Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method CRYSTALS _publ_contact_author_name 'Dr P. Mountford' _publ_contact_author_address ; Dr P. Mountford Chemistry Research Laboratory Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_phone '+44 1865 285140' _publ_contact_author_fax '+44 1865 285141' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_section_title ; Lanthanide mono(borohydride) complexes of diamide-diamine donor ligands: novel single site catalysts for the polymerisation of methyl methacrylate ; loop_ _publ_author_name 'Philip Mountford' 'Fanny Bonnet' 'Anna Collins' 'Andrew R. Cowley' 'Anna C. Hillier' data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 251360' # local code ach11 # CCDC 251360 _chemical_name_systematic ; [Sm({Nmes}2NN')Cl]2 ; _publ_section_exptl_refinement ; The slightly high residual electron density (1.18 e- / A^3) located 1.34 Angstroms from Sm(2)is attributed to an absorption artifact. ; _cell_length_a 16.165(3) _cell_angle_alpha 90 _cell_length_b 21.332(4) _cell_angle_beta 97.46(3) _cell_length_c 17.402(4) _cell_angle_gamma 90 _cell_volume 5949.8(21) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Sm ' -0.1638 3.4418 24.0042 2.4727 19.4258 0.1965 13.4396 14.3996 2.8960 128.0070 2.2096 International_Tables_Vol_IV_Table_2.2B _chemical_name_common (Sm((Nmes)2NN')Cl)2 _cell_formula_units_Z 4 _chemical_formula_sum ' C62 H78 Cl2 N8 Sm2 ' _chemical_formula_moiety ' C62 H78 Cl2 N8 Sm2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1307.06 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2656.000 _exptl_absorpt_coefficient_mu 2.089 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method '\f & \w scans' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.81 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 26058 _reflns_number_total 13576 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 13576 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13635 _diffrn_reflns_theta_min 2.980 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.481 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -0.99 _refine_diff_density_max 1.18 _refine_ls_number_reflns 7897 _refine_ls_number_parameters 667 #_refine_ls_R_factor_ref 0.0341 _refine_ls_wR_factor_ref 0.0387 _refine_ls_goodness_of_fit_ref 1.0952 _refine_ls_R_factor_all 0.0821 _refine_ls_wR_factor_all 0.0741 _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7900 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_gt 0.0387 _refine_ls_shift/su_max 0.001278 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 0.529 0.184 0.279 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Sm1 Sm 0.401258(15) 0.218853(12) 0.509785(14) 0.0250 1.0000 Uani . Sm2 Sm 0.406466(15) 0.313260(12) 0.283912(14) 0.0247 1.0000 Uani . Cl1 Cl 0.30683(8) 0.23465(7) 0.36472(7) 0.0357 1.0000 Uani . Cl2 Cl 0.49653(8) 0.30354(7) 0.43183(7) 0.0398 1.0000 Uani . N1 N 0.4614(3) 0.1256(2) 0.4936(2) 0.0301 1.0000 Uani . N2 N 0.2777(2) 0.2073(2) 0.5565(3) 0.0319 1.0000 Uani . N3 N 0.4205(3) 0.1571(2) 0.6369(2) 0.0304 1.0000 Uani . N4 N 0.4882(3) 0.2778(2) 0.6283(3) 0.0358 1.0000 Uani . N5 N 0.3444(3) 0.4081(2) 0.2848(2) 0.0289 1.0000 Uani . N6 N 0.5254(2) 0.3153(2) 0.2290(2) 0.0279 1.0000 Uani . N7 N 0.3797(3) 0.3596(2) 0.1457(2) 0.0308 1.0000 Uani . N8 N 0.3282(3) 0.2411(2) 0.1791(2) 0.0305 1.0000 Uani . C1 C 0.4930(4) 0.1152(3) 0.6340(3) 0.0394 1.0000 Uani . C2 C 0.4864(4) 0.0808(3) 0.5570(3) 0.0387 1.0000 Uani . C3 C 0.3416(3) 0.1217(3) 0.6366(3) 0.0384 1.0000 Uani . C4 C 0.2666(3) 0.1652(3) 0.6212(4) 0.0419 1.0000 Uani . C5 C 0.4351(4) 0.1975(3) 0.7068(3) 0.0386 1.0000 Uani . C6 C 0.4965(3) 0.2491(3) 0.6970(3) 0.0399 1.0000 Uani . C7 C 0.5542(4) 0.2680(3) 0.7591(3) 0.0468 1.0000 Uani . C8 C 0.6035(4) 0.3199(3) 0.7503(4) 0.0471 1.0000 Uani . C9 C 0.5919(4) 0.3523(3) 0.6822(4) 0.0486 1.0000 Uani . C10 C 0.5346(4) 0.3290(3) 0.6220(3) 0.0392 1.0000 Uani . C11 C 0.4742(3) 0.0988(2) 0.4210(3) 0.0310 1.0000 Uani . C12 C 0.5533(3) 0.1008(3) 0.3957(3) 0.0390 1.0000 Uani . C13 C 0.5652(4) 0.0738(3) 0.3254(3) 0.0426 1.0000 Uani . C14 C 0.5013(4) 0.0448(3) 0.2770(3) 0.0387 1.0000 Uani . C15 C 0.4231(3) 0.0428(3) 0.3021(3) 0.0370 1.0000 Uani . C16 C 0.4088(3) 0.0687(2) 0.3729(3) 0.0347 1.0000 Uani . C17 C 0.6250(4) 0.1336(4) 0.4443(4) 0.0557 1.0000 Uani . C18 C 0.5148(5) 0.0175(3) 0.2002(4) 0.0536 1.0000 Uani . C19 C 0.3239(3) 0.0628(3) 0.3992(4) 0.0489 1.0000 Uani . C20 C 0.2051(3) 0.2430(3) 0.5319(3) 0.0314 1.0000 Uani . C21 C 0.2041(3) 0.3075(3) 0.5447(3) 0.0405 1.0000 Uani . C22 C 0.1312(4) 0.3414(3) 0.5227(4) 0.0496 1.0000 Uani . C23 C 0.0593(3) 0.3141(3) 0.4866(4) 0.0454 1.0000 Uani . C24 C 0.0619(3) 0.2500(3) 0.4696(3) 0.0398 1.0000 Uani . C25 C 0.1323(3) 0.2147(3) 0.4915(3) 0.0356 1.0000 Uani . C26 C 0.2803(4) 0.3411(3) 0.5847(5) 0.0614 1.0000 Uani . C27 C -0.0200(4) 0.3527(4) 0.4664(5) 0.0658 1.0000 Uani . C28 C 0.1314(4) 0.1464(3) 0.4706(4) 0.0429 1.0000 Uani . C29 C 0.3820(4) 0.4283(3) 0.1560(3) 0.0391 1.0000 Uani . C30 C 0.3286(4) 0.4488(3) 0.2165(3) 0.0356 1.0000 Uani . C31 C 0.4479(3) 0.3390(3) 0.1020(3) 0.0322 1.0000 Uani . C32 C 0.5315(3) 0.3423(3) 0.1528(3) 0.0359 1.0000 Uani . C33 C 0.2988(3) 0.3377(3) 0.1073(3) 0.0355 1.0000 Uani . C34 C 