# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Marcus Cole' 'Aaron J. Davies' 'Cameron Jones' 'Peter Junk' _publ_contact_author_name 'Peter Junk' _publ_contact_author_address ; School of Chemistry Monash University Victoria 3800 AUSTRALIA ; _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Bulky formamidinate complexes of lithium: The first examples of eta2: eta1-C=N,N' metal amidinate coordination ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 281337' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Li{N(2,6-Me2C6H3)C(H)N(2,6-Me2C6H3)}(PMDETA)]' _chemical_melting_point 408 _chemical_formula_moiety 'C26 H42 Li1 N5' _chemical_formula_sum 'C52 H84 Li2 N10' _chemical_formula_weight 863.17 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n' _symmetry_int_tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.6759(2) _cell_length_b 17.6854(4) _cell_length_c 17.4137(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.146(2) _cell_angle_gamma 90.00 _cell_volume 2612.09(11) _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 prism _exptl_crystal_colour colourless _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 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9807 _exptl_absorpt_correction_T_max 0.9871 _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 23881 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10868 _reflns_number_gt 7825 _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^)+(0.0714P)^2^+0.0777P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(15) _refine_ls_number_reflns 10868 _refine_ls_number_parameters 675 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7491(2) 0.99443(11) 0.77913(12) 0.0295(4) Uani 1 1 d . . . N2 N 0.6995(2) 0.87435(11) 0.72596(12) 0.0285(4) Uani 1 1 d . . . N3 N 1.0499(2) 0.94843(11) 0.67556(11) 0.0283(4) Uani 1 1 d . . . N4 N 1.1537(2) 1.02182(12) 0.82721(13) 0.0361(5) Uani 1 1 d . . . N5 N 1.0941(3) 0.86779(14) 0.87291(14) 0.0452(6) Uani 1 1 d . . . N6 N 0.3123(2) 0.48225(11) 0.95664(11) 0.0282(4) Uani 1 1 d . . . N7 N 0.4248(3) 0.57901(13) 1.04313(13) 0.0429(6) Uani 1 1 d . . . N8 N 0.0370(2) 0.35492(11) 0.83919(12) 0.0311(5) Uani 1 1 d . . . N9 N 0.0346(2) 0.51233(11) 0.78520(11) 0.0289(4) Uani 1 1 d . . . N10 N 0.3358(2) 0.45663(10) 0.75745(11) 0.0248(4) Uani 1 1 d . . . C1 C 0.6759(3) 1.06212(14) 0.79791(16) 0.0340(6) Uani 1 1 d . . . C2 C 0.6814(3) 1.07879(15) 0.87723(17) 0.0396(6) Uani 1 1 d . . . C3 C 0.6180(3) 1.14704(17) 0.8965(2) 0.0534(8) Uani 1 1 d . . . H3 H 0.6224 1.1592 0.9500 0.064 Uiso 1 1 calc R . . C4 C 0.5487(4) 1.19742(17) 0.8381(2) 0.0585(9) Uani 1 1 d . . . H4 H 0.5065 1.2439 0.8519 0.070 Uiso 1 1 calc R . . C5 C 0.5411(3) 1.18034(16) 0.7618(2) 0.0514(8) Uani 1 1 d . . . H5 H 0.4926 1.2150 0.7223 0.062 Uiso 1 1 calc R . . C6 C 0.6030(3) 1.11285(14) 0.73948(17) 0.0394(6) Uani 1 1 d . . . C7 C 0.7490(4) 1.02218(18) 0.93915(19) 0.0531(8) Uani 1 1 d . . . H7A H 0.6829 0.9767 0.9326 0.080 Uiso 1 1 calc R . . H7B H 0.7523 1.0440 0.9912 0.080 Uiso 1 1 calc R . . H7C H 0.8560 1.0087 0.9342 0.080 Uiso 1 1 calc R . . C8 C 0.5874(4) 1.09596(17) 0.65348(19) 0.0521(8) Uani 1 1 d . . . H8A H 0.5279 1.0490 0.6403 0.078 Uiso 1 1 calc R . . H8B H 0.6926 1.0903 0.6418 0.078 Uiso 1 1 calc R . . H8C H 0.5318 1.1376 0.6223 0.078 Uiso 1 1 calc R . . C9 C 0.5795(2) 0.81923(13) 0.70301(14) 0.0274(5) Uani 1 1 d . . . C10 C 0.5113(2) 0.80853(14) 0.62365(14) 0.0287(5) Uani 1 1 d . . . C11 C 0.3971(3) 0.75259(14) 0.60173(16) 0.0344(6) Uani 1 1 d . . . H11 H 0.3507 0.7455 0.5477 0.041 Uiso 1 1 calc R . . C12 C 0.3502(3) 0.70716(15) 0.65752(18) 0.0399(6) Uani 1 1 d . . . H12 H 0.2737 0.6686 0.6421 0.048 Uiso 1 1 calc R . . C13 C 0.4162(3) 0.71867(15) 0.73552(17) 0.0397(6) Uani 1 1 d . . . H13 H 0.3828 0.6883 0.7739 0.048 Uiso 1 1 calc R . . C14 C 0.5304(3) 0.77357(15) 0.75967(15) 0.0343(6) Uani 1 1 d . . . C15 C 0.5613(3) 0.85511(16) 0.56116(15) 0.0377(6) Uani 1 1 d . . . H15A H 0.4909 0.8449 0.5104 0.056 Uiso 1 1 calc R . . H15B H 0.6697 0.8420 0.5583 0.056 Uiso 1 1 calc R . . H15C H 0.5559 0.9089 0.5739 0.056 Uiso 1 1 calc R . . C16 C 0.6014(4) 0.7823(2) 0.84568(17) 0.0536(8) Uani 1 1 d . . . H16A H 0.5333 0.7577 0.8765 0.080 Uiso 1 1 calc R . . H16B H 0.6112 0.8362 0.8590 0.080 Uiso 1 1 calc R . . H16C H 0.7059 0.7587 0.8575 0.080 Uiso 1 1 calc R . . C17 C 0.6517(2) 0.93874(13) 0.74941(14) 0.0272(5) Uani 1 1 d . . . H17 H 0.5417 0.9462 0.7450 0.033 Uiso 1 1 calc R . . C18A C 0.9323(6) 0.9965(4) 0.6250(4) 0.0346(13) Uani 0.584(9) 1 d P A 1 H18A H 0.9628 1.0041 0.5744 0.052 Uiso 0.584(9) 1 calc PR A 1 H18B H 0.9269 1.0455 0.6505 0.052 Uiso 0.584(9) 1 calc PR A 1 H18C H 0.8289 0.9718 0.6163 0.052 Uiso 0.584(9) 1 calc PR A 1 C18B C 0.9345(10) 0.9543(9) 0.6053(6) 0.060(3) Uani 0.416(9) 1 d P A 2 H18D H 0.9861 0.9623 