0382(9) Uani 1 1 d . U . . . H3AA H 0.225193 0.355692 0.282427 0.046 Uiso 0.55 1 calc R . P A 1 H3AB H 0.207868 0.461486 0.280151 0.046 Uiso 0.55 1 calc R . P A 1 H3BC H 0.196600 0.465140 0.291213 0.046 Uiso 0.45 1 calc R . P A 2 H3BD H 0.232953 0.383846 0.275011 0.046 Uiso 0.45 1 calc R . P A 2 C4 C 0.24112(11) 0.4249(2) 0.36419(13) 0.0249(6) Uani 1 1 d . . . . . H4A H 0.273698 0.449242 0.353776 0.030 Uiso 1 1 calc R . . . . H4B H 0.224583 0.471909 0.388664 0.030 Uiso 1 1 calc R . . . . O2 O 0.24750(7) 0.34234(13) 0.39913(8) 0.0197(4) Uani 1 1 d . . . . . C5A C 0.1272(2) 0.4500(4) 0.3508(3) 0.0221(12) Uiso 0.55 1 d . U P A 1 H5AA H 0.106350 0.476314 0.316959 0.027 Uiso 0.55 1 calc R . P A 1 H5AB H 0.147924 0.499910 0.368755 0.027 Uiso 0.55 1 calc R . P A 1 C6A C 0.0948(2) 0.4116(4) 0.3987(3) 0.0237(12) Uani 0.55 1 d . U P A 1 H6AA H 0.073782 0.460280 0.415286 0.028 Uiso 0.55 1 calc R . P A 1 H6AB H 0.073483 0.361909 0.381554 0.028 Uiso 0.55 1 calc R . P A 1 O3A O 0.12850(16) 0.3765(3) 0.4451(2) 0.0220(9) Uani 0.55 1 d D U P A 1 H3A H 0.112(2) 0.355(4) 0.474(2) 0.026 Uiso 0.55 1 d DR . P B 1 C5B C 0.1247(3) 0.3955(5) 0.3143(3) 0.0304(15) Uani 0.45 1 d . U P A 2 H5BA H 0.095566 0.358694 0.300850 0.036 Uiso 0.45 1 calc R . P A 2 H5BB H 0.126236 0.449490 0.287028 0.036 Uiso 0.45 1 calc R . P A 2 C6B C 0.1180(3) 0.4283(6) 0.3778(4) 0.0323(17) Uani 0.45 1 d . U P A 2 H6BA H 0.144030 0.472972 0.390179 0.039 Uiso 0.45 1 calc R . P A 2 H6BB H 0.085527 0.458419 0.380715 0.039 Uiso 0.45 1 calc R . P A 2 O3B O 0.1211(2) 0.3489(4) 0.4158(3) 0.0332(13) Uani 0.45 1 d D U P A 2 H3B H 0.115(3) 0.326(6) 0.453(2) 0.040 Uiso 0.45 1 d DR . P C 2 C7 C 0.19737(11) 0.1013(2) 0.30747(14) 0.0309(7) Uani 1 1 d . U . . . H7AA H 0.180957 0.045267 0.290889 0.037 Uiso 0.55 1 calc R . P A 1 H7AB H 0.221450 0.121211 0.277641 0.037 Uiso 0.55 1 calc R . P A 1 H7BC H 0.216563 0.145261 0.283638 0.037 Uiso 0.45 1 calc R . P A 2 H7BD H 0.190550 0.045859 0.282274 0.037 Uiso 0.45 1 calc R . P A 2 C8 C 0.22546(11) 0.0758(2) 0.36647(13) 0.0252(7) Uani 1 1 d . . . . . H8A H 0.204693 0.035787 0.391229 0.030 Uiso 1 1 calc R . . . . H8B H 0.255476 0.040992 0.357049 0.030 Uiso 1 1 calc R . . . . O4 O 0.23893(7) 0.15621(13) 0.40049(8) 0.0201(4) Uani 1 1 d . . . . . C9A C 0.1103(2) 0.1329(5) 0.3224(3) 0.0301(13) Uani 0.55 1 d . U P A 1 H9AA H 0.083714 0.173466 0.305834 0.036 Uiso 0.55 1 calc R . P A 1 H9AB H 0.108523 0.074668 0.299108 0.036 Uiso 0.55 1 calc R . P A 1 C10A C 0.1012(3) 0.1127(5) 0.3869(3) 0.0330(16) Uani 0.55 1 d . U P A 1 H10A H 0.066264 0.095340 0.390977 0.040 Uiso 0.55 1 calc R . P A 1 H10B H 0.122076 0.060735 0.401468 0.040 Uiso 0.55 1 calc R . P A 1 O5A O 0.11235(16) 0.1924(3) 0.4225(2) 0.0290(9) Uani 0.55 1 d D U P A 1 H5A H 0.110(3) 0.197(4) 0.4623(18) 0.035 Uiso 0.55 1 d DR . P D 1 C9B C 0.1135(2) 0.0828(5) 0.3506(3) 0.0226(13) Uani 0.45 1 d . U P A 2 H9BA H 0.129473 0.030108 0.372108 0.027 Uiso 0.45 1 calc R . P A 2 H9BB H 0.091737 0.058477 0.316933 0.027 Uiso 0.45 1 calc R . P A 2 C10B C 0.0828(3) 0.1384(7) 0.3954(4) 0.029(2) Uani 0.45 1 d . U P A 2 H10C H 0.068742 0.194604 0.375980 0.035 Uiso 0.45 1 calc R . P A 2 H10D H 0.055820 0.100917 0.411377 0.035 Uiso 0.45 1 calc R . P A 2 O5B O 0.1193(2) 0.1605(4) 0.4427(3) 0.0224(13) Uiso 0.45 1 d D U P A 2 H5B H 0.099(2) 0.185(4) 0.468(3) 0.027 Uiso 0.45 1 d DR . P E 2 O6 O 0.21146(8) 0.45783(13) 0.50412(10) 0.0314(5) Uani 1 1 d . . . . . O7 O 0.16360(7) 0.42222(14) 0.58053(9) 0.0226(4) Uani 1 1 d . . . . . C11 C 0.18092(10) 0.47758(19) 0.54408(13) 0.0198(6) Uani 1 1 d . . . . . C12 C 0.16620(12) 0.5798(2) 0.54717(14) 0.0319(7) Uani 1 1 d D . . . . C13A C 0.1319(3) 0.6060(5) 0.4926(3) 0.0320(16) Uiso 0.47 1 d D . P F 1 H13A H 0.146178 0.584942 0.454787 0.048 Uiso 0.47 1 calc R . P F 1 H13B H 0.099728 0.576950 0.496735 0.048 Uiso 0.47 1 calc R . P F 1 H13C H 0.127932 0.672962 0.491245 0.048 Uiso 0.47 1 calc R . P F 1 C14A C 0.1494(4) 0.6073(7) 0.6077(4) 0.049(2) Uiso 0.47 1 d D . P F 1 H14A H 0.173693 0.587500 0.639429 0.073 Uiso 0.47 1 calc R . P F 1 H14B H 0.145835 0.674252 0.609151 0.073 Uiso 0.47 1 calc R . P F 1 H14C H 0.117631 0.578240 0.614641 0.073 Uiso 0.47 1 calc R . P F 1 C15A C 0.2150(3) 0.6409(5) 0.5332(4) 0.0260(17) Uiso 0.47 1 d D U P F 1 H15A H 0.226858 0.623914 0.493168 0.039 Uiso 0.47 1 calc R . P F 1 H15B H 0.206451 0.706367 