# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Peter Junk' 'Marcus Cole' _publ_contact_author_name 'Assoc. Prof. Peter C. Junk' _publ_contact_author_address ; School of Chemistry Monash University Victoria 3800 Australia ; _publ_contact_author_email peter.junk@sci.monash.edu.au _publ_contact_author_phone '+61 (0)3 9905 4570' _publ_contact_author_fax '+61 (0)3 9905 4597' _publ_requested_journal 'Chemical Communications' _publ_section_title ; The synthesis of a sterically hindered samarium(II) bis(amidinate) and conversion to its homoleptic trivalent congener ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 262796' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Sm(DippForm)2(THF)2]' _chemical_melting_point '475 (dec.)' _chemical_formula_moiety 'C58 H86 N4 O2 Sm' _chemical_formula_sum 'C58 H86 N4 O2 Sm' _chemical_formula_weight 1021.66 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1023(2) _cell_length_b 12.7993(3) _cell_length_c 19.6691(5) _cell_angle_alpha 84.4520(10) _cell_angle_beta 86.800(2) _cell_angle_gamma 63.9530(10) _cell_volume 2724.19(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombohedral plate' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8962 _exptl_absorpt_correction_T_max 0.9461 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24871 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.28 _reflns_number_total 13029 _reflns_number_gt 10328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+4.6574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13029 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.825263(18) 0.795281(17) 0.740367(9) 0.01902(6) Uani 1 1 d . . . O1 O 1.0155(3) 0.6944(3) 0.66483(16) 0.0452(8) Uani 1 1 d . . . O2 O 0.9423(2) 0.9202(2) 0.75429(14) 0.0347(7) Uani 1 1 d . . . N1 N 0.6678(3) 0.9822(3) 0.68164(15) 0.0244(7) Uani 1 1 d . . . N2 N 0.6691(3) 0.8152(3) 0.64775(14) 0.0223(7) Uani 1 1 d . . . N3 N 0.7757(3) 0.6522(3) 0.82011(14) 0.0197(6) Uani 1 1 d . . . N4 N 0.8856(3) 0.7329(2) 0.86874(14) 0.0186(6) Uani 1 1 d . . . C1 C 0.6246(3) 1.1048(3) 0.67217(17) 0.0223(8) Uani 1 1 d . . . C2 C 0.6828(3) 1.1545(3) 0.62502(18) 0.0253(8) Uani 1 1 d . . . C3 C 0.6427(4) 1.2753(3) 0.62021(19) 0.0289(9) Uani 1 1 d . . . H3 H 0.6804 1.3099 0.5877 0.035 Uiso 1 1 calc R . . C4 C 0.5500(4) 1.3447(3) 0.6618(2) 0.0319(9) Uani 1 1 d . . . H4 H 0.5240 1.4266 0.6580 0.038 Uiso 1 1 calc R . . C5 C 0.4946(4) 1.2960(3) 0.7087(2) 0.0304(9) Uani 1 1 d . . . H5 H 0.4308 1.3449 0.7375 0.036 Uiso 1 1 calc R . . C6 C 0.5301(3) 1.1762(3) 0.71512(18) 0.0259(8) Uani 1 1 d . . . C7 C 0.7892(4) 1.0795(4) 0.5796(2) 0.0343(10) Uani 1 1 d . . . H7 H 0.8163 0.9962 0.5975 0.041 Uiso 1 1 calc R . . C8 C 0.8999(4) 1.1060(5) 0.5806(3) 0.0559(14) Uani 1 1 d . . . H8A H 0.8774 1.1859 0.5610 0.084 Uiso 1 1 calc R . . H8B H 0.9674 1.0512 0.5537 0.084 Uiso 1 1 calc R . . H8C H 0.9261 1.0979 0.6279 0.084 Uiso 1 1 calc R . . C9 C 0.7458(5) 1.0916(5) 0.5065(2) 0.0525(13) Uani 1 1 d . . . H9A H 0.6772 1.0704 0.5067 0.079 Uiso 1 1 calc R . . H9B H 0.8137 1.0398 0.4785 0.079 Uiso 1 1 calc R . . H9C H 0.7185 1.1725 0.4875 0.079 Uiso 1 1 calc R . . C10 C 0.4697(4) 1.1246(3) 0.7695(2) 0.0314(9) Uani 1 1 d . . . H10 H 0.5019 1.0395 0.7633 0.038 Uiso 1 1 calc R . . C11 C 0.5051(4) 1.1362(5) 0.8412(2) 0.0480(12) Uani 1 1 d . . . H11A H 0.5950 1.0998 0.8447 0.072 Uiso 1 1 calc R . . H11B H 0.4709 1.0973 0.8754 0.072 Uiso 1 1 calc R . . H11C H 0.4723 1.2190 0.8492 0.072 Uiso 1 1 calc R . . C12 C 0.3300(4) 1.1791(4) 0.7641(2) 0.0419(11) Uani 1 1 d . . . H12A H 0.2959 1.2626 0.7703 0.063 Uiso 1 1 calc R . . H12B H 0.2964 1.1412 0.7995 0.063 Uiso 1 1 calc R . . H12C H 0.3079 1.1685 0.7189 0.063 Uiso 1 1 calc R . . C13 C 0.6228(3) 0.7604(3) 0.60513(19) 0.0254(8) Uani 1 1 d . . . C14 C 0.5325(4) 0.7262(3) 0.6317(2) 0.0283(9) Uani 1 1 d . . . C15 C 0.4965(4) 0.6608(4) 0.5932(2) 0.0368(10) Uani 1 1 d . . . H15 H 0.4380 0.6348 0.6118 0.044 Uiso 1 1 calc R . . C16 C 0.5442(4) 0.6334(4) 0.5287(2) 0.0438(11) Uani 1 1 d . . . H16 H 0.5184 0.5892 0.5029 0.053 Uiso 1 1 calc R . . C17 C 0.6287(4) 0.6702(4) 0.5020(2) 0.0415(11) Uani 1 1 d . . . H17 H 0.6597 0.6525 0.4570 0.050 Uiso 1 1 calc R . . C18 C 0.6713(4) 0.7330(4) 0.5387(2) 0.0323(9) Uani 1 1 d . . . C19 C 0.4728(4) 0.7628(3) 0.7011(2) 0.0300(9) Uani 1 1 d . . . H19 H 0.5375 0.7605 0.7315 0.036 Uiso 1 1 calc R . . C20 C 0.4179(4) 0.6846(4) 0.7364(2) 0.0378(10) Uani 1 1 d . . . H20A H 0.3486 0.6912 0.7099 0.057 Uiso 1 1 calc R . . H20B H 0.3889 0.7089 0.7824 0.057 Uiso 1 1 calc R . . H20C H 0.4807 0.6035 0.7397 0.057 Uiso 1 1 calc R . . C21 C 0.3725(4) 0.8893(4) 0.6937(2) 0.0396(10) Uani 1 1 d . . . H21A H 0.3064 0.8937 0.6652 0.059 Uiso 1 1 calc R . . H21B H 0.4080 0.9401 0.6721 0.059 Uiso 1 1 calc R . . H21C H 0.3390 0.9146 0.7389 0.059 Uiso 1 1 calc R . . C22 C 0.7682(4) 0.7680(4) 0.5072(2) 0.0386(10) Uani 1 1 d . . . H22 H 0.7839 0.8150 0.5398 0.046 Uiso 1 1 calc R . . C23 C 0.8895(5) 0.6584(5) 0.4964(3) 0.0687(17) Uani 1 1 d . . . H23A H 0.9176 0.6134 0.5403 0.103 Uiso 1 1 calc R . . H23B H 0.9522 0.6821 0.4768 0.103 Uiso 1 1 calc R . . H23C H 0.8759 0.6103 0.4651 0.103 Uiso 1 1 calc R . . C24 C 0.7262(6) 0.8426(6) 0.4403(3) 0.0709(17) Uani 1 1 d . . . H24A H 0.7039 0.8005 0.4087 0.106 Uiso 1 1 calc R . . H24B H 0.7930 0.8596 0.4202 0.106 Uiso 1 1 calc R . . H24C H 0.6545 0.9159 0.4489 0.106 Uiso 1 1 calc R . . C25 C 0.6293(3) 0.9293(3) 0.64065(18) 0.0211(8) Uani 1 1 d . . . H25 H 0.5724 0.9740 0.6058 0.025 Uiso 1 1 calc R . . C26 C 0.7183(3) 0.5750(3) 0.82993(17) 0.0219(8) Uani 1 1 d . . . C27 C 0.6251(3) 0.5934(3) 0.88075(18) 0.0236(8) Uani 1 1 d . . . C28 C 0.5732(3) 0.5150(3) 0.88883(19) 0.0279(9) Uani 1 1 d . . . H28 H 0.5120 0.5248 0.9233 0.034 Uiso 1 1 calc R . . C29 C 0.6087(4) 0.4233(3) 0.8480(2) 0.0296(9) Uani 1 1 d . . . H29 H 0.5725 0.3705 0.8548 0.036 Uiso 1 1 calc R . . C30 C 0.6964(3) 0.4086(3) 0.7976(2) 0.0278(9) Uani 1 1 d . . . H30 H 0.7195 0.3459 0.7694 0.033 Uiso 1 1 calc R . . C31 C 0.7522(3) 0.4844(3) 0.78683(18) 0.0229(8) Uani 1 1 d . . . C32 C 0.5800(3) 0.6982(3) 0.92347(18) 0.0258(8) Uani 1 1 d . . . H32 H 0.6549 0.7029 0.9390 0.031 Uiso 1 1 calc R . . C33 C 0.5062(4) 0.8121(4) 0.8812(2) 0.0413(11) Uani 1 1 d . . . H33A H 0.5548 0.8192 0.8410 0.062 Uiso 1 1 calc R . . H33B H 0.4862 0.8779 0.9090 0.062 Uiso 1 1 calc R . . H33C H 0.4299 0.8126 0.8665 0.062 Uiso 1 1 calc R . . C34 C 0.5069(4) 0.6893(4) 0.9876(2) 0.0354(10) Uani 1 1 d . . . H34A H 0.4275 0.6946 0.9746 0.053 Uiso 1 1 calc R . . H34B H 0.4931 0.7532 1.0157 0.053 Uiso 1 1 calc R . . H34C H 0.5530 0.6145 1.0137 0.053 Uiso 1 1 calc R . . C35 C 0.8527(3) 0.4646(3) 0.73327(19) 0.0272(8) Uani 1 1 d . . . H35 H 0.8571 0.5405 0.7221 0.033 Uiso 1 1 calc R . . C36 C 0.8300(4) 0.4252(4) 0.6665(2) 0.0443(11) Uani 1 1 d . . . H36A H 0.8354 0.3464 0.6746 0.066 Uiso 1 1 calc R . . H36B H 0.8923 0.4250 0.6323 0.066 Uiso 1 1 calc R . . H36C H 0.7480 0.4791 0.6497 0.066 Uiso 1 1 calc R . . C37 C 0.9771(4) 0.3772(4) 0.7629(2) 0.0422(11) Uani 1 1 d . . . H37A H 0.9941 0.4075 0.8030 0.063 Uiso 1 1 calc R . . H37B H 1.0421 0.3659 0.7284 0.063 Uiso 1 1 calc R . . H37C H 0.9748 0.3025 0.7764 0.063 Uiso 1 1 calc R . . C38 C 0.9628(3) 0.7237(3) 0.92304(16) 0.0182(7) Uani 1 1 d . . . C39 C 0.9230(3) 0.8153(3) 0.96679(17) 0.0216(8) Uani 1 1 d . . . C40 C 0.9971(3) 0.8055(3) 1.02073(18) 0.0270(8) Uani 1 1 d . . . H40 H 0.9703 0.8662 1.0507 0.032 Uiso 1 1 calc R . . C41 C 1.1090(4) 0.7096(4) 1.03198(19) 0.0301(9) Uani 1 1 d . . . H41 H 1.1572 0.7036 1.0699 0.036 Uiso 1 1 calc R . . C42 C 1.1501(3) 0.6223(3) 0.98748(18) 0.0265(8) Uani 1 1 d . . . H42 H 1.2281 0.5575 0.9944 0.032 Uiso 1 1 calc R . . C43 C 1.0790(3) 0.6278(3) 0.93253(17) 0.0201(7) Uani 1 1 d . . . C44 C 0.7992(3) 0.9202(3) 0.95696(18) 0.0237(8) Uani 1 1 d . . . H44 H 0.7749 0.9254 0.9085 0.028 Uiso 1 1 calc R . . C45 C 0.8022(4) 1.0351(3) 0.9685(2) 0.0322(9) Uani 1 1 d . . . H45A H 0.8112 1.0385 1.0174 0.048 Uiso 1 1 calc R . . H45B H 0.7255 1.1004 0.9525 0.048 Uiso 1 1 calc R . . H45C H 0.8719 1.0402 0.9431 0.048 Uiso 1 1 calc R . . C46 C 0.7003(4) 0.9045(4) 1.0030(2) 0.0362(10) Uani 1 1 d . . . H46A H 0.6977 0.8314 0.9945 0.054 Uiso 1 1 calc R . . H46B H 0.6200 0.9700 0.9929 0.054 Uiso 1 1 calc R . . H46C H 0.7199 0.9020 1.0509 0.054 Uiso 1 1 calc R . . C47 C 1.1307(3) 0.5298(3) 0.88421(18) 0.0229(8) Uani 1 1 d . . . H47 H 1.0708 0.5502 0.8465 0.028 Uiso 1 1 calc R . . C48 C 1.2533(4) 0.5189(4) 0.8522(2) 0.0333(9) Uani 1 1 d . . . H48A H 1.3142 0.4970 0.8881 0.050 Uiso 1 1 calc R . . H48B H 1.2418 0.5939 0.8285 0.050 Uiso 1 1 calc R . . H48C H 1.2824 0.4589 0.8195 0.050 Uiso 1 1 calc R . . C49 C 1.1464(4) 0.4137(3) 0.9201(2) 0.0312(9) Uani 1 1 d . . . H49A H 1.2039 0.3923 0.9578 0.047 Uiso 1 1 calc R . . H49B H 1.1787 0.3535 0.8876 0.047 Uiso 1 1 calc R . . H49C H 1.0665 0.4206 0.9382 0.047 Uiso 1 1 calc R . . C50 C 0.8413(3) 0.6546(3) 0.87107(17) 0.0186(7) Uani 1 1 d . . . H50 H 0.8567 0.5997 0.9097 0.022 Uiso 1 1 calc R . . C51 C 1.0913(4) 0.5705(4) 0.6748(3) 0.0532(13) Uani 1 1 d . . . H51A H 1.0546 0.5276 0.6523 0.064 Uiso 1 1 calc R . . H51B H 1.0988 0.5448 0.7241 0.064 Uiso 1 1 calc R . . C52 C 1.2116(4) 0.5478(4) 0.6448(2) 0.0501(12) Uani 1 1 d . . . H52A H 1.2555 0.4668 0.6314 0.060 Uiso 1 1 calc R . . H52B H 1.2631 0.5622 0.6766 0.060 Uiso 1 1 calc R . . C53 C 1.1773(4) 0.6364(4) 0.5822(2) 0.0472(12) Uani 1 1 d . . . H53A H 1.2460 0.6562 0.5677 0.057 Uiso 1 1 calc R . . H53B H 1.1544 0.6063 0.5435 0.057 Uiso 1 1 calc R . . C54 C 1.0689(4) 0.7403(4) 0.6078(2) 0.0464(12) Uani 1 1 d . . . H54A H 1.0957 0.7967 0.6233 0.056 Uiso 1 1 calc R . . H54B H 1.0079 0.7800 0.5712 0.056 Uiso 1 1 calc R . . C55 C 1.0669(4) 0.8597(4) 0.7791(2) 0.0384(10) Uani 1 1 d . . . H55A H 1.1268 0.8470 0.7407 0.046 Uiso 1 1 calc R . . H55B H 1.0812 0.7831 0.8027 0.046 Uiso 1 1 calc R . . C56 C 1.0806(4) 0.9372(4) 0.8284(2) 0.0413(11) Uani 1 1 d . . . H56A H 1.1658 0.9291 0.8280 0.050 Uiso 1 1 calc R . . H56B H 1.0569 0.9196 0.8756 0.050 Uiso 1 1 calc R . . C57 C 0.9914(5) 1.0578(4) 0.7995(2) 0.0445(11) Uani 1 1 d . . . H57A H 0.9645 1.1146 0.8348 0.053 Uiso 1 1 calc R . . H57B H 1.0285 1.0864 0.7603 0.053 Uiso 1 1 calc R . . C58 C 0.8862(4) 1.0370(4) 0.7772(2) 0.0373(10) Uani 1 1 d . . . H58A H 0.8283 1.0424 0.8158 0.045 Uiso 1 1 calc R . . H58B H 0.8410 1.0950 0.7396 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02265(10) 0.01361(9) 0.02112(10) 0.00122(6) -0.00267(7) -0.00847(7) O1 0.0444(18) 0.0284(17) 0.0565(19) -0.0008(15) 0.0074(15) -0.0116(14) O2 0.0380(16) 0.0244(15) 0.0484(17) 0.0014(13) -0.0109(13) -0.0194(13) N1 0.0295(17) 0.0125(15) 0.0252(16) -0.0012(13) -0.0034(14) -0.0033(13) N2 0.0289(17) 0.0152(15) 0.0232(15) -0.0011(12) -0.0067(13) -0.0093(13) N3 0.0243(15) 0.0179(15) 0.0199(14) -0.0015(12) 0.0000(13) -0.0120(13) N4 0.0213(15) 0.0157(15) 0.0202(14) -0.0009(12) -0.0017(12) -0.0093(13) C1 0.0264(19) 0.0159(18) 0.0225(18) 0.0003(15) -0.0039(15) -0.0072(15) C2 0.0248(19) 0.024(2) 0.0238(19) 0.0007(16) -0.0023(16) -0.0075(16) C3 0.036(2) 0.022(2) 0.028(2) 0.0027(16) -0.0013(18) -0.0128(18) C4 0.045(2) 0.0160(19) 0.035(2) -0.0037(17) -0.0019(19) -0.0128(18) C5 0.033(2) 0.018(2) 0.033(2) -0.0070(17) 0.0040(18) -0.0041(17) C6 0.029(2) 0.022(2) 0.0264(19) -0.0040(16) -0.0011(16) -0.0096(17) C7 0.033(2) 0.025(2) 0.034(2) -0.0019(18) 0.0065(19) -0.0034(18) C8 0.034(3) 0.077(4) 0.052(3) -0.021(3) 0.013(2) -0.018(3) C9 0.051(3) 0.063(3) 0.040(3) -0.022(2) 0.013(2) -0.019(3) C10 0.034(2) 0.021(2) 0.038(2) -0.0060(17) 0.0113(19) -0.0117(18) C11 0.046(3) 0.064(3) 0.036(2) 0.011(2) -0.001(2) -0.029(3) C12 0.038(2) 0.052(3) 0.038(2) -0.009(2) 0.007(2) -0.022(2) C13 0.028(2) 0.0156(18) 0.030(2) -0.0003(15) -0.0111(17) -0.0062(16) C14 0.031(2) 0.0166(19) 0.035(2) 0.0046(16) -0.0144(18) -0.0086(17) C15 0.039(2) 0.028(2) 0.048(3) 0.001(2) -0.016(2) -0.017(2) C16 0.056(3) 0.034(3) 0.050(3) -0.013(2) -0.017(2) -0.025(2) C17 0.049(3) 0.036(3) 0.037(2) -0.014(2) -0.010(2) -0.014(2) C18 0.036(2) 0.026(2) 0.031(2) -0.0065(17) -0.0069(18) -0.0077(18) C19 0.035(2) 0.025(2) 0.033(2) 0.0059(17) -0.0101(18) -0.0169(18) C20 0.041(2) 0.035(2) 0.043(2) 0.012(2) -0.011(2) -0.023(2) C21 0.040(2) 0.032(2) 0.043(2) 0.003(2) 0.003(2) -0.015(2) C22 0.046(3) 0.042(3) 0.029(2) -0.014(2) 0.004(2) -0.019(2) C23 0.046(3) 0.063(4) 0.088(4) -0.029(3) 0.009(3) -0.013(3) C24 0.086(4) 0.087(5) 0.053(3) 0.020(3) -0.016(3) -0.053(4) C25 0.0205(18) 0.0151(18) 0.0234(18) 0.0009(15) -0.0015(15) -0.0040(15) C26 0.0241(19) 0.0174(18) 0.0239(18) 0.0044(15) -0.0074(15) -0.0093(15) C27 0.0256(19) 0.023(2) 0.0243(18) 0.0046(15) -0.0063(16) -0.0126(16) C28 0.028(2) 0.029(2) 0.030(2) 0.0062(17) -0.0036(17) -0.0164(18) C29 0.032(2) 0.027(2) 0.038(2) 0.0049(18) -0.0066(18) -0.0212(18) C30 0.033(2) 0.0185(19) 0.036(2) 0.0009(17) -0.0074(18) -0.0146(17) C31 0.0258(19) 0.0162(18) 0.0273(19) 0.0035(15) -0.0061(16) -0.0100(16) C32 0.028(2) 0.025(2) 0.0263(19) -0.0007(16) 0.0013(16) -0.0134(17) C33 0.055(3) 0.025(2) 0.037(2) -0.0036(19) 0.001(2) -0.011(2) C34 0.034(2) 0.032(2) 0.035(2) -0.0027(19) 0.0063(19) -0.0102(19) C35 0.031(2) 0.0179(19) 0.035(2) -0.0038(16) -0.0003(17) -0.0127(17) C36 0.046(3) 0.050(3) 0.043(3) -0.018(2) 0.007(2) -0.025(2) C37 0.030(2) 0.037(3) 0.057(3) -0.004(2) 0.000(2) -0.013(2) C38 0.0232(18) 0.0186(18) 0.0165(16) -0.0001(14) 0.0018(14) -0.0130(15) C39 0.0244(19) 0.0193(19) 0.0217(18) -0.0014(15) 0.0025(15) -0.0106(16) C40 0.034(2) 0.026(2) 0.0237(19) -0.0073(16) -0.0023(17) -0.0138(18) C41 0.032(2) 0.035(2) 0.027(2) -0.0027(17) -0.0067(17) -0.0161(19) C42 0.0229(19) 0.025(2) 0.030(2) 0.0017(16) -0.0053(16) -0.0089(16) C43 0.0200(18) 0.0196(18) 0.0219(18) -0.0004(15) 0.0023(15) -0.0102(15) C44 0.0272(19) 0.0174(19) 0.0257(19) -0.0052(15) -0.0011(16) -0.0084(16) C45 0.032(2) 0.021(2) 0.042(2) -0.0076(18) -0.0012(19) -0.0090(18) C46 0.030(2) 0.028(2) 0.049(3) -0.007(2) 0.005(2) -0.0115(19) C47 0.0213(18) 0.0208(19) 0.0232(18) -0.0023(15) 0.0026(15) -0.0063(15) C48 0.031(2) 0.028(2) 