0.5611 0.090 Uiso 0.416(9) 1 calc PR A 2 H18E H 0.8648 0.9971 0.6092 0.090 Uiso 0.416(9) 1 calc PR A 2 H18F H 0.8724 0.9076 0.5971 0.090 Uiso 0.416(9) 1 calc PR A 2 C19A C 1.0540(6) 0.8756(3) 0.6340(3) 0.0388(16) Uani 0.584(9) 1 d P A 1 H19A H 0.9477 0.8540 0.6211 0.058 Uiso 0.584(9) 1 calc PR A 1 H19B H 1.1250 0.8405 0.6679 0.058 Uiso 0.584(9) 1 calc PR A 1 H19C H 1.0921 0.8842 0.5856 0.058 Uiso 0.584(9) 1 calc PR A 1 C19B C 1.1648(9) 0.8875(4) 0.6649(4) 0.040(2) Uani 0.416(9) 1 d P A 2 H19D H 1.1096 0.8390 0.6558 0.061 Uiso 0.416(9) 1 calc PR A 2 H19E H 1.2487 0.8842 0.7122 0.061 Uiso 0.416(9) 1 calc PR A 2 H19F H 1.2109 0.8998 0.6197 0.061 Uiso 0.416(9) 1 calc PR A 2 C20A C 1.1997(6) 0.9846(5) 0.6932(3) 0.0315(18) Uani 0.577(14) 1 d P A 1 H20A H 1.2224 1.0062 0.6444 0.038 Uiso 0.577(14) 1 calc PR A 1 H20B H 1.2817 0.9463 0.7130 0.038 Uiso 0.577(14) 1 calc PR A 1 C20B C 1.1457(14) 1.0218(6) 0.6928(6) 0.051(3) Uani 0.423(14) 1 d P A 2 H20C H 1.2170 1.0258 0.6554 0.061 Uiso 0.423(14) 1 calc PR A 2 H20D H 1.0721 1.0652 0.6830 0.061 Uiso 0.423(14) 1 calc PR A 2 C21A C 1.209(2) 1.0469(8) 0.7537(9) 0.039(3) Uani 0.577(14) 1 d P A 1 H21A H 1.1442 1.0902 0.7297 0.046 Uiso 0.577(14) 1 calc PR A 1 H21B H 1.3200 1.0646 0.7690 0.046 Uiso 0.577(14) 1 calc PR A 1 C21B C 1.238(3) 1.0277(13) 0.7708(15) 0.054(6) Uani 0.423(14) 1 d P A 2 H21C H 1.3193 0.9876 0.7789 0.064 Uiso 0.423(14) 1 calc PR A 2 H21D H 1.2931 1.0771 0.7765 0.064 Uiso 0.423(14) 1 calc PR A 2 C22A C 1.1078(4) 1.0916(2) 0.8596(2) 0.0738(12) Uani 1 1 d . A . H22D H 1.2003 1.1243 0.8750 0.111 Uiso 1 1 calc R . . H22E H 1.0638 1.0804 0.9058 0.111 Uiso 1 1 calc R . . H22F H 1.0282 1.1174 0.8200 0.111 Uiso 1 1 calc R . . C23A C 1.2800(8) 0.9751(4) 0.8745(5) 0.0454(19) Uani 0.622(17) 1 d P A 1 H23A H 1.3715 0.9771 0.8488 0.054 Uiso 0.622(17) 1 calc PR A 1 H23B H 1.3130 0.9999 0.9264 0.054 Uiso 0.622(17) 1 calc PR A 1 C23B C 1.2335(16) 0.9872(7) 0.9056(9) 0.054(3) Uani 0.378(17) 1 d P A 2 H23C H 1.3486 0.9901 0.9085 0.064 Uiso 0.378(17) 1 calc PR A 2 H23D H 1.2107 1.0211 0.9471 0.064 Uiso 0.378(17) 1 calc PR A 2 C24A C 1.2510(10) 0.8984(6) 0.8882(12) 0.115(5) Uani 0.622(17) 1 d P A 1 H24A H 1.2978 0.8883 0.9442 0.138 Uiso 0.622(17) 1 calc PR A 1 H24B H 1.3120 0.8683 0.8570 0.138 Uiso 0.622(17) 1 calc PR A 1 C24B C 1.2058(15) 0.9238(8) 0.9238(6) 0.048(3) Uani 0.378(17) 1 d P A 2 H24C H 1.1678 0.9286 0.9733 0.057 Uiso 0.378(17) 1 calc PR A 2 H24D H 1.3092 0.8980 0.9375 0.057 Uiso 0.378(17) 1 calc PR A 2 C25A C 1.0329(18) 0.8634(7) 0.9409(7) 0.061(3) Uani 0.60(2) 1 d P A 1 H25A H 0.9223 0.8477 0.9270 0.091 Uiso 0.60(2) 1 calc PR A 1 H25B H 1.0403 0.9131 0.9663 0.091 Uiso 0.60(2) 1 calc PR A 1 H25C H 1.0934 0.8264 0.9770 0.091 Uiso 0.60(2) 1 calc PR A 1 C25B C 0.9966(19) 0.8362(12) 0.9294(14) 0.062(6) Uani 0.40(2) 1 d P A 2 H25D H 0.9454 0.7891 0.9080 0.093 Uiso 0.40(2) 1 calc PR A 2 H25E H 0.9161 0.8732 0.9358 0.093 Uiso 0.40(2) 1 calc PR A 2 H25F H 1.0659 0.8262 0.9805 0.093 Uiso 0.40(2) 1 calc PR A 2 C26A C 1.096(2) 0.7880(7) 0.8412(6) 0.074(3) Uani 0.60(2) 1 d P A 1 H26A H 1.1333 0.7890 0.7919 0.111 Uiso 0.60(2) 1 calc PR A 1 H26B H 0.9888 0.7671 0.8315 0.111 Uiso 0.60(2) 1 calc PR A 1 H26C H 1.1661 0.7565 0.8796 0.111 Uiso 0.60(2) 1 calc PR A 1 C26B C 1.174(2) 0.8107(8) 0.8418(8) 0.061(4) Uani 0.40(2) 1 d P A 2 H26D H 1.2413 0.7829 0.8848 0.092 Uiso 0.40(2) 1 calc PR A 2 H26E H 1.2387 0.8332 0.8081 0.092 Uiso 0.40(2) 1 calc PR A 2 H26F H 1.0971 0.7760 0.8108 0.092 Uiso 0.40(2) 1 calc PR A 2 C27 C 0.3277(3) 0.42621(14) 1.01626(14) 0.0277(5) Uani 1 1 d . . . C28 C 0.4416(3) 0.37002(14) 1.01891(14) 0.0294(5) Uani 1 1 d . . . C29 C 0.4445(3) 0.30878(15) 1.07000(15) 0.0353(6) Uani 1 1 d . . . H29 H 0.5195 0.2695 1.0705 0.042 Uiso 1 1 calc R . . C30 C 0.3399(3) 0.30453(16) 1.11971(15) 0.0391(6) Uani 1 1 d . . . H30 H 0.3444 0.2632 1.1550 0.047 Uiso 1 1 calc R . . C31 C 0.2286(3) 0.36084(17) 1.11768(15) 0.0391(7) Uani 1 1 d . . . H31 H 0.1570 0.3581 1.1521 0.047 Uiso 1 1 calc R . . C32 C 0.2198(3) 0.42178(15) 1.06579(14) 0.0319(6) Uani 1 1 d . . . C33 C 0.5620(3) 0.37598(16) 0.96749(16) 0.0380(6) Uani 1 1 d . . . H33A H 0.6344 0.3329 0.9777 0.057 Uiso 1 1 calc R . . H33B H 0.6217 0.4231 0.9794 0.057 Uiso 1 1 calc R . . H33C H 0.5078 0.3758 0.9121 0.057 Uiso 1 1 calc R . . C34 C 0.0915(3) 0.48004(17) 1.06083(17) 0.0442(7) Uani 1 1 d . . . H34A H 0.0367 0.4862 1.0059 0.066 Uiso 1 1 calc R . . H34B H 0.1381 0.5284 1.0811 0.066 Uiso 1 1 calc R . . H34C H 0.0163 0.4634 1.0922 0.066 Uiso 1 1 calc R . . C35 C 0.4833(3) 0.65473(15) 1.04618(17) 0.0414(6) Uani 1 1 d . . . C36 C 0.6318(3) 0.67039(15) 1.03054(15) 0.0369(6) Uani 1 1 d . . . C37 C 0.6971(3) 0.74177(15) 1.04814(16) 0.0413(6) Uani 1 1 d . . . H37 H 0.7999 0.7522 1.0400 0.050 Uiso 1 1 calc R . . C38 C 