0.533179 0.039 Uiso 0.47 1 calc R . P F 1 H15C H 0.240888 0.629050 0.564725 0.039 Uiso 0.47 1 calc R . P F 1 C14B C 0.1133(4) 0.5775(9) 0.5796(6) 0.043(3) Uiso 0.29 1 d D . P F 2 H14D H 0.089364 0.543299 0.553731 0.064 Uiso 0.29 1 calc R . P F 2 H14E H 0.117342 0.547401 0.619452 0.064 Uiso 0.29 1 calc R . P F 2 H14F H 0.101558 0.640550 0.585014 0.064 Uiso 0.29 1 calc R . P F 2 C13B C 0.1542(5) 0.6170(8) 0.4843(4) 0.031(3) Uiso 0.29 1 d D . P F 2 H13D H 0.131150 0.575437 0.462493 0.046 Uiso 0.29 1 calc R . P F 2 H13E H 0.139191 0.677925 0.487543 0.046 Uiso 0.29 1 calc R . P F 2 H13F H 0.184504 0.621838 0.461962 0.046 Uiso 0.29 1 calc R . P F 2 C15B C 0.2003(5) 0.6315(9) 0.5877(6) 0.051(3) Uiso 0.29 1 d D . P F 2 H15D H 0.204562 0.599307 0.626849 0.076 Uiso 0.29 1 calc R . P F 2 H15E H 0.232159 0.636950 0.568986 0.076 Uiso 0.29 1 calc R . P F 2 H15F H 0.186846 0.693037 0.594568 0.076 Uiso 0.29 1 calc R . P F 2 C13C C 0.2054(9) 0.6389(19) 0.5170(12) 0.093(11) Uiso 0.24 1 d D U P F 3 H13G H 0.237568 0.628701 0.537904 0.139 Uiso 0.24 1 calc R . P F 3 H13H H 0.207084 0.621506 0.473939 0.139 Uiso 0.24 1 calc R . P F 3 H13I H 0.196514 0.703968 0.519826 0.139 Uiso 0.24 1 calc R . P F 3 C14C C 0.1163(5) 0.5903(11) 0.5187(8) 0.046(4) Uiso 0.24 1 d D . P F 3 H14G H 0.116383 0.571189 0.475907 0.069 Uiso 0.24 1 calc R . P F 3 H14H H 0.093171 0.551896 0.540409 0.069 Uiso 0.24 1 calc R . P F 3 H14I H 0.106157 0.654826 0.521000 0.069 Uiso 0.24 1 calc R . P F 3 C15C C 0.1692(6) 0.6085(10) 0.6148(5) 0.029(3) Uiso 0.24 1 d D . P F 3 H15G H 0.202989 0.600193 0.631491 0.044 Uiso 0.24 1 calc R . P F 3 H15H H 0.159776 0.673234 0.618339 0.044 Uiso 0.24 1 calc R . P F 3 H15I H 0.146791 0.570304 0.637748 0.044 Uiso 0.24 1 calc R . P F 3 O8 O 0.30802(8) 0.44150(13) 0.49468(9) 0.0277(5) Uani 1 1 d . . . . . O9 O 0.35204(7) 0.38822(14) 0.41907(9) 0.0229(4) Uani 1 1 d . . . . . C16 C 0.34182(10) 0.44814(18) 0.45706(12) 0.0186(6) Uani 1 1 d . . . . . C17 C 0.37114(11) 0.53842(19) 0.45708(14) 0.0249(7) Uani 1 1 d . . . . . C18 C 0.35940(13) 0.6005(2) 0.51029(16) 0.0363(8) Uani 1 1 d . . . . . H18A H 0.378885 0.657064 0.508428 0.054 Uiso 1 1 calc R . . . . H18B H 0.324268 0.615942 0.507933 0.054 Uiso 1 1 calc R . . . . H18C H 0.367471 0.568605 0.548792 0.054 Uiso 1 1 calc R . . . . C19 C 0.42654(11) 0.5158(2) 0.45986(17) 0.0374(8) Uani 1 1 d . . . . . H19A H 0.434026 0.475793 0.425554 0.056 Uiso 1 1 calc R . . . . H19B H 0.445526 0.572856 0.457465 0.056 Uiso 1 1 calc R . . . . H19C H 0.435326 0.484340 0.498332 0.056 Uiso 1 1 calc R . . . . C20 C 0.35689(14) 0.5878(2) 0.39693(16) 0.0401(9) Uani 1 1 d . . . . . H20A H 0.364377 0.548108 0.362485 0.060 Uiso 1 1 calc R . . . . H20B H 0.321575 0.601706 0.395435 0.060 Uiso 1 1 calc R . . . . H20C H 0.375612 0.645185 0.394509 0.060 Uiso 1 1 calc R . . . . O10 O 0.18959(8) 0.33338(14) 0.70921(9) 0.0258(5) Uani 1 1 d . . . . . O11 O 0.17830(8) 0.18362(14) 0.70626(9) 0.0299(5) Uani 1 1 d . . . . . C21 C 0.18216(11) 0.2577(2) 0.73566(13) 0.0219(6) Uani 1 1 d D U . . . C22A C 0.1732(4) 0.2680(7) 0.8043(4) 0.030(3) Uani 0.5 1 d D U P G 1 C23 C 0.21888(13) 0.3140(3) 0.83548(14) 0.0401(9) Uani 1 1 d D U . . . H23A H 0.223205 0.375450 0.818252 0.060 Uiso 0.45 1 calc R . P G 1 H23B H 0.214317 0.319049 0.879406 0.060 Uiso 0.45 1 calc R . P G 1 H23C H 0.248125 0.276662 0.828594 0.060 Uiso 0.45 1 calc R . P G 1 H23D H 0.212884 0.376169 0.819656 0.060 Uiso 0.55 1 calc R . P G 2 H23E H 0.215741 0.313799 0.879804 0.060 Uiso 0.55 1 calc R . P G 2 H23F H 0.252159 0.294378 0.825980 0.060 Uiso 0.55 1 calc R . P G 2 C24A C 0.1257(4) 0.3240(7) 0.8106(5) 0.040(2) Uani 0.45 1 d D U P G 1 H24A H 0.129687 0.384878 0.792323 0.060 Uiso 0.45 1 calc R . P G 1 H24B H 0.098131 0.291967 0.789661 0.060 Uiso 0.45 1 calc R . P G 1 H24C H 0.119109 0.330918 0.853931 0.060 Uiso 0.45 1 calc R . P G 1 C25A C 0.1680(4) 0.1734(7) 0.8323(5) 0.042(3) Uani 0.45 1 d D U P G 1 H25A H 0.198560 0.138614 0.827955 0.062 Uiso 0.45 1 calc R . P G 1 H25B H 0.161596 0.179660 0.875732 0.062 Uiso 0.45 1 calc R . P G 1 H25C H 0.140618 0.140709 0.811463 0.062 Uiso 0.45 1 calc R . P G 1 C22B C 0.1808(4) 0.2471(7) 0.8056(4) 0.027(2) Uani 0.5 1 d D U P G 2 C24B C 0.1296(3) 0.2825(5) 0.8227(4) 0.0343(18) Uani 0.54 1 d D U P G 2 H24D H 0.125223 0.346047 0.808524 0.051 Uiso 0.54 1 calc R . P G 2 H24E H 0.103908 