0.037(2) -0.0046(18) 0.0086(19) -0.0103(18) C49 0.038(2) 0.022(2) 0.033(2) -0.0044(17) 0.0033(18) -0.0129(18) C50 0.0215(18) 0.0137(17) 0.0183(17) 0.0004(14) 0.0004(14) -0.0062(15) C51 0.051(3) 0.037(3) 0.064(3) -0.006(2) 0.008(3) -0.012(2) C52 0.047(3) 0.041(3) 0.049(3) -0.007(2) 0.005(2) -0.008(2) C53 0.040(3) 0.060(3) 0.043(3) -0.005(2) 0.006(2) -0.024(2) C54 0.052(3) 0.041(3) 0.048(3) -0.001(2) 0.004(2) -0.023(2) C55 0.030(2) 0.040(3) 0.047(3) 0.002(2) -0.004(2) -0.017(2) C56 0.038(2) 0.060(3) 0.035(2) -0.002(2) -0.003(2) -0.031(2) C57 0.067(3) 0.045(3) 0.038(2) 0.000(2) -0.007(2) -0.039(3) C58 0.052(3) 0.028(2) 0.034(2) 0.0001(18) -0.007(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.529(3) . ? Sm1 N3 2.546(3) . ? Sm1 O1 2.560(3) . ? Sm1 O2 2.599(3) . ? Sm1 N2 2.613(3) . ? Sm1 N4 2.617(3) . ? Sm1 C25 2.951(4) . ? Sm1 C50 2.957(3) . ? O1 C51 1.442(5) . ? O1 C54 1.465(5) . ? O2 C55 1.448(5) . ? O2 C58 1.450(5) . ? N1 C25 1.323(4) . ? N1 C1 1.415(4) . ? N2 C25 1.317(4) . ? N2 C13 1.422(4) . ? N3 C50 1.324(4) . ? N3 C26 1.431(4) . ? N4 C50 1.324(4) . ? N4 C38 1.421(4) . ? C1 C2 1.402(5) . ? C1 C6 1.408(5) . ? C2 C3 1.398(5) . ? C2 C7 1.527(5) . ? C3 C4 1.371(5) . ? C4 C5 1.370(5) . ? C5 C6 1.394(5) . ? C6 C10 1.522(5) . ? C7 C8 1.521(6) . ? C7 C9 1.528(6) . ? C10 C12 1.525(6) . ? C10 C11 1.535(6) . ? C13 C14 1.404(5) . ? C13 C18 1.413(5) . ? C14 C15 1.394(5) . ? C14 C19 1.524(5) . ? C15 C16 1.375(6) . ? C16 C17 1.364(6) . ? C17 C18 1.396(6) . ? C18 C22 1.512(6) . ? C19 C20 1.524(5) . ? C19 C21 1.538(6) . ? C22 C24 1.518(7) . ? C22 C23 1.544(7) . ? C26 C31 1.402(5) . ? C26 C27 1.419(5) . ? C27 C28 1.392(5) . ? C27 C32 1.525(5) . ? C28 C29 1.381(5) . ? C29 C30 1.374(5) . ? C30 C31 1.401(5) . ? C31 C35 1.513(5) . ? C32 C33 1.523(6) . ? C32 C34 1.523(5) . ? C35 C36 1.531(5) . ? C35 C37 1.533(6) . ? C38 C43 1.409(5) . ? C38 C39 1.414(5) . ? C39 C40 1.388(5) . ? C39 C44 1.517(5) . ? C40 C41 1.382(5) . ? C41 C42 1.383(5) . ? C42 C43 1.396(5) . ? C43 C47 1.532(5) . ? C44 C45 1.527(5) . ? C44 C46 1.532(5) . ? C47 C49 1.518(5) . ? C47 C48 1.533(5) . ? C51 C52 1.455(6) . ? C52 C53 1.532(7) . ? C53 C54 1.505(6) . ? C55 C56 1.516(6) . ? C56 C57 1.519(7) . ? C57 C58 1.505(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sm1 N3 125.17(10) . . ? N1 Sm1 O1 112.24(10) . . ? N3 Sm1 O1 112.94(9) . . ? N1 Sm1 O2 83.68(9) . . ? N3 Sm1 O2 134.07(9) . . ? O1 Sm1 O2 79.12(9) . . ? N1 Sm1 N2 52.92(9) . . ? N3 Sm1 N2 94.15(9) . . ? O1 Sm1 N2 94.55(10) . . ? O2 Sm1 N2 130.20(9) . . ? N1 Sm1 N4 131.96(9) . . ? N3 Sm1 N4 52.89(9) . . ? O1 Sm1 N4 109.15(9) . . ? O2 Sm1 N4 81.18(9) . . ? N2 Sm1 N4 144.63(9) . . ? N1 Sm1 C25 26.52(9) . . ? N3 Sm1 C25 112.49(9) . . ? O1 Sm1 C25 103.31(10) . . ? O2 Sm1 C25 106.67(9) . . ? N2 Sm1 C25 26.49(9) . . ? N4 Sm1 C25 147.52(9) . . ? N1 Sm1 C50 136.51(9) . . ? N3 Sm1 C50 26.52(9) . . ? O1 Sm1 C50 111.12(9) . . ? O2 Sm1 C50 107.64(9) . . ? N2 Sm1 C50 120.36(9) . . ? N4 Sm1 C50 26.59(9) . . ? C25 Sm1 C50 134.93(9) . . ? C51 O1 C54 107.6(3) . . ? C51 O1 Sm1 121.0(3) . . ? C54 O1 Sm1 131.5(2) . . ? C55 O2 C58 109.0(3) . . ? C55 O2 Sm1 117.3(2) . . ? C58 O2 Sm1 124.6(2) . . ? C25 N1 C1 119.3(3) . . ? C25 N1 Sm1 94.8(2) . . ? C1 N1 Sm1 145.1(2) . . ? C25 N2 C13 119.8(3) . . ? C25 N2 Sm1 91.3(2) . . ? C13 N2 Sm1 148.7(2) . . ? C50 N3 C26 117.3(3) . . ? C50 N3 Sm1 94.3(2) . . ? C26 N3 Sm1 148.3(2) . . ? C50 N4 C38 116.9(3) . . ? C50 N4 Sm1 91.2(2) . . ? C38 N4 Sm1 148.5(2) . . ? C2 C1 C6 119.8(3) . . ? C2 C1 N1 120.6(3) . . ? C6 C1 N1 119.3(3) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C7 119.6(3) . . ? C1 C2 C7 121.4(3) . . ? C4 C3 C2 120.9(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 121.2(3) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C10 119.8(3) . . ? C1 C6 C10 121.3(3) . . ? C8 C7 C2 113.1(4) . . ? C8 C7 C9 110.7(4) . . ? C2 C7 C9 110.3(3) . . ? C6 C10 C12 113.1(3) . . ? C6 C10 C11 110.5(3) . . ? C12 C10 C11 109.8(3) . . ? C14 C13 C18 119.7(3) . . ? C14 C13 N2 118.7(3) . . ? C18 C13 N2 121.5(3) . . ? C15 C14 C13 119.2(4) . . ? C15 C14 C19 120.6(4) . . ? C13 C14 C19 120.2(3) . . ? C16 C15 C14 121.2(4) . . ? C17 C16 C15 119.4(4) . . ? C16 C17 C18 122.2(4) . . ? C17 C18 C13 118.3(4) . . ? C17 C18 C22 119.6(4) . . ? C13 C18 C22 122.1(4) . . ? C20 C19 C14 114.4(3) . . ? C20 C19 C21 109.3(3) . . ? C14 C19 C21 109.7(3) . . ? C18 C22 C24 111.9(4) . . ? C18 C22 C23 110.1(4) . . ? C24 C22 C23 110.5(4) . . ? N2 C25 N1 120.6(3) . . ? N2 C25 Sm1 62.25(19) . . ? N1 C25 Sm1 58.65(18) . . ? C31 C26 C27 120.9(3) . . ? C31 C26 N3 118.9(3) . . ? C27 C26 N3 120.2(3) . . ? C28 C27 C26 117.9(3) . . ? C28 C27 C32 121.0(3) . . ? C26 C27 C32 121.0(3) . . ? C29 C28 C27 121.6(3) . . ? C30 C29 C28 119.9(4) . . ? C29 C30 C31 121.4(4) . . ? C30 C31 C26 118.2(3) . . ? C30 C31 C35 121.0(3) . . ? C26 C31 C35 120.6(3) . . ? C33 C32 C34 109.6(3) . . ? C33 C32 C27 111.8(3) . . ? C34 C32 C27 114.7(3) . . ? C31 C35 C36 114.2(3) . . ? C31 C35 C37 109.8(3) . . ? C36 C35 C37 110.5(3) . . ? C43 C38 C39 119.8(3) . . ? C43 C38 N4 121.5(3) . . ? C39 C38 N4 118.7(3) . . ? C40 C39 C38 118.8(3) . . ? C40 C39 C44 120.4(3) . . ? C38 C39 C44 120.7(3) . . ? C41 C40 C39 121.7(3) . . ? C40 C41 C42 119.4(4) . . ? C41 C42 C43 121.1(4) . . ? C42 C43 C38 119.0(3) . . ? C42 C43 C47 118.7(3) . . ? C38 C43 C47 122.3(3) . . ? C39 C44 C45 113.2(3) . . ? C39 C44 C46 111.1(3) . . ? C45 C44 C46 110.0(3) . . ? C49 C47 C43 111.8(3) . . ? C49 C47 C48 110.2(3) . . ? C43 C47 C48 110.8(3) . . ? N3 C50 N4 120.6(3) . . ? N3 C50 Sm1 59.14(18) . . ? N4 C50 Sm1 62.25(18) . . ? O1 C51 C52 107.2(4) . . ? C51 C52 C53 101.7(4) . . ? C54 C53 C52 102.8(3) . . ? O1 C54 C53 106.0(4) . . ? O2 C55 C56 106.3(3) . . ? C55 C56 C57 101.8(3) . . ? C58 C57 C56 102.4(4) . . ? O2 C58 C57 105.4(4) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.843 _refine_diff_density_min -1.615 _refine_diff_density_rms 0.122 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 262797' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Na(THF)5][Sm(I)2(DippForm)2(THF)]' _chemical_melting_point 451 _chemical_formula_moiety 'C74 H118 I2 N4 Na1 O6 Sm1' _chemical_formula_sum 'C148 H236 I4 N8 Na2 O12 Sm2' _chemical_formula_weight 3173.73 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.7632(3) _cell_length_b 14.3697(2) _cell_length_c 41.5794(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.7860(10) _cell_angle_gamma 90.00 _cell_volume 15982.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6536 _exptl_absorpt_coefficient_mu 1.560 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6518 _exptl_absorpt_correction_T_max 0.8596 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61917 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1134 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 28.30 _reflns_number_total 30037 _reflns_number_gt 16943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30037 _refine_ls_number_parameters 1618 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.2321 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.366770(15) 0.96582(3) 0.142540(11) 0.017 Uani 1 1 d . . . Sm2 Sm 0.867430(15) 1.01604(3) 0.141610(11) 0.016 Uani 1 1 d . . . I1 I 0.27391(2) 0.85163(4) 0.118690(15) 0.026 Uani 1 1 d . . . I2 I 0.45688(2) 1.07444(4) 0.172630(16) 0.027 Uani 1 1 d . . . I3 I 0.772920(19) 1.13643(4) 0.126410(15) 0.023 Uani 1 1 d . . . I4 I 0.96108(2) 0.90540(4) 0.164280(17) 0.031 Uani 1 1 d . . . Na1 Na 0.40189(12) 0.9179(2) 0.37644(9) 0.027 Uani 1 1 d . . . Na2 Na 0.90728(14) 1.0719(3) 0.38111(11) 0.044 Uani 1 1 d . . . O1 O 0.3298(2) 0.9504(4) 0.19639(15) 0.029 Uani 1 1 d . . . O2 O 0.3267(2) 1.0000(4) 0.37852(17) 0.038 Uani 1 1 d . . . O3 O 0.3747(2) 0.8183(4) 0.41586(18) 0.043 Uani 1 1 d . . . O4 O 0.4455(2) 1.0045(4) 0.41557(17) 0.037 Uani 1 1 d . . . O5 O 0.4496(2) 0.9946(4) 0.33816(16) 0.037 Uani 1 1 d . . . O6 O 0.3867(2) 0.8031(4) 0.33743(17) 0.036 Uani 1 1 d . . . O7 O 0.8356(2) 1.0064(4) 0.19736(14) 0.028 Uani 1 1 d . . . O8 O 0.8321(3) 0.9946(5) 0.3779(2) 0.054 Uani 1 1 d . . . O9 O 0.8868(3) 1.1831(5) 0.3438(2) 0.060 Uani 1 1 d . . . O10 O 0.8871(3) 1.1709(6) 0.4221(2) 0.078 Uani 1 1 d . . . O11 O 0.9551(3) 0.9796(4) 0.41608(19) 0.055 Uani 1 1 d . . . O12 O 0.9542(3) 1.0102(6) 0.3381(2) 0.072 Uani 1 1 d . . . N1 N 0.3138(2) 1.1095(4) 0.14576(17) 0.017 Uani 1 1 d . . . N2 N 0.3599(2) 1.0899(4) 0.10187(16) 0.017 Uani 1 1 d . . . N3 N 0.4107(2) 0.8197(4) 0.16160(17) 0.017 Uani 1 1 d . . . N4 N 0.4159(2) 0.8594(5) 0.10806(18) 0.022 Uani 1 1 d . . . N5 N 0.8151(2) 0.8699(4) 0.13939(17) 0.018 Uani 1 1 d . . . N6 N 0.8570(2) 0.9118(4) 0.09469(16) 0.016 Uani 1 1 d . . . N7 N 0.9105(2) 1.1565(4) 0.16583(17) 0.017 Uani 1 1 d . . . N8 N 0.9143(2) 1.1333(4) 0.11065(17) 0.018 Uani 1 1 d . . . C1 C 0.2770(3) 1.1550(5) 0.1626(2) 0.024 Uani 1 1 d . . . C2 C 0.2896(3) 1.1994(6) 0.1911(2) 0.025 Uani 1 1 d . . . C3 C 0.2530(3) 1.2392(6) 0.2109(3) 0.040 Uani 1 1 d . . . H3 H 0.2624 1.2689 0.2306 0.048 Uiso 1 1 calc R . . C4 C 0.2033(4) 1.2338(7) 0.2009(3) 0.051 Uani 1 1 d . . . H4 H 0.1781 1.2595 0.2138 0.061 Uiso 1 1 calc R . . C5 C 0.1897(3) 1.1881(6) 0.1702(3) 0.049 Uani 1 1 d . . . H5 H 0.1557 1.1857 0.1631 0.058 Uiso 1 1 calc R . . C6 C 0.2261(3) 1.1485(6) 0.1515(2) 0.025 Uani 1 1 d . . . C7 C 0.3434(3) 1.2157(7) 0.2009(2) 0.040 Uani 1 1 d . . . H7 H 0.3628 1.1633 0.1916 0.048 Uiso 1 1 calc R . . C8 C 0.3542(4) 1.2131(7) 0.2379(3) 0.058 Uani 1 1 d . . . H8A H 0.3390 1.2676 0.2480 0.087 Uiso 1 1 calc R . . H8B H 0.3904 1.2139 0.2423 0.087 Uiso 1 1 calc R . . H8C H 0.3399 1.1562 0.2469 0.087 Uiso 1 1 calc R . . C9 C 0.3625(4) 1.3024(8) 0.1861(3) 0.065 Uani 1 1 d . . . H9A H 0.3536 1.3028 0.1630 0.097 Uiso 1 1 calc R . . H9B H 0.3990 1.3049 0.1890 0.097 Uiso 1 1 calc R . . H9C H 0.3477 1.3566 0.1964 0.097 Uiso 1 1 calc R . . C10 C 0.2087(3) 1.1020(6) 0.1213(2) 0.029 Uani 1 1 d . . . H10 H 0.2376 1.0661 0.1129 0.035 Uiso 1 1 calc R . . C11 C 0.1658(3) 1.0345(7) 0.1248(3) 0.055 Uani 1 1 d . . . H11A H 0.1733 0.9921 0.1428 0.082 Uiso 1 1 calc R . . H11B H 0.1611 0.9986 0.1049 0.082 Uiso 1 1 calc R . . H11C H 0.1352 1.0692 0.1290 0.082 Uiso 1 1 calc R . . C12 C 0.1927(4) 1.1736(7) 0.0953(3) 0.043 Uani 1 1 d . . . H12A H 0.1629 1.2068 0.1020 0.065 Uiso 1 1 calc R . . H12B H 0.1853 1.1413 0.0749 0.065 Uiso 1 1 calc R . . H12C H 0.2199 1.2182 0.0923 0.065 Uiso 1 1 calc R . . C13 C 0.3765(3) 1.1290(5) 0.0727(2) 0.021 Uani 1 1 d . . . C14 C 0.3646(3) 1.0814(6) 0.0430(2) 0.028 Uani 1 1 d . . . C15 C 0.3812(3) 1.1164(6) 0.0141(2) 0.036 Uani 1 1 d . . . H15 H 0.3739 1.0845 -0.0055 0.043 Uiso 1 1 calc R . . C16 C 0.4094(3) 1.2010(7) 0.0143(3) 0.046 Uani 1 1 d . . . H16 H 0.4208 1.2260 -0.0053 0.055 Uiso 1 1 calc R . . C17 C 0.4199(3) 1.2465(6) 0.0430(3) 0.036 Uani 1 1 d . . . H17 H 0.4380 1.3033 0.0426 0.043 Uiso 1 1 calc R . . C18 C 0.4048(3) 1.2114(6) 0.0732(2) 0.030 Uani 1 1 d . . . C19 C 0.3310(3) 0.9991(6) 0.0422(2) 0.031 Uani 1 1 d . . . H19 H 0.3396 0.9619 0.0619 0.037 Uiso 1 1 calc R . . C20 C 0.3374(4) 0.9352(6) 0.0140(2) 0.038 Uani 1 1 d . . . H20A H 0.3291 0.9687 -0.0060 0.057 Uiso 1 1 calc R . . H20B H 0.3152 0.8814 0.0159 0.057 Uiso 1 1 calc R . . H20C H 0.3722 0.9139 0.0136 0.057 Uiso 1 1 calc R . . C21 C 0.2757(3) 1.0294(7) 0.0452(2) 0.039 Uani 1 1 d . . . H21A H 0.2721 1.0650 0.0651 0.058 Uiso 1 1 calc R . . H21B H 0.2543 0.9742 0.0456 0.058 Uiso 1 1 calc R . . H21C H 0.2658 1.0683 0.0267 0.058 Uiso 1 1 calc R . . C22 C 0.4187(3) 1.2639(5) 0.1040(2) 0.030 Uani 1 1 d . . . H22 H 0.4068 1.2264 0.1225 0.036 Uiso 1 1 calc R . . C23 C 0.4757(3) 1.2756(6) 0.1084(3) 0.043 Uani 1 1 d . . . H23A H 0.4913 1.2144 0.1114 0.064 Uiso 1 1 calc R . . H23B H 0.4832 1.3143 0.1274 0.064 Uiso 1 1 calc R . . H23C H 0.4889 1.3056 0.0893 0.064 Uiso 1 1 calc R . . C24 C 0.3928(4) 1.3604(6) 0.1052(3) 0.049 Uani 1 1 d . . . H24A H 0.4036 1.3930 0.1249 0.073 Uiso 1 1 calc R . . H24B H 0.3565 1.3521 0.1049 0.073 Uiso 1 1 calc R . . H24C H 0.4021 1.3972 0.0864 0.073 Uiso 1 1 calc R . . C25 C 0.3269(3) 1.1388(5) 0.1182(2) 0.017 Uani 1 1 d . . . H25 H 0.3132 1.1947 0.1095 0.021 Uiso 1 1 calc R . . C26 C 0.4271(3) 0.7651(5) 0.1882(2) 0.020 Uani 1 1 d . . . C27 C 0.3919(3) 0.7071(5) 0.2034(2) 0.020 Uani 1 1 d . . . C28 C 0.4066(3) 0.6560(6) 0.2301(2) 0.030 Uani 1 1 d . . . H28 H 0.3836 0.6159 0.2401 0.036 Uiso 1 1 calc R . . C29 C 0.4550(3) 0.6637(6) 0.2422(2) 0.028 Uani 1 1 d . . . H29 H 0.4650 0.6304 0.2610 0.033 Uiso 1 1 calc R . . C30 C 0.4885(3) 0.7183(5) 0.2273(2) 0.024 Uani 1 1 d . . . H30 H 0.5218 0.7209 0.2357 0.029 Uiso 1 1 calc R . . C31 C 0.4759(3) 0.7698(5) 0.2005(2) 0.020 Uani 1 1 d . . . C32 C 0.3385(3) 0.6974(6) 0.1892(2) 0.028 Uani 1 1 d . . . H32 H 0.3296 0.7578 0.1785 0.034 Uiso 1 1 calc R . . C33 C 0.2981(3) 0.6768(7) 0.2131(2) 0.042 Uani 1 1 d . . . H33A H 0.3017 0.6126 0.2207 0.063 Uiso 1 1 calc R . . H33B H 0.2652 0.6849 0.2026 0.063 Uiso 1 1 calc R . . H33C H 0.3016 0.7196 0.2313 0.063 Uiso 1 1 calc R . . C34 C 0.3386(4) 0.6218(7) 0.1624(3) 0.052 Uani 1 1 d . . . H34A H 0.3463 0.5611 0.1720 0.078 Uiso 1 1 calc R . . H34B H 0.3638 0.6373 0.1467 0.078 Uiso 1 1 calc R . . H34C H 0.3055 0.6193 0.1515 0.078 Uiso 1 1 calc R . . C35 C 0.5165(3) 0.8286(6) 0.1843(2) 0.025 Uani 1 1 d . . . H35 H 0.4998 0.8722 0.1686 0.030 Uiso 1 1 calc R . . C36 C 0.5470(3) 0.8852(6) 0.2086(3) 0.041 Uani 1 1 d . . . H36A H 0.5682 0.8434 0.2217 0.061 Uiso 1 1 calc R . . H36B H 0.5245 0.9195 0.2224 0.061 Uiso 1 1 calc R . . H36C H 0.5682 0.9292 0.1972 0.061 Uiso 1 1 calc R . . C37 C 0.5512(3) 0.7675(6) 0.1666(2) 0.035 Uani 1 1 d . . . H37A H 0.5737 0.8060 0.1540 0.052 Uiso 1 1 calc R . . H37B H 0.5319 0.7264 0.1521 0.052 Uiso 1 1 calc R . . H37C H 0.5710 0.7299 0.1820 0.052 Uiso 1 1 calc R . . C38 C 0.4303(3) 0.8345(5) 0.0767(2) 0.016 Uani 1 1 d . . . C39 C 0.4652(3) 0.8918(6) 0.0612(2) 0.022 Uani 1 1 d . . . C40 C 0.4789(3) 0.8681(6) 0.0303(2) 0.028 Uani 1 1 d . . . H40 H 0.5025 0.9062 0.0199 0.033 Uiso 1 1 calc R . . C41 C 0.4596(3) 0.7909(6) 0.0139(2) 0.028 Uani 1 1 d . . . H41 H 0.4690 0.7769 -0.0074 0.034 Uiso 1 