0.6143(4) 0.79754(17) 1.07719(17) 0.0495(8) Uani 1 1 d . . . H38 H 0.6593 0.8463 1.0884 0.059 Uiso 1 1 calc R . . C39 C 0.4661(3) 0.78221(16) 1.08984(16) 0.0438(7) Uani 1 1 d . . . H39 H 0.4094 0.8209 1.1097 0.053 Uiso 1 1 calc R . . C40 C 0.3979(3) 0.71153(15) 1.07425(17) 0.0402(6) Uani 1 1 d . . . C41 C 0.7243(3) 0.61089(17) 0.99802(19) 0.0515(8) Uani 1 1 d . . . H41A H 0.8367 0.6237 1.0113 0.077 Uiso 1 1 calc R . . H41B H 0.6889 0.6086 0.9408 0.077 Uiso 1 1 calc R . . H41C H 0.7077 0.5617 1.0208 0.077 Uiso 1 1 calc R . . C42 C 0.2372(3) 0.69575(18) 1.0898(2) 0.0552(8) Uani 1 1 d . . . H42A H 0.1994 0.7403 1.1137 0.083 Uiso 1 1 calc R . . H42B H 0.2431 0.6526 1.1256 0.083 Uiso 1 1 calc R . . H42C H 0.1642 0.6840 1.0402 0.083 Uiso 1 1 calc R . . C43 C 0.3633(3) 0.55272(16) 0.97633(15) 0.0349(6) Uani 1 1 d . . . H43 H 0.3515 0.5877 0.9341 0.042 Uiso 1 1 calc R . . C44 C 0.0241(3) 0.31187(16) 0.91000(16) 0.0439(7) Uani 1 1 d . . . H44A H 0.1208 0.2826 0.9282 0.066 Uiso 1 1 calc R . . H44B H -0.0662 0.2774 0.8975 0.066 Uiso 1 1 calc R . . H44C H 0.0092 0.3470 0.9514 0.066 Uiso 1 1 calc R . . C45 C 0.0613(3) 0.30120(16) 0.77865(16) 0.0420(7) Uani 1 1 d . . . H45A H 0.0669 0.3288 0.7305 0.063 Uiso 1 1 calc R . . H45B H -0.0268 0.2654 0.7678 0.063 Uiso 1 1 calc R . . H45C H 0.1600 0.2736 0.7972 0.063 Uiso 1 1 calc R . . C46 C -0.1087(3) 0.39860(15) 0.81134(15) 0.0350(6) Uani 1 1 d . . . H46A H -0.1395 0.4233 0.8569 0.042 Uiso 1 1 calc R . . H46B H -0.1944 0.3635 0.7876 0.042 Uiso 1 1 calc R . . C47 C -0.0913(3) 0.45829(15) 0.75165(15) 0.0334(6) Uani 1 1 d . . . H47A H -0.0658 0.4338 0.7047 0.040 Uiso 1 1 calc R . . H47B H -0.1923 0.4857 0.7350 0.040 Uiso 1 1 calc R . . C48 C -0.0281(3) 0.57267(16) 0.82881(17) 0.0427(7) Uani 1 1 d . . . H48A H -0.0807 0.5499 0.8677 0.064 Uiso 1 1 calc R . . H48B H -0.1039 0.6034 0.7920 0.064 Uiso 1 1 calc R . . H48C H 0.0588 0.6048 0.8556 0.064 Uiso 1 1 calc R . . C49 C 0.1085(3) 0.54638(14) 0.72410(15) 0.0317(5) Uani 1 1 d . . . H49A H 0.1716 0.5909 0.7462 0.038 Uiso 1 1 calc R . . H49B H 0.0251 0.5639 0.6798 0.038 Uiso 1 1 calc R . . C50 C 0.2145(3) 0.49006(14) 0.69397(14) 0.0293(5) Uani 1 1 d . . . H50A H 0.1486 0.4490 0.6656 0.035 Uiso 1 1 calc R . . H50B H 0.2673 0.5159 0.6561 0.035 Uiso 1 1 calc R . . C51 C 0.4596(3) 0.51162(14) 0.78815(15) 0.0323(6) Uani 1 1 d . . . H51A H 0.5079 0.5294 0.7454 0.049 Uiso 1 1 calc R . . H51B H 0.5401 0.4877 0.8288 0.049 Uiso 1 1 calc R . . H51C H 0.4136 0.5546 0.8109 0.049 Uiso 1 1 calc R . . C52 C 0.4093(3) 0.39178(14) 0.72522(15) 0.0333(6) Uani 1 1 d . . . H52A H 0.4928 0.3704 0.7663 0.050 Uiso 1 1 calc R . . H52B H 0.4546 0.4089 0.6812 0.050 Uiso 1 1 calc R . . H52C H 0.3293 0.3531 0.7068 0.050 Uiso 1 1 calc R . . Li1 Li 0.9593(4) 0.9421(2) 0.7829(2) 0.0302(8) Uani 1 1 d . A . Li2 Li 0.2082(4) 0.4449(2) 0.8516(2) 0.0279(8) 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 N1 0.0235(9) 0.0268(11) 0.0399(12) -0.0070(9) 0.0105(8) -0.0008(8) N2 0.0241(9) 0.0265(11) 0.0353(11) -0.0060(9) 0.0069(8) -0.0014(8) N3 0.0274(9) 0.0233(10) 0.0358(12) -0.0015(9) 0.0103(8) 0.0020(8) N4 0.0325(11) 0.0326(12) 0.0434(13) -0.0097(10) 0.0084(10) -0.0026(9) N5 0.0387(12) 0.0405(14) 0.0554(16) 0.0143(12) 0.0078(11) 0.0046(10) N6 0.0311(10) 0.0233(11) 0.0290(11) -0.0063(9) 0.0038(8) -0.0022(8) N7 0.0509(13) 0.0346(13) 0.0425(14) 0.0043(11) 0.0080(11) -0.0017(10) N8 0.0342(10) 0.0305(11) 0.0286(11) 0.0007(9) 0.0068(8) -0.0092(9) N9 0.0283(10) 0.0292(11) 0.0310(11) -0.0006(9) 0.0100(8) 0.0012(8) N10 0.0228(9) 0.0219(10) 0.0304(10) -0.0011(9) 0.0071(8) 0.0004(7) C1 0.0233(11) 0.0287(14) 0.0522(16) -0.0077(12) 0.0133(11) -0.0089(10) C2 0.0336(13) 0.0324(15) 0.0568(18) -0.0113(13) 0.0188(12) -0.0060(11) C3 0.0549(17) 0.0396(18) 0.073(2) -0.0228(17) 0.0302(16) -0.0111(14) C4 0.0553(18) 0.0238(15) 0.101(3) -0.0149(18) 0.0260(18) -0.0008(13) C5 0.0473(16) 0.0245(15) 0.085(2) -0.0025(16) 0.0184(15) -0.0018(12) C6 0.0289(12) 0.0286(14) 0.0636(19) -0.0037(13) 0.0167(12) -0.0058(11) C7 0.0594(18) 0.0515(19) 0.0538(19) -0.0157(16) 0.0242(15) -0.0064(15) C8 0.0561(18) 0.0351(16) 0.062(2) 0.0089(15) 0.0059(15) 0.0025(13) C9 0.0219(10) 0.0224(12) 0.0391(14) -0.0013(11) 0.0094(10) 0.0041(9) C10 0.0255(11) 0.0232(13) 0.0377(15) -0.0015(11) 0.0069(10) 0.0021(9) C11 0.0301(12) 0.0272(13) 0.0449(16) -0.0064(12) 0.0056(11) 0.0005(10) C12 0.0346(13) 0.0233(14) 0.064(2) -0.0022(13) 0.0147(12) -0.0026(10) C13 0.0390(13) 0.0263(14) 0.0579(19) 0.0070(13) 0.0196(13) -0.0029(11) C14 0.0344(13) 0.0318(14) 0.0394(15) 0.0033(12) 0.0136(11) 0.0023(10) C15 0.0409(14) 0.0363(15) 0.0343(14) 0.0028(12) 0.0046(11) -0.0057(11) C16 0.0608(18) 0.063(2) 0.0388(17) 0.0124(16) 0.0136(14) -0.0055(15) C17 0.0203(10) 0.0285(13) 0.0338(13) 0.0004(11) 0.0078(9) 0.0000(9) C18A 0.036(2) 0.031(3) 