0.243657 0.803233 0.051 Uiso 0.54 1 calc R . P G 2 H24F H 0.127074 0.280283 0.867062 0.051 Uiso 0.54 1 calc R . P G 2 C25B C 0.1874(3) 0.1488(6) 0.8275(4) 0.0296(17) Uani 0.54 1 d D U P G 2 H25D H 0.186208 0.147013 0.872069 0.044 Uiso 0.54 1 calc R . P G 2 H25E H 0.160970 0.110508 0.809331 0.044 Uiso 0.54 1 calc R . P G 2 H25F H 0.219312 0.125449 0.815312 0.044 Uiso 0.54 1 calc R . P G 2 O12 O 0.10082(8) 0.27596(17) 0.53396(10) 0.0334(5) Uani 1 1 d D . . . . O13 O 0.09159(8) 0.28153(17) 0.63286(10) 0.0339(5) Uani 1 1 d . . . . . C26 C 0.07374(12) 0.2856(3) 0.57922(15) 0.0386(8) Uani 1 1 d D U . . . C27A C 0.0166(3) 0.2816(6) 0.5686(4) 0.035(2) Uani 0.5 1 d D U P H 1 C28A C 0.0019(4) 0.3757(6) 0.5927(6) 0.073(3) Uani 0.5 1 d D U P H 1 H28A H 0.011515 0.380163 0.636214 0.109 Uiso 0.5 1 calc R . P H 1 H28B H 0.018601 0.423939 0.570271 0.109 Uiso 0.5 1 calc R . P H 1 H28C H -0.033813 0.383463 0.587092 0.109 Uiso 0.5 1 calc R . P H 1 C29A C 0.0032(5) 0.2690(14) 0.5021(5) 0.105(7) Uani 0.5 1 d D U P H 1 H29A H 0.019876 0.315880 0.478463 0.158 Uiso 0.5 1 calc R . P H 1 H29B H 0.013501 0.207776 0.489147 0.158 Uiso 0.5 1 calc R . P H 1 H29C H -0.032504 0.275255 0.495288 0.158 Uiso 0.5 1 calc R . P H 1 C30A C -0.0096(3) 0.2082(6) 0.6042(5) 0.059(2) Uani 0.5 1 d D U P H 1 H30A H -0.001274 0.215340 0.647849 0.089 Uiso 0.5 1 calc R . P H 1 H30B H -0.045306 0.214673 0.596886 0.089 Uiso 0.5 1 calc R . P H 1 H30C H 0.000700 0.147194 0.590745 0.089 Uiso 0.5 1 calc R . P H 1 C27B C 0.0205(3) 0.3249(6) 0.5655(4) 0.0355(19) Uani 0.5 1 d D U P H 2 C28B C -0.0053(3) 0.3396(8) 0.6252(4) 0.063(3) Uani 0.5 1 d D U P H 2 H28D H 0.011709 0.387989 0.648993 0.095 Uiso 0.5 1 calc R . P H 2 H28E H -0.039556 0.358000 0.616121 0.095 Uiso 0.5 1 calc R . P H 2 H28F H -0.004659 0.282297 0.648686 0.095 Uiso 0.5 1 calc R . P H 2 C29B C -0.0041(4) 0.2504(9) 0.5261(7) 0.079(5) Uani 0.5 1 d D U P H 2 H29D H -0.003859 0.192281 0.548766 0.119 Uiso 0.5 1 calc R . P H 2 H29E H -0.038234 0.268178 0.515544 0.119 Uiso 0.5 1 calc R . P H 2 H29F H 0.013815 0.242715 0.488739 0.119 Uiso 0.5 1 calc R . P H 2 C30B C 0.0195(3) 0.4141(6) 0.5292(4) 0.055(2) Uani 0.5 1 d D U P H 2 H30D H 0.035215 0.463022 0.553870 0.082 Uiso 0.5 1 calc R . P H 2 H30E H 0.037327 0.405651 0.491802 0.082 Uiso 0.5 1 calc R . P H 2 H30F H -0.014721 0.431114 0.518607 0.082 Uiso 0.5 1 calc R . P H 2 N31A N 0.0078(3) -0.0298(6) 0.6832(4) 0.071(2) Uani 0.5 1 d D U P I 1 C31A C 0.0387(3) 0.0196(6) 0.6961(3) 0.0430(18) Uani 0.5 1 d D U P I 1 C32A C 0.0768(8) 0.0889(19) 0.7174(8) 0.066(4) Uani 0.5 1 d D U P I 1 H32A H 0.097889 0.103688 0.683690 0.100 Uiso 0.5 1 calc GR . P I 1 H32B H 0.096883 0.063166 0.751437 0.100 Uiso 0.5 1 calc GR . P I 1 H32C H 0.060383 0.144857 0.730767 0.100 Uiso 0.5 1 calc GR . P I 1 N31B N -0.0227(4) 0.0572(8) 0.6548(4) 0.103(4) Uani 0.5 1 d D U P J 2 C31B C 0.0148(4) 0.0796(8) 0.6774(4) 0.069(3) Uani 0.5 1 d D U P J 2 C32B C 0.0664(8) 0.1025(19) 0.7021(8) 0.066(4) Uani 0.5 1 d D U P J 2 H32D H 0.068737 0.091381 0.746146 0.100 Uiso 0.5 1 calc GR . P J 2 H32E H 0.073476 0.167322 0.693959 0.100 Uiso 0.5 1 calc GR . P J 2 H32F H 0.090210 0.063647 0.681968 0.100 Uiso 0.5 1 calc GR . P J 2 C41 C -0.0031(5) 0.2480(4) 0.2668(4) 0.078(4) Uani 0.5 1 d . U P K -1 H41 H -0.004232 0.182873 0.269784 0.093 Uiso 0.5 1 calc R . P K -1 C42 C -0.0168(4) 0.3020(7) 0.3155(3) 0.076(4) Uani 0.5 1 d G U P K -1 H42 H -0.027240 0.273827 0.351722 0.091 Uiso 0.5 1 calc R . P K -1 C43 C -0.0152(6) 0.3973(7) 0.3111(6) 0.076(4) Uani 0.5 1 d G U P K -1 H43 H -0.024519 0.434222 0.344329 0.092 Uiso 0.5 1 calc R . P K -1 C44 C 0.0001(8) 0.4385(4) 0.2580(8) 0.072(4) Uani 0.5 1 d G U P K -1 H44 H 0.001210 0.503663 0.254998 0.087 Uiso 0.5 1 calc R . P K -1 C45 C 0.0138(6) 0.3845(7) 0.2093(6) 0.077(4) Uani 0.5 1 d G U P K -1 H45 H 0.024218 0.412711 0.173060 0.093 Uiso 0.5 1 calc R . P K -1 C46 C 0.0122(4) 0.2892(6) 0.2137(3) 0.076(4) Uani 0.5 1 d DG U P K -1 C47 C 0.0260(4) 0.2340(9) 0.1601(6) 0.114(5) Uani 0.5 1 d D U P K -1 H47A H -0.001433 0.233394 0.129580 0.172 Uiso 0.5 1 calc GR . P K -1 H47B H 0.033565 0.170908 0.173124 0.172 Uiso 0.5 1 calc GR . P K -1 H47C H 0.055039 0.261305 0.142359 0.172 Uiso 0.5 1 calc GR . P K -1 O51B O 0.1011(2) 0.4451(4) 0.7097(3) 0.0649(16) Uiso 0.5 1 d . . P L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01538(7) 0.02187(8) 