0.2915(3) 0.2676(3) 0.1123(3) 0.0324 1.0000 Uani . C35 C 0.2508(3) 0.2321(3) 0.0525(3) 0.0415 1.0000 Uani . C36 C 0.2480(4) 0.1670(3) 0.0606(4) 0.0481 1.0000 Uani . C37 C 0.2882(4) 0.1398(3) 0.1279(3) 0.0416 1.0000 Uani . C38 C 0.3253(3) 0.1789(3) 0.1843(3) 0.0364 1.0000 Uani . C39 C 0.3075(3) 0.4343(2) 0.3469(3) 0.0316 1.0000 Uani . C40 C 0.2223(3) 0.4250(2) 0.3544(3) 0.0348 1.0000 Uani . C41 C 0.1878(3) 0.4538(3) 0.4138(3) 0.0369 1.0000 Uani . C42 C 0.2340(4) 0.4902(3) 0.4694(3) 0.0386 1.0000 Uani . C43 C 0.3186(3) 0.4986(2) 0.4636(3) 0.0346 1.0000 Uani . C44 C 0.3551(3) 0.4721(2) 0.4033(3) 0.0339 1.0000 Uani . C45 C 0.1694(4) 0.3823(3) 0.2995(4) 0.0466 1.0000 Uani . C46 C 0.1933(4) 0.5192(3) 0.5344(4) 0.0477 1.0000 Uani . C47 C 0.4467(3) 0.4829(3) 0.3975(4) 0.0413 1.0000 Uani . C48 C 0.6038(3) 0.2910(2) 0.2628(3) 0.0299 1.0000 Uani . C49 C 0.6610(3) 0.3272(3) 0.3101(3) 0.0309 1.0000 Uani . C50 C 0.7372(3) 0.3010(3) 0.3416(3) 0.0371 1.0000 Uani . C51 C 0.7581(3) 0.2396(3) 0.3271(3) 0.0312 1.0000 Uani . C52 C 0.7014(3) 0.2045(3) 0.2782(3) 0.0378 1.0000 Uani . C53 C 0.6250(3) 0.2285(3) 0.2463(3) 0.0342 1.0000 Uani . C54 C 0.6415(4) 0.3944(3) 0.3277(4) 0.0471 1.0000 Uani . C55 C 0.8400(3) 0.2111(3) 0.3637(4) 0.0481 1.0000 Uani . C56 C 0.5638(4) 0.1890(3) 0.1947(4) 0.0465 1.0000 Uani . C101 C -0.0469(5) 0.0550(4) 0.3212(6) 0.0715 1.0000 Uani . C102 C -0.1115(6) 0.0548(4) 0.2639(5) 0.0777 1.0000 Uani . C103 C -0.1895(6) 0.0370(4) 0.2808(6) 0.0839 1.0000 Uani . C104 C -0.2004(5) 0.0198(4) 0.3538(6) 0.0745 1.0000 Uani . C105 C -0.1350(6) 0.0208(4) 0.4116(5) 0.0718 1.0000 Uani . C106 C -0.0581(5) 0.0394(3) 0.3957(5) 0.0637 1.0000 Uani . H11 H 0.5452(4) 0.1408(3) 0.6400(3) 0.0488 1.0000 Uiso . H12 H 0.4954(4) 0.0842(3) 0.6773(3) 0.0488 1.0000 Uiso . H21 H 0.5411(4) 0.0611(3) 0.5501(3) 0.0472 1.0000 Uiso . H22 H 0.4428(4) 0.0474(3) 0.5562(3) 0.0472 1.0000 Uiso . H31 H 0.3414(3) 0.1001(3) 0.6876(3) 0.0475 1.0000 Uiso . H32 H 0.3383(3) 0.0897(3) 0.5943(3) 0.0475 1.0000 Uiso . H41 H 0.2619(3) 0.1904(3) 0.6689(4) 0.0517 1.0000 Uiso . H42 H 0.2145(3) 0.1401(3) 0.6076(4) 0.0517 1.0000 Uiso . H51 H 0.4571(4) 0.1712(3) 0.7524(3) 0.0472 1.0000 Uiso . H52 H 0.3809(4) 0.2169(3) 0.7160(3) 0.0472 1.0000 Uiso . H71 H 0.5593(4) 0.2444(3) 0.8092(3) 0.0538 1.0000 Uiso . H81 H 0.6471(4) 0.3336(3) 0.7931(4) 0.0554 1.0000 Uiso . H91 H 0.6243(4) 0.3913(3) 0.6751(4) 0.0595 1.0000 Uiso . H101 H 0.5273(4) 0.3521(3) 0.5716(3) 0.0479 1.0000 Uiso . H131 H 0.6222(4) 0.0750(3) 0.3089(3) 0.0505 1.0000 Uiso . H151 H 0.3757(3) 0.0225(3) 0.2684(3) 0.0434 1.0000 Uiso . H171 H 0.6765(4) 0.1310(4) 0.4181(4) 0.0665 1.0000 Uiso . H172 H 0.6356(4) 0.1131(4) 0.4963(4) 0.0665 1.0000 Uiso . H173 H 0.6100(4) 0.1786(4) 0.4508(4) 0.0665 1.0000 Uiso . H181 H 0.4616(5) -0.0010(3) 0.1742(4) 0.0655 1.0000 Uiso . H182 H 0.5585(5) -0.0159(3) 0.2084(4) 0.0655 1.0000 Uiso . H183 H 0.5338(5) 0.0514(3) 0.1668(4) 0.0655 1.0000 Uiso . H191 H 0.2852(3) 0.0407(3) 0.3585(4) 0.0620 1.0000 Uiso . H192 H 0.3289(3) 0.0380(3) 0.4484(4) 0.0620 1.0000 Uiso . H193 H 0.3012(3) 0.1054(3) 0.4084(4) 0.0620 1.0000 Uiso . H221 H 0.1310(4) 0.3875(3) 0.5332(4) 0.0589 1.0000 Uiso . H241 H 0.0117(3) 0.2295(3) 0.4404(3) 0.0485 1.0000 Uiso . H261 H 0.2682(4) 0.3869(3) 0.5886(5) 0.0691 1.0000 Uiso . H262 H 0.2953(4) 0.3233(3) 0.6379(5) 0.0691 1.0000 Uiso . H263 H 0.3278(4) 0.3350(3) 0.5540(5) 0.0691 1.0000 Uiso . H271 H -0.0660(4) 0.3255(4) 0.4410(5) 0.0766 1.0000 Uiso . H272 H -0.0368(4) 0.3710(4) 0.5150(5) 0.0766 1.0000 Uiso . H273 H -0.0089(4) 0.3872(4) 0.4303(5) 0.0766 1.0000 Uiso . H281 H 0.0755(4) 0.1348(3) 0.4428(4) 0.0506 1.0000 Uiso . H282 H 0.1434(4) 0.1208(3) 0.5188(4) 0.0506 1.0000 Uiso . H283 H 0.1752(4) 0.1383(3) 0.4361(4) 0.0506 1.0000 Uiso . H291 H 0.4409(4) 0.4413(3) 0.1734(3) 0.0469 1.0000 Uiso . H292 H 0.3617(4) 0.4490(3) 0.1056(3) 0.0469 1.0000 Uiso . H301 H 0.3421(4) 0.4931(3) 0.2323(3) 0.0437 1.0000 Uiso . H302 H 0.2685(4) 0.4458(3) 0.1942(3) 0.0437 1.0000 Uiso . H311 H 0.4488(3) 0.3664(3) 0.0554(3) 0.0386 1.0000 Uiso . H312 H 0.4376(3) 0.2946(3) 0.0850(3) 0.0386 1.0000 Uiso . H321 H 0.5482(3) 0.3873(3) 0.1595(3) 0.0441 1.0000 Uiso . H322 H 0.5748(3) 0.3191(3) 0.1279(3) 0.0441 1.0000 Uiso . H331 H 0.2919(3) 0.3506(3) 0.0515(3) 0.0414 1.0000 Uiso . H332 H 0.2538(3) 0.3573(3) 0.1336(3) 0.0414 1.0000 Uiso . H351 H 0.2231(3) 0.2529(3) 0.0045(3) 0.0498 1.0000 Uiso . H361 H 0.2175(4) 0.1405(3) 0.0187(4) 0.0570 1.0000 Uiso . H371 H 0.2897(4) 0.0932(3) 0.1345(3) 0.0492 1.0000 Uiso . H381 H 0.3529(3) 0.1594(3) 0.2332(3) 0.0432 1.0000 Uiso . H411 H 0.1270(3) 0.4477(3) 0.4169(3) 0.0453 1.0000 Uiso . H431 H 0.3537(3) 0.5240(2) 0.5039(3) 0.0403 1.0000 Uiso . H451 H 0.1113(4) 0.3814(3) 0.3133(4) 0.0547 1.0000 Uiso . H452 H 0.1683(4) 0.3981(3) 0.2453(4) 0.0547 1.0000 Uiso . H453 H 0.1933(4) 0.3390(3) 0.3032(4) 0.0547 1.0000 Uiso . H461 H 0.2355(4) 0.5441(3) 0.5689(4) 0.0596 1.0000 Uiso . H462 H 0.1468(4) 0.5474(3) 0.5122(4) 0.0596 1.0000 Uiso . H463 H 0.1706(4) 0.4851(3) 0.5651(4) 0.0596 1.0000 Uiso . H471 H 0.4713(3) 0.5103(3) 0.4412(4) 0.0485 1.0000 Uiso . H472 H 0.4528(3) 0.5037(3) 0.3471(4) 0.0485 1.0000 Uiso . H473 H 0.4763(3) 0.4416(3) 0.4005(4) 0.0485 1.0000 Uiso . H501 H 0.7776(3) 0.3274(3) 0.3759(3) 0.0444 