0.035(3) 0.005(3) 0.004(2) 0.000(2) C18B 0.045(4) 0.092(9) 0.042(5) 0.007(6) 0.007(4) 0.022(6) C19A 0.041(3) 0.031(3) 0.044(3) -0.012(2) 0.010(2) 0.004(2) C19B 0.033(4) 0.041(4) 0.048(4) -0.002(3) 0.010(3) 0.006(3) C20A 0.025(3) 0.039(4) 0.034(3) -0.008(2) 0.0157(19) -0.007(2) C20B 0.072(6) 0.028(5) 0.072(6) 0.001(4) 0.057(5) -0.001(4) C21A 0.051(6) 0.035(6) 0.035(5) -0.014(4) 0.019(4) -0.020(4) C21B 0.042(8) 0.047(11) 0.085(15) -0.022(8) 0.040(9) -0.026(6) C22A 0.081(2) 0.052(2) 0.107(3) -0.042(2) 0.061(2) -0.0251(17) C23A 0.030(3) 0.051(4) 0.049(4) 0.002(3) -0.004(2) -0.004(2) C23B 0.026(6) 0.064(8) 0.062(8) -0.030(6) -0.010(5) -0.003(4) C24A 0.037(4) 0.083(7) 0.202(14) 0.042(8) -0.026(6) 0.012(4) C24B 0.032(6) 0.048(7) 0.050(6) 0.015(5) -0.020(4) -0.002(4) C25A 0.081(8) 0.049(6) 0.046(4) 0.013(5) 0.000(5) 0.018(5) C25B 0.040(5) 0.074(12) 0.072(11) 0.036(9) 0.013(6) -0.019(7) C26A 0.108(8) 0.049(6) 0.075(5) 0.019(4) 0.044(6) 0.030(5) C26B 0.074(9) 0.039(7) 0.067(7) 0.006(5) 0.008(6) 0.011(6) C27 0.0244(11) 0.0312(14) 0.0257(12) -0.0068(11) 0.0015(9) -0.0030(9) C28 0.0287(12) 0.0325(14) 0.0254(12) -0.0006(11) 0.0018(9) -0.0020(10) C29 0.0372(13) 0.0319(14) 0.0345(14) -0.0004(12) 0.0023(11) -0.0047(11) C30 0.0436(14) 0.0394(16) 0.0322(14) 0.0022(12) 0.0034(11) -0.0139(12) C31 0.0321(12) 0.0557(19) 0.0310(14) -0.0136(13) 0.0100(10) -0.0163(12) C32 0.0276(12) 0.0421(16) 0.0247(12) -0.0102(12) 0.0026(9) -0.0069(10) C33 0.0406(13) 0.0368(15) 0.0384(15) 0.0014(12) 0.0121(11) 0.0093(11) C34 0.0329(13) 0.0551(18) 0.0464(16) -0.0169(14) 0.0126(12) 0.0013(12) C35 0.0467(15) 0.0236(14) 0.0532(17) -0.0046(13) 0.0092(13) -0.0029(11) C36 0.0442(14) 0.0266(14) 0.0399(15) -0.0024(12) 0.0089(11) -0.0025(11) C37 0.0529(15) 0.0329(15) 0.0364(15) 0.0006(13) 0.0055(12) -0.0124(12) C38 0.0647(19) 0.0290(16) 0.0513(19) -0.0116(14) 0.0044(15) -0.0118(13) C39 0.0642(18) 0.0259(15) 0.0386(16) -0.0021(12) 0.0045(13) 0.0065(13) C40 0.0463(14) 0.0265(14) 0.0469(16) 0.0069(12) 0.0080(12) 0.0044(11) C41 0.0535(17) 0.0385(17) 0.067(2) -0.0119(15) 0.0235(15) -0.0073(13) C42 0.0487(16) 0.0340(17) 0.085(2) 0.0079(16) 0.0201(16) 0.0132(13) C43 0.0264(12) 0.0456(16) 0.0327(14) -0.0169(13) 0.0060(10) 0.0028(10) C44 0.0555(16) 0.0405(16) 0.0347(15) 0.0087(13) 0.0069(12) -0.0175(13) C45 0.0482(15) 0.0356(16) 0.0424(16) -0.0041(13) 0.0096(12) -0.0078(12) C46 0.0251(11) 0.0451(16) 0.0349(14) 0.0019(12) 0.0068(10) -0.0068(11) C47 0.0207(11) 0.0440(16) 0.0340(14) 0.0034(12) 0.0027(10) -0.0017(10) C48 0.0438(14) 0.0371(16) 0.0509(17) 0.0044(13) 0.0183(12) 0.0162(12) C49 0.0323(12) 0.0290(13) 0.0346(14) 0.0099(11) 0.0085(10) 0.0040(10) C50 0.0288(11) 0.0323(14) 0.0280(13) 0.0061(11) 0.0088(9) 0.0027(10) C51 0.0283(11) 0.0278(13) 0.0408(15) -0.0010(12) 0.0070(10) -0.0031(10) C52 0.0367(12) 0.0300(14) 0.0363(14) -0.0014(11) 0.0150(11) 0.0060(10) Li1 0.0272(17) 0.028(2) 0.037(2) 0.0028(18) 0.0106(16) 0.0040(15) Li2 0.0294(19) 0.028(2) 0.026(2) -0.0039(17) 0.0050(16) -0.0014(16) _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 N1 C17 1.330(3) . ? N1 C1 1.425(3) . ? N1 Li1 2.034(4) . ? N2 C17 1.307(3) . ? N2 C9 1.421(3) . ? N3 C18B 1.412(9) . ? N3 C20A 1.423(5) . ? N3 C18A 1.470(6) . ? N3 C19A 1.481(5) . ? N3 C19B 1.505(7) . ? N3 C20B 1.537(9) . ? N3 Li1 2.177(4) . ? N4 C21B 1.35(2) . ? N4 C22A 1.448(4) . ? N4 C23A 1.477(7) . ? N4 C23B 1.523(14) . ? N4 C21A 1.526(16) . ? N4 Li1 2.209(5) . ? N5 C26B 1.395(14) . ? N5 C25A 1.397(15) . ? N5 C24A 1.437(9) . ? N5 C26A 1.516(12) . ? N5 C24B 1.531(11) . ? N5 C25B 1.531(17) . ? N5 Li1 2.187(5) . ? N6 C43 1.343(3) . ? N6 C27 1.421(3) . ? N6 Li2 1.976(4) . ? N7 C43 1.262(3) . ? N7 C35 1.429(3) . ? N8 C45 1.467(3) . ? N8 C44 1.473(3) . ? N8 C46 1.474(3) . ? N8 Li2 2.157(4) . ? N9 C47 1.477(3) . ? N9 C48 1.478(3) . ? N9 C49 1.481(3) . ? N9 Li2 2.072(4) . ? N10 C51 1.464(3) . ? N10 C52 1.479(3) . ? N10 C50 1.480(3) . ? N10 Li2 2.172(4) . ? C1 C2 1.403(4) . ? C1 C6 1.403(4) . ? C2 C3 1.396(4) . ? C2 C7 1.498(4) . ? C3 C4 1.390(5) . ? C4 C5 1.352(5) . ? C5 C6 1.397(4) . ? C6 C8 1.505(4) . ? C9 C10 1.397(3) . ? C9 C14 1.408(3) . ? C10 C11 1.395(3) . ? C10 C15 1.500(3) . ? C11 C12 1.386(4) . ? C12 C13 1.374(4) . ? C13 C14 1.388(4) . ? C14 C16 1.503(4) . ? C20A C21A 1.515(18) . ? C20B C21B 1.43(3) . ? C23A C24A 1.409(11) . ? C23B C24B 1.203(17) . ? C27 C28 1.395(3) . ? C27 C32 1.402(3) . ? C28 C29 1.398(4) . ? C28 C33 1.516(3) . ? C29 C30 1.382(4) . ? C30 C31 1.382(4) . ? C31 C32 1.398(4) . ? C32 C34 1.505(4) . ? C35 C36 1.399(4) . ? C35 C40 1.397(4) . ? C36 C37 1.391(4) . ? C36 C41 1.504(4) . ? C37 C38 1.377(4) . ? C38 C39 1.376(4) . ? C39 C40 1.385(4) . ? C40 C42 1.501(4) . ? C46 C47 1.511(4) . ? C49 C50 1.521(3) . ? 