0.01106(7) -0.00206(5) 0.00079(5) -0.00124(6) Mn1 0.0166(2) 0.0130(2) 0.0155(2) -0.00018(15) 0.00283(16) -0.00033(15) Mn2 0.0156(2) 0.0438(3) 0.0136(2) 0.00385(19) -0.00228(17) -0.00148(19) O1 0.0138(9) 0.0146(9) 0.0132(9) 0.0010(7) -0.0008(7) 0.0006(7) N1A 0.020(3) 0.027(3) 0.016(2) -0.0012(19) -0.002(2) 0.002(2) C1A 0.028(3) 0.029(3) 0.019(3) 0.001(2) -0.009(2) 0.003(2) C2A 0.037(5) 0.030(4) 0.015(3) -0.003(3) -0.009(3) 0.004(4) N2A 0.016(3) 0.024(3) 0.017(3) -0.001(2) -0.003(2) -0.001(2) N1B 0.020(3) 0.031(3) 0.019(3) 0.003(2) -0.003(2) 0.001(2) C1B 0.032(5) 0.040(6) 0.017(4) 0.003(4) -0.009(3) 0.003(4) C2B 0.030(4) 0.036(4) 0.017(3) 0.000(3) -0.005(3) 0.003(3) N2B 0.018(3) 0.028(4) 0.014(3) -0.002(3) -0.001(2) -0.003(3) C3 0.0327(18) 0.049(2) 0.0315(19) 0.0239(16) -0.0143(15) -0.0149(15) C4 0.0219(15) 0.0301(16) 0.0228(16) 0.0126(12) 0.0003(12) -0.0006(12) O2 0.0190(10) 0.0246(10) 0.0154(10) 0.0073(8) -0.0004(8) 0.0011(8) C6A 0.021(3) 0.030(3) 0.020(3) 0.003(2) -0.002(2) 0.006(2) O3A 0.025(2) 0.028(2) 0.013(2) 0.0071(18) -0.0038(18) 0.0051(17) C5B 0.029(4) 0.031(4) 0.031(4) 0.005(3) -0.002(3) 0.010(3) C6B 0.030(5) 0.038(4) 0.029(4) 0.002(3) 0.003(4) 0.011(3) O3B 0.033(3) 0.047(4) 0.020(3) 0.004(3) 0.003(3) 0.013(3) C7 0.0223(16) 0.048(2) 0.0224(16) -0.0179(14) -0.0039(13) 0.0055(13) C8 0.0223(15) 0.0320(17) 0.0213(16) -0.0097(12) 0.0017(12) -0.0055(12) O4 0.0194(10) 0.0258(11) 0.0150(10) -0.0063(8) -0.0002(8) -0.0030(8) C9A 0.022(3) 0.038(4) 0.030(3) -0.010(3) -0.002(2) -0.010(2) C10A 0.036(5) 0.039(4) 0.024(4) -0.004(3) -0.001(3) -0.015(3) O5A 0.030(2) 0.033(3) 0.025(2) -0.007(2) 0.0045(19) -0.0085(19) C9B 0.022(3) 0.032(4) 0.013(3) -0.002(3) -0.001(3) -0.005(3) C10B 0.008(4) 0.056(6) 0.024(4) -0.021(4) 0.002(3) -0.001(3) O6 0.0415(13) 0.0184(10) 0.0364(13) 0.0062(9) 0.0222(11) 0.0091(9) O7 0.0185(10) 0.0313(11) 0.0179(10) 0.0027(8) 0.0012(8) 0.0027(8) C11 0.0194(14) 0.0227(15) 0.0171(14) -0.0028(11) -0.0027(11) 0.0016(11) C12 0.042(2) 0.0261(17) 0.0277(17) -0.0057(13) -0.0013(15) 0.0161(14) O8 0.0343(12) 0.0215(11) 0.0285(12) -0.0064(9) 0.0156(10) -0.0093(9) O9 0.0197(10) 0.0288(11) 0.0202(11) -0.0072(8) 0.0019(8) -0.0040(8) C16 0.0187(14) 0.0206(14) 0.0164(14) 0.0026(11) -0.0021(11) 0.0009(11) C17 0.0267(16) 0.0190(14) 0.0297(17) 0.0013(12) 0.0080(13) -0.0040(12) C18 0.043(2) 0.0242(17) 0.042(2) -0.0085(14) 0.0105(17) -0.0117(14) C19 0.0242(17) 0.0345(18) 0.054(2) 0.0030(16) 0.0035(16) -0.0070(14) C20 0.052(2) 0.0286(18) 0.040(2) 0.0117(15) 0.0060(18) -0.0055(16) O10 0.0344(12) 0.0260(11) 0.0167(10) -0.0020(8) -0.0012(9) -0.0008(9) O11 0.0463(14) 0.0266(12) 0.0171(10) -0.0004(9) 0.0051(10) -0.0106(10) C21 0.0198(14) 0.0321(16) 0.0138(13) -0.0026(11) 0.0015(11) -0.0069(12) C22A 0.045(5) 0.035(5) 0.011(4) -0.003(3) 0.007(3) -0.016(4) C23 0.052(2) 0.052(2) 0.0166(15) -0.0047(15) 0.0035(15) -0.0204(18) C24A 0.055(5) 0.041(6) 0.026(5) -0.008(4) 0.023(4) -0.007(5) C25A 0.062(8) 0.045(6) 0.017(4) 0.002(4) 0.003(5) -0.018(5) C22B 0.031(4) 0.036(5) 0.015(4) -0.006(3) 0.005(3) -0.003(3) C24B 0.036(4) 0.036(5) 0.032(4) -0.005(4) 0.015(3) -0.008(3) C25B 0.036(5) 0.040(4) 0.013(3) 0.003(3) 0.004(3) -0.010(3) O12 0.0212(11) 0.0576(15) 0.0213(11) -0.0101(10) -0.0008(9) 0.0055(10) O13 0.0202(11) 0.0591(15) 0.0228(11) -0.0066(10) 0.0034(9) 0.0017(10) C26 0.0198(16) 0.069(3) 0.0273(18) -0.0126(17) -0.0005(14) 0.0056(15) C27A 0.016(3) 0.049(5) 0.038(4) -0.007(4) 0.003(3) 0.002(4) C28A 0.033(5) 0.050(5) 0.134(11) -0.018(6) -0.016(6) 0.015(4) C29A 0.017(6) 0.24(2) 0.054(5) -0.031(8) -0.012(5) 0.019(8) C30A 0.016(3) 0.056(5) 0.105(7) 0.006(5) 0.002(4) -0.005(3) C27B 0.013(3) 0.045(5) 0.049(5) -0.015(4) 0.000(3) 0.000(4) C28B 0.032(5) 0.079(7) 0.081(7) 0.003(5) 0.027(5) 0.009(5) C29B 0.018(5) 0.068(7) 0.151(14) -0.060(8) -0.015(7) -0.004(4) C30B 0.028(4) 0.065(5) 0.072(6) 0.006(4) 0.003(4) 0.018(4) N31A 0.059(5) 0.088(6) 0.063(5) 0.006(4) -0.011(4) -0.036(4) C31A 0.038(4) 0.060(5) 0.031(4) 0.009(4) 0.000(3) -0.012(3) C32A 0.096(8) 0.094(8) 0.008(9) 0.004(5) -0.007(4) -0.061(8) N31B 0.093(6) 0.143(9) 0.074(6) -0.049(6) 0.023(5) -0.065(7) C31B 0.076(6) 0.087(7) 0.046(5) -0.017(5) 0.025(4) -0.043(6) C32B 0.096(8) 0.094(8) 0.008(9) 0.004(5) -0.007(4) -0.061(8) C41 0.034(6) 0.094(7) 0.102(10) -0.016(5) -0.036(8) 0.029(7) C42 0.038(6) 0.104(7) 0.082(9) -0.001(7) -0.039(7) 0.015(6) C43 0.049(7) 0.102(7) 0.074(10) -0.035(6) -0.039(6) 0.025(6) C44 0.036(4) 0.093(6) 0.084(10) -0.025(7) -0.034(6) 0.026(8) C45 0.034(6) 0.119(8) 0.076(10) -0.026(7) -0.027(6) 0.022(7) C46 0.033(7) 0.114(8) 0.076(8) -0.047(7) -0.038(6) 0.027(8) C47 0.059(7) 0.170(13) 0.112(9) -0.071(9) -0.022(7) 0.034(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 O1 Sm1 O2 71.61(6) . 