1 calc R . . C42 C 0.4258(3) 0.7349(6) 0.0300(2) 0.027 Uani 1 1 d . . . H42 H 0.4131 0.6806 0.0195 0.033 Uiso 1 1 calc R . . C43 C 0.4101(3) 0.7552(6) 0.0602(2) 0.023 Uani 1 1 d . . . C44 C 0.4897(3) 0.9744(6) 0.0790(2) 0.023 Uani 1 1 d . . . H44 H 0.4641 1.0019 0.0932 0.027 Uiso 1 1 calc R . . C45 C 0.5062(3) 1.0510(6) 0.0560(2) 0.031 Uani 1 1 d . . . H45A H 0.5141 1.1076 0.0683 0.047 Uiso 1 1 calc R . . H45B H 0.4792 1.0640 0.0402 0.047 Uiso 1 1 calc R . . H45C H 0.5360 1.0304 0.0449 0.047 Uiso 1 1 calc R . . C46 C 0.5329(3) 0.9399(7) 0.1004(2) 0.036 Uani 1 1 d . . . H46A H 0.5599 0.9176 0.0870 0.054 Uiso 1 1 calc R . . H46B H 0.5214 0.8890 0.1140 0.054 Uiso 1 1 calc R . . H46C H 0.5453 0.9910 0.1141 0.054 Uiso 1 1 calc R . . C47 C 0.3701(3) 0.6923(5) 0.0748(2) 0.023 Uani 1 1 d . . . H47 H 0.3606 0.7203 0.0958 0.028 Uiso 1 1 calc R . . C48 C 0.3227(3) 0.6831(6) 0.0537(2) 0.036 Uani 1 1 d . . . H48A H 0.3106 0.7452 0.0477 0.055 Uiso 1 1 calc R . . H48B H 0.2971 0.6505 0.0657 0.055 Uiso 1 1 calc R . . H48C H 0.3301 0.6478 0.0343 0.055 Uiso 1 1 calc R . . C49 C 0.3912(3) 0.5969(6) 0.0817(2) 0.038 Uani 1 1 d . . . H49A H 0.4057 0.5719 0.0621 0.057 Uiso 1 1 calc R . . H49B H 0.3645 0.5556 0.0886 0.057 Uiso 1 1 calc R . . H49C H 0.4172 0.6012 0.0987 0.057 Uiso 1 1 calc R . . C50 C 0.4276(3) 0.8012(6) 0.1324(2) 0.020 Uani 1 1 d . . . H50 H 0.4475 0.7477 0.1289 0.025 Uiso 1 1 calc R . . C51 C 0.3569(3) 0.9452(7) 0.2283(2) 0.038 Uani 1 1 d . . . H51A H 0.3789 1.0001 0.2314 0.045 Uiso 1 1 calc R . . H51B H 0.3779 0.8885 0.2295 0.045 Uiso 1 1 calc R . . C52 C 0.3173(4) 0.9427(8) 0.2547(3) 0.049 Uani 1 1 d . . . H52A H 0.3265 0.9840 0.2730 0.058 Uiso 1 1 calc R . . H52B H 0.3119 0.8787 0.2628 0.058 Uiso 1 1 calc R . . C53 C 0.2707(3) 0.9795(7) 0.2354(2) 0.039 Uani 1 1 d . . . H53A H 0.2396 0.9558 0.2448 0.046 Uiso 1 1 calc R . . H53B H 0.2699 1.0484 0.2357 0.046 Uiso 1 1 calc R . . C54 C 0.2756(3) 0.9441(6) 0.2015(2) 0.029 Uani 1 1 d . . . H54A H 0.2637 0.8791 0.1994 0.034 Uiso 1 1 calc R . . H54B H 0.2565 0.9836 0.1859 0.034 Uiso 1 1 calc R . . C55 C 0.3215(4) 1.0642(6) 0.4043(3) 0.054 Uani 1 1 d . . . H55A H 0.3326 1.1271 0.3979 0.064 Uiso 1 1 calc R . . H55B H 0.3417 1.0442 0.4234 0.064 Uiso 1 1 calc R . . C56 C 0.2644(4) 1.0648(6) 0.4119(3) 0.051 Uani 1 1 d . . . H56A H 0.2560 1.0151 0.4272 0.061 Uiso 1 1 calc R . . H56B H 0.2538 1.1257 0.4205 0.061 Uiso 1 1 calc R . . C57 C 0.2405(4) 1.0462(7) 0.3780(3) 0.042 Uani 1 1 d . . . H57A H 0.2074 1.0163 0.3795 0.050 Uiso 1 1 calc R . . H57B H 0.2368 1.1047 0.3655 0.050 Uiso 1 1 calc R . . C58 C 0.2774(4) 0.9818(7) 0.3628(3) 0.046 Uani 1 1 d . . . H58A H 0.2675 0.9161 0.3661 0.056 Uiso 1 1 calc R . . H58B H 0.2786 0.9937 0.3394 0.056 Uiso 1 1 calc R . . C59 C 0.3951(4) 0.7300(7) 0.4200(3) 0.064 Uani 1 1 d . . . H59A H 0.4261 0.7334 0.4336 0.076 Uiso 1 1 calc R . . H59B H 0.4035 0.7033 0.3989 0.076 Uiso 1 1 calc R . . C60 C 0.3561(4) 0.6681(6) 0.4363(3) 0.045 Uani 1 1 d . . . H60A H 0.3364 0.6319 0.4201 0.055 Uiso 1 1 calc R . . H60B H 0.3725 0.6246 0.4518 0.055 Uiso 1 1 calc R . . C61 C 0.3235(4) 0.7374(6) 0.4534(3) 0.041 Uani 1 1 d . . . H61A H 0.2880 0.7174 0.4527 0.049 Uiso 1 1 calc R . . H61B H 0.3348 0.7456 0.4761 0.049 Uiso 1 1 calc R . . C62 C 0.3303(4) 0.8239(7) 0.4346(3) 0.059 Uani 1 1 d . . . H62A H 0.3008 0.8339 0.4201 0.071 Uiso 1 1 calc R . . H62B H 0.3331 0.8776 0.4495 0.071 Uiso 1 1 calc R . . C63 C 0.4560(5) 0.9876(7) 0.4489(3) 0.069 Uani 1 1 d . . . H63A H 0.4891 0.9574 0.4516 0.083 Uiso 1 1 calc R . . H63B H 0.4306 0.9447 0.4573 0.083 Uiso 1 1 calc R . . C64 C 0.4558(5) 1.0725(8) 0.4669(3) 0.075 Uani 1 1 d . . . H64A H 0.4885 1.0826 0.4782 0.090 Uiso 1 1 calc R . . H64B H 0.4292 1.0718 0.4829 0.090 Uiso 1 1 calc R . . C65 C 0.4458(4) 1.1477(8) 0.4417(3) 0.055 Uani 1 1 d . . . H65A H 0.4111 1.1707 0.4427 0.066 Uiso 1 1 calc R . . H65B H 0.4690 1.2007 0.4450 0.066 Uiso 1 1 calc R . . C66 C 0.4544(4) 1.1015(6) 0.4096(3) 0.043 Uani 1 1 d . . . H66A H 0.4309 1.1258 0.3928 0.051 Uiso 1 1 calc R . . H66B H 0.4891 1.1118 0.4028 0.051 Uiso 1 1 calc R . . C67 C 0.5031(4) 1.0037(7) 0.3333(3) 0.044 Uani 1 1 d . . . H67A H 0.5226 0.9820 0.3525 0.053 Uiso 1 1 calc R . . H67B H 0.5120 1.0692 0.3289 0.053 Uiso 1 1 calc R . . C68 C 0.5127(4) 0.9438(7) 0.3050(3) 0.051 Uani 1 1 d . . . H68A H 0.5169 0.8778 0.3114 0.061 Uiso 1 1 calc R . . H68B H 0.5430 0.9644 0.2939 0.061 Uiso 1 1 calc R . . C69 C 0.4635(4) 0.9581(7) 0.2827(3) 0.052 Uani 1 1 d . . . H69A H 0.4693 1.0033 0.2653 0.062 Uiso 1 1 calc R . . H69B H 0.4519 0.8985 0.2732 0.062 Uiso 1 1 calc R . . C70 C 0.4261(4) 0.9956(7) 0.3064(3) 0.044 Uani 1 1 d . . . H70A H 0.4162 1.0599 0.3004 0.052 Uiso 1 1 calc R . . H70B H 0.3957 0.9563 0.3060 0.052 Uiso 1 1 calc R . . C71 C 0.4213(3) 0.7384(6) 0.3254(2) 0.032 Uani 1 1 d . . . H71A H 0.4497 0.7293 0.3409 0.038 Uiso 1 1 calc R . . H71B H 0.4344 0.7600 0.3047 0.038 Uiso 1 1 calc R . . C72 C 0.3917(3) 0.6488(6) 0.3209(2) 0.035 Uani 1 1 d . . . H72A H 0.3911 0.6124 0.3411 0.042 Uiso 1 1 calc R . . H72B H 0.4056 0.6096 0.3038 0.042 Uiso 1 1 calc R . . C73 C 0.3393(3) 0.6852(6) 0.3112(2) 0.036 Uani 1 1 d . . . H73A H 0.3365 0.6978 0.2878 0.043 Uiso 1 1 calc R . . H73B H 0.3131 0.6402 0.3170 0.043 Uiso 1 1 calc R . . C74 C 0.3353(3) 0.7735(6) 0.3303(2) 0.037 Uani 1 1 d . . . H74A H 0.3170 0.8216 0.3176 0.045 Uiso 1 1 calc R . . H74B H 0.3174 0.7622 0.3504 0.045 Uiso 1 1 calc R . . C75 C 0.7802(3) 0.8120(5) 0.1546(2) 0.018 Uani 1 1 d . . . C76 C 0.7973(3) 0.7493(6) 0.1784(2) 0.028 Uani 1 1 d . . . C77 C 0.7617(4) 0.6950(6) 0.1940(2) 0.040 Uani 1 1 d . . . H77 H 0.7728 0.6535 0.2106 0.048 Uiso 1 1 calc R . . C78 C 0.7113(3) 0.6999(6) 0.1862(3) 0.041 Uani 1 1 d . . . H78 H 0.6882 0.6617 0.1970 0.050 Uiso 1 1 calc R . . C79 C 0.6949(3) 0.7599(6) 0.1627(2) 0.037 Uani 1 1 d . . . H79 H 0.6603 0.7624 0.1570 0.045 Uiso 1 1 calc R . . C80 C 0.7284(3) 0.8186(6) 0.1468(2) 0.030 Uani 1 1 d . . . C81 C 0.8538(3) 0.7389(6) 0.1853(2) 0.035 Uani 1 1 d . . . H81 H 0.8697 0.7985 0.1787 0.042 Uiso 1 1 calc R . . C82 C 0.8696(4) 0.7220(8) 0.2204(3) 0.061 Uani 1 1 d . . . H82A H 0.8609 0.7764 0.2334 0.091 Uiso 1 1 calc R . . H82B H 0.9058 0.7118 0.2221 0.091 Uiso 1 1 calc R . . H82C H 0.8522 0.6670 0.2285 0.091 Uiso 1 1 calc R . . C83 C 0.8737(3) 0.6609(7) 0.1626(3) 0.049 Uani 1 1 d . . . H83A H 0.8589 0.6010 0.1684 0.073 Uiso 1 1 calc R . . H83B H 0.9101 0.6570 0.1651 0.073 Uiso 1 1 calc R . . H83C H 0.8644 0.6759 0.1403 0.073 Uiso 1 1 calc R . . C84 C 0.7075(3) 0.8863(6) 0.1218(3) 0.033 Uani 1 1 d . . . H84 H 0.7351 0.9285 0.1152 0.039 Uiso 1 1 calc R . . C85 C 0.6669(3) 0.9457(6) 0.1373(3) 0.050 Uani 1 1 d . . . H85A H 0.6377 0.9068 0.1413 0.075 Uiso 1 1 calc R . . H85B H 0.6572 0.9966 0.1227 0.075 Uiso 1 1 calc R . . H85C H 0.6801 0.9714 0.1577 0.075 Uiso 1 1 calc R . . C86 C 0.6854(3) 0.8382(6) 0.0913(2) 0.039 Uani 1 1 d . . . H86A H 0.7116 0.8020 0.0811 0.058 Uiso 1 1 calc R . . H86B H 0.6725 0.8855 0.0762 0.058 Uiso 1 1 calc R . . H86C H 0.6582 0.7967 0.0973 0.058 Uiso 1 1 calc R . . C87 C 0.8711(3) 0.8899(6) 0.0628(2) 0.023 Uani 1 1 d . . . C88 C 0.8547(3) 0.9509(6) 0.0371(2) 0.023 Uani 1 1 d . . . C89 C 0.8691(3) 0.9290(6) 0.0065(2) 0.030 Uani 1 1 d . . . H89 H 0.8589 0.9691 -0.0107 0.037 Uiso 1 1 calc R . . C90 C 0.8977(3) 0.8513(6) -0.0007(2) 0.036 Uani 1 1 d . . . H90 H 0.9064 0.8389 -0.0223 0.043 Uiso 1 1 calc R . . C91 C 0.9136(3) 0.7915(6) 0.0243(2) 0.032 Uani 1 1 d . . . H91 H 0.9332 0.7383 0.0196 0.038 Uiso 1 1 calc R . . C92 C 0.9010(3) 0.8095(6) 0.0558(2) 0.024 Uani 1 1 d . . . C93 C 0.8199(3) 1.0309(6) 0.0448(2) 0.025 Uani 1 1 d . . . H93 H 0.8310 1.0582 0.0660 0.030 Uiso 1 1 calc R . . C94 C 0.8197(4) 1.1089(6) 0.0192(2) 0.038 Uani 1 1 d . . . H94A H 0.8530 1.1367 0.0185 0.057 Uiso 1 1 calc R . . H94B H 0.7954 1.1567 0.0248 0.057 Uiso 1 1 calc R . . H94C H 0.8104 1.0826 -0.0019 0.057 Uiso 1 1 calc R . . C95 C 0.7658(3) 0.9918(6) 0.0480(2) 0.031 Uani 1 1 d . . . H95A H 0.7555 0.9599 0.0280 0.046 Uiso 1 1 calc R . . H95B H 0.7427 1.0432 0.0520 0.046 Uiso 1 1 calc R . . H95C H 0.7652 0.9477 0.0660 0.046 Uiso 1 1 calc R . . C96 C 0.9188(3) 0.7428(5) 0.0815(2) 0.027 Uani 1 1 d . . . H96 H 0.9078 0.7666 0.1027 0.033 Uiso 1 1 calc R . . C97 C 0.9750(3) 0.7358(6) 0.0827(3) 0.045 Uani 1 1 d . . . H97A H 0.9867 0.7185 0.0614 0.067 Uiso 1 1 calc R . . H97B H 0.9855 0.6884 0.0985 0.067 Uiso 1 1 calc R . . H97C H 0.9894 0.7961 0.0890 0.067 Uiso 1 1 calc R . . C98 C 0.8975(4) 0.6481(6) 0.0765(3) 0.046 Uani 1 1 d . . . H98A H 0.8610 0.6511 0.0771 0.069 Uiso 1 1 calc R . . H98B H 0.9103 0.6066 0.0936 0.069 Uiso 1 1 calc R . . H98C H 0.9073 0.6242 0.0556 0.069 Uiso 1 1 calc R . . C99 C 0.8265(3) 0.8547(5) 0.1094(2) 0.017 Uani 1 1 d . . . H99 H 0.8127 0.8026 0.0982 0.021 Uiso 1 1 calc R . . C100 C 0.9280(3) 1.2058(5) 0.1932(2) 0.019 Uani 1 1 d . . . C101 C 0.8934(3) 1.2545(5) 0.2119(2) 0.021 Uani 1 1 d . . . C102 C 0.9107(3) 1.3026(6) 0.2392(2) 0.030 Uani 1 1 d . . . H102 H 0.8875 1.3355 0.2518 0.036 Uiso 1 1 calc R . . C103 C 0.9605(3) 1.3035(6) 0.2482(2) 0.031 Uani 1 1 d . . . H103 H 0.9714 1.3361 0.2670 0.038 Uiso 1 1 calc R . . C104 C 0.9942(3) 1.2571(6) 0.2299(2) 0.024 Uani 1 1 d . . . H104 H 1.0288 1.2602 0.2356 0.029 Uiso 1 1 calc R . . C105 C 0.9785(3) 1.2052(5) 0.2029(2) 0.022 Uani 1 1 d . . . C106 C 0.8389(3) 1.2616(6) 0.2003(2) 0.025 Uani 1 1 d . . . H106 H 0.8322 1.2075 0.1857 0.030 Uiso 1 1 calc R . . C107 C 0.8019(3) 1.2548(6) 0.2275(2) 0.032 Uani 1 1 d . . . H10A H 0.8069 1.3075 0.2422 0.048 Uiso 1 1 calc R . . H10B H 0.8074 1.1965 0.2393 0.048 Uiso 1 1 calc R . . H10C H 0.7677 1.2562 0.2185 0.048 Uiso 1 1 calc R . . C108 C 0.8292(4) 1.3469(7) 0.1811(2) 0.045 Uani 1 1 d . . . H10D H 0.8359 1.4018 0.1946 0.068 Uiso 1 1 calc R . . H10E H 0.7943 1.3476 0.1734 0.068 Uiso 1 1 calc R . . H10F H 0.8512 1.3477 0.1627 0.068 Uiso 1 1 calc R . . C109 C 1.0190(3) 1.1542(6) 0.1832(2) 0.022 Uani 1 1 d . . . H109 H 1.0013 1.1138 0.1668 0.027 Uiso 1 1 calc R . . C110 C 1.0526(3) 1.0931(6) 0.2036(2) 0.036 Uani 1 1 d . . . H11D H 1.0753 1.0587 0.1899 0.054 Uiso 1 1 calc R . . H11E H 1.0323 1.0490 0.2156 0.054 Uiso 1 1 calc R . . H11F H 1.0722 1.1317 0.2188 0.054 Uiso 1 1 calc R . . C111 C 1.0496(3) 1.2264(6) 0.1650(2) 0.031 Uani 1 1 d . . . H11G H 1.0702 1.2624 0.1804 0.046 Uiso 1 1 calc R . . H11H H 1.0269 1.2684 0.1531 0.046 Uiso 1 1 calc R . . H11I H 1.0712 1.1945 0.1499 0.046 Uiso 1 1 calc R . . C112 C 0.9256(3) 1.1719(6) 0.0800(2) 0.020 Uani 1 1 d . . . C113 C 0.9589(3) 1.1223(5) 0.0606(2) 0.018 Uani 1 1 d . . . C114 C 0.9690(3) 1.1573(6) 0.0308(2) 0.028 Uani 1 1 d . . . H114 H 0.9908 1.1235 0.0174 0.033 Uiso 1 1 calc R . . C115 C 0.9492(3) 1.2377(6) 0.0199(2) 0.033 Uani 1 1 d . . . H115 H 0.9564 1.2600 -0.0010 0.039 Uiso 1 1 calc R . . C116 C 0.9180(3) 1.2876(6) 0.0396(2) 0.025 Uani 1 1 d . . . H116 H 0.9052 1.3457 0.0323 0.030 Uiso 1 1 calc R . . C117 C 0.9052(3) 1.2559(5) 0.0695(2) 0.018 Uani 1 1 d . . . C118 C 0.9859(3) 1.0364(5) 0.0727(2) 0.023 Uani 1 1 d . . . H118 H 0.9618 1.0003 0.0857 0.028 Uiso 1 1 calc R . . C119 C 1.0029(3) 0.9729(6) 0.0459(2) 0.031 Uani 1 1 d . . . H11J H 0.9746 0.9594 0.0312 0.046 Uiso 1 1 calc R . . H11K H 1.0157 0.9146 0.0553 0.046 Uiso 1 1 calc R . . H11L H 1.0294 1.0036 0.0342 0.046 Uiso 1 1 calc R . . C120 C 1.0305(3) 1.0645(6) 0.0955(2) 0.036 Uani 1 1 d . . . H12D H 1.0458 1.0084 0.1049 0.055 Uiso 1 1 calc R . . H12E H 1.0184 1.1043 0.1127 0.055 Uiso 1 1 calc R . . H12F H 1.0554 1.0984 0.0833 0.055 Uiso 1 1 calc R . . C121 C 0.8690(3) 1.3132(5) 0.0894(2) 0.019 Uani 1 1 d . . . H121 H 0.8604 1.2749 0.1086 0.023 Uiso 1 1 calc R . . C122 C 0.8210(3) 1.3362(6) 0.0716(2) 0.035 Uani 1 1 d . . . H12G H 0.8277 1.3795 0.0540 0.053 Uiso 1 1 calc R . . H12H H 0.7977 1.3650 0.0863 0.053 Uiso 1 1 calc R . . H12I H 0.8061 1.2790 0.0627 0.053 Uiso 1 1 calc R . . C123 C 0.8940(3) 1.4017(6) 0.1019(2) 0.038 Uani 1 1 d . . . H12J H 0.9238 1.3856 0.1151 0.057 Uiso 1 1 calc R . . H12K H 0.8706 1.4365 0.1150 0.057 Uiso 1 1 calc R . . H12L H 0.9039 1.4401 0.0837 0.057 Uiso 1 1 calc R . . C124 C 0.9257(3) 1.1832(5) 0.1370(2) 0.018 Uani 1 1 d . . . H124 H 0.9449 1.2385 0.1352 0.021 Uiso 1 1 calc R . . C125 C 0.8650(4) 0.9977(7) 0.2268(2) 0.043 Uani 1 1 d . . . H12M H 0.8838 1.0557 0.2315 0.051 Uiso 1 1 calc R . . H12N H 0.8889 0.9454 0.2254 0.051 Uiso 1 1 calc R . . C126 C 0.8274(4) 0.9794(7) 0.2520(3) 0.053 Uani 1 1 d . . . H12O H 0.8207 1.0369 0.2643 0.064 Uiso 1 1 calc R . . H12P H 0.8398 0.9309 0.2672 0.064 Uiso 1 1 calc R . . C127 C 0.7806(4) 0.9468(7) 0.2342(2) 0.048 Uani 1 1 d . . . H12Q H 0.7817 0.8792 0.2297 0.058 Uiso 1 1 calc R . . H12R H 0.7502 0.9614 0.2462 0.058 Uiso 1 1 calc R . . C128 C 0.7833(3) 1.0025(6) 0.2043(2) 0.032 Uani 1 1 d . . . H12S H 0.7640 0.9724 0.1865 0.039 Uiso 1 1 calc R . . H12T H 0.7698 1.0658 0.2076 0.039 Uiso 1 1 calc R . . C129 C 0.8205(5) 0.9337(10) 0.3565(4) 0.128 Uani 1 1 d . . . H12U H 0.8355 0.8727 0.3621 0.154 Uiso 1 1 calc R . . H12V H 0.8322 0.9531 0.3352 0.154 Uiso 1 1 calc R . . C130 C 0.7616(5) 0.9280(9) 0.3564(4) 0.122 Uani 1 1 d . . . H13A H 0.7469 0.9710 0.3400 0.147 Uiso 1 1 calc R . . H13B H 0.7504 0.8640 0.3511 0.147 Uiso 1 1 calc R . . C131 C 0.7475(5) 0.9511(9) 0.3848(4) 0.084 Uani 1 1 d . . . H13C H 0.7454 0.8963 0.3992 0.101 Uiso 1 1 calc R . . H13D H 0.7150 0.9840 0.3840 0.101 Uiso 1 1 calc R . . C132 C 0.7868(5) 1.0104(11) 0.3943(3) 0.092 Uani 1 1 d . . . H13E H 0.7935 1.0028 0.4177 0.111 Uiso 1 1 calc R . . H13F H 0.7761 1.0756 0.3905 0.111 Uiso 1 1 calc R . . C133 C 0.8401(4) 1.2072(8) 0.3276(4) 0.084 Uani 1 1 d . . . H13G H 0.8357 1.1703 0.3076 0.101 Uiso 1 1 calc R . . H13H H 0.8119 1.1934 0.3416 0.101 Uiso 1 1 calc R . . C134 C 0.8412(3) 1.3051(7) 0.3200(3) 0.042 Uani 1 1 d . . . H13I H 0.8172 1.3395 0.3333 0.051 Uiso 1 1 calc R . . H13J H 0.8322 1.3155 0.2970 0.051 Uiso 1 1 calc R . . C135 C 0.8950(3) 1.3381(6) 0.3276(3) 0.040 Uani 1 1 d . . . H13K H 0.9084 1.3742 0.3095 0.048 Uiso 1 1 calc R . . H13L H 0.8968 1.3766 0.3474 0.048 Uiso 1 1 calc R . . C136 C 0.9231(4) 1.2459(7) 0.3324(3) 0.062 Uani 1 1 d . . . H13M H 0.9366 1.2238 0.3119 0.075 Uiso 1 1 calc R . . H13N H 0.9511 1.2530 0.3484 0.075 Uiso 1 1 calc R . . C137 C 0.8666(5) 1.1433(9) 0.4504(3) 0.083 Uani 1 1 d . . . H13O H 0.8921 1.1419 0.4681 0.100 Uiso 1 1 calc R . . H13P H 0.8512 1.0809 0.4482 0.100 Uiso 1 1 calc R . . C138 C 0.8254(5) 1.2202(8) 0.4567(3) 0.080 Uani 1 1 d . . . H13Q H 0.7938 1.2077 0.4445 0.096 Uiso 1 1 calc R . . H13R H 0.8187 1.2268 0.4799 0.096 Uiso 1 1 calc R . . C139 C 0.8524(5) 1.3031(10) 0.4439(3) 0.085 Uani 1 1 d . . . H13S H 0.8286 1.3530 0.4375 0.102 Uiso 1 1 calc R . . H13T H 0.8766 1.3280 0.4602 0.102 Uiso 1 1 calc R . . C140 C 0.8782(6) 1.2677(9) 0.4158(4) 0.095 Uani 1 1 d . . . H14A H 0.8572 1.2757 0.3960 0.114 Uiso 1 1 calc R . . H14B H 0.9102 1.3011 0.4131 0.114 Uiso 1 1 calc R . . C141 C 0.9741(4) 0.9977(8) 0.4468(3) 0.056 Uani 1 1 d . . . H14C H 0.9649 1.0610 0.4540 0.067 Uiso 1 1 calc R . . H14D H 1.0109 0.9913 0.4480 0.067 Uiso 1 1 calc R . . C142 C 0.9488(5) 0.9224(9) 0.4671(3) 0.077 Uani 1 1 d . . . H14E H 0.9210 0.9489 0.4793 0.092 Uiso 1 1 calc R . . H14F H 0.9731 0.8931 0.4824 0.092 Uiso 1 1 calc R . . C143 C 0.9286(6) 0.8490(9) 0.4408(4) 0.104 Uani 1 1 d . . . H14G H 0.9403 0.7853 0.4460 0.124 Uiso 1 1 calc R . . H14H H 0.8916 0.8492 0.4392 0.124 Uiso 1 1 calc R . . C144 C 0.9491(5) 0.8812(7) 0.4125(3) 0.071 Uani 1 1 d . . . H14I H 0.9266 0.8670 0.3938 0.085 Uiso 1 1 calc R . . H14J H 0.9818 0.8512 0.4091 0.085 Uiso 1 1 calc R . . C145 C 0.9353(5) 0.9978(9) 0.3037(3) 0.079 Uani 1 1 d . . . H14K H 0.9230 0.9337 0.2999 0.095 Uiso 1 1 calc R . . H14L H 0.9081 1.0423 0.2983 0.095 Uiso 1 1 calc R . . C146 C 0.9787(6) 1.0164(10) 0.2851(4) 0.120 Uani 1 1 d . . . H14M H 0.9783 0.9758 0.2658 0.144 Uiso 1 1 calc R . . H14N H 0.9780 1.0819 0.2777 0.144 Uiso 1 1 calc R . . C147 C 1.0228(6) 1.0002(17) 0.3037(4) 0.197 Uani 1 1 d . . . H14O H 1.0386 0.9410 0.2973 0.236 Uiso 1 1 calc R . . H14P H 1.0470 1.0515 0.3009 0.236 Uiso 1 1 calc R . . C148 C 1.0082(5) 0.9961(11) 0.3338(5) 0.147 Uani 1 1 d . . . H14Q H 1.0268 1.0439 0.3465 0.176 Uiso 1 1 calc R . . H14R H 1.0177 0.9346 0.3428 0.176 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.016 0.018 0.016 0.001 0.002 0.001 Sm2 0.015 0.017 0.016 0.000 0.001 0.000 I1 0.020 0.029 0.029 -0.003 0.000 0.001 I2 0.020 0.025 0.037 -0.001 -0.004 -0.001 I3 0.018 0.025 0.026 -0.001 0.001 0.002 I4 0.022 0.026 0.045 0.004 -0.008 0.003 Na1 0.026 0.028 0.028 -0.003 0.005 -0.007 Na2 0.041 0.042 0.050 0.011 0.006 -0.001 O1 0.026 0.042 0.018 -0.001 0.005 -0.002 O2 0.034 0.030 0.049 -0.010 0.000 -0.002 O3 0.043 0.039 0.048 0.017 0.007 -0.002 O4 0.044 0.034 0.033 -0.006 -0.003 -0.004 O5 0.034 0.052 0.024 0.001 0.006 -0.005 O6 0.033 0.030 0.047 -0.014 0.013 -0.006 O7 0.033 0.036 0.014 0.005 0.005 -0.001 O8 0.046 0.049 0.068 -0.033 0.015 -0.023 O9 0.035 0.047 0.099 0.029 -0.005 -0.010 O10 0.078 0.071 0.087 -0.006 0.026 0.022 O11 0.095 0.030 0.040 0.010 -0.008 -0.005 O12 0.048 0.121 0.046 0.031 0.007 0.017 N1 0.020 0.017 0.016 -0.001 0.006 0.002 N2 0.022 0.018 0.012 0.009 0.005 -0.002 N3 0.018 0.018 0.016 0.003 0.008 -0.001 N4 0.020 0.025 0.021 0.000 0.003 0.000 N5 0.017 0.015 0.022 -0.001 0.005 0.002 N6 0.019 0.020 0.011 0.000 0.000 -0.002 N7 0.015 0.018 0.019 -0.004 -0.001 -0.001 N8 0.011 0.018 0.023 0.000 0.004 0.003 C1 0.021 0.016 0.035 -0.005 0.004 0.002 C2 0.028 0.023 0.024 -0.003 0.013 -0.001 C3 0.037 0.044 0.039 -0.007 0.005 0.007 C4 0.046 0.042 0.068 0.008 0.033 0.015 C5 0.024 0.023 0.100 0.002 0.006 0.000 C6 0.018 0.024 0.032 0.001 0.005 0.004 C7 0.025 0.054 0.042 -0.029 0.006 0.002 C8 0.055 0.053 0.064 -0.026 -0.015 0.003 C9 0.037 0.084 0.073 0.011 0.006 -0.022 C10 0.029 0.021 0.037 -0.003 0.008 -0.001 C11 0.020 0.050 0.094 -0.022 0.003 -0.008 C12 0.042 0.042 0.046 -0.002 -0.005 0.008 C13 0.022 0.016 0.024 0.008 0.004 0.010 C14 0.025 0.034 0.023 0.008 0.004 0.010 C15 0.036 0.044 0.028 0.005 0.001 0.012 C16 0.034 0.061 0.043 0.034 0.015 0.018 C17 0.032 0.031 0.045 0.018 0.007 0.004 C18 0.023 0.033 0.033 0.013 0.012 0.015 C19 0.040 0.036 0.017 0.010 -0.004 0.005 C20 0.058 0.031 0.023 -0.010 -0.004 0.011 C21 0.038 0.045 0.032 -0.002 -0.011 0.005 C22 0.029 0.015 0.046 -0.002 0.003 -0.003 C23 0.028 0.038 0.063 -0.004 0.013 0.000 C24 0.043 0.019 0.085 0.004 0.007 0.003 C25 0.020 0.015 0.017 0.011 0.005 0.003 C26 0.023 0.017 0.020 0.005 0.005 0.006 C27 0.021 0.019 0.022 0.006 0.009 0.007 C28 0.030 0.030 0.030 0.012 0.012 0.004 C29 0.038 0.039 0.005 0.008 0.000 0.017 C30 0.017 0.020 0.035 0.004 0.003 0.003 C31 0.017 0.018 0.025 0.004 -0.003 0.006 C32 0.030 0.023 0.032 0.009 -0.004 -0.006 C33 0.029 0.055 0.043 0.026 0.011 -0.002 C34 0.050 0.042 0.063 0.010 -0.016 -0.022 C35 0.026 0.019 0.028 0.006 -0.005 0.002 C36 0.031 0.033 0.057 0.005 -0.014 -0.006 C37 0.033 0.033 0.038 0.017 0.017 0.010 C38 0.018 0.022 0.008 0.002 0.002 0.009 C39 0.023 0.028 0.015 0.005 0.006 0.011 C40 0.029 0.025 0.030 0.009 0.012 0.006 C41 0.033 0.035 0.017 -0.007 0.008 0.007 C42 0.036 0.025 0.021 -0.008 0.001 0.007 C43 0.020 0.026 0.023 0.004 0.003 0.006 C44 0.022 0.027 0.020 -0.002 0.011 -0.005 C45 0.036 0.029 0.028 0.000 0.005 -0.003 C46 0.029 0.045 0.034 0.012 0.004 0.003 C47 0.035 0.020 0.016 0.002 0.005 0.001 C48 0.026 0.040 0.043 -0.014 0.001 0.003 C49 0.041 0.020 0.054 0.012 0.010 0.002 C50 0.015 0.021 0.026 0.005 0.004 0.000 C51 0.040 0.039 0.034 -0.004 -0.010 0.004 C52 0.050 0.065 0.031 0.001 0.006 -0.017 C53 0.040 0.047 0.030 -0.008 0.017 -0.006 C54 0.027 0.040 0.020 -0.001 0.009 -0.001 C55 0.041 0.024 0.094 0.005 -0.006 -0.003 C56 0.048 0.016 0.089 -0.002 0.018 -0.001 C57 0.032 0.037 0.056 0.018 -0.001 0.002 C58 0.048 0.041 0.050 -0.003 -0.002 -0.001 C59 0.067 0.060 0.066 0.024 0.029 0.031 C60 0.041 0.031 0.064 0.005 0.004 -0.002 C61 0.038 0.035 0.051 0.012 0.013 0.002 C62 0.064 0.046 0.072 0.019 0.038 0.017 C63 0.101 0.049 0.054 -0.014 -0.038 0.009 C64 0.131 0.064 0.029 -0.015 -0.009 -0.001 C65 0.051 0.063 0.051 -0.032 -0.002 -0.016 C66 0.028 0.042 0.058 -0.004 0.000 -0.020 C67 0.032 0.053 0.048 0.013 0.001 -0.009 C68 0.049 0.040 0.065 0.009 0.032 0.000 C69 0.074 0.047 0.034 0.004 0.008 -0.005 C70 0.045 0.038 0.047 0.006 -0.003 -0.011 C71 0.032 0.032 0.033 -0.008 0.012 -0.007 C72 0.047 0.035 0.023 -0.006 0.014 -0.009 C73 0.031 0.042 0.036 -0.006 0.008 0.000 C74 0.040 0.040 0.033 -0.014 0.009 0.000 C75 0.030 0.007 0.018 -0.002 -0.001 -0.002 C76 0.034 0.026 0.026 -0.001 0.008 -0.005 C77 0.063 0.033 0.025 0.016 0.015 -0.008 C78 0.032 0.041 0.053 0.007 0.029 -0.004 C79 0.030 0.036 0.046 0.014 0.017 0.000 C80 0.026 0.019 0.047 -0.001 0.007 0.000 C81 0.042 0.037 0.026 0.020 -0.013 -0.007 C82 0.087 0.066 0.028 0.022 -0.009 -0.002 C83 0.029 0.058 0.060 0.011 -0.003 -0.006 C84 0.013 0.013 0.072 -0.004 0.005 0.003 C85 0.031 0.020 0.099 -0.002 0.010 0.009 C86 0.035 0.024 0.058 0.009 -0.007 -0.003 C87 0.021 0.033 0.015 -0.007 0.006 -0.010 C88 0.024 0.024 0.022 0.001 0.002 -0.011 C89 0.034 0.045 0.012 0.005 0.007 -0.005 C90 0.038 0.051 0.018 -0.013 0.019 -0.006 C91 0.032 0.034 0.029 -0.015 0.006 -0.012 C92 0.019 0.027 0.028 -0.004 0.007 -0.006 C93 0.034 0.029 0.011 0.004 -0.003 0.002 C94 0.045 0.048 0.021 -0.002 -0.001 -0.002 C95 0.032 0.042 0.020 -0.003 0.001 -0.001 C96 0.030 0.021 0.031 0.009 0.012 0.001 C97 0.041 0.041 0.053 0.005 0.007 0.013 C98 0.072 0.017 0.049 -0.005 0.007 -0.003 C99 0.013 0.013 0.026 -0.004 -0.005 -0.002 C100 0.020 0.023 0.013 -0.001 0.000 -0.002 C101 0.025 0.015 0.023 -0.006 0.000 -0.001 C102 0.028 0.032 0.029 -0.004 0.002 0.005 C103 0.036 0.034 0.024 -0.017 0.003 -0.006 C104 0.024 0.035 0.014 -0.009 -0.001 -0.011 C105 0.029 0.022 0.016 0.003 0.001 -0.001 C106 0.014 0.032 0.028 -0.007 0.003 0.005 C107 0.027 0.037 0.033 -0.016 0.012 0.002 C108 0.045 0.060 0.031 0.001 0.002 0.014 C109 0.014 0.032 0.020 -0.011 -0.005 0.001 C110 0.027 0.032 0.048 -0.005 -0.015 0.008 C111 0.010 0.040 0.042 -0.010 0.002 -0.004 C112 0.022 0.026 0.013 0.001 0.005 -0.012 C113 0.015 0.024 0.017 0.001 0.008 -0.003 C114 0.034 0.029 0.020 -0.001 0.007 0.000 C115 0.037 0.046 0.016 -0.006 0.010 -0.004 C116 0.025 0.020 0.029 0.010 0.002 0.000 C117 0.024 0.012 0.017 0.006 0.001 -0.003 C118 0.018 0.023 0.029 -0.005 0.010 -0.005 C119 0.037 0.026 0.031 0.000 0.016 0.006 C120 0.037 0.032 0.041 -0.006 -0.002 0.000 C121 0.025 0.012 0.022 0.009 0.006 0.002 C122 0.037 0.034 0.034 0.001 0.007 0.011 C123 0.045 0.026 0.045 -0.010 0.019 -0.003 C124 0.013 0.011 0.028 -0.003 0.002 -0.002 C125 0.061 0.054 0.013 0.007 -0.014 -0.007 C126 0.097 0.044 0.019 0.016 0.007 0.004 C127 0.078 0.042 0.026 0.003 0.023 -0.011 C128 0.037 0.037 0.024 -0.002 0.016 -0.011 C129 0.093 0.097 0.197 -0.066 0.034 -0.010 C130 0.066 0.060 0.236 -0.065 -0.064 0.022 C131 0.074 0.048 0.132 -0.021 0.019 -0.016 C132 0.064 0.160 0.053 -0.031 0.014 -0.028 C133 0.048 0.055 0.146 0.008 -0.037 -0.003 C134 0.034 0.059 0.034 0.004 0.005 0.006 C135 0.034 0.029 0.058 0.009 0.014 0.010 C136 0.044 0.065 0.078 0.023 0.003 0.006 C137 0.120 0.080 0.047 -0.033 -0.027 0.017 C138 0.065 0.088 0.087 -0.024 0.027 -0.018 C139 0.063 0.130 0.061 -0.028 -0.005 0.015 C140 0.118 0.070 0.099 -0.022 0.050 0.019 C141 0.066 0.055 0.046 0.017 0.010 0.003 C142 0.080 0.083 0.069 0.027 0.029 0.025 C143 0.123 0.067 0.123 -0.014 0.041 -0.051 C144 0.103 0.041 0.069 0.008 0.010 -0.010 C145 0.118 0.077 0.041 0.000 -0.015 0.031 C146 0.175 0.075 0.117 0.021 0.117 0.004 C147 0.082 0.402 0.110 -0.110 0.066 -0.130 C148 0.053 0.086 0.298 0.098 -0.050 -0.018 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.460(6) . ? Sm1 O1 2.486(6) . ? Sm1 N4 2.497(7) . ? Sm1 N1 2.511(6) . ? Sm1 N3 2.522(6) . ? Sm1 C25 2.877(7) . ? Sm1 C50 2.909(8) . ? Sm1 I2 3.1031(7) . ? Sm1 I1 3.1143(7) . ? Sm2 N6 2.469(6) . ? Sm2 N8 2.485(7) . ? Sm2 O7 2.498(6) . ? Sm2 N7 2.519(6) . ? Sm2 N5 2.525(6) . ? Sm2 C124 2.874(8) . ? Sm2 C99 2.878(8) . ? Sm2 I4 3.0904(7) . ? Sm2 I3 3.1129(6) . ? Na1 O3 2.311(7) . ? Na1 O4 2.331(7) . ? Na1 O2 2.337(7) . ? Na1 O6 2.340(7) . ? Na1 O5 2.346(7) . ? Na2 O9 2.283(8) . ? Na2 O10 2.297(10) . ? Na2 O8 2.299(8) . ? Na2 O11 2.322(8) . ? Na2 O12 2.387(9) . ? O1 C54 1.475(9) . ? O1 C51 1.494(10) . ? O2 C55 1.424(12) . ? O2 C58 1.478(11) . ? O3 C59 1.390(11) . ? O3 C62 1.445(12) . ? O4 C63 1.427(12) . ? O4 C66 1.437(11) . ? O5 C70 1.445(11) . ? O5 C67 1.457(11) . ? O6 C71 1.414(10) . ? O6 C74 1.463(10) . ? O7 C125 1.438(10) . ? O7 C128 1.439(10) . ? O8 C129 1.278(15) . ? O8 C132 1.428(14) . ? O9 C136 1.416(12) . ? O9 C133 1.443(12) . ? O10 C137 1.373(15) . ? O10 C140 1.434(14) . ? O11 C141 1.386(12) . ? O11 C144 1.431(12) . ? O12 C148 1.478(16) . ? O12 C145 1.513(14) . ? N1 C25 1.280(10) . ? N1 C1 1.389(10) . ? N2 C25 1.331(10) . ? N2 C13 1.422(10) . ? N3 C50 1.334(10) . ? N3 C26 1.414(10) . ? N4 C50 1.344(10) . ? N4 C38 1.417(10) . ? N5 C99 1.313(10) . ? N5 C75 1.414(10) . ? N6 C99 1.321(10) . ? N6 C87 1.425(10) . ? N7 C124 1.334(10) . ? N7 C100 1.407(10) . ? N8 C124 1.337(10) . ? N8 C112 1.431(10) . ? C1 C2 1.378(12) . ? C1 C6 1.428(11) . ? C2 C3 1.420(12) . ? C2 C7 1.503(11) . ? C3 C4 1.383(13) . ? C4 C5 1.470(14) . ? C5 C6 1.387(13) . ? C6 C10 1.484(12) . ? C7 C9 1.489(14) . ? C7 C8 1.558(14) . ? C10 C11 1.513(12) . ? C10 C12 1.544(13) . ? C13 C18 1.405(12) . ? C13 C14 1.440(12) . ? C14 C15 1.385(13) . ? C14 C19 1.486(12) . ? C15 C16 1.432(13) . ? C16 C17 1.382(13) . ? C17 C18 1.422(13) . ? C18 C22 1.525(12) . ? C19 C20 1.506(12) . ? C19 C21 1.550(12) . ? C22 C23 1.541(11) . ? C22 C24 1.551(11) . ? C26 C31 1.392(11) . ? C26 C27 1.420(11) . ? C27 C28 1.380(11) . ? C27 C32 1.537(11) . ? C28 C29 1.379(11) . ? C29 C30 1.355(12) . ? C30 C31 1.368(11) . ? C31 C35 1.548(12) . ? C32 C33 1.519(12) . ? C32 C34 1.556(13) . ? C35 C37 1.490(12) . ? C35 C36 1.515(11) . ? C38 C39 1.416(11) . ? C38 C43 1.428(11) . ? C39 C40 1.388(12) . ? C39 C44 1.534(11) . ? C40 C41 1.393(12) . ? C41 C42 1.396(12) . ? C42 C43 1.367(12) . ? C43 C47 1.540(11) . ? C44 C46 1.523(11) . ? C44 C45 1.531(11) . ? C47 C49 1.506(11) . ? C47 C48 1.525(11) . ? C51 C52 1.551(14) . ? C52 C53 1.555(13) . ? C53 C54 1.510(12) . ? C55 C56 1.570(13) . ? C56 C57 1.551(14) . ? C57 C58 1.504(14) . ? C59 C60 1.543(14) . ? C60 C61 1.517(13) . ? C61 C62 1.482(13) . ? C63 C64 1.431(15) . ? C64 C65 1.524(16) . ? C65 C66 1.511(14) . ? C67 C68 1.486(14) . ? C68 C69 1.601(14) . ? C69 C70 1.524(15) . ? C71 C72 1.522(12) . ? C72 C73 1.539(12) . ? C73 C74 1.501(12) . ? C75 C76 1.404(11) . ? C75 C80 1.417(11) . ? C76 C77 1.406(12) . ? C76 C81 1.535(12) . ? C77 C78 1.382(12) . ? C78 C79 1.363(13) . ? C79 C80 1.410(12) . ? C80 C84 1.520(12) . ? C81 C82 1.528(13) . ? C81 C83 1.568(14) . ? C84 C85 1.538(12) . ? C84 C86 1.544(13) . ? C87 C88 1.440(11) . ? C87 C92 1.441(11) . ? C88 C89 1.377(12) . ? C88 C93 1.521(12) . ? C89 C90 1.392(12) . ? C90 C91 1.405(13) . ? C91 C92 1.388(12) . ? C92 C96 1.502(11) . ? C93 C94 1.545(12) . ? C93 C95 1.562(11) . ? C96 C98 1.486(11) . ? C96 C97 1.508(11) . ? C100 C105 1.398(11) . ? C100 C101 1.414(11) . ? C101 C102 1.395(11) . ? C101 C106 1.525(10) . ? C102 C103 1.373(11) . ? C103 C104 1.373(12) . ? C104 C105 1.401(11) . ? C105 C109 1.563(12) . ? C106 C108 1.480(12) . ? C106 C107 1.530(12) . ? C109 C110 1.504(11) . ? C109 C111 1.534(12) . ? C112 C117 1.389(11) . ? C112 C113 1.413(11) . ? C113 C114 1.372(12) . ? C113 C118 1.508(11) . ? C114 C115 1.345(12) . ? C115 C116 1.387(12) . ? C116 C117 1.378(11) . ? C117 C121 1.532(11) . ? C118 C119 1.519(12) . ? C118 C120 1.557(11) . ? C121 C122 1.502(11) . ? C121 C123 1.521(11) . ? C125 C126 1.500(14) . ? C126 C127 1.509(14) . ? C127 C128 1.482(12) . ? C129 C130 1.577(17) . ? C130 C131 1.30(2) . ? C131 C132 1.402(15) . ? C133 C134 1.442(14) . ? C134 C135 1.539(12) . ? C135 C136 1.534(13) . ? C137 C138 1.588(16) . ? C138 C139 1.500(17) . ? C139 C140 1.465(17) . ? C141 C142 1.542(15) . ? C142 C143 1.603(18) . ? C143 C144 1.394(17) . ? C145 C146 1.441(18) . ? C146 C147 1.41(2) . ? C147 C148 1.33(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sm1 O1 131.3(2) . . ? N2 Sm1 N4 