1.0000 Uiso . H521 H 0.7161(3) 0.1606(3) 0.2653(3) 0.0445 1.0000 Uiso . H541 H 0.6893(4) 0.4130(3) 0.3625(4) 0.0559 1.0000 Uiso . H542 H 0.6321(4) 0.4188(3) 0.2782(4) 0.0559 1.0000 Uiso . H543 H 0.5901(4) 0.3960(3) 0.3540(4) 0.0559 1.0000 Uiso . H551 H 0.8438(3) 0.1666(3) 0.3464(4) 0.0573 1.0000 Uiso . H552 H 0.8872(3) 0.2357(3) 0.3470(4) 0.0573 1.0000 Uiso . H553 H 0.8432(3) 0.2125(3) 0.4214(4) 0.0573 1.0000 Uiso . H561 H 0.5880(4) 0.1463(3) 0.1896(4) 0.0533 1.0000 Uiso . H562 H 0.5530(4) 0.2091(3) 0.1424(4) 0.0533 1.0000 Uiso . H563 H 0.5101(4) 0.1854(3) 0.2173(4) 0.0533 1.0000 Uiso . H1011 H 0.0101(5) 0.0671(4) 0.3102(6) 0.0842 1.0000 Uiso . H1021 H -0.1017(6) 0.0669(4) 0.2103(5) 0.0939 1.0000 Uiso . H1031 H -0.2376(6) 0.0373(4) 0.2384(6) 0.1019 1.0000 Uiso . H1041 H -0.2569(5) 0.0066(4) 0.3652(6) 0.0923 1.0000 Uiso . H1051 H -0.1423(6) 0.0074(4) 0.4653(5) 0.0916 1.0000 Uiso . H1061 H -0.0099(5) 0.0420(3) 0.4378(5) 0.0767 1.0000 Uiso . 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 0.02456(12) 0.02695(13) 0.02304(13) 0.00226(11) 0.00170(9) 0.00058(11) Sm2 0.02545(12) 0.02709(13) 0.02093(12) 0.0016(1) 0.00068(9) 0.00297(11) Cl1 0.0301(6) 0.0507(8) 0.0252(6) 0.0056(5) -0.0004(5) -0.0091(6) Cl2 0.0387(7) 0.0535(8) 0.0247(6) 0.0079(6) -0.0054(5) -0.0167(6) N1 0.031(2) 0.032(2) 0.027(2) 0.0000(18) 0.0039(17) 0.0090(18) N2 0.023(2) 0.041(3) 0.033(2) 0.0102(19) 0.0076(17) 0.0051(18) N3 0.032(2) 0.033(2) 0.026(2) 0.0037(18) 0.0021(17) 0.0023(19) N4 0.036(2) 0.042(3) 0.028(2) 0.001(2) -0.0027(18) -0.007(2) N5 0.032(2) 0.029(2) 0.025(2) -0.0014(17) 0.0001(17) 0.0064(18) N6 0.028(2) 0.031(2) 0.023(2) 0.0019(18) 0.0011(16) 0.0017(18) N7 0.035(2) 0.033(2) 0.023(2) 0.0031(18) -0.0004(17) 0.0040(19) N8 0.032(2) 0.034(2) 0.026(2) -0.0009(18) 0.0059(17) -0.0017(19) C1 0.039(3) 0.039(3) 0.040(3) 0.003(3) 0.003(2) 0.006(3) C2 0.044(3) 0.034(3) 0.039(3) 0.005(2) 0.005(2) 0.013(2) C3 0.036(3) 0.040(3) 0.039(3) 0.014(3) 0.003(2) -0.001(2) C4 0.029(3) 0.055(4) 0.042(3) 0.011(3) 0.008(2) 0.001(3) C5 0.045(3) 0.050(3) 0.021(2) 0.004(2) 0.004(2) 0.003(3) C6 0.038(3) 0.044(3) 0.036(3) -0.002(3) -0.001(2) 0.004(3) C7 0.048(3) 0.057(4) 0.032(3) -0.009(3) -0.007(3) 0.018(3) C8 0.032(3) 0.057(4) 0.049(4) -0.023(3) -0.006(3) 0.004(3) C9 0.043(3) 0.049(4) 0.054(4) -0.021(3) 0.009(3) -0.011(3) C10 0.044(3) 0.045(3) 0.030(3) -0.009(2) 0.009(2) -0.004(3) C11 0.027(2) 0.032(3) 0.032(3) 0.002(2) -0.003(2) 0.002(2) C12 0.033(3) 0.049(3) 0.035(3) -0.005(3) 0.004(2) -0.005(3) C13 0.037(3) 0.049(4) 0.041(3) -0.005(3) 0.006(3) -0.004(3) C14 0.053(3) 0.031(3) 0.031(3) 0.002(2) 0.003(2) -0.004(3) C15 0.038(3) 0.033(3) 0.038(3) -0.004(2) -0.002(2) -0.004(2) C16 0.031(3) 0.026(3) 0.047(3) 0.004(2) 0.002(2) 0.002(2) C17 0.035(3) 0.087(5) 0.044(4) -0.020(4) 0.002(3) -0.012(3) C18 0.067(4) 0.056(4) 0.040(4) -0.009(3) 0.012(3) -0.012(3) C19 0.031(3) 0.050(4) 0.067(4) -0.025(3) 0.009(3) -0.006(3) C20 0.028(2) 0.044(3) 0.023(2) 0.009(2) 0.009(2) 0.008(2) C21 0.027(3) 0.050(4) 0.043(3) 0.008(3) 0.003(2) 0.001(3) C22 0.041(3) 0.041(3) 0.068(4) 0.007(3) 0.012(3) 0.011(3) C23 0.030(3) 0.063(4) 0.043(3) 0.018(3) 0.007(2) 0.007(3) C24 0.025(3) 0.059(4) 0.035(3) 0.005(3) 0.003(2) 0.003(3) C25 0.031(3) 0.044(3) 0.033(3) 0.001(2) 0.009(2) 0.002(2) C26 0.044(4) 0.042(4) 0.094(6) 0.004(4) -0.004(4) -0.003(3) C27 0.038(3) 0.072(5) 0.085(6) 0.019(4) -0.001(3) 0.016(3) C28 0.032(3) 0.057(4) 0.040(3) -0.010(3) 0.005(2) -0.006(3) C29 0.050(3) 0.031(3) 0.034(3) 0.007(2) -0.003(3) 0.002(3) C30 0.043(3) 0.035(3) 0.027(3) 0.000(2) -0.002(2) 0.008(2) C31 0.037(3) 0.041(3) 0.018(2) 0.007(2) 0.003(2) 0.001(2) C32 0.039(3) 0.044(3) 0.026(3) 0.005(2) 0.007(2) 0.003(3) C33 0.028(3) 0.046(3) 0.031(3) 0.001(2) -0.002(2) 0.009(2) C34 0.025(2) 0.044(3) 0.029(3) 0.000(2) 0.004(2) 0.007(2) C35 0.036(3) 0.060(4) 0.027(3) -0.003(3) -0.001(2) -0.004(3) C36 0.046(3) 0.051(4) 0.047(4) -0.011(3) 0.006(3) -0.009(3) C37 0.045(3) 0.039(3) 0.042(3) -0.009(3) 0.010(3) -0.000(3) C38 0.041(3) 0.038(3) 0.030(3) -0.005(2) 0.003(2) -0.008(2) C39 0.037(3) 0.026(2) 0.030(3) 0.005(2) -0.002(2) 0.005(2) C40 0.032(3) 0.030(3) 0.039(3) -0.003(2) -0.006(2) 0.003(2) C41 0.029(3) 0.034(3) 0.047(3) -0.003(2) 0.002(2) 0.008(2) C42 0.040(3) 0.034(3) 0.042(3) -0.001(2) 0.003(2) 0.009(2) C43 0.043(3) 0.025(3) 0.034(3) -0.003(2) -0.004(2) 0.003(2) C44 0.037(3) 0.027(3) 0.036(3) -0.002(2) -0.002(2) 0.004(2) C45 0.038(3) 0.050(4) 0.049(4) -0.018(3) -0.003(3) 0.006(3) C46 0.048(3) 0.047(4) 0.048(4) -0.009(3) 0.008(3) 0.000(3) C47 0.035(3) 0.040(3) 0.046(3) -0.013(3) -0.003(3) -0.006(2) C48 0.023(2) 0.037(3) 0.030(3) 0.003(2) 0.006(2) -0.002(2) C49 0.031(3) 0.036(3) 0.026(3) 0.002(2) 0.006(2) 0.001(2) C50 0.032(3) 0.043(3) 0.035(3) -0.000(2) -0.001(2) -0.004(2) C51 0.025(2) 0.042(3) 0.027(3) 0.010(2) 0.003(2) 0.007(2) C52 0.037(3) 0.036(3) 0.041(3) -0.002(2) 0.006(2) 0.003(2) C53 0.031(3) 0.035(3) 0.036(3) 0.000(2) 0.003(2) -0.001(2) C54 0.043(3) 0.039(3) 0.057(4) -0.002(3) -0.002(3) -0.007(3) C55 0.030(3) 0.058(4) 0.054(4) 0.012(3) -0.003(3) 0.007(3) C56 0.039(3) 0.040(3) 0.057(4) -0.014(3) -0.008(3) 0.006(3) C101 0.060(5) 0.052(4) 0.105(7) 0.005(4) 0.020(5) 0.005(4) C102 0.089(7) 0.070(5) 0.074(6) -0.002(4) 0.011(5) 0.026(5) C103 0.078(6) 0.077(6) 0.090(7) -0.031(5) -0.013(5) 0.018(5) C104 0.056(5) 0.052(5) 0.117(8) -0.021(5) 0.022(5) -0.013(4) C105 0.093(6) 0.050(4) 0.076(6) -0.004(4) 0.022(5) -0.001(4) C106 0.065(5) 0.046(4) 0.078(5) -0.003(4) 0.001(4) 0.004(4) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm1 . Cl1 . 