7_556 O1 Sm1 O4 71.34(6) . 7_556 O1 Sm1 O7 82.49(6) . . O1 Sm1 O9 82.38(6) . 7_556 O1 Sm1 O10 148.65(6) . . O1 Sm1 O11 147.26(6) . . O1 Sm1 O12 71.72(6) . . O1 Sm1 O13 122.30(7) . . O2 Sm1 O4 65.75(6) 7_556 7_556 O2 Sm1 O12 130.21(6) 7_556 . O2 Sm1 O13 147.14(7) 7_556 . O4 Sm1 O12 129.16(7) 7_556 . O4 Sm1 O13 144.42(7) 7_556 . O7 Sm1 O2 135.48(6) . 7_556 O7 Sm1 O4 71.97(6) . 7_556 O7 Sm1 O10 79.93(7) . . O7 Sm1 O11 129.54(7) . . O7 Sm1 O12 69.67(7) . . O7 Sm1 O13 77.38(7) . . O9 Sm1 O2 73.22(6) 7_556 7_556 O9 Sm1 O4 136.32(6) 7_556 7_556 O9 Sm1 O7 139.13(7) 7_556 . O9 Sm1 O10 127.10(7) 7_556 . O9 Sm1 O11 76.06(7) 7_556 . O9 Sm1 O12 69.57(7) 7_556 . O9 Sm1 O13 79.20(7) 7_556 . O10 Sm1 O2 104.12(6) . 7_556 O10 Sm1 O4 78.61(6) . 7_556 O10 Sm1 O12 124.53(7) . . O10 Sm1 O13 78.63(7) . . O11 Sm1 O2 78.68(7) . 7_556 O11 Sm1 O4 108.69(7) . 7_556 O11 Sm1 O10 52.50(7) . . O11 Sm1 O12 121.28(7) . . O11 Sm1 O13 77.62(7) . . O13 Sm1 O12 50.59(7) . . O1 Mn1 O1 81.44(8) 7_556 . O1 Mn1 O2 88.41(7) . . O1 Mn1 O2 88.25(7) 7_556 . O1 Mn1 O4 88.38(7) 7_556 7_556 O1 Mn1 O4 88.07(7) . 7_556 O1 Mn1 O6 97.51(8) . . O1 Mn1 O6 177.87(8) 7_556 . O1 Mn1 O8 96.97(8) 7_556 . O1 Mn1 O8 178.12(8) . . O4 Mn1 O2 175.45(8) 7_556 . O6 Mn1 O2 93.57(8) . . O6 Mn1 O4 89.74(8) . 7_556 O6 Mn1 O8 84.11(9) . . O8 Mn1 O2 90.54(8) . . O8 Mn1 O4 92.90(8) . 7_556 O1 Mn2 N1A 135.43(13) . . O1 Mn2 N2A 148.42(15) . . O1 Mn2 N1B 150.43(17) . . O1 Mn2 N2B 135.00(17) . . O1 Mn2 O3A 76.38(11) . . O1 Mn2 O5B 77.81(15) . . N1A Mn2 O3A 69.07(16) . . N2A Mn2 N1A 75.98(19) . . N2A Mn2 O3A 123.24(18) . . N1B Mn2 N2B 74.6(2) . . N1B Mn2 O5B 123.6(2) . . O2 Mn2 O1 80.05(6) . . O2 Mn2 N1A 77.17(13) . . O2 Mn2 N2A 117.33(14) . . O2 Mn2 N1B 78.11(16) . . O2 Mn2 N2B 127.98(17) . . O2 Mn2 O3A 96.95(12) . . O2 Mn2 O4 77.29(7) . . O2 Mn2 O5A 166.65(12) . . O2 Mn2 O5B 157.69(15) . . O3B Mn2 O1 92.20(17) . . O3B Mn2 N1B 76.0(2) . . O3B Mn2 N2B 107.1(3) . . O3B Mn2 O2 107.95(19) . . O3B Mn2 O4 169.65(16) . . O3B Mn2 O5B 75.8(2) . . O4 Mn2 O1 79.76(6) . . O4 Mn2 N1A 130.25(14) . . O4 Mn2 N2A 79.03(16) . . O4 Mn2 N1B 114.14(17) . . O4 Mn2 N2B 74.94(18) . . O4 Mn2 O3A 156.09(12) . . O4 Mn2 O5A 108.56(15) . . O4 Mn2 O5B 95.94(14) . . O5A Mn2 O1 89.08(13) . . O5A Mn2 N1A 106.04(18) . . O5A Mn2 N2A 75.90(17) . . O5A Mn2 O3A 72.78(16) . . O5B Mn2 N2B 68.7(2) . . Mn1 O1 Sm1 103.41(7) 7_556 . Mn1 O1 Sm1 103.76(8) . . Mn1 O1 Mn1 98.57(8) 7_556 . Mn1 O1 Mn2 97.20(7) . . Mn1 O1 Mn2 97.42(7) 7_556 . Mn2 O1 Sm1 147.64(8) . . C1A N1A Mn2 107.9(3) . . C1A N1A C3 108.1(4) . . C3 N1A Mn2 101.0(3) . . C5A N1A Mn2 113.7(4) . . C5A N1A C1A 108.1(5) . . C5A N1A C3 117.5(4) . . N1A C1A H1AA 109.1 . . N1A C1A H1AB 109.1 . . N1A C1A C2A 112.5(5) . . H1AA C1A H1AB 107.8 . . C2A C1A H1AA 109.1 . . C2A C1A H1AB 109.1 . . C1A C2A H2AA 109.1 . . C1A C2A H2AB 109.1 . . H2AA C2A H2AB 107.9 . . N2A C2A C1A 112.4(6) . . N2A C2A H2AA 109.1 . . N2A C2A H2AB 109.1 . . C2A N2A Mn2 110.4(4) . . C2A N2A C7 114.9(5) . . C7 N2A Mn2 105.3(3) . . C9A N2A Mn2 107.3(4) . . C9A N2A C2A 110.3(6) . . C9A N2A C7 108.2(5) . . C1B N1B Mn2 111.4(5) . . C3 N1B Mn2 105.6(3) . . C3 N1B C1B 118.8(6) . . C5B N1B Mn2 105.4(4) . . C5B N1B C1B 109.1(7) . . C5B N1B C3 105.6(6) . . N1B C1B H1BA 108.9 . . N1B C1B H1BB 108.9 . . N1B C1B C2B 113.5(8) . . H1BA C1B H1BB 107.7 . . C2B C1B H1BA 108.9 . . C2B C1B H1BB 108.9 . . C1B C2B H2BA 109.1 . . C1B C2B H2BB 109.1 . . H2BA C2B H2BB 107.8 . . N2B C2B C1B 112.7(7) . . N2B C2B H2BA 109.1 . . N2B C2B H2BB 109.1 . . C2B N2B Mn2 108.0(5) . . C2B N2B C9B 110.1(6) . . C7 N2B Mn2 102.2(4) . . C7 N2B C2B 105.9(5) . . C7 N2B C9B 118.1(6) . . C9B N2B Mn2 111.9(5) . . N1A C3 H3AA 110.6 . . N1A C3 H3AB 110.6 . . N1B C3 H3BC 107.5 . . N1B C3 H3BD 107.5 . . N1B C3 C4 119.2(3) . . H3AA C3 H3AB 108.7 . . H3BC C3 H3BD 107.0 . . C4 C3 N1A 105.7(3) . . C4 C3 H3AA 110.6 . . C4 C3 H3AB 110.6 . . C4 C3 H3BC 107.5 . . C4 C3 H3BD 107.5 . . C3 C4 H4A 109.6 . . C3 C4 H4B 109.6 . . H4A C4 H4B 108.1 . . O2 C4 C3 110.2(2) . . O2 C4 H4A 109.6 . . O2 C4 H4B 109.6 . . Mn1 O2 Sm1 92.18(7) . 