94.5(2) . . ? O1 Sm1 N4 133.9(2) . . ? N2 Sm1 N1 53.9(2) . . ? O1 Sm1 N1 77.5(2) . . ? N4 Sm1 N1 147.4(2) . . ? N2 Sm1 N3 147.5(2) . . ? O1 Sm1 N3 80.6(2) . . ? N4 Sm1 N3 54.7(2) . . ? N1 Sm1 N3 157.9(2) . . ? N2 Sm1 C25 27.5(2) . . ? O1 Sm1 C25 103.9(2) . . ? N4 Sm1 C25 121.5(2) . . ? N1 Sm1 C25 26.4(2) . . ? N3 Sm1 C25 173.8(2) . . ? N2 Sm1 C50 121.4(2) . . ? O1 Sm1 C50 107.3(2) . . ? N4 Sm1 C50 27.4(2) . . ? N1 Sm1 C50 174.7(2) . . ? N3 Sm1 C50 27.3(2) . . ? C25 Sm1 C50 148.8(2) . . ? N2 Sm1 I2 87.34(15) . . ? O1 Sm1 I2 90.43(13) . . ? N4 Sm1 I2 97.07(15) . . ? N1 Sm1 I2 89.90(15) . . ? N3 Sm1 I2 86.77(14) . . ? C25 Sm1 I2 89.01(15) . . ? C50 Sm1 I2 92.08(15) . . ? N2 Sm1 I1 96.94(15) . . ? O1 Sm1 I1 84.49(13) . . ? N4 Sm1 I1 85.62(15) . . ? N1 Sm1 I1 90.20(14) . . ? N3 Sm1 I1 91.18(14) . . ? C25 Sm1 I1 93.40(15) . . ? C50 Sm1 I1 88.27(15) . . ? I2 Sm1 I1 174.78(2) . . ? N6 Sm2 N8 92.8(2) . . ? N6 Sm2 O7 131.8(2) . . ? N8 Sm2 O7 135.3(2) . . ? N6 Sm2 N7 147.3(2) . . ? N8 Sm2 N7 55.3(2) . . ? O7 Sm2 N7 80.7(2) . . ? N6 Sm2 N5 54.4(2) . . ? N8 Sm2 N5 146.5(2) . . ? O7 Sm2 N5 77.5(2) . . ? N7 Sm2 N5 158.1(2) . . ? N6 Sm2 C124 120.2(2) . . ? N8 Sm2 C124 27.7(2) . . ? O7 Sm2 C124 108.0(2) . . ? N7 Sm2 C124 27.7(2) . . ? N5 Sm2 C124 174.1(2) . . ? N6 Sm2 C99 27.2(2) . . ? N8 Sm2 C99 119.8(2) . . ? O7 Sm2 C99 104.6(2) . . ? N7 Sm2 C99 174.1(2) . . ? N5 Sm2 C99 27.1(2) . . ? C124 Sm2 C99 147.4(2) . . ? N6 Sm2 I4 89.95(14) . . ? N8 Sm2 I4 95.11(14) . . ? O7 Sm2 I4 89.16(13) . . ? N7 Sm2 I4 86.20(14) . . ? N5 Sm2 I4 91.56(14) . . ? C124 Sm2 I4 90.78(14) . . ? C99 Sm2 I4 91.22(14) . . ? N6 Sm2 I3 96.08(14) . . ? N8 Sm2 I3 86.45(14) . . ? O7 Sm2 I3 85.45(13) . . ? N7 Sm2 I3 89.69(14) . . ? N5 Sm2 I3 90.47(14) . . ? C124 Sm2 I3 87.78(14) . . ? C99 Sm2 I3 93.31(14) . . ? I4 Sm2 I3 173.69(2) . . ? O3 Na1 O4 89.8(3) . . ? O3 Na1 O2 89.8(3) . . ? O4 Na1 O2 96.7(3) . . ? O3 Na1 O6 90.2(3) . . ? O4 Na1 O6 158.7(3) . . ? O2 Na1 O6 104.5(3) . . ? O3 Na1 O5 164.2(3) . . ? O4 Na1 O5 87.2(3) . . ? O2 Na1 O5 106.0(3) . . ? O6 Na1 O5 87.0(3) . . ? O9 Na2 O10 90.8(3) . . ? O9 Na2 O8 96.2(3) . . ? O10 Na2 O8 96.7(3) . . ? O9 Na2 O11 160.3(3) . . ? O10 Na2 O11 91.5(3) . . ? O8 Na2 O11 102.9(3) . . ? O9 Na2 O12 82.6(3) . . ? O10 Na2 O12 158.0(4) . . ? O8 Na2 O12 104.8(3) . . ? O11 Na2 O12 88.0(3) . . ? C54 O1 C51 108.8(6) . . ? C54 O1 Sm1 123.7(5) . . ? C51 O1 Sm1 127.5(5) . . ? C55 O2 C58 109.9(7) . . ? C55 O2 Na1 117.4(5) . . ? C58 O2 Na1 130.7(6) . . ? C59 O3 C62 108.1(7) . . ? C59 O3 Na1 121.5(6) . . ? C62 O3 Na1 129.1(6) . . ? C63 O4 C66 107.6(7) . . ? C63 O4 Na1 131.8(6) . . ? C66 O4 Na1 118.7(6) . . ? C70 O5 C67 105.9(7) . . ? C70 O5 Na1 113.2(5) . . ? C67 O5 Na1 133.9(6) . . ? C71 O6 C74 111.1(6) . . ? C71 O6 Na1 127.4(5) . . ? C74 O6 Na1 119.2(5) . . ? C125 O7 C128 109.6(7) . . ? C125 O7 Sm2 126.9(6) . . ? C128 O7 Sm2 123.5(5) . . ? C129 O8 C132 104.4(10) . . ? C129 O8 Na2 124.4(9) . . ? C132 O8 Na2 130.5(7) . . ? C136 O9 C133 106.6(9) . . ? C136 O9 Na2 121.3(6) . . ? C133 O9 Na2 132.1(7) . . ? C137 O10 C140 111.6(10) . . ? C137 O10 Na2 124.5(8) . . ? C140 O10 Na2 120.5(8) . . ? C141 O11 C144 108.6(8) . . ? C141 O11 Na2 130.5(6) . . ? C144 O11 Na2 116.2(7) . . ? C148 O12 C145 99.7(11) . . ? C148 O12 Na2 132.9(10) . . ? C145 O12 Na2 125.8(7) . . ? C25 N1 C1 120.9(7) . . ? C25 N1 Sm1 93.0(5) . . ? C1 N1 Sm1 145.5(6) . . ? C25 N2 C13 117.2(6) . . ? C25 N2 Sm1 93.9(5) . . ? C13 N2 Sm1 148.7(5) . . ? C50 N3 C26 119.6(7) . . ? C50 N3 Sm1 92.7(5) . . ? C26 N3 Sm1 146.9(5) . . ? C50 N4 C38 118.2(7) . . ? C50 N4 Sm1 93.6(5) . . ? C38 N4 Sm1 147.8(5) . . ? C99 N5 C75 120.3(7) . . ? C99 N5 Sm2 91.6(5) . . ? C75 N5 Sm2 147.8(5) . . ? C99 N6 C87 118.6(7) . . ? C99 N6 Sm2 93.9(5) . . ? C87 N6 Sm2 147.4(5) . . ? C124 N7 C100 118.5(7) . . ? C124 N7 Sm2 91.2(5) . . ? C100 N7 Sm2 149.7(5) . . ? C124 N8 C112 118.2(7) . . ? C124 N8 Sm2 92.6(5) . . ? C112 N8 Sm2 148.1(5) . . ? C2 C1 N1 119.5(7) . . ? C2 C1 C6 121.0(8) . . ? N1 C1 C6 119.3(8) . . ? C1 C2 C3 122.0(8) . . ? C1 C2 C7 120.9(8) . . ? C3 C2 C7 116.8(8) . . ? C4 C3 C2 118.5(10) . . ? C3 C4 C5 119.7(9) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 C1 118.0(9) . . ? C5 C6 C10 116.9(8) . . ? C1 C6 C10 125.1(8) . . ? C9 C7 C2 110.9(9) . . ? C9 C7 C8 112.0(8) . . ? C2 C7 C8 114.4(8) . . ? C6 C10 C11 115.2(8) . . ? C6 C10 C12 111.4(7) . . ? C11 C10 C12 107.5(8) . . ? C18 C13 N2 120.3(8) . . ? C18 C13 C14 121.1(8) . . ? N2 C13 C14 118.6(7) . . ? C15 C14 C13 120.1(9) . . ? C15 C14 C19 118.8(9) . . ? C13 C14 C19 120.9(8) . . ? C14 C15 C16 119.2(10) . . ? C17 C16 C15 119.9(10) . . ? C16 C17 C18 122.6(9) . . ? C13 C18 C17 117.0(9) . . ? C13 C18 C22 123.1(8) . . ? C17 C18 C22 119.9(8) . . ? C14 C19 C20 114.7(8) . . ? C14 C19 C21 110.6(7) . . ? C20 C19 C21 111.5(7) . . ? C18 C22 C23 111.6(8) . . ? C18 C22 C24 111.8(8) . . ? C23 C22 C24 109.9(7) . . ? N1 C25 N2 119.2(7) . . ? N1 C25 Sm1 60.6(4) . . ? N2 C25 Sm1 58.6(4) . . ? C31 C26 N3 121.8(7) . . ? C31 C26 C27 119.5(8) . . ? N3 C26 C27 118.6(7) . . ? C28 C27 C26 119.6(8) . . ? C28 C27 C32 120.0(8) . . ? C26 C27 C32 120.3(8) . . ? C29 C28 C27 119.5(8) . . ? C30 C29 C28 120.4(8) . . ? C29 C30 C31 122.4(8) . . ? C30 C31 C26 118.5(8) . . ? C30 C31 C35 119.5(7) . . ? C26 C31 C35 121.9(8) . . ? C33 C32 C27 116.0(8) . . ? C33 C32 C34 110.5(7) . . ? C27 C32 C34 108.4(7) . . ? C37 C35 C36 108.3(8) . . ? C37 C35 C31 110.6(7) . . ? C36 C35 C31 111.9(8) . . ? C39 C38 N4 118.3(7) . . ? C39 C38 C43 119.3(8) . . ? N4 C38 C43 122.3(8) . . ? C40 C39 C38 118.4(8) . . ? C40 C39 C44 120.9(8) . . ? C38 C39 C44 120.6(8) . . ? C39 C40 C41 122.9(8) . . ? C40 C41 C42 117.5(9) . . ? C43 C42 C41 122.5(8) . . ? C42 C43 C38 119.3(8) . . ? C42 C43 C47 118.3(8) . . ? C38 C43 C47 122.4(8) . . ? C46 C44 C45 111.7(7) . . ? C46 C44 C39 109.6(7) . . ? C45 C44 C39 112.6(7) . . ? C49 C47 C48 109.3(7) . . ? C49 C47 C43 110.3(7) . . ? C48 C47 C43 113.5(8) . . ? N3 C50 N4 119.0(7) . . ? N3 C50 Sm1 60.0(4) . . ? N4 C50 Sm1 59.0(4) . . ? O1 C51 C52 107.9(7) . . ? C51 C52 C53 100.4(8) . . ? C54 C53 C52 106.0(8) . . ? O1 C54 C53 103.2(7) . . ? O2 C55 C56 105.8(7) . . ? C57 C56 C55 101.1(9) . . ? C58 C57 C56 103.3(8) . . ? O2 C58 C57 107.1(8) . . ? O3 C59 C60 108.2(8) . . ? C61 C60 C59 103.6(8) . . ? C62 C61 C60 102.8(8) . . ? O3 C62 C61 110.8(8) . . ? O4 C63 C64 111.1(10) . . ? C63 C64 C65 104.3(10) . . ? C66 C65 C64 105.5(9) . . ? O4 C66 C65 104.1(9) . . ? O5 C67 C68 104.8(8) . . ? C67 C68 C69 102.8(8) . . ? C70 C69 C68 102.6(9) . . ? O5 C70 C69 108.1(8) . . ? O6 C71 C72 104.8(7) . . ? C71 C72 C73 102.2(7) . . ? C74 C73 C72 103.2(7) . . ? O6 C74 C73 105.7(7) . . ? C76 C75 N5 119.1(7) . . ? C76 C75 C80 120.0(8) . . ? N5 C75 C80 120.9(7) . . ? C75 C76 C77 118.0(8) . . ? C75 C76 C81 119.5(8) . . ? C77 C76 C81 122.4(9) . . ? C78 C77 C76 122.3(9) . . ? C79 C78 C77 119.4(9) . . ? C78 C79 C80 121.3(9) . . ? C79 C80 C75 119.0(9) . . ? C79 C80 C84 118.6(8) . . ? C75 C80 C84 122.4(8) . . ? C82 C81 C76 115.9(9) . . ? C82 C81 C83 111.8(8) . . ? C76 C81 C83 107.9(7) . . ? C80 C84 C85 108.5(9) . . ? C80 C84 C86 113.5(7) . . ? C85 C84 C86 109.6(7) . . ? N6 C87 C88 118.3(7) . . ? N6 C87 C92 122.0(8) . . ? C88 C87 C92 119.8(8) . . ? C89 C88 C87 117.4(8) . . ? C89 C88 C93 124.0(8) . . ? C87 C88 C93 118.5(8) . . ? C88 C89 C90 123.6(9) . . ? C89 C90 C91 119.2(9) . . ? C92 C91 C90 120.5(9) . . ? C91 C92 C87 119.5(8) . . ? C91 C92 C96 118.2(8) . . ? C87 C92 C96 122.3(8) . . ? C88 C93 C94 113.0(8) . . ? C88 C93 C95 108.8(7) . . ? C94 C93 C95 109.6(7) . . ? C98 C96 C92 111.9(8) . . ? C98 C96 C97 108.8(7) . . ? C92 C96 C97 111.1(7) . . ? N5 C99 N6 120.1(7) . . ? N5 C99 Sm2 61.3(4) . . ? N6 C99 Sm2 58.8(4) . . ? C105 C100 N7 121.7(7) . . ? C105 C100 C101 119.2(8) . . ? N7 C100 C101 119.1(7) . . ? C102 C101 C100 119.1(8) . . ? C102 C101 C106 120.9(8) . . ? C100 C101 C106 119.7(8) . . ? C103 C102 C101 121.5(9) . . ? C104 C103 C102 119.6(9) . . ? C103 C104 C105 121.1(8) . . ? C100 C105 C104 119.5(8) . . ? C100 C105 C109 122.0(8) . . ? C104 C105 C109 118.3(7) . . ? C108 C106 C101 112.0(7) . . ? C108 C106 C107 110.2(7) . . ? C101 C106 C107 113.4(8) . . ? C110 C109 C111 110.8(7) . . ? C110 C109 C105 112.9(8) . . ? C111 C109 C105 109.4(7) . . ? C117 C112 C113 120.5(8) . . ? C117 C112 N8 121.6(8) . . ? C113 C112 N8 117.9(7) . . ? C114 C113 C112 118.5(8) . . ? C114 C113 C118 119.6(8) . . ? C112 C113 C118 121.7(8) . . ? C115 C114 C113 122.1(9) . . ? C114 C115 C116 118.9(9) . . ? C117 C116 C115 122.3(8) . . ? C116 C117 C112 117.6(8) . . ? C116 C117 C121 119.3(7) . . ? C112 C117 C121 123.1(8) . . ? C113 C118 C119 113.6(8) . . ? C113 C118 C120 110.0(7) . . ? C119 C118 C120 111.1(7) . . ? C122 C121 C123 110.2(7) . . ? C122 C121 C117 113.3(7) . . ? C123 C121 C117 110.8(7) . . ? N7 C124 N8 120.9(7) . . ? N7 C124 Sm2 61.2(4) . . ? N8 C124 Sm2 59.7(4) . . ? O7 C125 C126 104.4(8) . . ? C125 C126 C127 106.0(9) . . ? C128 C127 C126 100.5(8) . . ? O7 C128 C127 105.3(8) . . ? O8 C129 C130 105.1(11) . . ? C131 C130 C129 107.6(12) . . ? C130 C131 C132 100.1(13) . . ? C131 C132 O8 114.2(12) . . ? C134 C133 O9 108.2(9) . . ? C133 C134 C135 106.2(8) . . ? C136 C135 C134 102.3(8) . . ? O9 C136 C135 104.8(8) . . ? O10 C137 C138 103.8(10) . . ? C139 C138 C137 98.6(10) . . ? C140 C139 C138 104.6(12) . . ? O10 C140 C139 105.8(12) . . ? O11 C141 C142 102.6(10) . . ? C141 C142 C143 103.4(11) . . ? C144 C143 C142 103.1(10) . . ? C143 C144 O11 106.5(11) . . ? C146 C145 O12 103.7(12) . . ? C147 C146 C145 110.4(15) . . ? C148 C147 C146 105.1(14) . . ? C147 C148 O12 115.2(14) . . ? _diffrn_measured_fraction_theta_max 0.755 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.798 _refine_diff_density_max 2.369 _refine_diff_density_min -1.989 _refine_diff_density_rms 0.319 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 262798' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Sm(DippForm)3].5/2C7H8' _chemical_melting_point 494 _chemical_formula_moiety 'C92.50 H125 N6 Sm' _chemical_formula_sum 'C92.50 H125 N6 Sm' _chemical_formula_weight 1471.34 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1662(2) _cell_length_b 37.9133(8) _cell_length_c 16.4994(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.1070(10) _cell_angle_gamma 90.00 _cell_volume 8189.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8621 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44716 _diffrn_reflns_av_R_equivalents 0.1993 _diffrn_reflns_av_sigmaI/netI 0.3504 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.37 _reflns_number_total 18160 _reflns_number_gt 6734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18160 _refine_ls_number_parameters 939 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2713 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2011 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.76954(3) 0.143840(13) 0.89342(2) 0.02341(14) Uani 1 1 d . . . N1 N 0.8494(4) 0.20017(17) 0.8648(3) 0.0190(16) Uani 1 1 d . . . N2 N 0.6877(4) 0.20151(18) 0.9090(4) 0.0236(17) Uani 1 1 d . . . N3 N 0.8384(4) 0.10431(17) 0.7943(4) 0.0223(17) Uani 1 1 d . . . N4 N 0.6701(4) 0.12103(18) 0.7691(4) 0.0223(16) Uani 1 1 d . . . N5 N 0.8715(4) 0.12789(17) 1.0224(4) 0.0233(16) Uani 1 1 d . . . N6 N 0.7038(4) 0.11029(17) 1.0043(4) 0.0207(16) Uani 1 1 d . . . C1 C 0.9278(6) 0.2226(2) 0.8364(5) 0.026(2) Uani 1 1 d . . . C2 C 1.0255(6) 0.2222(2) 0.8808(5) 0.031(2) Uani 1 1 d . . . C3 C 1.0984(6) 0.2458(3) 0.8563(5) 0.037(3) Uani 1 1 d . . . H3 H 1.1649 0.2457 0.8849 0.044 Uiso 1 1 calc R . . C4 C 1.0776(6) 0.2689(3) 0.7928(6) 0.043(3) Uani 1 1 d . . . H4 H 1.1286 0.2849 0.7792 0.052 Uiso 1 1 calc R . . C5 C 0.9827(6) 0.2688(2) 0.7487(5) 0.039(3) Uani 1 1 d . . . H5 H 0.9689 0.2845 0.7040 0.047 Uiso 1 1 calc R . . C6 C 0.9053(6) 0.2455(2) 0.7696(5) 0.028(2) Uani 1 1 d . . . C7 C 1.0493(5) 0.2000(2) 0.9545(5) 0.025(2) Uani 1 1 d . . . H7 H 1.0101 0.1775 0.9456 0.030 Uiso 1 1 calc R . . C8 C 1.1618(5) 0.1904(2) 0.9730(5) 0.037(3) Uani 1 1 d . . . H8A H 1.1859 0.1792 0.9250 0.055 Uiso 1 1 calc R . . H8B H 1.1702 0.1740 1.0191 0.055 Uiso 1 1 calc R . . H8C H 1.2017 0.2118 0.9867 0.055 Uiso 1 1 calc R . . C9 C 1.0141(6) 0.2179(3) 1.0301(5) 0.041(3) Uani 1 1 d . . . H9A H 1.0487 0.2407 1.0388 0.062 Uiso 1 1 calc R . . H9B H 1.0309 0.2029 1.0779 0.062 Uiso 1 1 calc R . . H9C H 0.9400 0.2217 1.0218 0.062 Uiso 1 1 calc R . . C10 C 0.8024(6) 0.2467(3) 0.7169(5) 0.035(2) Uani 1 1 d . . . H10 H 0.7600 0.2266 0.7331 0.042 Uiso 1 1 calc R . . C11 C 0.8134(6) 0.2433(3) 0.6269(5) 0.051(3) Uani 1 1 d . . . H11A H 0.8530 0.2632 0.6093 0.077 Uiso 1 1 calc R . . H11B H 0.7456 0.2432 0.5961 0.077 Uiso 1 1 calc R . . H11C H 0.8488 0.2212 0.6171 0.077 Uiso 1 1 calc R . . C12 C 0.7432(6) 0.2813(2) 0.7286(5) 0.046(3) Uani 1 1 d . . . H12A H 0.7333 0.2841 0.7863 0.069 Uiso 1 1 calc R . . H12B H 0.6765 0.2803 0.6961 0.069 Uiso 1 1 calc R . . H12C H 0.7822 0.3013 0.7110 0.069 Uiso 1 1 calc R . . C13 C 0.6095(6) 0.2260(2) 0.9288(5) 0.028(2) Uani 1 1 d . . . C14 C 0.5113(6) 0.2215(3) 0.8866(5) 0.029(2) Uani 1 1 d . . . C15 C 0.4350(6) 0.2457(3) 0.9033(5) 0.038(3) Uani 1 1 d . . . H15 H 0.3679 0.2433 0.8764 0.046 Uiso 1 1 calc R . . C16 C 0.4560(7) 0.2728(3) 0.9579(6) 0.048(3) Uani 1 1 d . . . H16 H 0.4042 0.2893 0.9671 0.058 Uiso 1 1 calc R . . C17 C 0.5516(7) 0.2761(3) 0.9992(5) 0.043(3) Uani 1 1 d . . . H17 H 0.5646 0.2950 1.0366 0.052 Uiso 1 1 calc R . . C18 C 0.6299(6) 0.2527(2) 0.9881(5) 0.030(2) Uani 1 1 d . . . C19 C 0.4879(5) 0.1942(3) 0.8210(5) 0.035(3) Uani 1 1 d . . . H19 H 0.5281 0.1725 0.8378 0.042 Uiso 1 1 calc R . . C20 C 0.3758(5) 0.1838(3) 0.8067(5) 0.041(3) Uani 1 1 d . . . H20A H 0.3521 0.1762 0.8583 0.062 Uiso 1 1 calc R . . H20B H 0.3677 0.1643 0.7674 0.062 Uiso 1 1 calc R . . H20C H 0.3353 0.2040 0.7852 0.062 Uiso 1 1 calc R . . C21 C 0.5244(5) 0.2077(2) 0.7401(5) 0.039(3) Uani 1 1 d . . . H21A H 0.4914 0.2303 0.7253 0.059 Uiso 1 1 calc R . . H21B H 0.5061 0.1905 0.6968 0.059 Uiso 1 1 calc R . . H21C H 0.5987 0.2109 0.7473 0.059 Uiso 1 1 calc R . . C22 C 0.7338(6) 0.2577(3) 1.0373(5) 0.041(3) Uani 