2.7956(12) yes Sm1 . Cl2 . 2.8317(13) yes Sm1 . N1 . 2.247(4) yes Sm1 . N2 . 2.265(4) yes Sm1 . N3 . 2.559(4) yes Sm1 . N4 . 2.656(4) yes Sm2 . Cl1 . 2.8234(13) yes Sm2 . Cl2 . 2.7954(12) yes Sm2 . N5 . 2.260(4) yes Sm2 . N6 . 2.255(4) yes Sm2 . N7 . 2.585(4) yes Sm2 . N8 . 2.589(4) yes N1 . C2 . 1.477(7) yes N1 . C11 . 1.427(7) yes N2 . C4 . 1.469(7) yes N2 . C20 . 1.418(6) yes N3 . C1 . 1.480(7) yes N3 . C3 . 1.481(7) yes N3 . C5 . 1.484(7) yes N4 . C6 . 1.335(7) yes N4 . C10 . 1.338(7) yes N5 . C30 . 1.467(6) yes N5 . C39 . 1.415(7) yes N6 . C32 . 1.463(6) yes N6 . C48 . 1.423(6) yes N7 . C29 . 1.475(7) yes N7 . C31 . 1.484(7) yes N7 . C33 . 1.466(7) yes N8 . C34 . 1.358(6) yes N8 . C38 . 1.330(7) yes C1 . C2 . 1.519(8) yes C3 . C4 . 1.524(8) yes C5 . C6 . 1.507(8) yes C6 . C7 . 1.392(8) yes C7 . C8 . 1.39(1) yes C8 . C9 . 1.36(1) yes C9 . C10 . 1.397(8) yes C11 . C12 . 1.406(7) yes C11 . C16 . 1.413(7) yes C12 . C13 . 1.388(8) yes C12 . C17 . 1.515(8) yes C13 . C14 . 1.389(8) yes C14 . C15 . 1.391(8) yes C14 . C18 . 1.501(8) yes C15 . C16 . 1.397(8) yes C16 . C19 . 1.509(8) yes C20 . C21 . 1.395(8) yes C20 . C25 . 1.423(8) yes C21 . C22 . 1.393(8) yes C21 . C26 . 1.514(9) yes C22 . C23 . 1.376(9) yes C23 . C24 . 1.400(9) yes C23 . C27 . 1.526(8) yes C24 . C25 . 1.378(8) yes C25 . C28 . 1.500(8) yes C29 . C30 . 1.511(8) yes C31 . C32 . 1.518(7) yes C33 . C34 . 1.503(8) yes C34 . C35 . 1.383(8) yes C35 . C36 . 1.398(9) yes C36 . C37 . 1.390(9) yes C37 . C38 . 1.366(8) yes C39 . C40 . 1.414(8) yes C39 . C44 . 1.418(7) yes C40 . C41 . 1.380(8) yes C40 . C45 . 1.505(7) yes C41 . C42 . 1.382(8) yes C42 . C43 . 1.397(8) yes C42 . C46 . 1.512(8) yes C43 . C44 . 1.389(8) yes C44 . C47 . 1.513(8) yes C48 . C49 . 1.389(7) yes C48 . C53 . 1.416(7) yes C49 . C50 . 1.399(7) yes C49 . C54 . 1.507(8) yes C50 . C51 . 1.384(8) yes C51 . C52 . 1.386(8) yes C51 . C55 . 1.519(7) yes C52 . C53 . 1.383(8) yes C53 . C56 . 1.505(8) yes C101 . C102 . 1.346(12) yes C101 . C106 . 1.372(12) yes C102 . C103 . 1.384(13) yes C103 . C104 . 1.357(13) yes C104 . C105 . 1.360(12) yes C105 . C106 . 1.368(11) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Sm1 . Cl2 . 75.97(4) yes Cl1 . Sm1 . N1 . 100.83(11) yes Cl2 . Sm1 . N1 . 103.49(12) yes Cl1 . Sm1 . N2 . 86.20(11) yes Cl2 . Sm1 . N2 . 143.24(11) yes N1 . Sm1 . N2 . 111.37(16) yes Cl1 . Sm1 . N3 . 146.5(1) yes Cl2 . Sm1 . N3 . 136.9(1) yes N1 . Sm1 . N3 . 69.31(15) yes N2 . Sm1 . N3 . 69.37(14) yes Cl1 . Sm1 . N4 . 144.66(11) yes Cl2 . Sm1 . N4 . 78.7(1) yes N1 . Sm1 . N4 . 108.80(15) yes N2 . Sm1 . N4 . 100.10(15) yes N3 . Sm1 . N4 . 65.15(14) yes Cl1 . Sm2 . Cl2 . 76.11(4) yes Cl1 . Sm2 . N5 . 104.22(11) yes Cl2 . Sm2 . N5 . 103.79(11) yes Cl1 . Sm2 . N6 . 142.65(11) yes Cl2 . Sm2 . N6 . 91.2(1) yes N5 . Sm2 . N6 . 112.93(15) yes Cl1 . Sm2 . N7 . 130.8(1) yes Cl2 . Sm2 . N7 . 152.8(1) yes N5 . Sm2 . N7 . 69.11(14) yes N6 . Sm2 . N7 . 69.34(14) yes Cl1 . Sm2 . N8 . 74.9(1) yes Cl2 . Sm2 . N8 . 138.9(1) yes N5 . Sm2 . N8 . 111.17(14) yes N6 . Sm2 . N8 . 94.50(14) yes N7 . Sm2 . N8 . 64.18(14) yes Sm1 . Cl1 . Sm2 . 103.97(4) yes Sm1 . Cl2 . Sm2 . 103.76(4) yes Sm1 . N1 . C2 . 124.1(3) yes Sm1 . N1 . C11 . 125.5(3) yes C2 . N1 . C11 . 110.2(4) yes Sm1 . N2 . C4 . 122.9(3) yes Sm1 . N2 . C20 . 124.6(3) yes C4 . N2 . C20 . 112.3(4) yes Sm1 . N3 . C1 . 106.8(3) yes Sm1 . N3 . C3 . 104.6(3) yes C1 . N3 . C3 . 112.1(4) yes Sm1 . N3 . C5 . 113.4(3) yes C1 . N3 . C5 . 109.7(4) yes C3 . N3 . C5 . 110.1(4) yes Sm1 . N4 . C6 . 117.4(4) yes Sm1 . N4 . C10 . 124.7(4) yes C6 . N4 . C10 . 117.1(5) yes Sm2 . N5 . C30 . 123.7(3) yes Sm2 . N5 . C39 . 126.2(3) yes C30 . N5 . C39 . 109.8(4) yes Sm2 . N6 . C32 . 123.6(3) yes Sm2 . N6 . C48 . 125.5(3) yes C32 . N6 . C48 . 110.9(4) yes Sm2 . N7 . C29 . 105.5(3) yes Sm2 . N7 . C31 . 108.5(3) yes C29 . N7 . C31 . 110.4(4) yes Sm2 . N7 . C33 . 109.5(3) yes C29 . N7 . C33 . 112.2(4) yes C31 . N7 . C33 . 110.5(4) yes Sm2 . N8 . C34 . 118.3(3) yes Sm2 . N8 . C38 . 124.3(3) yes C34 . N8 . C38 . 117.3(5) yes N3 . C1 . C2 . 111.0(4) yes N1 . C2 . C1 . 109.1(4) yes N3 . C3 . C4 . 110.8(5) yes N2 . C4 . C3 . 109.4(4) yes N3 . C5 . C6 . 111.7(4) yes N4 . C6 . C5 . 116.4(5) yes N4 . C6 . C7 . 122.9(6) yes C5 . C6 . C7 . 120.5(5) yes C6 . C7 . C8 . 118.8(6) yes C7 . C8 . C9 . 119.0(5) yes C8 . C9 . C10 . 118.3(6) yes N4 . C10 . C9 . 123.6(6) yes N1 . C11 . C12 . 120.4(5) yes N1 . C11 . C16 . 121.6(5) yes C12 . C11 . C16 . 118.0(5) yes C11 . C12 . C13 . 119.9(5) yes C11 . C12 . C17 . 120.1(5) yes C13 . C12 . C17 . 120.0(5) yes C12 . C13 . C14 . 122.7(5) yes C13 . C14 . C15 . 117.3(5) yes C13 . C14 . C18 . 121.9(6) yes C15 . C14 . C18 . 120.8(5) yes C14 . C15 . C16 . 121.7(5) yes C11 . C16 . C15 . 120.4(5) yes C11 . C16 . C19 . 119.9(5) yes C15 . C16 . C19 . 119.7(5) yes N2 . C20 . C21 . 120.5(5) yes N2 . C20 . C25 . 121.3(5) yes C21 . C20 . C25 . 118.1(5) yes C20 . C21 . C22 . 119.7(6) yes C20 . C21 . C26 . 