7_556 Mn2 O2 Sm1 108.62(8) . 7_556 Mn2 O2 Mn1 92.56(7) . . C4 O2 Sm1 124.45(16) . 7_556 C4 O2 Mn1 120.08(17) . . C4 O2 Mn2 113.11(16) . . N1A C5A H5AA 109.6 . . N1A C5A H5AB 109.6 . . N1A C5A C6A 110.5(5) . . H5AA C5A H5AB 108.1 . . C6A C5A H5AA 109.6 . . C6A C5A H5AB 109.6 . . C5A C6A H6AA 110.8 . . C5A C6A H6AB 110.8 . . H6AA C6A H6AB 108.9 . . O3A C6A C5A 104.6(5) . . O3A C6A H6AA 110.8 . . O3A C6A H6AB 110.8 . . Mn2 O3A H3A 112(4) . . C6A O3A Mn2 109.3(3) . . C6A O3A H3A 109(4) . . N1B C5B H5BA 108.7 . . N1B C5B H5BB 108.7 . . N1B C5B C6B 114.0(6) . . H5BA C5B H5BB 107.6 . . C6B C5B H5BA 108.7 . . C6B C5B H5BB 108.7 . . C5B C6B H6BA 110.5 . . C5B C6B H6BB 110.5 . . H6BA C6B H6BB 108.7 . . O3B C6B C5B 106.3(6) . . O3B C6B H6BA 110.5 . . O3B C6B H6BB 110.5 . . Mn2 O3B H3B 95(6) . . C6B O3B Mn2 115.5(5) . . C6B O3B H3B 145(6) . . N2A C7 H7AA 108.3 . . N2A C7 H7AB 108.3 . . N2B C7 H7BC 110.6 . . N2B C7 H7BD 110.6 . . N2B C7 C8 105.8(4) . . H7AA C7 H7AB 107.4 . . H7BC C7 H7BD 108.7 . . C8 C7 N2A 116.1(3) . . C8 C7 H7AA 108.3 . . C8 C7 H7AB 108.3 . . C8 C7 H7BC 110.6 . . C8 C7 H7BD 110.6 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . H8A C8 H8B 108.1 . . O4 C8 C7 110.7(2) . . O4 C8 H8A 109.5 . . O4 C8 H8B 109.5 . . Mn1 O4 Sm1 92.47(7) 7_556 7_556 Mn2 O4 Sm1 108.24(8) . 7_556 Mn2 O4 Mn1 92.67(7) . 7_556 C8 O4 Sm1 124.13(16) . 7_556 C8 O4 Mn1 120.10(16) . 7_556 C8 O4 Mn2 113.48(16) . . N2A C9A H9AA 108.5 . . N2A C9A H9AB 108.5 . . H9AA C9A H9AB 107.5 . . C10A C9A N2A 114.9(6) . . C10A C9A H9AA 108.5 . . C10A C9A H9AB 108.5 . . C9A C10A H10A 109.9 . . C9A C10A H10B 109.9 . . H10A C10A H10B 108.3 . . O5A C10A C9A 108.8(6) . . O5A C10A H10A 109.9 . . O5A C10A H10B 109.9 . . Mn2 O5A H5A 107(4) . . C10A O5A Mn2 114.1(4) . . C10A O5A H5A 126(4) . . N2B C9B H9BA 109.8 . . N2B C9B H9BB 109.8 . . N2B C9B C10B 109.2(7) . . H9BA C9B H9BB 108.3 . . C10B C9B H9BA 109.8 . . C10B C9B H9BB 109.8 . . C9B C10B H10C 111.5 . . C9B C10B H10D 111.5 . . H10C C10B H10D 109.3 . . O5B C10B C9B 101.5(6) . . O5B C10B H10C 111.5 . . O5B C10B H10D 111.5 . . Mn2 O5B H5B 117(4) . . C10B O5B Mn2 109.0(5) . . C10B O5B H5B 97(4) . . C11 O6 Mn1 128.85(18) . . C11 O7 Sm1 134.21(17) . . O6 C11 C12 115.4(2) . . O7 C11 O6 125.3(3) . . O7 C11 C12 119.3(2) . . C11 C12 C15A 107.5(3) . . C11 C12 C14B 103.6(5) . . C11 C12 C13C 109.4(12) . . C13A C12 C11 110.8(4) . . C13A C12 C15A 100.8(5) . . C14A C12 C11 113.1(4) . . C14A C12 C13A 115.7(5) . . C14A C12 C15A 107.9(5) . . C13B C12 C11 110.7(5) . . C13B C12 C14B 104.4(7) . . C15B C12 C11 111.4(6) . . C15B C12 C14B 106.9(7) . . C15B C12 C13B 118.5(8) . . C14C C12 C11 108.5(7) . . C14C C12 C13C 113.6(13) . . C14C C12 C15C 112.7(9) . . C15C C12 C11 107.5(6) . . C15C C12 C13C 104.8(13) . . C12 C13A H13A 109.5 . . C12 C13A H13B 109.5 . . C12 C13A H13C 109.5 . . H13A C13A H13B 109.5 . . H13A C13A H13C 109.5 . . H13B C13A H13C 109.5 . . C12 C14A H14A 109.5 . . C12 C14A H14B 109.5 . . C12 C14A H14C 109.5 . . H14A C14A H14B 109.5 . . H14A C14A H14C 109.5 . . H14B C14A H14C 109.5 . . C12 C15A H15A 109.5 . . C12 C15A H15B 109.5 . . C12 C15A H15C 109.5 . . H15A C15A H15B 109.5 . . H15A C15A H15C 109.5 . . H15B C15A H15C 109.5 . . C12 C14B H14D 109.5 . . C12 C14B H14E 109.5 . . C12 C14B H14F 109.5 . . H14D C14B H14E 109.5 . . H14D C14B H14F 109.5 . . H14E C14B H14F 109.5 . . C12 C13B H13D 109.5 . . C12 C13B H13E 109.5 . . C12 C13B H13F 109.5 . . H13D C13B H13E 109.5 . . H13D C13B H13F 109.5 . . H13E C13B H13F 109.5 . . C12 C15B H15D 109.5 . . C12 C15B H15E 109.5 . . C12 C15B H15F 109.5 . . H15D C15B H15E 109.5 . . H15D C15B H15F 109.5 . . H15E C15B H15F 109.5 . . C12 C13C H13G 109.5 . . C12 C13C H13H 109.5 . . C12 C13C H13I 109.5 . . H13G C13C H13H 109.5 . . H13G C13C H13I 109.5 . . H13H C13C H13I 109.5 . . C12 C14C H14G 109.5 . . C12 C14C H14H 109.5 . . C12 C14C H14I 109.5 . . H14G C14C H14H 109.5 . . H14G C14C H14I 109.5 . . H14H C14C H14I 109.5 . . C12 C15C H15G 109.5 . . C12 C15C H15H 109.5 . . C12 C15C H15I 109.5 . . H15G C15C H15H 109.5 . . H15G C15C H15I 109.5 . . H15H C15C H15I 109.5 . . C16 O8 Mn1 129.75(18) . . C16 O9 Sm1 134.29(17) . 