1 1 d . . . H22 H 0.7772 0.2368 1.0279 0.049 Uiso 1 1 calc R . . C23 C 0.7233(7) 0.2600(3) 1.1284(5) 0.059(3) Uani 1 1 d . . . H23A H 0.6819 0.2807 1.1390 0.089 Uiso 1 1 calc R . . H23B H 0.7912 0.2623 1.1586 0.089 Uiso 1 1 calc R . . H23C H 0.6901 0.2386 1.1459 0.089 Uiso 1 1 calc R . . C24 C 0.7901(7) 0.2909(3) 1.0137(6) 0.062(3) Uani 1 1 d . . . H24A H 0.8027 0.2894 0.9564 0.093 Uiso 1 1 calc R . . H24B H 0.8555 0.2929 1.0480 0.093 Uiso 1 1 calc R . . H24C H 0.7483 0.3118 1.0219 0.093 Uiso 1 1 calc R . . C25 C 0.7688(6) 0.2185(2) 0.8837(4) 0.026(2) Uani 1 1 d . . . H25 H 0.7684 0.2434 0.8793 0.032 Uiso 1 1 calc R . . C26 C 0.9201(5) 0.0830(3) 0.7645(5) 0.026(2) Uani 1 1 d . . . C27 C 1.0075(6) 0.1014(3) 0.7438(5) 0.032(2) Uani 1 1 d . . . C28 C 1.0842(6) 0.0806(3) 0.7152(5) 0.038(3) Uani 1 1 d . . . H28 H 1.1440 0.0920 0.7009 0.045 Uiso 1 1 calc R . . C29 C 1.0776(7) 0.0452(3) 0.7068(6) 0.052(3) Uani 1 1 d . . . H29 H 1.1322 0.0322 0.6881 0.063 Uiso 1 1 calc R . . C30 C 0.9907(7) 0.0280(3) 0.7258(6) 0.052(3) Uani 1 1 d . . . H30 H 0.9847 0.0032 0.7181 0.063 Uiso 1 1 calc R . . C31 C 0.9121(6) 0.0466(3) 0.7560(5) 0.036(2) Uani 1 1 d . . . C32 C 1.0171(6) 0.1409(3) 0.7475(5) 0.033(2) Uani 1 1 d . . . H32 H 0.9861 0.1489 0.7971 0.040 Uiso 1 1 calc R . . C33 C 1.1259(5) 0.1550(2) 0.7541(5) 0.042(3) Uani 1 1 d . . . H33A H 1.1680 0.1422 0.7970 0.064 Uiso 1 1 calc R . . H33B H 1.1256 0.1802 0.7677 0.064 Uiso 1 1 calc R . . H33C H 1.1540 0.1518 0.7020 0.064 Uiso 1 1 calc R . . C34 C 0.9557(6) 0.1581(3) 0.6736(6) 0.047(3) Uani 1 1 d . . . H34A H 0.9828 0.1502 0.6235 0.070 Uiso 1 1 calc R . . H34B H 0.9615 0.1838 0.6780 0.070 Uiso 1 1 calc R . . H34C H 0.8838 0.1512 0.6720 0.070 Uiso 1 1 calc R . . C35 C 0.8194(6) 0.0250(3) 0.7786(6) 0.041(3) Uani 1 1 d . . . H35 H 0.7785 0.0404 0.8123 0.049 Uiso 1 1 calc R . . C36 C 0.8514(7) -0.0079(3) 0.8284(6) 0.065(3) Uani 1 1 d . . . H36A H 0.7910 -0.0189 0.8476 0.098 Uiso 1 1 calc R . . H36B H 0.8996 -0.0013 0.8753 0.098 Uiso 1 1 calc R . . H36C H 0.8843 -0.0247 0.7943 0.098 Uiso 1 1 calc R . . C37 C 0.7507(7) 0.0133(3) 0.7046(6) 0.060(3) Uani 1 1 d . . . H37A H 0.7896 -0.0015 0.6702 0.090 Uiso 1 1 calc R . . H37B H 0.7244 0.0340 0.6737 0.090 Uiso 1 1 calc R . . H37C H 0.6935 -0.0003 0.7219 0.090 Uiso 1 1 calc R . . C38 C 0.5774(6) 0.1169(2) 0.7145(5) 0.026(2) Uani 1 1 d . . . C39 C 0.4907(6) 0.1029(2) 0.7453(5) 0.029(2) Uani 1 1 d . . . C40 C 0.4016(6) 0.0999(2) 0.6928(6) 0.040(3) Uani 1 1 d . . . H40 H 0.3425 0.0904 0.7131 0.047 Uiso 1 1 calc R . . C41 C 0.3956(7) 0.1101(3) 0.6124(5) 0.052(3) Uani 1 1 d . . . H41 H 0.3337 0.1076 0.5777 0.063 Uiso 1 1 calc R . . C42 C 0.4815(6) 0.1241(3) 0.5831(5) 0.042(3) Uani 1 1 d . . . H42 H 0.4786 0.1310 0.5276 0.050 Uiso 1 1 calc R . . C43 C 0.5728(6) 0.1281(2) 0.6342(5) 0.028(2) Uani 1 1 d . . . C44 C 0.4968(6) 0.0885(3) 0.8307(5) 0.031(2) Uani 1 1 d . . . H44 H 0.5417 0.1046 0.8665 0.037 Uiso 1 1 calc R . . C45 C 0.3931(5) 0.0866(2) 0.8658(5) 0.036(2) Uani 1 1 d . . . H45A H 0.3597 0.1097 0.8607 0.054 Uiso 1 1 calc R . . H45B H 0.4039 0.0799 0.9234 0.054 Uiso 1 1 calc R . . H45C H 0.3497 0.0689 0.8356 0.054 Uiso 1 1 calc R . . C46 C 0.5452(6) 0.0521(3) 0.8374(6) 0.056(3) Uani 1 1 d . . . H46A H 0.5067 0.0361 0.7990 0.084 Uiso 1 1 calc R . . H46B H 0.5442 0.0432 0.8930 0.084 Uiso 1 1 calc R . . H46C H 0.6160 0.0536 0.8244 0.084 Uiso 1 1 calc R . . C47 C 0.6613(6) 0.1445(3) 0.5952(5) 0.032(2) Uani 1 1 d . . . H47 H 0.7149 0.1513 0.6401 0.038 Uiso 1 1 calc R . . C48 C 0.6307(7) 0.1778(3) 0.5463(5) 0.061(3) Uani 1 1 d . . . H48A H 0.5797 0.1718 0.5008 0.092 Uiso 1 1 calc R . . H48B H 0.6911 0.1879 0.5252 0.092 Uiso 1 1 calc R . . H48C H 0.6017 0.1950 0.5817 0.092 Uiso 1 1 calc R . . C49 C 0.7103(6) 0.1187(3) 0.5386(5) 0.048(3) Uani 1 1 d . . . H49A H 0.6580 0.1102 0.4964 0.072 Uiso 1 1 calc R . . H49B H 0.7399 0.0987 0.5705 0.072 Uiso 1 1 calc R . . H49C H 0.7641 0.1309 0.5127 0.072 Uiso 1 1 calc R . . C50 C 0.7507(6) 0.1025(2) 0.7480(5) 0.025(2) Uani 1 1 d . . . H50 H 0.7443 0.0884 0.7001 0.030 Uiso 1 1 calc R . . C51 C 0.9651(6) 0.1272(2) 1.0787(5) 0.031(2) Uani 1 1 d . . . C52 C 1.0521(6) 0.1108(2) 1.0524(5) 0.026(2) Uani 1 1 d . . . C53 C 1.1399(6) 0.1094(3) 1.1072(6) 0.041(3) Uani 1 1 d . . . H53 H 1.1994 0.0983 1.0913 0.049 Uiso 1 1 calc R . . C54 C 1.1423(7) 0.1240(3) 1.1849(6) 0.054(3) Uani 1 1 d . . . H54 H 1.2022 0.1224 1.2224 0.065 Uiso 1 1 calc R . . C55 C 1.0566(6) 0.1405(3) 1.2063(5) 0.052(3) Uani 1 1 d . . . H55 H 1.0594 0.1509 1.2589 0.063 Uiso 1 1 calc R . . C56 C 0.9675(6) 0.1430(3) 1.1561(5) 0.037(2) Uani 1 1 d . . . C57 C 1.0492(5) 0.0938(3) 0.9713(5) 0.035(3) Uani 1 1 d . . . H57 H 1.0038 0.1083 0.9319 0.042 Uiso 1 1 calc R . . C58 C 1.1532(5) 0.0906(3) 0.9380(5) 0.048(3) Uani 1 1 d . . . H58A H 1.1845 0.1140 0.9363 0.072 Uiso 1 1 calc R . . H58B H 1.1437 0.0807 0.8829 0.072 Uiso 1 1 calc R . . H58C H 1.1977 0.0751 0.9735 0.072 Uiso 1 1 calc R . . C59 C 1.0031(6) 0.0570(3) 0.9732(5) 0.043(3) Uani 1 1 d . . . H59A H 1.0430 0.0428 1.0148 0.065 Uiso 1 1 calc R . . H59B H 1.0043 0.0459 0.9198 0.065 Uiso 1 1 calc R . . H59C H 0.9324 0.0588 0.9863 0.065 Uiso 1 1 calc R . . C60 C 0.8772(6) 0.1618(3) 1.1856(5) 0.037(2) Uani 1 1 d . . . H60 H 0.8250 0.1660 1.1380 0.044 Uiso 1 1 calc R . . C61 C 0.9083(7) 0.1976(3) 1.2243(6) 0.070(4) Uani 1 1 d . . . H61A H 0.8483 0.2090 1.2434 0.105 Uiso 1 1 calc R . . H61B H 0.9359 0.2127 1.1837 0.105 Uiso 1 1 calc R . . H61C H 0.9605 0.1940 1.2705 0.105 Uiso 1 1 calc R . . C62 C 0.8275(6) 0.1405(3) 1.2501(5) 0.061(3) Uani 1 1 d . . . H62A H 0.8004 0.1184 1.2260 0.092 Uiso 1 1 calc R . . H62B H 0.7718 0.1542 1.2694 0.092 Uiso 1 1 calc R . . H62C H 0.8788 0.1353 1.2961 0.092 Uiso 1 1 calc R . . C63 C 0.6273(5) 0.0912(2) 1.0415(4) 0.023(2) Uani 1 1 d . . . C64 C 0.5371(5) 0.1094(3) 1.0587(5) 0.029(2) Uani 1 1 d . . . C65 C 0.4636(6) 0.0906(3) 1.0980(5) 0.034(2) Uani 1 1 d . . . H65 H 0.4030 0.1024 1.1096 0.041 Uiso 1 1 calc R . . C66 C 0.4774(6) 0.0557(3) 1.1202(5) 0.038(2) Uani 1 1 d . . . H66 H 0.4273 0.0437 1.1472 0.045 Uiso 1 1 calc R . . C67 C 0.5643(6) 0.0383(3) 1.1029(5) 0.037(2) Uani 1 1 d . . . H67 H 0.5741 0.0143 1.1186 0.045 Uiso 1 1 calc R . . C68 C 0.6391(6) 0.0556(3) 1.0620(5) 0.032(2) Uani 1 1 d . . . C69 C 0.5222(5) 0.1481(2) 1.0407(5) 0.026(2) Uani 1 1 d . . . H69 H 0.5476 0.1526 0.9867 0.031 Uiso 1 1 calc R . . C70 C 0.4114(5) 0.1603(2) 1.0341(5) 0.038(3) Uani 1 1 d . . . H70A H 0.3704 0.1460 0.9934 0.057 Uiso 1 1 calc R . . H70B H 0.4076 0.1852 1.0176 0.057 Uiso 1 1 calc R . . H70C H 0.3850 0.1577 1.0871 0.057 Uiso 1 1 calc R . . C71 C 0.5866(6) 0.1706(2) 1.1034(5) 0.038(2) Uani 1 1 d . . . H71A H 0.6586 0.1638 1.1044 0.057 Uiso 1 1 calc R . . H71B H 0.5640 0.1668 1.1574 0.057 Uiso 1 1 calc R . . H71C H 0.5787 0.1955 1.0885 0.057 Uiso 1 1 calc R . . C72 C 0.7323(6) 0.0330(3) 1.0469(5) 0.036(3) Uani 1 1 d . . . H72 H 0.7732 0.0471 1.0108 0.043 Uiso 1 1 calc R . . C73 C 0.7033(6) -0.0009(3) 1.0023(6) 0.050(3) Uani 1 1 d . . . H73A H 0.6723 -0.0171 1.0389 0.076 Uiso 1 1 calc R . . H73B H 0.7646 -0.0118 0.9844 0.076 Uiso 1 1 calc R . . H73C H 0.6544 0.0041 0.9548 0.076 Uiso 1 1 calc R . . C74 C 0.8029(6) 0.0249(3) 1.1247(5) 0.051(3) Uani 1 1 d . . . H74A H 0.7662 0.0103 1.1611 0.077 Uiso 1 1 calc R . . H74B H 0.8243 0.0470 1.1522 0.077 Uiso 1 1 calc R . . H74C H 0.8632 0.0121 1.1105 0.077 Uiso 1 1 calc R . . C75 C 0.7924(5) 0.1113(2) 1.0498(5) 0.025(2) Uani 1 1 d . . . H75 H 0.7999 0.1002 1.1018 0.030 Uiso 1 1 calc R . . C76 C 0.3795(10) -0.0771(4) 0.6853(7) 0.114(5) Uani 1 1 d . . . H76A H 0.3824 -0.0520 0.6718 0.172 Uiso 1 1 calc R . . H76B H 0.3719 -0.0798 0.7434 0.172 Uiso 1 1 calc R . . H76C H 0.3211 -0.0880 0.6529 0.172 Uiso 1 1 calc R . . C77 C 0.4787(10) -0.0952(5) 0.6660(7) 0.076(4) Uani 1 1 d . . . C78 C 0.4892(11) -0.1324(4) 0.6682(6) 0.079(4) Uani 1 1 d . . . H78 H 0.4344 -0.1468 0.6815 0.094 Uiso 1 1 calc R . . C79 C 0.5800(12) -0.1475(4) 0.6507(6) 0.083(4) Uani 1 1 d . . . H79 H 0.5868 -0.1724 0.6525 0.099 Uiso 1 1 calc R . . C80 C 0.6599(10) -0.1277(4) 0.6309(7) 0.083(4) Uani 1 1 d . . . H80 H 0.7220 -0.1385 0.6197 0.099 Uiso 1 1 calc R . . C81 C 0.6481(10) -0.0905(4) 0.6274(7) 0.080(4) Uani 1 1 d . . . H81 H 0.7024 -0.0762 0.6126 0.095 Uiso 1 1 calc R . . C82 C 0.5584(11) -0.0749(4) 0.6452(6) 0.081(4) Uani 1 1 d . . . H82 H 0.5516 -0.0499 0.6430 0.098 Uiso 1 1 calc R . . C83A C -0.134(3) -0.1023(14) 0.507(3) 0.36(4) Uani 0.58(3) 1 d P A 1 H83A H -0.1913 -0.0994 0.5403 0.535 Uiso 0.58(3) 1 calc PR A 1 H83B H -0.1090 -0.1266 0.5120 0.535 Uiso 0.58(3) 1 calc PR A 1 H83C H -0.1576 -0.0972 0.4501 0.535 Uiso 0.58(3) 1 calc PR A 1 C83B C 0.145(3) -0.0203(13) 0.514(2) 0.17(3) Uani 0.42(3) 1 d P A 2 H83D H 0.1504 -0.0270 0.4572 0.261 Uiso 0.42(3) 1 calc PR A 2 H83E H 0.2134 -0.0161 0.5418 0.261 Uiso 0.42(3) 1 calc PR A 2 H83F H 0.1042 0.0013 0.5152 0.261 Uiso 0.42(3) 1 calc PR A 2 C84 C -0.063(4) -0.081(2) 0.5322(15) 0.77(9) Uani 1 1 d . . . C85 C 0.034(2) -0.0695(9) 0.5077(15) 0.200(13) Uani 1 1 d . A . H85 H 0.0539 -0.0789 0.4584 0.240 Uiso 1 1 calc R . . C87 C 0.0963(15) -0.0510(5) 0.6359(13) 0.159(7) Uani 1 1 d . A . H87 H 0.1467 -0.0419 0.6758 0.190 Uiso 1 1 calc R . . C88 C 0.005(2) -0.0725(7) 0.6593(16) 0.222(15) Uani 1 1 d . . . H88 H -0.0127 -0.0761 0.7129 0.267 Uiso 1 1 calc R A . C89 C -0.051(3) -0.0872(12) 0.581(4) 0.47(5) Uani 1 1 d . A . H89 H -0.0803 -0.1095 0.5897 0.562 Uiso 1 1 calc R . . C90 C 0.3301(19) 0.0149(8) 0.6079(18) 0.153(15) Uani 0.50 1 d P . . H90A H 0.2716 -0.0002 0.5900 0.230 Uiso 0.50 1 calc PR . . H90B H 0.3086 0.0397 0.6056 0.230 Uiso 0.50 1 calc PR . . H90C H 0.3564 0.0089 0.6639 0.230 Uiso 0.50 1 calc PR . . C91 C 0.4188(14) 0.0091(5) 0.5485(10) 0.116(6) Uani 1 1 d . . . C92 C 0.5076(15) 0.0265(5) 0.5560(10) 0.121(6) Uani 1 1 d . . . H92 H 0.5169 0.0451 0.5947 0.145 Uiso 1 1 calc R . . C93 C 0.5889(13) 0.0184(4) 0.5084(11) 0.118(6) Uani 1 1 d . . . H93 H 0.6497 0.0321 0.5154 0.141 Uiso 1 1 calc R . . C94 C 0.101(3) -0.0455(10) 0.5504(15) 0.235(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0211(2) 0.0277(3) 0.0222(2) 0.0010(3) 0.00564(14) -0.0009(3) N1 0.015(3) 0.019(5) 0.024(4) 0.004(3) 0.009(3) 0.002(3) N2 0.014(3) 0.029(5) 0.028(4) 0.007(3) 0.006(3) -0.003(3) N3 0.023(4) 0.019(5) 0.025(4) -0.001(3) 0.002(3) -0.003(3) N4 0.023(4) 0.015(4) 0.030(4) 0.001(3) 0.007(3) 0.002(3) N5 0.027(4) 0.011(4) 0.033(4) 0.004(3) 0.005(3) 0.003(3) N6 0.013(3) 0.019(5) 0.030(4) -0.003(3) 0.002(3) -0.002(3) C1 0.031(5) 0.013(6) 0.035(5) 0.001(4) 0.008(4) -0.002(4) C2 0.022(5) 0.036(7) 0.034(5) -0.008(5) 0.004(4) 0.009(5) C3 0.024(5) 0.054(8) 0.034(6) 0.000(5) 0.009(4) -0.008(5) C4 0.039(6) 0.038(8) 0.057(7) 0.001(6) 0.024(5) -0.015(5) C5 0.031(5) 0.045(8) 0.041(6) 0.019(5) 0.004(4) -0.004(5) C6 0.024(5) 0.030(7) 0.031(5) -0.005(4) 0.011(4) 0.006(4) C7 0.017(4) 0.027(6) 0.030(5) 0.010(4) -0.003(4) 0.002(4) C8 0.016(4) 0.046(8) 0.048(6) 0.001(5) 0.003(4) -0.005(4) C9 0.031(5) 0.060(8) 0.032(6) 0.003(5) 0.000(4) -0.008(5) C10 0.033(5) 0.040(7) 0.034(6) 0.000(5) 0.013(4) -0.001(5) C11 0.045(6) 0.076(9) 0.033(6) -0.001(6) 0.006(4) 0.011(6) C12 0.037(5) 0.044(8) 0.057(7) 0.017(5) 0.010(5) 0.014(5) C13 0.022(5) 0.036(7) 0.030(5) 0.001(4) 0.015(4) 0.008(4) C14 0.025(5) 0.041(7) 0.022(5) 0.012(4) 0.006(4) 0.002(5) C15 0.030(5) 0.049(8) 0.039(6) -0.002(5) 0.016(4) 0.008(5) C16 0.051(7) 0.048(9) 0.049(7) 0.010(6) 0.019(5) 0.024(6) C17 0.055(6) 0.033(7) 0.045(6) -0.010(5) 0.022(5) 0.008(6) C18 0.034(5) 0.024(6) 0.037(6) -0.001(4) 0.022(4) 0.002(5) C19 0.016(4) 0.046(8) 0.043(6) -0.006(5) -0.001(4) 0.002(5) C20 0.020(5) 0.052(8) 0.051(6) 0.007(5) -0.002(4) 0.001(5) C21 0.027(5) 0.042(8) 0.048(6) 0.004(5) 0.005(4) -0.002(5) C22 0.043(6) 0.040(8) 0.043(6) -0.012(5) 0.022(5) -0.004(5) C23 0.098(8) 0.055(9) 0.024(6) -0.007(5) 0.005(5) 0.002(7) C24 0.063(7) 0.048(9) 0.078(8) -0.026(7) 0.019(6) -0.021(6) C25 0.027(4) 0.026(6) 0.026(5) -0.005(4) 0.004(4) 0.004(5) C26 0.014(4) 0.027(7) 0.037(5) -0.001(4) 0.001(4) -0.006(4) C27 0.030(5) 0.034(7) 0.032(5) 0.001(5) 0.005(4) 0.009(5) C28 0.041(5) 0.020(7) 0.057(6) 0.007(5) 0.025(5) 0.012(5) C29 0.049(6) 0.037(8) 0.076(8) -0.004(6) 0.033(6) 0.022(6) C30 0.057(6) 0.030(7) 0.076(8) -0.009(6) 0.034(6) 0.018(6) C31 0.040(6) 0.034(7) 0.037(6) -0.006(5) 0.009(4) -0.011(5) C32 0.032(5) 0.029(7) 0.042(6) -0.008(5) 0.017(4) 0.000(5) C33 0.024(5) 0.054(8) 0.051(6) 0.001(5) 0.011(4) -0.004(5) C34 0.034(5) 0.046(8) 0.060(7) 0.006(6) 0.005(5) -0.011(5) C35 0.044(6) 0.020(7) 0.061(7) -0.002(5) 0.018(5) -0.002(5) C36 0.066(7) 0.051(9) 0.080(9) 0.003(7) 0.012(6) -0.010(6) C37 0.063(7) 0.052(9) 0.064(8) -0.009(6) 0.000(6) -0.015(6) C38 0.025(5) 0.027(6) 0.025(5) -0.001(4) 0.000(4) -0.009(4) C39 0.022(5) 0.034(7) 0.031(5) 0.007(4) 0.001(4) -0.007(4) C40 0.023(5) 0.042(8) 0.054(7) 0.002(5) 0.007(4) -0.012(5) C41 0.039(6) 0.086(10) 0.030(6) -0.001(6) -0.010(4) -0.012(6) C42 0.040(6) 0.051(8) 0.034(6) 0.002(5) 0.001(5) 0.004(5) C43 0.023(5) 0.032(7) 0.031(5) 0.001(4) 0.009(4) 0.003(4) C44 0.024(5) 0.039(7) 0.031(5) 0.005(5) 0.004(4) 0.004(5) C45 0.024(5) 0.035(7) 0.048(6) 0.019(5) 0.003(4) -0.006(4) C46 0.045(6) 0.072(10) 0.051(7) 0.016(6) 0.008(5) -0.002(6) C47 0.039(5) 0.032(6) 0.024(5) 0.000(5) -0.001(4) -0.005(5) C48 0.071(7) 0.079(10) 0.036(6) 0.004(6) 0.009(5) -0.013(7) C49 0.054(6) 0.075(9) 0.017(5) 0.005(5) 0.012(4) -0.003(6) C50 0.039(5) 0.015(5) 0.019(4) 0.003(4) 0.001(4) -0.006(4) C51 0.025(5) 0.027(7) 0.039(6) 0.002(4) -0.002(4) -0.014(4) C52 0.022(5) 0.027(6) 0.029(5) 0.005(4) -0.001(4) -0.003(4) C53 0.023(5) 0.051(8) 0.048(7) 0.010(6) -0.001(4) 0.002(5) C54 0.037(6) 0.071(10) 0.051(7) 0.014(6) -0.014(5) -0.013(6) C55 0.037(5) 0.080(10) 0.039(6) 0.000(6) 0.000(4) -0.008(6) C56 0.029(5) 0.057(8) 0.025(5) -0.006(6) -0.004(4) -0.019(6) C57 0.018(5) 0.051(8) 0.035(6) -0.004(5) 0.001(4) 0.006(5) C58 0.028(5) 0.051(8) 0.067(7) -0.002(6) 0.010(5) 0.007(5) C59 0.035(5) 0.043(8) 0.054(7) -0.014(5) 0.013(4) 0.000(5) C60 0.042(5) 0.036(7) 0.033(6) -0.011(5) 0.007(4) -0.008(5) C61 