121.0(5) yes C22 . C21 . C26 . 119.3(6) yes C21 . C22 . C23 . 122.6(6) yes C22 . C23 . C24 . 117.6(5) yes C22 . C23 . C27 . 120.8(7) yes C24 . C23 . C27 . 121.6(6) yes C23 . C24 . C25 . 121.4(5) yes C20 . C25 . C24 . 120.3(6) yes C20 . C25 . C28 . 120.8(5) yes C24 . C25 . C28 . 118.8(5) yes N7 . C29 . C30 . 111.4(5) yes N5 . C30 . C29 . 109.8(4) yes N7 . C31 . C32 . 110.6(4) yes N6 . C32 . C31 . 110.5(4) yes N7 . C33 . C34 . 111.3(4) yes N8 . C34 . C33 . 115.9(5) yes N8 . C34 . C35 . 121.8(5) yes C33 . C34 . C35 . 122.3(5) yes C34 . C35 . C36 . 119.2(5) yes C35 . C36 . C37 . 118.8(6) yes C36 . C37 . C38 . 117.6(6) yes N8 . C38 . C37 . 125.2(5) yes N5 . C39 . C40 . 121.8(5) yes N5 . C39 . C44 . 120.5(5) yes C40 . C39 . C44 . 117.7(5) yes C39 . C40 . C41 . 119.9(5) yes C39 . C40 . C45 . 120.5(5) yes C41 . C40 . C45 . 119.6(5) yes C40 . C41 . C42 . 122.8(5) yes C41 . C42 . C43 . 117.8(5) yes C41 . C42 . C46 . 120.4(5) yes C43 . C42 . C46 . 121.7(5) yes C42 . C43 . C44 . 121.2(5) yes C39 . C44 . C43 . 120.6(5) yes C39 . C44 . C47 . 119.2(5) yes C43 . C44 . C47 . 120.2(5) yes N6 . C48 . C49 . 122.0(5) yes N6 . C48 . C53 . 119.0(4) yes C49 . C48 . C53 . 119.0(5) yes C48 . C49 . C50 . 119.6(5) yes C48 . C49 . C54 . 120.6(5) yes C50 . C49 . C54 . 119.9(5) yes C49 . C50 . C51 . 122.1(5) yes C50 . C51 . C52 . 117.7(5) yes C50 . C51 . C55 . 121.5(5) yes C52 . C51 . C55 . 120.8(5) yes C51 . C52 . C53 . 122.1(5) yes C48 . C53 . C52 . 119.6(5) yes C48 . C53 . C56 . 119.3(5) yes C52 . C53 . C56 . 121.1(5) yes C102 . C101 . C106 . 121.0(8) yes C101 . C102 . C103 . 118.9(9) yes C102 . C103 . C104 . 120.4(9) yes C103 . C104 . C105 . 120.3(8) yes C104 . C105 . C106 . 119.6(9) yes C101 . C106 . C105 . 119.7(8) yes ##end data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 251361' # Local code AC3 # CCDC 251361 _chemical_name_systematic ; [Sm(N2NN_Mes)(BH4)2Li]2 ; _chemical_melting_point ? _chemical_name_common (Sm(N2NN_Mes)(BH4)2Li)2 _cell_length_a 10.57200(10) _cell_length_b 11.6396(2) _cell_length_c 12.6413(2) _cell_angle_alpha 101.4560(6) _cell_angle_beta 105.0218(7) _cell_angle_gamma 93.5125(10) _cell_volume 1461.99(4) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Sm -0.1638 3.4418 24.0042 2.4727 19.4258 0.1965 13.4396 14.3996 2.8960 128.0070 2.2096 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Li -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C28 H44 B2 Li1 N4 Sm1' _chemical_formula_moiety 'C28 H44 B2 Li1 N4 Sm1' _chemical_compound_source ? _chemical_formula_weight 615.65 _cell_measurement_reflns_used 7956 _cell_measurement_theta_min 5 _cell_measurement_theta_max 31 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 2.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.78 # Sheldrick geometric definitions 0.75 0.78 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15945 _reflns_number_total 8786 _diffrn_reflns_av_R_equivalents 0.018 # Number of reflections with Friedels Law is 8786 # Number of reflections without Friedels Law is 8786 # Theoretical number of reflections is about 8962 _diffrn_reflns_theta_min 5.130 _diffrn_reflns_theta_max 30.552 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.719 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.81 _refine_diff_density_max 1.46 _refine_ls_number_reflns 8786 _refine_ls_number_restraints 137 _refine_ls_number_parameters 351 #_refine_ls_R_factor_ref 0.0293 _refine_ls_wR_factor_ref 0.0540 _refine_ls_goodness_of_fit_ref 0.9926 #_reflns_number_all 8786 _refine_ls_R_factor_all 0.0293 _refine_ls_wR_factor_all 0.0540 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 8016 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_gt 0.0524 _refine_ls_shift/su_max 0.001001 _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.688E-02 0.748 0.00 0.00 0.00 0.333 ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_reference ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Sm1 Sm -0.160797(8) -0.178590(8) 0.210440(7) 0.0174 1.0000 Uani . . . . . . Li1 Li -0.0204(4) -0.1515(3) 0.5271(3) 0.0347 1.0000 Uani . . . . . . N1 N -0.12708(15) -0.00539(14) 0.15318(12) 0.0211 1.0000 Uani D . . . . . N2 N -0.37297(15) -0.26125(15) 0.15458(13) 0.0240 1.0000 Uani D . . . . . N3 N -0.25448(15) -0.21357(14) -0.00552(13) 0.0218 1.0000 Uani D . . . . . N4 N -0.01759(15) -0.29105(14) 0.09424(13) 0.0237 1.0000 Uani D . . . . . C1 C -0.20044(19) 0.00410(18) 0.04014(16) 0.0265 1.0000 Uani D . . . . . C2 C -0.2029(2) -0.11126(19) -0.04179(16) 0.0273 1.0000 Uani D . . . . . C3 C -0.45299(19) -0.2948(2) 0.03807(17) 0.0324 1.0000 Uani D . . . . . C4 C -0.40045(18) -0.2208(2) -0.03134(16) 0.0296 1.0000 Uani D . . . . . C5 C -0.2159(2) -0.32301(18) -0.06213(16) 0.0279 1.0000 Uani D . . . . . C6 C -0.07138(19) -0.33308(17) -0.01659(16) 0.0242 1.0000 Uani D . . . . . C7 C 0.0008(2) -0.38734(18) -0.08590(17) 0.0301 1.0000 Uani D . . . . . C8 C 0.1320(2) -0.39797(18) -0.0398(2) 0.0350 1.0000 Uani D . . . . . C9 C 0.1881(2) -0.35561(17) 0.07402(19) 0.0311 1.0000 Uani D . . . . . C10 C 0.11029(19) -0.30334(17) 0.13785(17) 0.0264 1.0000 Uani D . . . . . C11 C -0.05743(17) 0.10100(16) 0.22371(15) 0.0199 1.0000 Uani . . . . . . C12 C -0.11672(18) 0.20542(17) 0.24859(15) 0.0223 1.0000 Uani D . . . . . C13 