7_556 O8 C16 C17 117.2(2) . . O9 C16 O8 125.0(3) . . O9 C16 C17 117.8(2) . . C16 C17 C19 108.9(2) . . C16 C17 C20 106.8(3) . . C18 C17 C16 112.4(2) . . C18 C17 C19 109.6(3) . . C18 C17 C20 109.1(3) . . C20 C17 C19 110.0(3) . . C17 C18 H18A 109.5 . . C17 C18 H18B 109.5 . . C17 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C17 C19 H19A 109.5 . . C17 C19 H19B 109.5 . . C17 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C17 C20 H20A 109.5 . . C17 C20 H20B 109.5 . . C17 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C21 O10 Sm1 92.65(16) . . C21 O11 Sm1 93.02(17) . . O10 C21 Sm1 60.97(14) . . O10 C21 C22A 113.5(4) . . O10 C21 C22B 123.7(4) . . O11 C21 Sm1 60.77(14) . . O11 C21 O10 121.4(3) . . O11 C21 C22A 124.8(4) . . O11 C21 C22B 114.8(4) . . C22A C21 Sm1 167.6(4) . . C22B C21 Sm1 175.1(4) . . C23 C22A C21 108.4(6) . . C24A C22A C21 108.0(7) . . C24A C22A C23 113.1(8) . . C25A C22A C21 109.2(8) . . C25A C22A C23 107.6(8) . . C25A C22A C24A 110.5(8) . . C22A C23 H23A 109.5 . . C22A C23 H23B 109.5 . . C22A C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . H23D C23 H23E 109.5 . . H23D C23 H23F 109.5 . . H23E C23 H23F 109.5 . . C22B C23 H23D 109.5 . . C22B C23 H23E 109.5 . . C22B C23 H23F 109.5 . . C22A C24A H24A 109.5 . . C22A C24A H24B 109.5 . . C22A C24A H24C 109.5 . . H24A C24A H24B 109.5 . . H24A C24A H24C 109.5 . . H24B C24A H24C 109.5 . . C22A C25A H25A 109.5 . . C22A C25A H25B 109.5 . . C22A C25A H25C 109.5 . . H25A C25A H25B 109.5 . . H25A C25A H25C 109.5 . . H25B C25A H25C 109.5 . . C21 C22B C23 108.3(6) . . C21 C22B C24B 105.6(7) . . C23 C22B C24B 106.3(7) . . C25B C22B C21 113.7(7) . . C25B C22B C23 113.1(8) . . C25B C22B C24B 109.3(7) . . C22B C24B H24D 109.5 . . C22B C24B H24E 109.5 . . C22B C24B H24F 109.5 . . H24D C24B H24E 109.5 . . H24D C24B H24F 109.5 . . H24E C24B H24F 109.5 . . C22B C25B H25D 109.5 . . C22B C25B H25E 109.5 . . C22B C25B H25F 109.5 . . H25D C25B H25E 109.5 . . H25D C25B H25F 109.5 . . H25E C25B H25F 109.5 . . C26 O12 Sm1 91.53(19) . . C26 O13 Sm1 96.80(18) . . O12 C26 Sm1 62.90(16) . . O12 C26 C27A 119.2(4) . . O12 C26 C27B 116.9(4) . . O13 C26 Sm1 58.17(16) . . O13 C26 O12 121.0(3) . . O13 C26 C27A 118.5(4) . . O13 C26 C27B 120.7(4) . . C27A C26 Sm1 170.9(4) . . C27B C26 Sm1 165.2(4) . . C28A C27A C26 100.9(6) . . C29A C27A C26 110.2(7) . . C29A C27A C28A 112.9(10) . . C29A C27A C30A 108.4(9) . . C30A C27A C26 116.0(6) . . C30A C27A C28A 108.4(7) . . C27A C28A H28A 109.5 . . C27A C28A H28B 109.5 . . C27A C28A H28C 109.5 . . H28A C28A H28B 109.5 . . H28A C28A H28C 109.5 . . H28B C28A H28C 109.5 . . C27A C29A H29A 109.5 . . C27A C29A H29B 109.5 . . C27A C29A H29C 109.5 . . H29A C29A H29B 109.5 . . H29A C29A H29C 109.5 . . H29B C29A H29C 109.5 . . C27A C30A H30A 109.5 . . C27A C30A H30B 109.5 . . C27A C30A H30C 109.5 . . H30A C30A H30B 109.5 . . H30A C30A H30C 109.5 . . H30B C30A H30C 109.5 . . C28B C27B C26 110.0(7) . . C29B C27B C26 103.1(7) . . C29B C27B C28B 112.3(9) . . C29B C27B C30B 108.3(9) . . C30B C27B C26 113.8(6) . . C30B C27B C28B 109.3(7) . . C27B C28B H28D 109.5 . . C27B C28B H28E 109.5 . . C27B C28B H28F 109.5 . . H28D C28B H28E 109.5 . . H28D C28B H28F 109.5 . . H28E C28B H28F 109.5 . . C27B C29B H29D 109.5 . . C27B C29B H29E 109.5 . . C27B C29B H29F 109.5 . . H29D C29B H29E 109.5 . . H29D C29B H29F 109.5 . . H29E C29B H29F 109.5 . . C27B C30B H30D 109.5 . . C27B C30B H30E 109.5 . . C27B C30B H30F 109.5 . . H30D C30B H30E 109.5 . . H30D C30B H30F 109.5 . . H30E C30B H30F 109.5 . . N31A C31A C32A 175.0(15) . . C31A C32A H32A 109.5 . . C31A C32A H32B 109.5 . . C31A C32A H32C 109.5 . . H32A C32A H32B 109.5 . . H32A C32A H32C 109.5 . . H32B C32A H32C 109.5 . . N31B C31B C32B 173.8(16) . . C31B C32B H32D 109.5 . . C31B C32B H32E 109.5 . . C31B C32B H32F 109.5 . . H32D C32B H32E 109.5 . . H32D C32B H32F 109.5 . . H32E C32B H32F 109.5 . . C42 C41 H41 120.0 . . C42 C41 C46 120.0 . . C46 C41 H41 120.0 . . C41 C42 H42 120.0 . . C41 C42 C43 120.0 . . C43 C42 H42 120.0 . . C42 C43 H43 120.0 . . C42 C43 C44 120.0 . . C44 C43 H43 120.0 . . C43 C44 H44 120.0 . . C45 C44 C43 120.0 . . C45 C44 H44 120.0 . . C44 C45 H45 120.0 . . C46 C45 C44 120.0 . . C46 C45 H45 120.0 . . C41 C46 C47 121.7(9) . . C45 C46 C41 120.0 . . C45 C46 C47 118.3(9) . . C46 C47 H47A 109.5 . . C46 C47 H47B 109.5 . . C46 C47 H47C 109.5 . . H47A C47 H47B 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sm1 O1 2.3996(17) . Sm1 O2 2.4991(19) 7_556 Sm1 O4 2.5072(19) 7_556 Sm1 O7 