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 C17 N1 C1 115.76(18) . . ? C17 N1 Li1 99.66(18) . . ? C1 N1 Li1 144.5(2) . . ? C17 N2 C9 115.08(18) . . ? C18B N3 C20A 127.1(6) . . ? C18B N3 C18A 33.1(5) . . ? C20A N3 C18A 110.9(4) . . ? C18B N3 C19A 74.1(6) . . ? C20A N3 C19A 112.4(4) . . ? C18A N3 C19A 107.1(3) . . ? C18B N3 C19B 108.3(6) . . ? C20A N3 C19B 75.5(5) . . ? C18A N3 C19B 137.2(4) . . ? C19A N3 C19B 39.9(3) . . ? C18B N3 C20B 111.3(8) . . ? C20A N3 C20B 31.4(3) . . ? C18A N3 C20B 84.7(6) . . ? C19A N3 C20B 139.7(5) . . ? C19B N3 C20B 106.5(6) . . ? C18B N3 Li1 115.4(4) . . ? C20A N3 Li1 108.4(3) . . ? C18A N3 Li1 102.3(3) . . ? C19A N3 Li1 115.1(2) . . ? C19B N3 Li1 115.9(3) . . ? C20B N3 Li1 98.9(4) . . ? C21B N4 C22A 117.0(10) . . ? C21B N4 C23A 89.8(11) . . ? C22A N4 C23A 119.5(5) . . ? C21B N4 C23B 118.1(12) . . ? C22A N4 C23B 96.0(6) . . ? C23A N4 C23B 29.7(4) . . ? C21B N4 C21A 18.0(12) . . ? C22A N4 C21A 103.9(6) . . ? C23A N4 C21A 107.6(7) . . ? C23B N4 C21A 134.8(10) . . ? C21B N4 Li1 106.7(11) . . ? C22A N4 Li1 115.3(2) . . ? C23A N4 Li1 105.1(3) . . ? C23B N4 Li1 103.1(5) . . ? C21A N4 Li1 104.2(7) . . ? C26B N5 C25A 126.6(8) . . ? C26B N5 C24A 79.5(11) . . ? C25A N5 C24A 112.2(11) . . ? C26B N5 C26A 30.9(5) . . ? C25A N5 C26A 106.9(5) . . ? C24A N5 C26A 109.7(9) . . ? C26B N5 C24B 112.8(10) . . ? C25A N5 C24B 81.5(8) . . ? C24A N5 C24B 35.8(6) . . ? C26A N5 C24B 139.4(9) . . ? C26B N5 C25B 111.8(9) . . ? C25A N5 C25B 22.5(8) . . ? C24A N5 C25B 130.4(11) . . ? C26A N5 C25B 86.8(8) . . ? C24B N5 C25B 103.4(10) . . ? C26B N5 Li1 113.0(6) . . ? C25A N5 Li1 113.6(5) . . ? C24A N5 Li1 104.4(4) . . ? C26A N5 Li1 110.1(4) . . ? C24B N5 Li1 101.7(5) . . ? C25B N5 Li1 113.3(8) . . ? C43 N6 C27 119.0(2) . . ? C43 N6 Li2 127.5(2) . . ? C27 N6 Li2 113.43(18) . . ? C43 N7 C35 117.2(2) . . ? C45 N8 C44 108.3(2) . . ? C45 N8 C46 110.2(2) . . ? C44 N8 C46 109.60(19) . . ? C45 N8 Li2 110.46(17) . . ? C44 N8 Li2 118.01(19) . . ? C46 N8 Li2 99.86(17) . . ? C47 N9 C48 110.41(19) . . ? C47 N9 C49 112.04(18) . . ? C48 N9 C49 109.71(19) . . ? C47 N9 Li2 103.81(18) . . ? C48 N9 Li2 115.59(19) . . ? C49 N9 Li2 105.12(17) . . ? C51 N10 C52 108.17(17) . . ? C51 N10 C50 111.06(19) . . ? C52 N10 C50 108.79(18) . . ? C51 N10 Li2 103.83(17) . . ? C52 N10 Li2 122.76(18) . . ? C50 N10 Li2 101.91(16) . . ? C2 C1 C6 119.7(2) . . ? C2 C1 N1 118.6(2) . . ? C6 C1 N1 121.7(2) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C7 121.3(3) . . ? C1 C2 C7 119.7(2) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 121.5(3) . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C8 119.1(3) . . ? C1 C6 C8 121.8(2) . . ? C10 C9 C14 119.2(2) . . ? C10 C9 N2 120.3(2) . . ? C14 C9 N2 120.5(2) . . ? C11 C10 C9 119.7(2) . . ? C11 C10 C15 119.2(2) . . ? C9 C10 C15 121.1(2) . . ? C12 C11 C10 121.0(2) . . ? C13 C12 C11 119.0(2) . . ? C12 C13 C14 121.7(2) . . ? C13 C14 C9 119.4(2) . . ? C13 C14 C16 119.4(2) . . ? C9 C14 C16 121.2(2) . . ? N2 C17 N1 123.3(2) . . ? N3 C20A C21A 113.1(8) . . ? C21B C20B N3 114.8(12) . . ? C20A C21A N4 113.0(11) . . ? N4 C21B C20B 114.0(17) . . ? C24A C23A N4 119.6(5) . . ? C24B C23B N4 122.1(9) . . ? C23A C24A N5 121.8(6) . . ? C23B C24B N5 126.0(9) . . ? C28 C27 C32 120.0(2) . . ? C28 C27 N6 118.5(2) . . ? C32 C27 N6 121.1(2) . . ? C27 C28 C29 119.4(2) . . ? C27 C28 C33 120.2(2) . . ? C29 C28 C33 120.5(2) . . ? C30 C29 C28 120.9(2) . . ? C31 C30 C29 119.5(2) . . ? C30 C31 C32 121.0(2) . . ? C31 C32 C27 119.2(2) . . ? C31 C32 C34 120.3(2) . . ? C27 C32 C34 120.5(2) . . ? C36 C35 C40 120.3(2) . . ? C36 C35 N7 120.8(2) . . ? C40 C35 N7 118.4(2) . . ? C37 C36 C35 119.0(2) . . ? C37 C36 C41 119.5(2) . . ? C35 C36 C41 121.4(2) . . ? C38 C37 C36 120.7(3) . . ? C37 C38 C39 119.6(3) . . ? C38 C39 C40 121.4(3) . . ? C39 C40 C35 118.7(2) . . ? C39 C40 C42 120.5(3) . . ? C35 C40 C42 120.7(2) . . ? N7 C43 N6 129.1(3) . . ? N8 C46 C47 112.95(18) . . ? N9 C47 C46 110.65(19) . . ? N9 C49 C50 111.46(19) . . ? N10 C50 C49 112.97(19) . . ? N1 Li1 N3 115.6(2) . . ? N1 Li1 N5 129.6(2) . . ? N3 Li1 N5 114.26(18) . . ? N1 Li1 N4 109.56(19) . . ? N3 Li1 N4 83.12(15) . . ? N5 Li1 N4 83.06(16) . . ? N6 Li2 N9 117.4(2) . . ? N6 Li2 N8 120.7(2) . . ? N9 Li2 N8 87.96(16) . . ? N6 Li2 N10 117.42(18) . . ? N9 Li2 N10 87.15(16) . . ? N8 Li2 N10 116.42(18) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.557 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.047 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 281338' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Li{N(2,6-Et2C6H3)C(H)N(2,6-Et2C6H3)}(PMDETA)]' _chemical_melting_point 348 _chemical_formula_moiety 'C30 H50 Li N5' _chemical_formula_sum 'C30 H50 Li N5' _chemical_formula_weight 487.69 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' Li Li -0.0003 0.0001 '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' _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 