C -0.0396(2) 0.30788(17) 0.31724(16) 0.0255 1.0000 Uani D . . . . . C14 C 0.09551(19) 0.31311(17) 0.36472(16) 0.0254 1.0000 Uani D . . . . . C15 C 0.15182(18) 0.20904(17) 0.34570(16) 0.0234 1.0000 Uani D . . . . . C16 C 0.07855(17) 0.10384(16) 0.27792(15) 0.0206 1.0000 Uani D . . . . . C17 C -0.26364(19) 0.20533(19) 0.20727(18) 0.0308 1.0000 Uani D . . . . . C18 C 0.1774(2) 0.42646(19) 0.43376(19) 0.0366 1.0000 Uani D . . . . . C19 C 0.14569(18) -0.00562(17) 0.26175(16) 0.0250 1.0000 Uani D . . . . . C20 C -0.44399(17) -0.27170(17) 0.23498(16) 0.0224 1.0000 Uani . . . . . . C21 C -0.51187(17) -0.17813(18) 0.27274(17) 0.0254 1.0000 Uani D . . . . . C22 C -0.56686(18) -0.18249(18) 0.36086(17) 0.0278 1.0000 Uani D . . . . . C23 C -0.56264(18) -0.27902(19) 0.41069(17) 0.0283 1.0000 Uani D . . . . . C24 C -0.50332(19) -0.37401(17) 0.36780(17) 0.0264 1.0000 Uani D . . . . . C25 C -0.44361(17) -0.37222(17) 0.28136(16) 0.0235 1.0000 Uani D . . . . . C26 C -0.5242(2) -0.0726(2) 0.2199(2) 0.0335 1.0000 Uani D . . . . . C27 C -0.6181(2) -0.2788(2) 0.5094(2) 0.0425 1.0000 Uani D . . . . . C28 C -0.3790(2) -0.47715(18) 0.24096(18) 0.0302 1.0000 Uani D . . . . . B1 B -0.1662(2) -0.0142(2) 0.41661(18) 0.0221 1.0000 Uani . . . . . . B2 B -0.0387(2) -0.3067(2) 0.3618(2) 0.0268 1.0000 Uani . . . . . . H1 H -0.072(2) -0.039(2) 0.3922(19) 0.035(3) 1.0000 Uiso . . . . . . H2 H -0.176(2) -0.056(2) 0.486(2) 0.035(3) 1.0000 Uiso . . . . . . H3 H -0.247(2) -0.048(2) 0.339(2) 0.035(3) 1.0000 Uiso . . . . . . H4 H -0.167(2) 0.082(2) 0.4424(19) 0.035(3) 1.0000 Uiso . . . . . . H5 H -0.130(2) -0.274(2) 0.375(2) 0.040(3) 1.0000 Uiso . . . . . . H6 H 0.019(2) -0.228(2) 0.348(2) 0.040(3) 1.0000 Uiso . . . . . . H7 H 0.017(2) -0.340(2) 0.434(2) 0.040(3) 1.0000 Uiso . . . . . . H8 H -0.075(2) -0.369(2) 0.282(2) 0.040(3) 1.0000 Uiso . . . . . . H11 H -0.2901 0.0212 0.0372 0.0318 1.0000 Uiso D . . . . . H12 H -0.1566 0.0680 0.0191 0.0318 1.0000 Uiso D . . . . . H21 H -0.2567 -0.1099 -0.1171 0.0333 1.0000 Uiso D . . . . . H22 H -0.1132 -0.1194 -0.0451 0.0333 1.0000 Uiso D . . . . . H31 H -0.5441 -0.2779 0.0325 0.0375 1.0000 Uiso D . . . . . H32 H -0.4533 -0.3794 0.0068 0.0375 1.0000 Uiso D . . . . . H41 H -0.4385 -0.2528 -0.1129 0.0342 1.0000 Uiso D . . . . . H42 H -0.4256 -0.1402 -0.0130 0.0342 1.0000 Uiso D . . . . . H51 H -0.2685 -0.3903 -0.0518 0.0316 1.0000 Uiso D . . . . . H52 H -0.2367 -0.3254 -0.1424 0.0316 1.0000 Uiso D . . . . . H71 H -0.0416 -0.4171 -0.1653 0.0378 1.0000 Uiso D . . . . . H81 H 0.1842 -0.4363 -0.0873 0.0458 1.0000 Uiso D . . . . . H91 H 0.2788 -0.3604 0.1088 0.0392 1.0000 Uiso D . . . . . H101 H 0.1483 -0.2738 0.2188 0.0310 1.0000 Uiso D . . . . . H131 H -0.0828 0.3777 0.3327 0.0313 1.0000 Uiso D . . . . . H151 H 0.2450 0.2086 0.3817 0.0289 1.0000 Uiso D . . . . . H171 H -0.2893 0.2706 0.2538 0.0365 1.0000 Uiso D . . . . . H172 H -0.3092 0.1299 0.2110 0.0365 1.0000 Uiso D . . . . . H173 H -0.2871 0.2133 0.1286 0.0365 1.0000 Uiso D . . . . . H181 H 0.2603 0.4145 0.4813 0.0413 1.0000 Uiso D . . . . . H182 H 0.1317 0.4700 0.4812 0.0413 1.0000 Uiso D . . . . . H183 H 0.1959 0.4798 0.3893 0.0413 1.0000 Uiso D . . . . . H191 H 0.2401 0.0133 0.2869 0.0312 1.0000 Uiso D . . . . . H192 H 0.1255 -0.0610 0.3035 0.0312 1.0000 Uiso D . . . . . H193 H 0.1242 -0.0492 0.1838 0.0312 1.0000 Uiso D . . . . . H221 H -0.6088 -0.1163 0.3900 0.0342 1.0000 Uiso D . . . . . H241 H -0.5088 -0.4506 0.3884 0.0323 1.0000 Uiso D . . . . . H261 H -0.5310 -0.0020 0.2740 0.0427 1.0000 Uiso D . . . . . H262 H -0.6040 -0.0864 0.1585 0.0427 1.0000 Uiso D . . . . . H263 H -0.4502 -0.0564 0.1916 0.0427 1.0000 Uiso D . . . . . H271 H -0.5952 -0.3446 0.5434 0.0546 1.0000 Uiso D . . . . . H272 H -0.7140 -0.2882 0.4877 0.0546 1.0000 Uiso D . . . . . H273 H -0.5914 -0.2085 0.5699 0.0546 1.0000 Uiso D . . . . . H281 H -0.4178 -0.5473 0.2568 0.0360 1.0000 Uiso D . . . . . H282 H -0.3882 -0.4924 0.1614 0.0360 1.0000 Uiso D . . . . . H283 H -0.2860 -0.4692 0.2765 0.0360 1.0000 Uiso 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 0.01626(5) 0.02027(5) 0.01474(5) 0.00386(3) 0.00276(3) 0.00210(3) Li1 0.0361(19) 0.034(2) 0.0309(19) 0.0018(16) 0.0083(16) -0.0003(15) N1 0.0232(7) 0.0220(8) 0.0167(7) 0.0040(6) 0.0030(6) 0.0031(6) N2 0.0182(7) 0.0332(9) 0.0200(8) 0.0071(7) 0.0041(6) 0.0002(6) N3 0.0203(7) 0.0266(8) 0.0173(7) 0.0056(6) 0.0032(6) 0.0007(6) N4 0.0239(8) 0.0241(8) 0.0221(8) 0.0005(6) 0.0076(6) 0.0041(6) C1 0.0310(10) 0.0274(10) 0.0199(9) 0.0084(8) 0.0028(8) 0.0040(8) C2 0.0298(10) 0.0336(11) 0.0189(9) 0.0093(8) 0.0056(8) 0.0005(8) C3 0.0208(9) 0.0480(14) 0.0244(10) 0.0090(9) 0.0011(8) -0.0072(9) C4 0.0200(9) 0.0455(13) 0.0206(9) 0.0099(9) -0.0002(7) 0.0005(8) C5 0.0321(10) 0.0276(10) 0.0193(9) 0.0012(8) 0.0028(8) 0.0001(8) C6 0.0316(10) 0.0210(9) 0.0206(9) 0.0042(7) 0.0090(8) 0.0013(7) C7 0.0421(12) 0.0267(10) 0.0250(10) 0.0038(8) 0.0175(9) 0.0015(9) C8 0.0427(12) 0.0283(11) 0.0430(13) 0.0052(9) 0.0296(11) 0.0043(9) C9 0.0264(10) 0.0251(10) 0.0449(13) 0.0054(9) 0.0168(9) 0.0043(8) C10 0.0240(9) 0.0224(10) 0.0314(10) 0.0021(8) 0.0080(8) 0.0038(7) C11 0.0227(8) 0.0224(9) 0.0179(8) 0.0088(7) 0.0077(7) 0.0034(7) C12 0.0241(9) 0.0235(9) 0.0217(9) 0.0095(7) 0.0064(7) 0.0058(7) C13 