0.072(7) 0.087(11) 0.056(7) -0.034(7) 0.029(6) -0.016(7) C62 0.059(6) 0.076(10) 0.051(7) -0.018(7) 0.021(5) -0.011(7) C63 0.023(5) 0.028(6) 0.018(5) 0.001(4) 0.006(3) -0.010(4) C64 0.017(4) 0.040(7) 0.031(5) -0.003(5) 0.004(4) -0.008(5) C65 0.030(5) 0.038(7) 0.037(6) 0.000(5) 0.013(4) -0.001(5) C66 0.040(5) 0.034(7) 0.041(6) 0.009(5) 0.014(4) -0.007(5) C67 0.039(5) 0.036(7) 0.037(6) 0.010(5) 0.000(4) -0.003(5) C68 0.025(5) 0.037(7) 0.034(5) 0.008(5) 0.008(4) -0.007(5) C69 0.023(4) 0.019(6) 0.038(5) 0.006(4) 0.009(4) -0.005(5) C70 0.030(5) 0.049(8) 0.037(6) -0.001(5) 0.018(4) 0.014(5) C71 0.038(5) 0.031(7) 0.046(6) -0.005(5) 0.015(4) 0.002(5) C72 0.028(5) 0.041(8) 0.042(6) 0.005(5) 0.016(4) -0.002(5) C73 0.056(6) 0.036(8) 0.061(7) 0.004(6) 0.009(5) -0.001(6) C74 0.045(6) 0.049(8) 0.060(7) 0.013(6) 0.009(5) 0.003(6) C75 0.027(5) 0.036(7) 0.016(5) -0.004(4) 0.014(4) -0.007(4) C76 0.126(11) 0.130(16) 0.092(11) -0.031(10) 0.033(9) -0.002(11) C77 0.084(10) 0.103(14) 0.042(7) -0.014(8) 0.005(6) -0.009(11) C78 0.106(11) 0.088(14) 0.042(7) 0.010(7) 0.012(7) -0.025(10) C79 0.105(10) 0.089(13) 0.049(7) 0.001(8) -0.015(7) 0.013(11) C80 0.070(9) 0.093(15) 0.077(9) 0.013(9) -0.029(7) -0.022(9) C81 0.089(10) 0.071(13) 0.077(10) -0.008(8) 0.001(7) -0.014(9) C82 0.098(10) 0.090(13) 0.057(8) -0.011(8) 0.014(7) -0.022(10) C83A 0.26(5) 0.47(9) 0.30(6) 0.07(5) -0.19(4) -0.19(5) C83B 0.23(5) 0.20(6) 0.11(4) 0.07(4) 0.13(4) 0.11(4) C84 0.31(5) 2.0(3) 0.035(15) -0.17(5) 0.08(2) -0.35(8) C85 0.16(2) 0.29(4) 0.15(2) -0.11(2) 0.017(17) 0.00(2) C87 0.200(19) 0.15(2) 0.125(18) -0.029(14) 0.010(14) 0.050(16) C88 0.25(3) 0.19(3) 0.26(3) 0.16(2) 0.18(2) 0.14(2) C89 0.22(4) 0.34(5) 0.77(11) 0.14(6) -0.31(6) -0.05(3) C90 0.11(2) 0.18(4) 0.18(3) -0.06(3) 0.07(2) 0.03(2) C91 0.120(14) 0.090(16) 0.127(15) -0.035(11) -0.033(11) -0.011(11) C92 0.101(12) 0.132(19) 0.123(14) -0.023(12) -0.020(11) 0.032(14) C93 0.141(15) 0.064(13) 0.136(15) -0.027(11) -0.045(12) -0.010(11) C94 0.37(4) 0.27(4) 0.097(19) -0.04(2) 0.14(2) -0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N1 2.448(6) . ? Sm1 N6 2.460(6) . ? Sm1 N3 2.462(6) . ? Sm1 N2 2.463(7) . ? Sm1 N5 2.467(6) . ? Sm1 N4 2.469(6) . ? Sm1 C25 2.833(9) . ? Sm1 C75 2.848(8) . ? Sm1 C50 2.854(9) . ? N1 C25 1.331(8) . ? N1 C1 1.452(9) . ? N2 C25 1.351(8) . ? N2 C13 1.449(9) . ? N3 C50 1.317(9) . ? N3 C26 1.470(9) . ? N4 C50 1.349(9) . ? N4 C38 1.446(9) . ? N5 C75 1.337(8) . ? N5 C51 1.464(9) . ? N6 C75 1.319(8) . ? N6 C63 1.432(9) . ? C1 C6 1.410(11) . ? C1 C2 1.411(10) . ? C2 C3 1.402(11) . ? C2 C7 1.485(11) . ? C3 C4 1.371(11) . ? C4 C5 1.377(11) . ? C5 C6 1.420(10) . ? C6 C10 1.530(10) . ? C7 C8 1.525(9) . ? C7 C9 1.535(10) . ? C10 C11 1.513(10) . ? C10 C12 1.547(11) . ? C13 C14 1.412(10) . ? C13 C18 1.412(11) . ? C14 C15 1.409(11) . ? C14 C19 1.506(11) . ? C15 C16 1.374(12) . ? C16 C17 1.372(11) . ? C17 C18 1.387(11) . ? C18 C22 1.527(11) . ? C19 C20 1.522(9) . ? C19 C21 1.553(10) . ? C22 C23 1.525(11) . ? C22 C24 1.533(11) . ? C26 C31 1.391(11) . ? C26 C27 1.417(10) . ? C27 C28 1.402(10) . ? C27 C32 1.504(12) . ? C28 C29 1.351(12) . ? C29 C30 1.381(11) . ? C30 C31 1.388(11) . ? C31 C35 1.549(11) . ? C32 C33 1.523(10) . ? C32 C34 1.535(11) . ? C35 C37 1.507(11) . ? C35 C36 1.528(12) . ? C38 C43 1.386(10) . ? C38 C39 1.402(10) . ? C39 C40 1.387(10) . ? C39 C44 1.507(10) . ? C40 C41 1.376(11) . ? C41 C42 1.382(11) . ? C42 C43 1.401(10) . ? C43 C47 1.524(10) . ? C44 C46 1.516(12) . ? C44 C45 1.541(9) . ? C47 C48 1.528(12) . ? C47 C49 1.542(11) . ? C51 C56 1.407(11) . ? C51 C52 1.413(10) . ? C52 C53 1.390(10) . ? C52 C57 1.481(11) . ? C53 C54 1.394(12) . ? C54 C55 1.370(12) . ? C55 C56 1.366(10) . ? C56 C60 1.512(11) . ? C57 C59 1.523(11) . ? C57 C58 1.533(9) . ? C60 C61 1.537(12) . ? C60 C62 1.537(11) . ? C63 C68 1.397(11) . ? C63 C64 1.428(10) . ? C64 C65 1.414(10) . ? C64 C69 1.504(11) . ? C65 C66 1.381(11) . ? C66 C67 1.376(10) . ? C67 C68 1.413(10) . ? C68 C72 1.537(11) . ? C69 C70 1.524(9) . ? C69 C71 1.526(10) . ? C72 C73 1.512(12) . ? C72 C74 1.535(11) . ? C76 C77 1.539(15) . ? C77 C82 1.376(15) . ? C77 C78 1.415(16) . ? C78 C79 1.384(15) . ? C79 C80 1.359(15) . ? C80 C81 1.421(15) . ? C81 C82 1.380(14) . ? C83A C84 1.27(6) . ? C83B C94 1.30(4) . ? C84 C89 0.83(7) . ? C84 C85 1.45(5) . ? C85 C94 1.41(3) . ? C87 C94 1.43(2) . ? C87 C88 1.53(2) . ? C88 C89 1.53(4) . ? C90 C91 1.62(2) . ? C91 C92 1.337(18) . ? C91 C93 1.399(18) 3_656 ? C92 C93 1.427(17) . ? C93 C91 1.399(18) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sm1 N6 141.9(2) . . ? N1 Sm1 N3 101.9(2) . . ? N6 Sm1 N3 111.3(2) . . ? N1 Sm1 N2 56.45(18) . . ? N6 Sm1 N2 100.9(2) . . ? N3 Sm1 N2 143.7(2) . . ? N1 Sm1 N5 100.1(2) . . ? N6 Sm1 N5 55.53(19) . . ? N3 Sm1 N5 102.6(2) . . ? N2 Sm1 N5 109.4(2) . . ? N1 Sm1 N4 110.2(2) . . ? N6 Sm1 N4 103.8(2) . . ? N3 Sm1 N4 55.62(19) . . ? N2 Sm1 N4 101.4(2) . . ? N5 Sm1 N4 145.3(2) . . ? N1 Sm1 C25 28.00(17) . . ? N6 Sm1 C25 124.0(2) . . ? N3 Sm1 C25 124.7(2) . . ? N2 Sm1 C25 28.46(17) . . ? N5 Sm1 C25 107.0(2) . . ? N4 Sm1 C25 107.7(2) . . ? N1 Sm1 C75 123.2(2) . . ? N6 Sm1 C75 27.55(17) . . ? N3 Sm1 C75 109.1(2) . . ? N2 Sm1 C75 107.2(2) . . ? N5 Sm1 C75 27.98(18) . . ? N4 Sm1 C75 126.6(2) . . ? C25 Sm1 C75 118.9(2) . . ? N1 Sm1 C50 108.5(2) . . ? N6 Sm1 C50 109.6(2) . . ? N3 Sm1 C50 27.44(19) . . ? N2 Sm1 C50 125.1(2) . . ? N5 Sm1 C50 125.5(2) . . ? N4 Sm1 C50 28.18(19) . . ? C25 Sm1 C50 120.0(2) . . ? C75 Sm1 C50 121.0(2) . . ? C25 N1 C1 112.5(7) . . ? C25 N1 Sm1 92.3(5) . . ? C1 N1 Sm1 155.0(5) . . ? C25 N2 C13 111.7(7) . . ? C25 N2 Sm1 91.2(5) . . ? C13 N2 Sm1 157.1(5) . . ? C50 N3 C26 113.9(7) . . ? C50 N3 Sm1 93.1(5) . . ? C26 N3 Sm1 152.9(5) . . ? C50 N4 C38 114.7(7) . . ? C50 N4 Sm1 92.0(5) . . ? C38 N4 Sm1 153.2(5) . . ? C75 N5 C51 114.2(7) . . ? C75 N5 Sm1 92.1(5) . . ? C51 N5 Sm1 153.7(5) . . ? C75 N6 C63 112.9(6) . . ? C75 N6 Sm1 92.9(4) . . ? C63 N6 Sm1 154.2(5) . . ? C6 C1 C2 121.0(8) . . ? C6 C1 N1 121.0(7) . . ? C2 C1 N1 117.8(7) . . ? C3 C2 C1 117.3(8) . . ? C3 C2 C7 120.3(7) . . ? C1 C2 C7 122.2(8) . . ? C4 C3 C2 122.7(8) . . ? C3 C4 C5 120.0(8) . . ? C4 C5 C6 120.4(8) . . ? C1 C6 C5 118.5(7) . . ? C1 C6 C10 124.2(8) . . ? C5 C6 C10 117.2(8) . . ? C2 C7 C8 114.6(6) . . ? C2 C7 C9 111.1(7) . . ? C8 C7 C9 108.4(6) . . ? C11 C10 C6 112.5(6) . . ? C11 C10 C12 107.3(7) . . ? C6 C10 C12 112.5(7) . . ? C14 C13 C18 121.6(8) . . ? C14 C13 N2 116.6(8) . . ? C18 C13 N2 121.8(7) . . ? C15 C14 C13 117.4(9) . . ? C15 C14 C19 119.5(7) . . ? C13 C14 C19 122.9(8) . . ? C16 C15 C14 121.0(9) . . ? C17 C16 C15 120.3(9) . . ? C16 C17 C18 122.1(9) . . ? C17 C18 C13 117.4(8) . . ? C17 C18 C22 119.1(8) . . ? C13 C18 C22 123.5(8) . . ? C14 C19 C20 114.3(7) . . ? C14 C19 C21 109.4(7) . . ? C20 C19 C21 109.6(7) . . ? C23 C22 C18 111.2(7) . . ? C23 C22 C24 107.4(8) . . ? C18 C22 C24 113.5(8) . . ? N1 C25 N2 120.1(8) . . ? N1 C25 Sm1 59.7(4) . . ? N2 C25 Sm1 60.4(4) . . ? C31 C26 C27 121.1(8) . . ? C31 C26 N3 121.9(7) . . ? C27 C26 N3 117.0(8) . . ? C28 C27 C26 116.0(9) . . ? C28 C27 C32 120.8(8) . . ? C26 C27 C32 123.1(8) . . ? C29 C28 C27 123.4(9) . . ? C28 C29 C30 119.5(9) . . ? C29 C30 C31 120.5(10) . . ? C30 C31 C26 119.3(8) . . ? C30 C31 C35 117.0(9) . . ? C26 C31 C35 123.6(8) . . ? C27 C32 C33 115.4(7) . . ? C27 C32 C34 110.9(7) . . ? C33 C32 C34 108.6(7) . . ? C37 C35 C36 107.6(8) . . ? C37 C35 C31 112.4(8) . . ? C36 C35 C31 112.4(8) . . ? C43 C38 C39 120.5(7) . . ? C43 C38 N4 120.7(7) . . ? C39 C38 N4 118.7(7) . . ? C40 C39 C38 118.2(8) . . ? C40 C39 C44 120.8(7) . . ? C38 C39 C44 120.8(7) . . ? C41 C40 C39 122.5(8) . . ? C40 C41 C42 118.7(8) . . ? C41 C42 C43 120.8(8) . . ? C38 C43 C42 119.4(7) . . ? C38 C43 C47 124.8(7) . . ? C42 C43 C47 115.8(7) . . ? C39 C44 C46 112.3(7) . . ? C39 C44 C45 114.0(7) . . ? C46 C44 C45 108.2(7) . . ? C43 C47 C48 113.0(7) . . ? C43 C47 C49 112.6(8) . . ? C48 C47 C49 107.9(7) . . ? N3 C50 N4 119.3(8) . . ? N3 C50 Sm1 59.5(4) . . ? N4 C50 Sm1 59.8(4) . . ? C56 C51 C52 121.7(7) . . ? C56 C51 N5 120.3(7) . . ? C52 C51 N5 117.9(7) . . ? C53 C52 C51 117.6(8) . . ? C53 C52 C57 120.7(8) . . ? C51 C52 C57 121.7(7) . . ? C52 C53 C54 121.2(8) . . ? C55 C54 C53 118.7(9) . . ? C56 C55 C54 123.6(9) . . ? C55 C56 C51 117.1(8) . . ? C55 C56 C60 119.5(8) . . ? C51 C56 C60 123.4(7) . . ? C52 C57 C59 110.5(7) . . ? C52 C57 C58 114.9(7) . . ? C59 C57 C58 107.9(7) . . ? C56 C60 C61 111.6(7) . . ? C56 C60 C62 112.4(8) . . ? C61 C60 C62 106.9(7) . . ? C68 C63 C64 119.6(7) . . ? C68 C63 N6 121.8(7) . . ? C64 C63 N6 118.6(8) . . ? C65 C64 C63 118.1(9) . . ? C65 C64 C69 120.0(7) . . ? C63 C64 C69 121.8(7) . . ? C66 C65 C64 121.8(8) . . ? C67 C66 C65 119.6(8) . . ? C66 C67 C68 121.0(9) . . ? C63 C68 C67 119.9(8) . . ? C63 C68 C72 124.7(7) . . ? C67 C68 C72 115.4(8) . . ? C64 C69 C70 114.5(7) . . ? C64 C69 C71 111.1(7) . . ? C70 C69 C71 109.7(7) . . ? C73 C72 C74 109.5(8) . . ? C73 C72 C68 112.8(7) . . ? C74 C72 C68 113.6(7) . . ? N6 C75 N5 119.5(7) . . ? N6 C75 Sm1 59.6(4) . . ? N5 C75 Sm1 59.9(4) . . ? C82 C77 C78 119.3(13) . . ? C82 C77 C76 119.2(16) . . ? C78 C77 C76 121.5(14) . . ? C79 C78 C77 119.3(13) . . ? C80 C79 C78 122.0(15) . . ? C79 C80 C81 118.3(14) . . ? C82 C81 C80 120.6(14) . . ? C77 C82 C81 120.4(14) . . ? C89 C84 C83A 102(8) . . ? C89 C84 C85 106(6) . . ? C83A C84 C85 138(4) . . ? C94 C85 C84 126(3) . . ? C94 C87 C88 116(2) . . ? C87 C88 C89 107(3) . . ? C84 C89 C88 138(8) . . ? C92 C91 C93 115.5(17) . 3_656 ? C92 C91 C90 123.8(19) . . ? C93 C91 C90 120(2) 3_656 . ? C91 C92 C93 122.9(17) . . ? C91 C93 C92 121.6(16) 3_656 . ? C83B C94 C85 122(3) . . ? C83B C94 C87 129(4) . . ? C85 C94 C87 108(3) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.200 _refine_diff_density_min -1.646 _refine_diff_density_rms 0.150 #===END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 262799' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Sm(F)(DippForm)2(THF)]' _chemical_melting_point '549 (dec.)' _chemical_formula_moiety 'C54 H78 F N4 O Sm' _chemical_formula_sum 'C54 H78 F N4 O Sm' _chemical_formula_weight 968.55 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.4714(2) _cell_length_b 12.1996(2) _cell_length_c 21.6593(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.0650(10) _cell_angle_gamma 90.00 _cell_volume 5080.93(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombohedral prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7149 _exptl_absorpt_correction_T_max 0.7954 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32459 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 28.24 _reflns_number_total 12173 _reflns_number_gt 10645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+1.7551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12173 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.568731(7) 0.600983(12) 0.264671(7) 0.01787(9) Uani 1 1 d . . . F1 F 0.66911(11) 0.54461(18) 0.27761(11) 0.0329(5) Uani 1 1 d . . . O1 O 0.62172(13) 0.77893(19) 0.25711(13) 0.0287(5) Uani 1 1 d . . . N1 N 0.48501(14) 0.4719(2) 0.19389(13) 0.0206(5) Uani 1 1 d . . . N2 N 0.51011(14) 0.6251(2) 0.14593(14) 0.0201(5) Uani 1 1 d . . . N3 N 0.51767(13) 0.7004(2) 0.33506(13) 0.0203(5) Uani 1 1 d . . . N4 N 0.55513(13) 0.5248(2) 0.36440(13) 0.0196(5) Uani 1 1 d . . . C1 C 0.45241(17) 0.3672(3) 0.18811(15) 0.0217(6) Uani 1 1 d . . . C2 C 0.49212(18) 0.2761(3) 0.22000(16) 0.0250(6) Uani 1 1 d . . . C3 C 0.4598(2) 0.1747(3) 0.21565(19) 0.0314(8) Uani 1 1 d . . . H3 H 0.4864 0.1128 0.2365 0.038 Uiso 1 1 calc R . . C4 C 0.3893(2) 0.1627(3) 0.1813(2) 0.0342(8) Uani 1 1 d . . . H4 H 0.3679 0.0930 0.1786 0.041 Uiso 1 1 calc R . . C5 C 0.3503(2) 0.2522(3) 0.15094(19) 0.0330(8) Uani 1 1 d . . . H5 H 0.3020 0.2431 0.1274 0.040 Uiso 1 1 calc R . . C6 C 0.38011(17) 0.3554(3) 0.15411(17) 0.0264(7) Uani 1 1 d . . . C7 C 0.57010(18) 0.2878(3) 0.25634(19) 0.0318(8) Uani 1 1 d . . . H7 H 0.5782 0.3622 0.2769 0.038 Uiso 1 1 calc R . . C8 C 0.5993(2) 0.2035(3) 0.3116(2) 0.0397(9) Uani 1 1 d . . . H8A H 0.5972 0.1302 0.2925 0.060 Uiso 1 1 calc R . . H8B H 0.5717 0.2048 0.3406 0.060 Uiso 1 1 calc R . . H8C H 0.6478 0.2217 0.3369 0.060 Uiso 1 1 calc R . . C9 C 0.6096(2) 0.2821(4) 0.2088(2) 0.0440(10) Uani 1 1 d . . . H9A H 0.6032 0.2095 0.1882 0.066 Uiso 1 1 calc R . . H9B H 0.6592 0.2946 0.2327 0.066 Uiso 1 1 calc R . . H9C H 0.5921 0.3383 0.1749 0.066 Uiso 1 1 calc R . . C10 C 0.33477(19) 0.4534(3) 0.1261(2) 0.0364(9) Uani 1 1 d . . . H10 H 0.3623 0.5054 0.1090 0.044 Uiso 1 1 calc R . . C11 C 0.3171(3) 0.5114(4) 0.1800(3) 0.0674(17) Uani 1 1 d . . . H11A H 0.2844 0.4667 0.1932 0.101 Uiso 1 1 calc R . . H11B H 0.2959 0.5825 0.1638 0.101 Uiso 1 1 calc R . . H11C H 0.3597 0.5227 0.2179 0.101 Uiso 1 1 calc R . . C12 C 0.2682(2) 0.4265(5) 0.0696(2) 0.0487(11) Uani 1 1 d . . . H12A H 0.2788 0.3763 0.0390 0.073 Uiso 1 1 calc R . . H12B H 0.2480 0.4941 0.0465 0.073 Uiso 1 1 calc R . . H12C H 0.2349 0.3917 0.0870 0.073 Uiso 1 1 calc R . . C13 C 0.52151(16) 0.6743(2) 0.09073(15) 0.0208(6) Uani 1 1 d . . . C14 C 0.48062(18) 0.7643(3) 0.05946(16) 0.0246(6) Uani 1 1 d . . . C15 C 0.4919(2) 0.8121(3) 0.00542(19) 0.0317(8) Uani 1 1 d . . . H15 H 0.4641 0.8725 -0.0161 0.038 Uiso 1 1 calc R . . C16 C 0.5432(2) 0.7730(3) -0.01735(18) 0.0330(8) Uani 1 1 d . . . H16 H 0.5496 0.8052 -0.0548 0.040 Uiso 1 1 calc R . . C17 C 0.58474(19) 0.6871(3) 0.01486(17) 0.0293(7) Uani 1 1 d . . . H17 H 0.6202 0.6611 -0.0005 0.035 Uiso 1 1 calc R . . C18 C 0.57585(17) 0.6376(3) 0.06959(15) 0.0228(6) Uani 1 1 d . . . C19 C 0.42262(18) 0.8070(3) 0.08275(17) 0.0265(7) Uani 1 1 d . . . H19 H 0.4360 0.7889 0.1305 0.032 Uiso 1 1 calc R . . C20 C 0.4136(2) 0.9311(3) 0.0761(2) 0.0387(9) Uani 1 1 d . . . H20A H 0.4581 0.9670 0.0993 0.058 Uiso 1 1 calc R . . H20B H 0.3790 0.9547 0.0953 0.058 Uiso 1 1 calc R . . H20C H 0.3978 0.9514 0.0295 0.058 Uiso 1 1 calc R . . C21 C 0.35429(19) 0.7487(3) 0.04724(19) 0.0333(8) Uani 1 1 d . . . H21A H 0.3408 0.7617 -0.0001 0.050 Uiso 1 1 calc R . . H21B H 0.3181 0.7769 0.0631 0.050 Uiso 1 1 calc R . . H21C H 0.3600 