13.889(3) _cell_length_b 15.094(3) _cell_length_c 15.379(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.31(3) _cell_angle_gamma 90.00 _cell_volume 3003.6(10) _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 colourless _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 1.078 _exptl_crystal_density_method empirical _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9874 _exptl_absorpt_correction_T_max 0.9937 _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 11714 _diffrn_reflns_av_R_equivalents 0.1647 _diffrn_reflns_av_sigmaI/netI 0.3072 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5646 _reflns_number_gt 1167 _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^)+(0.0994P)^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 5646 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3643 _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_ref 0.2948 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _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 N1 N -0.2452(4) 0.2054(3) 0.0235(4) 0.0588(15) Uani 1 1 d . . . N2 N -0.1816(4) 0.1599(3) -0.0902(4) 0.0671(16) Uani 1 1 d . . . N3 N -0.1293(5) 0.1825(4) 0.2638(4) 0.0720(16) Uani 1 1 d . . . N4 N 0.0006(4) 0.1186(4) 0.1663(4) 0.0701(16) Uani 1 1 d . D . N5 N -0.1651(5) -0.0101(4) 0.1135(5) 0.0815(18) Uani 1 1 d . . . C1 C -0.3111(5) 0.2676(5) 0.0398(4) 0.0568(17) Uani 1 1 d . . . C2 C -0.3929(6) 0.2360(6) 0.0612(5) 0.081(2) Uani 1 1 d . B . C3 C -0.4605(6) 0.2941(7) 0.0787(5) 0.096(3) Uani 1 1 d . . . H3 H -0.5162 0.2714 0.0941 0.115 Uiso 1 1 calc R . . C4 C -0.4488(6) 0.3830(7) 0.0745(5) 0.087(3) Uani 1 1 d . . . H4 H -0.4960 0.4225 0.0862 0.104 Uiso 1 1 calc R . . C5 C -0.3689(6) 0.4148(5) 0.0532(4) 0.078(2) Uani 1 1 d . . . H5 H -0.3608 0.4771 0.0496 0.093 Uiso 1 1 calc R . . C6 C -0.2987(5) 0.3589(5) 0.0367(4) 0.0608(18) Uani 1 1 d . . . C7 C -0.4054(8) 0.1379(8) 0.0706(12) 0.155(6) Uani 1 1 d . . . H7A H -0.4228 0.1140 0.0068 0.186 Uiso 1 1 calc R A 1 H7B H -0.3350 0.1160 0.1069 0.186 Uiso 1 1 calc R A 1 C8A C -0.4681(13) 0.0943(8) 0.1058(14) 0.137(8) Uani 0.67(2) 1 d P B 1 H8A1 H -0.4520 0.1123 0.1708 0.205 Uiso 0.67(2) 1 calc PR B 1 H8A2 H -0.4574 0.0304 0.1031 0.205 Uiso 0.67(2) 1 calc PR B 1 H8A3 H -0.5402 0.1088 0.0691 0.205 Uiso 0.67(2) 1 calc PR B 1 C8B C -0.481(3) 0.1207(14) 0.0228(17) 0.077(12) Uani 0.33(2) 1 d P B 2 H8B1 H -0.5057 0.0685 0.0461 0.116 Uiso 0.33(2) 1 calc PR B 2 H8B2 H -0.4773 0.1074 -0.0384 0.116 Uiso 0.33(2) 1 calc PR B 2 H8B3 H -0.5281 0.1704 0.0170 0.116 Uiso 0.33(2) 1 calc PR B 2 C9 C -0.2036(5) 0.3951(4) 0.0222(5) 0.081(2) Uani 1 1 d . . . H9A H -0.1480 0.3502 0.0439 0.097 Uiso 1 1 calc R . . H9B H -0.2204 0.4037 -0.0456 0.097 Uiso 1 1 calc R . . C10 C -0.1631(6) 0.4814(5) 0.0716(5) 0.108(3) Uani 1 1 d . . . H10A H -0.2136 0.5285 0.0445 0.162 Uiso 1 1 calc R . . H10B H -0.0978 0.4964 0.0643 0.162 Uiso 1 1 calc R . . H10C H -0.1515 0.4752 0.1381 0.162 Uiso 1 1 calc R . . C11 C -0.1884(5) 0.1761(5) -0.1831(5) 0.0632(18) Uani 1 1 d . . . C12 C -0.2462(6) 0.1202(6) -0.2547(7) 0.080(2) Uani 1 1 d . . . C13 C -0.2514(6) 0.1341(7) -0.3461(6) 0.099(3) Uani 1 1 d . . . H13 H -0.2881 0.0938 -0.3941 0.118 Uiso 1 1 calc R . . C14 C -0.2035(7) 0.2059(8) -0.3662(7) 0.108(3) Uani 1 1 d . . . H14 H -0.2095 0.2173 -0.4287 0.130 Uiso 1 1 calc R . . C15 C -0.1478(7) 0.2604(6) -0.2971(7) 0.105(3) Uani 1 1 d . . . H15 H -0.1138 0.3096 -0.3118 0.126 Uiso 1 1 calc R . . C16 C -0.1387(6) 0.2474(6) -0.2077(6) 0.081(2) Uani 1 1 d . . . C17 C -0.2977(6) 0.0396(6) -0.2344(5) 0.104(3) Uani 1 1 d . . . H17A H -0.3047 -0.0058 -0.2827 0.125 Uiso 1 1 calc R . . H17B H -0.2537 0.0147 -0.1733 0.125 Uiso 1 1 calc R . . C18 C -0.3996(6) 0.0594(5) -0.2323(5) 0.111(3) Uani 1 1 d . . . H18A H -0.3933 0.1048 -0.1850 0.167 Uiso 1 1 calc R . . H18B H -0.4293 0.0055 -0.2168 0.167 Uiso 1 1 calc R . . H18C H -0.4447 0.0811 -0.2937 0.167 Uiso 1 1 calc R . . C19 C -0.0683(7) 0.3063(5) -0.1315(6) 0.094(2) Uani 1 1 d . . . H19A H -0.0897 0.3687 -0.1464 0.113 Uiso 1 1 calc R . . H19B H -0.0765 0.2914 -0.0719 0.113 Uiso 1 1 calc R . . C20 C 0.0415(6) 0.2977(5) -0.1192(6) 0.117(3) Uani 1 1 d . . . H20A H 0.0672 0.2396 -0.0922 0.176 Uiso 1 1 calc R . . H20B H 0.0814 0.3444 -0.0773 0.176 Uiso 1 1 calc R . . H20C H 0.0490 0.3033 -0.1799 0.176 Uiso 1 1 calc R . . C21 C -0.2371(5) 0.2105(4) -0.0590(5) 0.0606(18) Uani 1 1 d . . . H21 H -0.2758 0.2558 -0.0997 0.073 Uiso 1 1 calc R . . C22 C -0.1318(8) 0.2774(5) 0.2638(5) 0.147(4) Uani 1 1 d . . . H22A H -0.1033 0.2991 0.3282 0.221 Uiso 1 1 calc R . . H22B H -0.2034 0.2977 0.2343 0.221 Uiso 1 1 calc R . . H22C H -0.0906 0.3003 0.2289 0.221 Uiso 1 1 calc R . . C23 C -0.1866(7) 0.1475(6) 0.3147(5) 0.158(4) Uani 1 1 d . . . H23A H -0.1922 0.0831 0.3064 0.237 Uiso 1 1 calc R . . H23B H -0.2559 0.1737 0.2922 0.237 Uiso 1 1 calc R . . H23C H -0.1517 0.1613 0.3811 0.237 Uiso 1 1 calc R . . C24 C -0.0240(9) 0.1552(9) 0.3094(6) 0.188(6) Uani 1 1 d . . . H24A H 0.0086 0.1998 0.3586 0.226 Uiso 1 1 calc R . . H24B H -0.0260 0.0991 0.3420 0.226 Uiso 1 1 calc R . . C25 C 0.0421(6) 0.1421(6) 0.2654(5) 0.115(3) Uani 1 1 d . . . H25A H 0.0903 0.0945 0.2989 0.138 Uiso 1 1 calc R . . H25B H 0.0835 0.1968 0.2720 0.138 Uiso 1 1 calc R . . C26 C 0.0438(5) 0.1716(5) 0.1100(5) 0.108(3) Uani 1 1 d . . . H26A H 0.1186 0.1618 0.1313 0.161 Uiso 1 1 calc R . . H26B H 0.0301 0.2345 0.1165 0.161 Uiso 1 1 calc R . . H26C H 0.0117 0.1542 0.0443 0.161 Uiso 1 1 calc R . . C27 C 0.0137(7) 0.0262(6) 0.1533(6) 0.102(3) Uani 1 1 d . . . H27A H 0.0121 0.0190 0.0888 0.123 Uiso 1 1 calc R C 1 H27B H 0.0845 0.0105 0.1955 0.123 Uiso 1 1 calc R C 1 C28A C -0.0522(17) -0.0378(15) 0.166(4) 0.133(14) Uani 0.50(3) 1 d P D 1 H28A H -0.0394 -0.0442 0.2335 0.160 Uiso 0.50(3) 1 calc PR D 1 H28B H -0.0388 -0.0957 0.1424 0.160 Uiso 0.50(3) 1 calc PR D 1 C28B C -0.0743(17) -0.0170(13) 0.087(2) 0.070(8) Uani 0.50(3) 1 d P D 2 H28C H -0.0580 -0.0803 0.0832 0.084 Uiso 0.50(3) 1 calc PR D 2 H28D H -0.0900 0.0100 0.0251 0.084 Uiso 0.50(3) 1 calc PR D 2 C29A C -0.254(4) -0.0301(18) 0.023(2) 0.099(8) Uani 0.56(7) 1 d P D 1 H29A H -0.2528 0.0123 -0.0253 0.148 Uiso 0.56(7) 1 calc PR D 1 H29B H -0.3195 -0.0251 0.0324 0.148 Uiso 0.56(7) 1 calc PR D 1 H29C H -0.2463 -0.0904 0.0023 0.148 Uiso 0.56(7) 1 calc PR D 1 C29B C -0.203(4) -0.023(2) 0.017(2) 0.069(10) Uani 0.44(7) 1 d P D 2 H29D H -0.1740 0.0218 -0.0125 0.104 Uiso 0.44(7) 1 calc PR D 2 H29E H -0.2789 -0.0172 -0.0072 0.104 Uiso 0.44(7) 1 calc PR D 2 H29F H -0.1844 -0.0822 0.0027 0.104 Uiso 0.44(7) 1 calc PR D 2 C30 C -0.1969(8) -0.0683(6) 0.1719(6) 0.146(4) Uani 1 1 d . D . H30A H -0.2014 -0.1290 0.1483 0.218 Uiso 1 1 calc R . . H30B H -0.2647 -0.0497 0.1713 0.218 Uiso 1 1 calc R . . H30C H -0.1464 -0.0657 0.2359 0.218 Uiso 1 1 calc R . . Li1 Li -0.1582(8) 0.1324(7) 0.1275(7) 0.065(3) Uani 1 1 d . 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 N1 0.058(4) 0.061(4) 0.062(4) 0.001(3) 0.026(3) 0.002(3) N2 0.066(4) 0.058(4) 0.064(4) -0.012(3) 0.006(3) 0.007(3) N3 0.079(5) 0.068(5) 0.060(4) 0.003(3) 0.015(3) 0.004(4) N4 0.065(4) 0.051(4) 0.080(4) -0.008(3) 0.009(3) -0.001(3) N5 0.089(6) 0.051(4) 0.098(6) 0.003(4) 0.026(5) -0.017(4) C1 0.057(5) 0.068(6) 0.041(4) 0.008(4) 0.012(4) -0.005(4) C2 0.080(6) 0.072(6) 0.105(6) 0.027(5) 0.050(5) 0.022(5) C3 0.086(6) 0.114(8) 0.091(6) 0.019(6) 0.036(5) -0.002(6) C4 0.076(6) 0.117(9) 0.060(5) -0.022(5) 0.017(5) 0.020(6) C5 0.082(6) 0.069(6) 0.073(5) -0.023(4) 0.017(5) 0.015(5) C6 0.066(5) 0.058(6) 0.057(4) -0.012(4) 0.020(4) -0.010(4) C7 0.081(8) 0.143(12) 0.231(15) 0.057(11) 0.044(10) -0.028(8) C8A 0.211(16) 0.081(10) 0.18(2) -0.013(10) 0.147(15) -0.056(10) C8B 0.16(3) 0.022(14) 0.046(16) 0.014(12) 0.033(18) 0.019(17) C9 0.088(6) 0.047(5) 0.096(5) -0.016(4) 0.021(5) -0.003(4) C10 0.113(7) 0.068(6) 0.133(7) 0.003(5) 0.034(6) -0.016(5) C11 0.063(5) 0.057(5) 0.065(6) -0.005(5) 0.018(4) 0.012(4) C12 0.066(6) 0.080(7) 0.082(6) -0.015(6) 0.012(5) -0.004(5) C13 0.083(7) 0.126(9) 0.073(7) -0.032(6) 0.012(5) 0.022(6) C14 0.080(7) 0.154(10) 0.096(8) -0.016(8) 0.038(7) 0.001(6) C15 0.097(7) 0.147(9) 0.081(7) 0.000(7) 0.042(6) -0.008(6) C16 0.085(6) 0.095(7) 0.070(6) 0.000(5) 0.036(5) 0.012(5) C17 0.064(6) 0.128(9) 0.101(6) -0.028(6) 0.007(5) 0.035(6) C18 0.098(7) 0.112(7) 0.113(6) -0.011(5) 0.025(5) 0.007(5) C19 0.098(7) 0.084(6) 0.104(6) -0.002(5) 0.040(6) 0.002(5) C20 0.096(7) 0.095(7) 0.146(7) -0.019(5) 0.026(6) 0.008(5) C21 0.054(5) 0.037(5) 0.092(6) -0.008(4) 0.027(4) -0.008(3) C22 0.247(12) 0.053(7) 0.084(6) -0.008(5) -0.010(6) -0.006(7) C23 0.211(11) 0.187(10) 0.108(7) -0.020(6) 0.097(8) -0.074(8) C24 0.127(10) 0.345(17) 0.068(7) -0.035(8) 0.006(7) 0.056(10) C25 0.075(7) 0.171(9) 0.064(6) -0.034(6) -0.016(5) 0.019(6) C26 0.069(6) 0.109(7) 0.145(7) 0.001(6) 0.040(5) -0.012(5) C27 0.081(7) 0.083(8) 0.113(7) -0.015(6) 0.001(6) 0.024(6) C28A 0.090(18) 0.075(17) 0.17(4) -0.005(18) -0.026(17) 0.054(13) C28B 0.059(14) 0.048(11) 0.087(17) -0.007(11) 0.007(13) -0.004(9) C29A 0.11(2) 0.077(13) 0.117(16) -0.023(11) 0.056(17) -0.056(15) C29B 0.06(2) 0.081(17) 0.055(16) 0.020(11) 0.012(14) -0.019(14) C30 0.214(11) 0.093(8) 0.137(8) 0.036(6) 0.073(8) 0.032(7) Li1 0.058(7) 0.063(8) 0.065(7) 0.009(6) 0.011(6) -0.009(6) _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 N1 C21 1.316(7) . ? N1 C1 1.395(7) . ? N1 Li1 1.956(11) . ? N2 C21 1.295(7) . ? N2 C11 1.419(7) . ? N3 C23 1.407(7) . ? N3 C22 1.433(8) . ? N3 C24 1.434(10) . ? N3 Li1 2.124(11) . ? N4 C27 1.431(8) . ? N4 C26 1.459(7) . ? N4 C25 1.463(8) . ? N4 