0.0322(10) 0.0209(9) 0.0249(9) 0.0077(8) 0.0079(8) 0.0063(8) C14 0.0309(10) 0.0232(10) 0.0213(9) 0.0071(7) 0.0048(8) 0.0000(8) C15 0.0221(8) 0.0282(10) 0.0215(9) 0.0098(8) 0.0058(7) 0.0017(7) C16 0.0228(8) 0.0222(9) 0.0199(8) 0.0082(7) 0.0082(7) 0.0044(7) C17 0.0259(9) 0.0282(11) 0.0376(11) 0.0071(9) 0.0071(9) 0.0077(8) C18 0.0397(12) 0.0267(11) 0.0370(12) 0.0054(9) 0.0023(10) -0.0024(9) C19 0.0228(9) 0.0264(10) 0.0283(10) 0.0085(8) 0.0090(8) 0.0062(7) C20 0.0171(8) 0.0268(10) 0.0224(9) 0.0059(7) 0.0042(7) 0.0004(7) C21 0.0168(8) 0.0291(10) 0.0313(10) 0.0114(8) 0.0048(8) 0.0036(7) C22 0.0207(9) 0.0309(11) 0.0335(11) 0.0080(9) 0.0091(8) 0.0071(8) C23 0.0234(9) 0.0348(11) 0.0296(10) 0.0089(9) 0.0111(8) 0.0034(8) C24 0.0277(9) 0.0225(10) 0.0302(10) 0.0092(8) 0.0085(8) -0.0004(7) C25 0.0205(8) 0.0237(10) 0.0235(9) 0.0034(7) 0.0029(7) 0.0002(7) C26 0.0249(10) 0.0362(12) 0.0461(13) 0.0209(10) 0.0113(9) 0.0111(8) C27 0.0508(14) 0.0441(14) 0.0432(14) 0.0125(11) 0.0288(12) 0.0074(11) C28 0.0325(10) 0.0258(10) 0.0325(11) 0.0044(8) 0.0113(9) 0.0025(8) B1 0.0223(10) 0.0254(11) 0.0182(9) 0.0042(8) 0.0055(8) 0.0032(8) B2 0.0302(11) 0.0270(12) 0.0238(11) 0.0088(9) 0.0051(9) 0.0086(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.39735(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm1 . N1 . 2.3110(15) yes Sm1 . N2 . 2.2584(15) yes Sm1 . N3 . 2.5898(15) yes Sm1 . N4 . 2.6068(15) yes Sm1 . B1 . 2.927(2) yes Sm1 . B2 . 2.764(2) yes Sm1 . H1 . 2.45(2) no Sm1 . H3 . 2.39(2) no Sm1 . H5 . 2.50(2) no Sm1 . H6 . 2.40(2) no Sm1 . H8 . 2.67(2) no Li1 . C14 2_556 2.728(4) yes Li1 . C15 2_556 2.537(4) yes Li1 . C16 2_556 2.654(4) yes Li1 . B1 . 2.637(5) yes Li1 . B1 2_556 2.525(4) yes Li1 . B2 . 2.432(4) yes Li1 . H2 . 2.06(2) no Li1 . H4 2_556 2.00(2) no Li1 . H5 . 2.16(2) no N1 . C1 . 1.468(2) yes N1 . C11 . 1.407(2) yes N2 . C3 . 1.457(2) yes N2 . C20 . 1.430(2) yes N3 . C2 . 1.481(2) yes N3 . C4 . 1.486(2) yes N3 . C5 . 1.468(3) yes N4 . C6 . 1.344(2) yes N4 . C10 . 1.349(2) yes C1 . C2 . 1.519(3) yes C1 . H11 . 0.974 no C1 . H12 . 0.969 no C2 . H21 . 0.978 no C2 . H22 . 0.970 no C3 . C4 . 1.522(3) yes C3 . H31 . 0.983 no C3 . H32 . 0.985 no C4 . H41 . 0.989 no C4 . H42 . 0.990 no C5 . C6 . 1.507(3) yes C5 . H51 . 0.982 no C5 . H52 . 0.975 no C6 . C7 . 1.391(3) yes C7 . C8 . 1.382(3) yes C7 . H71 . 0.969 no C8 . C9 . 1.380(3) yes C8 . H81 . 0.979 no C9 . C10 . 1.381(3) yes C9 . H91 . 0.957 no C10 . H101 . 0.979 no C11 . C12 . 1.419(3) yes C11 . C16 . 1.418(2) yes C12 . C13 . 1.394(3) yes C12 . C17 . 1.505(3) yes C13 . C14 . 1.391(3) yes C13 . H131 . 0.967 no C14 . C15 . 1.388(3) yes C14 . C18 . 1.504(3) yes C15 . C16 . 1.399(3) yes C15 . H151 . 0.973 no C16 . C19 . 1.500(3) yes C17 . H171 . 0.963 no C17 . H172 . 0.991 no C17 . H173 . 0.985 no C18 . H181 . 0.962 no C18 . H182 . 0.954 no C18 . H183 . 0.959 no C19 . H191 . 0.962 no C19 . H192 . 0.956 no C19 . H193 . 0.975 no C20 . C21 . 1.413(3) yes C20 . C25 . 1.409(3) yes C21 . C22 . 1.391(3) yes C21 . C26 . 1.507(3) yes C22 . C23 . 1.391(3) yes C22 . H221 . 0.969 no C23 . C24 . 1.390(3) yes C23 . C27 . 1.510(3) yes C24 . C25 . 1.399(3) yes C24 . H241 . 0.979 no C25 . C28 . 1.502(3) yes C26 . H261 . 0.979 no C26 . H262 . 0.967 no C26 . H263 . 0.964 no C27 . H271 . 0.963 no C27 . H272 . 0.972 no C27 . H273 . 0.973 no C28 . H281 . 0.970 no C28 . H282 . 0.964 no C28 . H283 . 0.959 no B1 . H1 . 1.15(2) no B1 . H2 . 1.10(2) no B1 . H3 . 1.10(2) no B1 . H4 . 1.10(2) no B2 . H5 . 1.10(2) no B2 . H6 . 1.14(2) no B2 . H7 . 1.11(2) no B2 . H8 . 1.08(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Sm1 . N2 . 114.22(6) yes N1 . Sm1 . N3 . 70.13(5) yes N2 . Sm1 . N3 . 69.17(5) yes N1 . Sm1 . N4 . 93.56(5) yes N2 . Sm1 . N4 . 112.27(5) yes N3 . Sm1 . N4 . 64.87(5) yes N1 . Sm1 . B1 . 82.39(6) yes N2 . Sm1 . B1 . 98.89(6) yes N3 . Sm1 . B1 . 140.46(6) yes N4 . Sm1 . B1 . 147.16(5) yes N1 . Sm1 . B2 . 141.12(6) yes N2 . Sm1 . B2 . 103.30(7) yes N3 . Sm1 . B2 . 136.63(6) yes N4 . Sm1 . B2 . 80.90(6) yes B1 . Sm1 . B2 . 82.14(7) yes N1 . Sm1 . H1 . 79.0(5) no N2 . Sm1 . H1 . 120.8(5) no N3 . Sm1 . H1 . 148.5(5) no N4 . Sm1 . H1 . 124.6(5) no B1 . Sm1 . H1 . 22.6(5) no N1 . Sm1 . H3 . 80.8(5) no N2 . Sm1 . H3 . 80.6(6) no N3 . Sm1 . H3 . 122.8(6) no N4 . Sm1 . H3 . 167.2(6) no B1 . Sm1 . H3 . 21.0(6) no N1 . Sm1 . H5 . 145.5(6) no N2 . Sm1 . H5 . 87.5(6) no N3 . Sm1 . H5 . 144.4(6) no N4 . Sm1 . H5 . 102.8(6) no B1 . Sm1 . H5 . 67.3(6) no N1 . Sm1 . H6 . 117.1(6) no N2 . Sm1 . H6 . 127.5(6) no N3 . Sm1 . H6 . 139.8(6) no N4 . Sm1 . H6 . 75.1(6) no B1 . Sm1 . H6 . 77.9(6) no N1 . Sm1 . H8 . 151.9(5) no N2 . Sm1 . H8 . 92.2(5) no N3 . Sm1 . H8 . 114.1(5) no N4 . Sm1 . H8 . 66.3(5) no B1 . Sm1 . H8 . 103.6(5) no B2 . Sm1 . H1 . 73.2(5) no B2 . Sm1 . H3 . 96.2(6) no H1 . Sm1 . H3 . 43.1(8) no B2 . Sm1 . H5 . 23.4(6) no H1 . Sm1 . H5 . 66.7(8) no H3 . Sm1 . H5 . 76.6(8) no B2 . Sm1 . H6 . 24.3(6) no H1 . Sm1 . H6 . 61.3(8) no H3 . Sm1 . H6 . 97.1(8) no H5 . Sm1 . H6 . 42.3(8) no B2 . Sm1 . H8 . 22.9(5) no H1 . Sm1 . H8 . 96.0(8) no H3 . Sm1 . H8 . 114.5(8) no H5 . Sm1 . H8 . 37.9(7) no H6 . Sm1 . H8 . 41.0(8) no C14 2_556 Li1 . C15 2_556 30.29(7) yes C14 2_556 Li1 . C16 2_556 53.89(9) yes C15 2_556 Li1 . C16 2_556 31.16(7) yes C14 2_556 Li1 . H2 . 