0.6698 0.0559 0.050 Uiso 1 1 calc R . . C22 C 0.62552(17) 0.5461(3) 0.10476(16) 0.0249(6) Uani 1 1 d . . . H22 H 0.6144 0.5256 0.1448 0.030 Uiso 1 1 calc R . . C23 C 0.7015(2) 0.5840(3) 0.1274(2) 0.0346(8) Uani 1 1 d . . . H23A H 0.7152 0.5978 0.0890 0.052 Uiso 1 1 calc R . . H23B H 0.7314 0.5270 0.1547 0.052 Uiso 1 1 calc R . . H23C H 0.7065 0.6516 0.1531 0.052 Uiso 1 1 calc R . . C24 C 0.6158(2) 0.4439(3) 0.06156(19) 0.0342(8) Uani 1 1 d . . . H24A H 0.5670 0.4208 0.0472 0.051 Uiso 1 1 calc R . . H24B H 0.6453 0.3847 0.0868 0.051 Uiso 1 1 calc R . . H24C H 0.6287 0.4606 0.0230 0.051 Uiso 1 1 calc R . . C25 C 0.48565(15) 0.5223(2) 0.14020(15) 0.0209(6) Uani 1 1 d . . . H25 H 0.4692 0.4868 0.0987 0.025 Uiso 1 1 calc R . . C26 C 0.49770(17) 0.8039(3) 0.35315(16) 0.0232(6) Uani 1 1 d . . . C27 C 0.42818(19) 0.8391(3) 0.3237(2) 0.0317(8) Uani 1 1 d . . . C28 C 0.4094(2) 0.9420(4) 0.3414(2) 0.0470(11) Uani 1 1 d . . . H28 H 0.3628 0.9667 0.3223 0.056 Uiso 1 1 calc R . . C29 C 0.4576(2) 1.0076(3) 0.3860(3) 0.0480(11) Uani 1 1 d . . . H29 H 0.4436 1.0761 0.3983 0.058 Uiso 1 1 calc R . . C30 C 0.5256(2) 0.9751(3) 0.4128(2) 0.0408(10) Uani 1 1 d . . . H30 H 0.5585 1.0220 0.4427 0.049 Uiso 1 1 calc R . . C31 C 0.54727(19) 0.8727(3) 0.39651(19) 0.0284(7) Uani 1 1 d . . . C32 C 0.37322(19) 0.7681(3) 0.2758(2) 0.0376(9) Uani 1 1 d . . . H32 H 0.3971 0.7059 0.2622 0.045 Uiso 1 1 calc R . . C33 C 0.3310(3) 0.8323(4) 0.2138(2) 0.0518(11) Uani 1 1 d . . . H33A H 0.3005 0.8848 0.2249 0.078 Uiso 1 1 calc R . . H33B H 0.3027 0.7811 0.1804 0.078 Uiso 1 1 calc R . . H33C H 0.3628 0.8717 0.1966 0.078 Uiso 1 1 calc R . . C34 C 0.3241(3) 0.7208(4) 0.3078(3) 0.0570(13) Uani 1 1 d . . . H34A H 0.3501 0.6732 0.3444 0.086 Uiso 1 1 calc R . . H34B H 0.2877 0.6781 0.2754 0.086 Uiso 1 1 calc R . . H34C H 0.3026 0.7806 0.3243 0.086 Uiso 1 1 calc R . . C35 C 0.62389(18) 0.8428(3) 0.42513(19) 0.0287(7) Uani 1 1 d . . . H35 H 0.6309 0.7739 0.4031 0.034 Uiso 1 1 calc R . . C36 C 0.6699(2) 0.9311(4) 0.4115(2) 0.0385(9) Uani 1 1 d . . . H36A H 0.6559 0.9435 0.3640 0.058 Uiso 1 1 calc R . . H36B H 0.7186 0.9073 0.4285 0.058 Uiso 1 1 calc R . . H36C H 0.6649 0.9994 0.4333 0.058 Uiso 1 1 calc R . . C37 C 0.6456(2) 0.8197(3) 0.4984(2) 0.0371(9) Uani 1 1 d . . . H37A H 0.6348 0.8834 0.5208 0.056 Uiso 1 1 calc R . . H37B H 0.6957 0.8051 0.5161 0.056 Uiso 1 1 calc R . . H37C H 0.6202 0.7556 0.5056 0.056 Uiso 1 1 calc R . . C38 C 0.56257(17) 0.4333(3) 0.40716(15) 0.0205(6) Uani 1 1 d . . . C39 C 0.6297(2) 0.3929(2) 0.44192(18) 0.0240(7) Uani 1 1 d . . . C40 C 0.63688(19) 0.3055(3) 0.48500(17) 0.0286(7) Uani 1 1 d . . . H40 H 0.6820 0.2787 0.5090 0.034 Uiso 1 1 calc R . . C41 C 0.5797(2) 0.2569(3) 0.49358(17) 0.0296(7) Uani 1 1 d . . . H41 H 0.5854 0.1989 0.5243 0.035 Uiso 1 1 calc R . . C42 C 0.51370(19) 0.2938(3) 0.45681(17) 0.0268(7) Uani 1 1 d . . . H42 H 0.4743 0.2587 0.4617 0.032 Uiso 1 1 calc R . . C43 C 0.50345(18) 0.3813(3) 0.41280(17) 0.0233(6) Uani 1 1 d . . . C44 C 0.69314(18) 0.4452(3) 0.43243(18) 0.0289(7) Uani 1 1 d . . . H44 H 0.6802 0.4628 0.3846 0.035 Uiso 1 1 calc R . . C45 C 0.7571(2) 0.3704(4) 0.4506(2) 0.0386(9) Uani 1 1 d . . . H45A H 0.7925 0.4035 0.4355 0.058 Uiso 1 1 calc R . . H45B H 0.7437 0.2987 0.4296 0.058 Uiso 1 1 calc R . . H45C H 0.7759 0.3611 0.4985 0.058 Uiso 1 1 calc R . . C46 C 0.7128(2) 0.5528(3) 0.4698(3) 0.0447(10) Uani 1 1 d . . . H46A H 0.6721 0.6012 0.4579 0.067 Uiso 1 1 calc R . . H46B H 0.7501 0.5883 0.4584 0.067 Uiso 1 1 calc R . . H46C H 0.7288 0.5383 0.5172 0.067 Uiso 1 1 calc R . . C47 C 0.42957(19) 0.4148(3) 0.37226(18) 0.0249(7) Uani 1 1 d . . . H47 H 0.4322 0.4696 0.3389 0.030 Uiso 1 1 calc R . . C48 C 0.38644(19) 0.3170(3) 0.33527(19) 0.0315(7) Uani 1 1 d . . . H48A H 0.4103 0.2822 0.3081 0.047 Uiso 1 1 calc R . . H48B H 0.3405 0.3426 0.3071 0.047 Uiso 1 1 calc R . . H48C H 0.3810 0.2636 0.3670 0.047 Uiso 1 1 calc R . . C49 C 0.3931(2) 0.4694(3) 0.4153(2) 0.0343(8) Uani 1 1 d . . . H49A H 0.3880 0.4162 0.4472 0.051 Uiso 1 1 calc R . . H49B H 0.3470 0.4952 0.3875 0.051 Uiso 1 1 calc R . . H49C H 0.4209 0.5317 0.4386 0.051 Uiso 1 1 calc R . . C50 C 0.52883(17) 0.6173(2) 0.37729(16) 0.0201(6) Uani 1 1 d . . . H50 H 0.5180 0.6245 0.4164 0.024 Uiso 1 1 calc R . . C51 C 0.5803(2) 0.8744(3) 0.2270(2) 0.0355(8) Uani 1 1 d . . . H51A H 0.5639 0.9130 0.2592 0.043 Uiso 1 1 calc R . . H51B H 0.5393 0.8523 0.1890 0.043 Uiso 1 1 calc R . . C52 C 0.6279(3) 0.9475(4) 0.2050(3) 0.0554(13) Uani 1 1 d . . . H52A H 0.6032 0.9778 0.1607 0.067 Uiso 1 1 calc R . . H52B H 0.6455 1.0090 0.2361 0.067 Uiso 1 1 calc R . . C53 C 0.6867(3) 0.8742(4) 0.2041(3) 0.0537(13) Uani 1 1 d . . . H53A H 0.7300 0.9164 0.2118 0.064 Uiso 1 1 calc R . . H53B H 0.6750 0.8345 0.1618 0.064 Uiso 1 1 calc R . . C54 C 0.6934(2) 0.7958(3) 0.2605(2) 0.0352(8) Uani 1 1 d . . . H54A H 0.7150 0.7258 0.2546 0.042 Uiso 1 1 calc R . . H54B H 0.7216 0.8285 0.3032 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01784(12) 0.01574(13) 0.01768(12) -0.00207(5) 0.00309(8) -0.00166(5) F1 0.0273(10) 0.0357(11) 0.0349(12) 0.0039(9) 0.0095(9) 0.0055(9) O1 0.0274(12) 0.0232(11) 0.0346(13) -0.0023(10) 0.0097(10) -0.0060(9) N1 0.0218(13) 0.0166(12) 0.0201(13) -0.0003(10) 0.0028(10) -0.0021(10) N2 0.0204(12) 0.0143(11) 0.0234(13) 0.0001(10) 0.0047(10) 0.0000(10) N3 0.0214(12) 0.0153(12) 0.0222(13) -0.0010(10) 0.0047(10) 0.0013(10) N4 0.0205(12) 0.0159(12) 0.0208(12) -0.0008(10) 0.0048(10) 0.0004(10) C1 0.0269(16) 0.0159(13) 0.0209(15) -0.0037(12) 0.0063(12) -0.0056(12) C2 0.0315(17) 0.0189(14) 0.0230(15) -0.0012(12) 0.0071(13) 0.0021(13) C3 0.044(2) 0.0177(15) 0.0328(19) -0.0012(13) 0.0141(16) 0.0004(14) C4 0.046(2) 0.0215(16) 0.037(2) -0.0066(14) 0.0162(17) -0.0130(15) C5 0.0310(18) 0.0317(19) 0.0320(19) -0.0052(15) 0.0052(15) -0.0130(15) C6 0.0256(16) 0.0268(17) 0.0233(16) 0.0004(13) 0.0039(13) -0.0045(13) C7 0.0318(19) 0.0184(17) 0.039(2) 0.0020(13) 0.0045(16) 0.0040(12) C8 0.045(2) 0.0267(18) 0.033(2) -0.0012(15) -0.0057(17) 0.0089(16) C9 0.037(2) 0.035(2) 0.058(3) 0.0083(19) 0.015(2) 0.0083(17) C10 0.0253(17) 0.0293(18) 0.042(2) 0.0120(16) -0.0042(15) -0.0067(14) C11 0.084(4) 0.040(2) 0.048(3) -0.016(2) -0.016(3) 0.030(3) C12 0.039(2) 0.067(3) 0.031(2) -0.002(2) -0.0003(18) 0.008(2) C13 0.0247(15) 0.0163(14) 0.0185(14) -0.0016(11) 0.0037(12) -0.0038(11) C14 0.0275(16) 0.0208(15) 0.0218(15) -0.0015(12) 0.0037(12) -0.0028(12) C15 0.039(2) 0.0240(16) 0.0290(18) 0.0082(13) 0.0082(15) 0.0030(14) C16 0.043(2) 0.0311(18) 0.0254(17) 0.0048(14) 0.0121(15) -0.0045(15) C17 0.0318(17) 0.0303(17) 0.0265(17) -0.0005(13) 0.0110(14) -0.0034(14) C18 0.0274(16) 0.0177(14) 0.0204(15) -0.0025(12) 0.0045(12) -0.0029(12) C19 0.0291(17) 0.0205(15) 0.0257(16) -0.0012(12) 0.0039(13) 0.0040(13) C20 0.044(2) 0.0243(17) 0.044(2) -0.0008(17) 0.0104(18) 0.0068(17) C21 0.0294(18) 0.0306(18) 0.036(2) -0.0023(15) 0.0071(15) 0.0030(14) C22 0.0255(16) 0.0250(16) 0.0222(15) -0.0018(12) 0.0057(12) 0.0017(12) C23 0.0254(18) 0.0341(18) 0.039(2) -0.0082(16) 0.0047(16) 0.0013(14) C24 0.041(2) 0.0252(18) 0.0315(19) -0.0043(14) 0.0061(16) 0.0029(15) C25 0.0195(14) 0.0193(14) 0.0195(14) -0.0040(11) 0.0011(11) 0.0021(11) C26 0.0266(16) 0.0166(14) 0.0257(16) -0.0022(12) 0.0080(13) -0.0004(12) C27 0.0264(17) 0.0252(17) 0.037(2) -0.0075(14) 0.0026(15) 0.0050(14) C28 0.037(2) 0.034(2) 0.061(3) -0.011(2) 0.004(2) 0.0166(18) C29 0.049(2) 0.0251(19) 0.063(3) -0.0163(19) 0.011(2) 0.0097(18) C30 0.040(2) 0.0208(17) 0.056(3) -0.0147(17) 0.0090(19) -0.0026(15) C31 0.0285(17) 0.0183(14) 0.038(2) -0.0060(14) 0.0110(15) -0.0015(14) C32 0.0272(18) 0.036(2) 0.041(2) -0.0123(17) 0.0010(15) 0.0058(15) C33 0.052(3) 0.063(3) 0.034(2) 0.002(2) 0.0060(19) -0.001(2) C34 0.072(3) 0.044(3) 0.045(3) 0.003(2) 0.008(2) -0.024(2) C35 0.0266(16) 0.0226(16) 0.0354(19) -0.0085(14) 0.0087(14) -0.0065(13) C36 0.038(2) 0.046(2) 0.0285(19) -0.0033(17) 0.0076(16) -0.0175(19) C37 0.0334(19) 0.036(2) 0.043(2) 0.0089(17) 0.0140(17) 0.0011(16) C38 0.0280(16) 0.0137(13) 0.0170(14) -0.0030(11) 0.0040(12) 0.0015(12) C39 0.0262(17) 0.0204(16) 0.0211(16) -0.0024(11) 0.0027(13) 0.0012(11) C40 0.0342(18) 0.0235(16) 0.0215(16) -0.0001(12) 0.0012(13) 0.0037(13) C41 0.042(2) 0.0182(15) 0.0236(16) 0.0013(12) 0.0051(14) 0.0008(14) C42 0.0349(18) 0.0209(15) 0.0240(16) -0.0015(12) 0.0093(13) -0.0055(13) C43 0.0262(16) 0.0179(14) 0.0220(16) -0.0015(12) 0.0035(13) 0.0014(12) C44 0.0247(16) 0.0286(18) 0.0307(18) 0.0020(14) 0.0060(14) 0.0039(14) C45 0.0300(19) 0.039(2) 0.041(2) -0.0005(18) 0.0050(16) 0.0074(17) C46 0.031(2) 0.034(2) 0.066(3) -0.007(2) 0.014(2) -0.0041(16) C47 0.0242(16) 0.0220(15) 0.0261(17) 0.0023(12) 0.0055(13) -0.0010(12) C48 0.0286(17) 0.0335(19) 0.0306(18) -0.0042(15) 0.0080(14) -0.0073(14) C49 0.0331(19) 0.0272(17) 0.044(2) -0.0035(15) 0.0151(16) 0.0022(14) C50 0.0208(15) 0.0170(13) 0.0202(15) -0.0011(11) 0.0040(12) -0.0030(11) C51 0.037(2) 0.0246(16) 0.037(2) 0.0004(16) 0.0026(16) -0.0021(16) C52 0.069(3) 0.032(2) 0.067(3) 0.014(2) 0.027(3) 0.000(2) C53 0.070(3) 0.038(2) 0.071(4) 0.005(2) 0.048(3) -0.007(2) C54 0.0306(18) 0.0333(19) 0.044(2) -0.0043(16) 0.0157(16) -0.0085(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 F1 2.093(2) . ? Sm1 N1 2.443(3) . ? Sm1 N3 2.446(3) . ? Sm1 N4 2.454(3) . ? Sm1 N2 2.454(3) . ? Sm1 O1 2.457(2) . ? Sm1 C25 2.817(3) . ? Sm1 C50 2.833(3) . ? O1 C51 1.457(5) . ? O1 C54 1.457(4) . ? N1 C25 1.320(4) . ? N1 C1 1.426(4) . ? N2 C25 1.340(4) . ? N2 C13 1.426(4) . ? N3 C50 1.332(4) . ? N3 C26 1.423(4) . ? N4 C50 1.321(4) . ? N4 C38 1.424(4) . ? C1 C2 1.410(5) . ? C1 C6 1.416(4) . ? C2 C3 1.391(5) . ? C2 C7 1.525(5) . ? C3 C4 1.386(6) . ? C4 C5 1.379(6) . ? C5 C6 1.391(5) . ? C6 C10 1.508(5) . ? C7 C9 1.513(6) . ? C7 C8 1.535(5) . ? C10 C11 1.511(7) . ? C10 C12 1.522(6) . ? C13 C14 1.406(4) . ? C13 C18 1.413(4) . ? C14 C15 1.397(5) . ? C14 C19 1.532(5) . ? C15 C16 1.388(6) . ? C16 C17 1.379(5) . ? C17 C18 1.397(5) . ? C18 C22 1.526(5) . ? C19 C21 1.522(5) . ? C19 C20 1.527(5) . ? C22 C24 1.531(5) . ? C22 C23 1.533(5) . ? C26 C31 1.401(5) . ? C26 C27 1.412(5) . ? C27 C28 1.404(5) . ? C27 C32 1.514(5) . ? C28 C29 1.376(6) . ? C29 C30 1.371(6) . ? C30 C31 1.410(5) . ? C31 C35 1.520(5) . ? C32 C34 1.519(7) . ? C32 C33 1.538(6) . ? C35 C37 1.521(6) . ? C35 C36 1.525(5) . ? C38 C43 1.408(5) . ? C38 C39 1.411(5) . ? C39 C40 1.391(5) . ? C39 C44 1.522(5) . ? C40 C41 1.381(5) . ? C41 C42 1.387(5) . ? C42 C43 1.398(5) . ? C43 C47 1.521(5) . ? C44 C46 1.522(5) . ? C44 C45 1.532(5) . ? C47 C49 1.532(5) . ? C47 C48 1.536(5) . ? C51 C52 1.515(6) . ? C52 C53 1.504(7) . ? C53 C54 1.522(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Sm1 N1 108.51(9) . . ? F1 Sm1 N3 133.59(9) . . ? N1 Sm1 N3 110.68(9) . . ? F1 Sm1 N4 99.23(8) . . ? N1 Sm1 N4 92.35(9) . . ? N3 Sm1 N4 55.75(8) . . ? F1 Sm1 N2 106.53(9) . . ? N1 Sm1 N2 55.55(9) . . ? N3 Sm1 N2 115.71(9) . . ? N4 Sm1 N2 143.67(9) . . ? F1 Sm1 O1 82.16(8) . . ? N1 Sm1 O1 139.35(9) . . ? N3 Sm1 O1 84.05(8) . . ? N4 Sm1 O1 125.41(8) . . ? N2 Sm1 O1 83.82(9) . . ? F1 Sm1 C25 105.01(9) . . ? N1 Sm1 C25 27.92(9) . . ? N3 Sm1 C25 121.24(9) . . ? N4 Sm1 C25 119.99(9) . . ? N2 Sm1 C25 28.41(9) . . ? O1 Sm1 C25 111.87(9) . . ? F1 Sm1 C50 117.89(9) . . ? N1 Sm1 C50 103.78(9) . . ? N3 Sm1 C50 28.01(9) . . ? N4 Sm1 C50 27.77(8) . . ? N2 Sm1 C50 135.41(9) . . ? O1 Sm1 C50 105.05(8) . . ? C25 Sm1 C50 126.18(9) . . ? C51 O1 C54 109.4(3) . . ? C51 O1 Sm1 122.2(2) . . ? C54 O1 Sm1 125.5(2) . . ? C25 N1 C1 119.1(3) . . ? C25 N1 Sm1 92.01(18) . . ? C1 N1 Sm1 147.0(2) . . ? C25 N2 C13 118.6(3) . . ? C25 N2 Sm1 91.00(19) . . ? C13 N2 Sm1 140.1(2) . . ? C50 N3 C26 119.0(3) . . ? C50 N3 Sm1 92.37(19) . . ? C26 N3 Sm1 146.7(2) . . ? C50 N4 C38 119.5(3) . . ? C50 N4 Sm1 92.29(19) . . ? C38 N4 Sm1 148.2(2) . . ? C2 C1 C6 119.9(3) . . ? C2 C1 N1 119.3(3) . . ? C6 C1 N1 120.7(3) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 C7 120.5(3) . . ? C1 C2 C7 120.3(3) . . ? C4 C3 C2 120.9(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C10 119.9(3) . . ? C1 C6 C10 121.2(3) . . ? C9 C7 C2 110.7(3) . . ? C9 C7 C8 110.0(3) . . ? C2 C7 C8 113.5(3) . . ? C6 C10 C11 109.7(3) . . ? C6 C10 C12 114.2(3) . . ? C11 C10 C12 109.7(4) . . ? C14 C13 C18 119.7(3) . . ? C14 C13 N2 119.4(3) . . ? C18 C13 N2 120.8(3) . . ? C15 C14 C13 119.2(3) . . ? C15 C14 C19 120.3(3) . . ? C13 C14 C19 120.5(3) . . ? C16 C15 C14 121.2(3) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 121.4(3) . . ? C17 C18 C13 119.0(3) . . ? C17 C18 C22 118.8(3) . . ? C13 C18 C22 122.2(3) . . ? C21 C19 C20 110.8(3) . . ? C21 C19 C14 110.9(3) . . ? C20 C19 C14 112.9(3) . . ? C18 C22 C24 111.5(3) . . ? C18 C22 C23 111.6(3) . . ? C24 C22 C23 110.3(3) . . ? N1 C25 N2 118.1(3) . . ? N1 C25 Sm1 60.06(16) . . ? N2 C25 Sm1 60.59(17) . . ? C31 C26 C27 120.4(3) . . ? C31 C26 N3 120.4(3) . . ? C27 C26 N3 119.1(3) . . ? C28 C27 C26 118.5(3) . . ? C28 C27 C32 119.3(3) . . ? C26 C27 C32 122.2(3) . . ? C29 C28 C27 121.0(4) . . ? C28 C29 C30 120.5(4) . . ? C29 C30 C31 120.8(4) . . ? C26 C31 C30 118.7(3) . . ? C26 C31 C35 122.6(3) . . ? C30 C31 C35 118.7(3) . . ? C27 C32 C34 110.9(4) . . ? C27 C32 C33 111.8(4) . . ? C34 C32 C33 109.3(4) . . ? C31 C35 C37 111.2(3) . . ? C31 C35 C36 111.8(3) . . ? C37 C35 C36 110.7(3) . . ? C43 C38 C39 120.4(3) . . ? C43 C38 N4 120.4(3) . . ? C39 C38 N4 119.2(3) . . ? C40 C39 C38 119.0(3) . . ? C40 C39 C44 120.9(3) . . ? C38 C39 C44 120.1(3) . . ? C41 C40 C39 121.4(3) . . ? C40 C41 C42 119.1(3) . . ? C41 C42 C43 121.9(3) . . ? C42 C43 C38 118.1(3) . . ? C42 C43 C47 119.0(3) . . ? C38 C43 C47 122.9(3) . . ? C46 C44 C39 111.8(3) . . ? C46 C44 C45 109.3(3) . . ? C39 C44 C45 114.0(3) . . ? C43 C47 C49 111.2(3) . . ? C43 C47 C48 111.9(3) . . ? C49 C47 C48 110.0(3) . . ? N4 C50 N3 119.5(3) . . ? N4 C50 Sm1 59.94(17) . . ? N3 C50 Sm1 59.62(17) . . ? O1 C51 C52 105.8(3) . . ? C53 C52 C51 104.9(4) . . ? C52 C53 C54 102.5(4) . . ? O1 C54 C53 103.6(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 3.806 _refine_diff_density_min -5.153 _refine_diff_density_rms 0.175 #===END