2.423(2) . Sm1 O9 2.4173(19) 7_556 Sm1 O10 2.4894(19) . Sm1 O11 2.485(2) . Sm1 C21 2.844(3) . Sm1 O12 2.620(2) . Sm1 O13 2.518(2) . Mn1 O1 1.9102(17) . Mn1 O1 1.9053(17) 7_556 Mn1 O2 2.2012(18) . Mn1 O4 2.1972(19) 7_556 Mn1 O6 1.976(2) . Mn1 O8 1.984(2) . Mn2 O1 2.2923(18) . Mn2 N1A 2.410(5) . Mn2 N2A 2.340(6) . Mn2 N1B 2.359(6) . Mn2 N2B 2.468(8) . Mn2 O2 2.1746(19) . Mn2 O3A 2.451(4) . Mn2 O3B 2.122(6) . Mn2 O4 2.177(2) . Mn2 O5A 2.178(4) . Mn2 O5B 2.424(5) . N1A C1A 1.481(7) . N1A C3 1.548(6) . N1A C5A 1.479(7) . C1A H1AA 0.9900 . C1A H1AB 0.9900 . C1A C2A 1.516(10) . C2A H2AA 0.9900 . C2A H2AB 0.9900 . C2A N2A 1.487(10) . N2A C7 1.541(7) . N2A C9A 1.479(7) . N1B C1B 1.479(12) . N1B C3 1.479(7) . N1B C5B 1.469(9) . C1B H1BA 0.9900 . C1B H1BB 0.9900 . C1B C2B 1.508(11) . C2B H2BA 0.9900 . C2B H2BB 0.9900 . C2B N2B 1.473(9) . N2B C7 1.464(8) . N2B C9B 1.478(9) . C3 H3AA 0.9900 . C3 H3AB 0.9900 . C3 H3BC 0.9900 . C3 H3BD 0.9900 . C3 C4 1.519(4) . C4 H4A 0.9900 . C4 H4B 0.9900 . C4 O2 1.431(3) . C5A H5AA 0.9900 . C5A H5AB 0.9900 . C5A C6A 1.508(8) . C6A H6AA 0.9900 . C6A H6AB 0.9900 . C6A O3A 1.431(7) . O3A H3A 0.85(3) . C5B H5BA 0.9900 . C5B H5BB 0.9900 . C5B C6B 1.491(10) . C6B H6BA 0.9900 . C6B H6BB 0.9900 . C6B O3B 1.425(10) . O3B H3B 0.910(19) . C7 H7AA 0.9900 . C7 H7AB 0.9900 . C7 H7BC 0.9900 . C7 H7BD 0.9900 . C7 C8 1.518(4) . C8 H8A 0.9900 . C8 H8B 0.9900 . C8 O4 1.426(3) . C9A H9AA 0.9900 . C9A H9AB 0.9900 . C9A C10A 1.478(9) . C10A H10A 0.9900 . C10A H10B 0.9900 . C10A O5A 1.422(8) . O5A H5A 0.88(3) . C9B H9BA 0.9900 . C9B H9BB 0.9900 . C9B C10B 1.548(9) . C10B H10C 0.9900 . C10B H10D 0.9900 . C10B O5B 1.439(10) . O5B H5B 0.86(3) . O6 C11 1.268(3) . O7 C11 1.242(3) . C11 C12 1.541(4) . C12 C13A 1.532(7) . C12 C14A 1.479(8) . C12 C15A 1.638(7) . C12 C14B 1.633(10) . C12 C13B 1.503(9) . C12 C15B 1.463(10) . C12 C13C 1.543(14) . C12 C14C 1.475(11) . C12 C15C 1.541(10) . C13A H13A 0.9800 . C13A H13B 0.9800 . C13A H13C 0.9800 . C14A H14A 0.9800 . C14A H14B 0.9800 . C14A H14C 0.9800 . C15A H15A 0.9800 . C15A H15B 0.9800 . C15A H15C 0.9800 . C14B H14D 0.9800 . C14B H14E 0.9800 . C14B H14F 0.9800 . C13B H13D 0.9800 . C13B H13E 0.9800 . C13B H13F 0.9800 . C15B H15D 0.9800 . C15B H15E 0.9800 . C15B H15F 0.9800 . C13C H13G 0.9800 . C13C H13H 0.9800 . C13C H13I 0.9800 . C14C H14G 0.9800 . C14C H14H 0.9800 . C14C H14I 0.9800 . C15C H15G 0.9800 . C15C H15H 0.9800 . C15C H15I 0.9800 . O8 C16 1.267(3) . O9 C16 1.246(3) . C16 C17 1.536(4) . C17 C18 1.522(4) . C17 C19 1.540(4) . C17 C20 1.537(4) . 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 . O10 C21 1.265(3) . O11 C21 1.258(3) . C21 C22A 1.544(10) . C21 C22B 1.543(10) . C22A C23 1.542(10) . C22A C24A 1.539(11) . C22A C25A 1.516(10) . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C23 H23D 0.9800 . C23 H23E 0.9800 . C23 H23F 0.9800 . C23 C22B 1.544(10) . C24A H24A 0.9800 . C24A H24B 0.9800 . C24A H24C 0.9800 . C25A H25A 0.9800 . C25A H25B 0.9800 . C25A H25C 0.9800 . C22B C24B 1.548(10) . C22B C25B 1.517(10) . C24B H24D 0.9800 . C24B H24E 0.9800 . C24B H24F 0.9800 . C25B H25D 0.9800 . C25B H25E 0.9800 . C25B H25F 0.9800 . O12 C26 1.271(4) . O13 C26 1.254(4) . C26 C27A 1.560(8) . C26 C27B 1.573(8) . C27A C28A 1.528(10) . C27A C29A 1.499(12) . C27A C30A 1.519(10) . C28A H28A 0.9800 . C28A H28B 0.9800 . C28A H28C 0.9800 . C29A H29A 0.9800 . C29A H29B 0.9800 . C29A H29C 0.9800 . C30A H30A 0.9800 . C30A H30B 0.9800 . C30A H30C 0.9800 . C27B C28B 1.528(10) . C27B C29B 1.522(10) . C27B C30B 1.522(11) . C28B H28D 0.9800 . C28B H28E 0.9800 . C28B H28F 0.9800 . C29B H29D 0.9800 . C29B H29E 0.9800 . C29B H29F 0.9800 . C30B H30D 0.9800 . C30B H30E 0.9800 . C30B H30F 0.9800 . N31A C31A 1.132(9) . C31A C32A 1.503(13) . C32A H32A 0.9800 . C32A H32B 0.9800 . C32A H32C 0.9800 . N31B C31B 1.159(10) . C31B C32B 1.517(13) . C32B H32D 0.9800 . C32B H32E 0.9800 . C32B H32F 0.9800 . C41 H41 0.9500 . C41 C42 1.3900 . C41 C46 1.3900 . C42 H42 0.9500 . C42 C43 1.3900 . C43 H43 0.9500 . C43 C44 1.3900 . C44 H44 0.9500 . C44 C45 1.3900 . C45 H45 0.9500 . C45 C46 1.3900 . C46 C47 1.487(11) . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3A H3A O12 0.85(3) 1.78(4) 2.577(5) 154(6) yes O3B H3B O12 0.910(19) 1.967(18) 2.877(6) 180(11) yes O5A H5A O12 0.88(3) 1.971(19) 2.762(5) 148(6) yes O5B H5B O12 0.86(3) 1.966(19) 2.679(6) 139(5) yes