107.2(7) no C15 2_556 Li1 . H2 . 81.1(7) no C16 2_556 Li1 . H2 . 80.3(7) no C14 2_556 Li1 . H4 2_556 123.4(7) no C15 2_556 Li1 . H4 2_556 132.3(7) no C16 2_556 Li1 . H4 2_556 106.4(7) no C14 2_556 Li1 . H5 . 85.7(6) no C15 2_556 Li1 . H5 . 97.5(6) no C16 2_556 Li1 . H5 . 127.7(7) no H2 . Li1 . H4 2_556 121.9(9) no H2 . Li1 . H5 . 82.7(9) no H4 2_556 Li1 . H5 . 124.5(9) no Sm1 . N1 . C1 . 119.08(12) yes Sm1 . N1 . C11 . 125.16(11) yes C1 . N1 . C11 . 114.93(15) yes Sm1 . N2 . C3 . 124.48(11) yes Sm1 . N2 . C20 . 120.79(12) yes C3 . N2 . C20 . 114.35(14) yes Sm1 . N3 . C2 . 108.07(11) yes Sm1 . N3 . C4 . 107.59(10) yes C2 . N3 . C4 . 109.77(15) yes Sm1 . N3 . C5 . 110.92(11) yes C2 . N3 . C5 . 110.19(15) yes C4 . N3 . C5 . 110.23(15) yes Sm1 . N4 . C6 . 118.35(12) yes Sm1 . N4 . C10 . 123.59(12) yes C6 . N4 . C10 . 117.94(16) yes N1 . C1 . C2 . 108.63(16) yes N1 . C1 . H11 . 111.595 no C2 . C1 . H11 . 109.996 no N1 . C1 . H12 . 109.309 no C2 . C1 . H12 . 109.473 no H11 . C1 . H12 . 107.817 no C1 . C2 . N3 . 111.53(15) yes C1 . C2 . H21 . 110.593 no N3 . C2 . H21 . 109.371 no C1 . C2 . H22 . 107.683 no N3 . C2 . H22 . 109.435 no H21 . C2 . H22 . 108.151 no N2 . C3 . C4 . 109.70(16) yes N2 . C3 . H31 . 110.380 no C4 . C3 . H31 . 106.371 no N2 . C3 . H32 . 110.910 no C4 . C3 . H32 . 110.192 no H31 . C3 . H32 . 109.189 no C3 . C4 . N3 . 111.29(16) yes C3 . C4 . H41 . 111.912 no N3 . C4 . H41 . 108.392 no C3 . C4 . H42 . 108.127 no N3 . C4 . H42 . 108.989 no H41 . C4 . H42 . 108.038 no N3 . C5 . C6 . 112.16(16) yes N3 . C5 . H51 . 108.516 no C6 . C5 . H51 . 109.327 no N3 . C5 . H52 . 108.777 no C6 . C5 . H52 . 109.958 no H51 . C5 . H52 . 108.006 no C5 . C6 . N4 . 116.80(16) yes C5 . C6 . C7 . 121.16(18) yes N4 . C6 . C7 . 121.99(18) yes C6 . C7 . C8 . 119.17(19) yes C6 . C7 . H71 . 119.569 no C8 . C7 . H71 . 121.262 no C7 . C8 . C9 . 119.30(18) yes C7 . C8 . H81 . 120.239 no C9 . C8 . H81 . 120.456 no C8 . C9 . C10 . 118.40(19) yes C8 . C9 . H91 . 121.695 no C10 . C9 . H91 . 119.895 no C9 . C10 . N4 . 123.19(19) yes C9 . C10 . H101 . 119.375 no N4 . C10 . H101 . 117.434 no N1 . C11 . C12 . 123.75(16) yes N1 . C11 . C16 . 118.83(16) yes C12 . C11 . C16 . 117.35(17) yes C11 . C12 . C13 . 119.94(17) yes C11 . C12 . C17 . 120.75(17) yes C13 . C12 . C17 . 119.22(17) yes C12 . C13 . C14 . 122.79(18) yes C12 . C13 . H131 . 118.051 no C14 . C13 . H131 . 119.156 no C13 . C14 . C15 . 117.11(18) yes C13 . C14 . C18 . 121.59(18) yes C15 . C14 . C18 . 121.30(18) yes C14 . C15 . C16 . 122.20(17) yes C14 . C15 . H151 . 119.131 no C16 . C15 . H151 . 118.655 no C11 . C16 . C15 . 120.36(17) yes C11 . C16 . C19 . 120.30(17) yes C15 . C16 . C19 . 119.33(16) yes C12 . C17 . H171 . 108.723 no C12 . C17 . H172 . 109.726 no H171 . C17 . H172 . 110.155 no C12 . C17 . H173 . 109.270 no H171 . C17 . H173 . 110.134 no H172 . C17 . H173 . 108.820 no C14 . C18 . H181 . 113.185 no C14 . C18 . H182 . 111.090 no H181 . C18 . H182 . 107.163 no C14 . C18 . H183 . 113.325 no H181 . C18 . H183 . 107.454 no H182 . C18 . H183 . 104.035 no C16 . C19 . H191 . 110.906 no C16 . C19 . H192 . 113.499 no H191 . C19 . H192 . 105.489 no C16 . C19 . H193 . 113.796 no H191 . C19 . H193 . 106.613 no H192 . C19 . H193 . 105.937 no N2 . C20 . C21 . 120.00(17) yes N2 . C20 . C25 . 121.23(17) yes C21 . C20 . C25 . 118.72(16) yes C20 . C21 . C22 . 119.68(18) yes C20 . C21 . C26 . 120.94(17) yes C22 . C21 . C26 . 119.38(18) yes C21 . C22 . C23 . 122.16(18) yes C21 . C22 . H221 . 119.864 no C23 . C22 . H221 . 117.974 no C22 . C23 . C24 . 117.61(17) yes C22 . C23 . C27 . 120.85(19) yes C24 . C23 . C27 . 121.53(19) yes C23 . C24 . C25 . 122.17(18) yes C23 . C24 . H241 . 123.391 no C25 . C24 . H241 . 114.037 no C20 . C25 . C24 . 119.42(17) yes C20 . C25 . C28 . 121.39(17) yes C24 . C25 . C28 . 119.18(17) yes C21 . C26 . H261 . 110.903 no C21 . C26 . H262 . 109.662 no H261 . C26 . H262 . 106.959 no C21 . C26 . H263 . 112.144 no H261 . C26 . H263 . 108.327 no H262 . C26 . H263 . 108.681 no C23 . C27 . H271 . 111.856 no C23 . C27 . H272 . 112.501 no H271 . C27 . H272 . 104.094 no C23 . C27 . H273 . 115.923 no H271 . C27 . H273 . 106.237 no H272 . C27 . H273 . 105.291 no C25 . C28 . H281 . 109.779 no C25 . C28 . H282 . 113.110 no H281 . C28 . H282 . 107.624 no C25 . C28 . H283 . 113.202 no H281 . C28 . H283 . 107.021 no H282 . C28 . H283 . 105.754 no Sm1 . B1 . H1 . 55.0(12) no Sm1 . B1 . H2 . 115.2(12) no H1 . B1 . H2 . 109.6(17) no Sm1 . B1 . H3 . 51.0(12) no H1 . B1 . H3 . 104.5(17) no H2 . B1 . H3 . 112.4(17) no Sm1 . B1 . H4 . 135.6(12) no H1 . B1 . H4 . 112.8(16) no H2 . B1 . H4 . 109.1(17) no H3 . B1 . H4 . 108.4(17) no Sm1 . B2 . H5 . 64.7(13) no Sm1 . B2 . H6 . 59.9(12) no H5 . B2 . H6 . 104.6(18) no Sm1 . B2 . H7 . 168.1(13) no H5 . B2 . H7 . 112.3(17) no H6 . B2 . H7 . 111.9(17) no Sm1 . B2 . H8 . 73.8(13) no H5 . B2 . H8 . 101.4(18) no H6 . B2 . H8 . 107.5(17) no H7 . B2 . H8 . 118.0(18) no Sm1 . H1 . B1 . 102.5(14) no Li1 . H2 . B1 . 109.1(15) no Sm1 . H3 . B1 . 108.0(15) no Li1 2_556 H4 . B1 . 105.2(15) no Sm1 . H5 . Li1 . 110.6(10) no Sm1 . H5 . B2 . 91.9(14) no Li1 . H5 . B2 . 90.8(14) no Sm1 . H6 . B2 . 95.8(14) no Sm1 . H8 . B2 . 83.4(14) no ##end