Li1 2.074(11) . ? N5 C29B 1.40(3) . ? N5 C30 1.437(9) . ? N5 C28B 1.458(16) . ? N5 C29A 1.52(3) . ? N5 C28A 1.54(2) . ? N5 Li1 2.161(11) . ? C1 C2 1.378(8) . ? C1 C6 1.391(8) . ? C2 C3 1.381(9) . ? C2 C7 1.504(11) . ? C3 C4 1.357(9) . ? C4 C5 1.354(9) . ? C5 C6 1.381(8) . ? C6 C9 1.519(8) . ? C7 C8B 1.07(2) . ? C7 C8A 1.352(13) . ? C9 C10 1.510(8) . ? C11 C12 1.387(9) . ? C11 C16 1.403(9) . ? C12 C13 1.397(9) . ? C12 C17 1.501(9) . ? C13 C14 1.364(10) . ? C14 C15 1.343(10) . ? C15 C16 1.350(9) . ? C16 C19 1.512(9) . ? C17 C18 1.458(8) . ? C19 C20 1.472(8) . ? C24 C25 1.338(9) . ? C27 C28A 1.39(3) . ? C27 C28B 1.43(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 C21 N1 C1 115.2(5) . . ? C21 N1 Li1 125.3(6) . . ? C1 N1 Li1 118.8(5) . . ? C21 N2 C11 116.2(6) . . ? C23 N3 C22 110.9(7) . . ? C23 N3 C24 107.7(7) . . ? C22 N3 C24 107.9(7) . . ? C23 N3 Li1 118.3(6) . . ? C22 N3 Li1 111.1(5) . . ? C24 N3 Li1 100.0(5) . . ? C27 N4 C26 110.5(6) . . ? C27 N4 C25 111.0(6) . . ? C26 N4 C25 113.2(6) . . ? C27 N4 Li1 103.5(5) . . ? C26 N4 Li1 113.5(5) . . ? C25 N4 Li1 104.5(5) . . ? C29B N5 C30 120(2) . . ? C29B N5 C28B 75(3) . . ? C30 N5 C28B 128.4(13) . . ? C29B N5 C29A 29.2(11) . . ? C30 N5 C29A 97.0(16) . . ? C28B N5 C29A 103(2) . . ? C29B N5 C28A 116(3) . . ? C30 N5 C28A 89(2) . . ? C28B N5 C28A 46.2(12) . . ? C29A N5 C28A 140(2) . . ? C29B N5 Li1 103.3(13) . . ? C30 N5 Li1 124.0(6) . . ? C28B N5 Li1 95.0(8) . . ? C29A N5 Li1 106.3(11) . . ? C28A N5 Li1 102.6(9) . . ? C2 C1 C6 118.2(7) . . ? C2 C1 N1 117.6(7) . . ? C6 C1 N1 124.2(6) . . ? C1 C2 C3 120.4(8) . . ? C1 C2 C7 119.8(7) . . ? C3 C2 C7 119.7(8) . . ? C4 C3 C2 121.1(8) . . ? C5 C4 C3 119.1(7) . . ? C4 C5 C6 121.5(7) . . ? C5 C6 C1 119.7(7) . . ? C5 C6 C9 121.1(7) . . ? C1 C6 C9 119.1(6) . . ? C8B C7 C8A 62.9(14) . . ? C8B C7 C2 106.9(18) . . ? C8A C7 C2 129.1(11) . . ? C10 C9 C6 114.9(6) . . ? C12 C11 C16 116.9(8) . . ? C12 C11 N2 120.2(8) . . ? C16 C11 N2 122.9(7) . . ? C11 C12 C13 120.6(8) . . ? C11 C12 C17 120.7(8) . . ? C13 C12 C17 118.5(9) . . ? C14 C13 C12 119.8(9) . . ? C15 C14 C13 119.6(10) . . ? C14 C15 C16 122.1(9) . . ? C15 C16 C11 120.8(8) . . ? C15 C16 C19 120.0(9) . . ? C11 C16 C19 119.1(8) . . ? C18 C17 C12 112.3(7) . . ? C20 C19 C16 113.3(6) . . ? N2 C21 N1 126.4(7) . . ? C25 C24 N3 124.1(8) . . ? C24 C25 N4 118.6(7) . . ? C28A C27 C28B 49.3(13) . . ? C28A C27 N4 122.2(13) . . ? C28B C27 N4 115.0(12) . . ? C27 C28A N5 109(3) . . ? C27 C28B N5 112.1(16) . . ? N1 Li1 N4 124.6(5) . . ? N1 Li1 N3 116.4(6) . . ? N4 Li1 N3 87.3(4) . . ? N1 Li1 N5 119.2(5) . . ? N4 Li1 N5 86.1(4) . . ? N3 Li1 N5 116.0(5) . . ? _diffrn_measured_fraction_theta_max 0.759 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.829 _refine_diff_density_max 0.150 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.038 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 281339' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Li{N(2,6-iPr2C6H3)C(H)N(2,6-iPr2C6H3)}(PMDETA)]' _chemical_melting_point 422 _chemical_formula_moiety 'C34 H58 Li N5' _chemical_formula_sum 'C34 H58 Li N5' _chemical_formula_weight 543.79 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.7197(2) _cell_length_b 16.5509(2) _cell_length_c 17.5383(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3401.93(9) _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 prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9756 _exptl_absorpt_correction_T_max 0.9877 _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 31582 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8298 _reflns_number_gt 5411 _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^)+(0.0545P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1.5(17) _refine_ls_number_reflns 8298 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.12005(12) 0.84804(7) 0.15494(8) 0.0214(3) Uani 1 1 d . . . N2 N 0.11255(12) 0.98347(7) 0.12369(8) 0.0235(3) Uani 1 1 d . . . N3 N 0.07352(13) 0.97066(8) 0.32945(8) 0.0273(4) Uani 1 1 d . . . N4 N -0.05666(13) 0.82240(8) 0.32366(9) 0.0300(4) Uani 1 1 d . . . N5 N -0.17213(13) 0.90744(8) 0.20208(8) 0.0281(4) Uani 1 1 d . . . C1 C 0.15477(14) 0.77009(9) 0.13031(9) 0.0204(4) Uani 1 1 d . . . C2 C 0.23306(14) 0.72576(9) 0.17544(9) 0.0210(4) Uani 1 1 d . . . C3 C 0.26659(15) 0.64911(10) 0.15171(10) 0.0232(4) Uani 1 1 d . . . H3 H 0.3200 0.6196 0.1815 0.028 Uiso 1 1 calc R . . C4 C 0.22368(15) 0.61516(9) 0.08566(10) 0.0244(4) Uani 1 1 d . . . H4 H 0.2484 0.5632 0.0697 0.029 Uiso 1 1 calc R . . C5 C 0.14489(15) 0.65723(10) 0.04318(10) 0.0244(4) Uani 1 1 d . . . H5 H 0.1138 0.6330 -0.0013 0.029 Uiso 1 1 calc R . . C6 C 0.10962(14) 0.73442(9) 0.06376(10) 0.0209(4) Uani 1 1 d . . . C7 C 0.28393(15) 0.76395(9) 0.24603(10) 0.0255(4) Uani 1 1 d . . . H7 H 0.2256 0.8019 0.2671 0.031 Uiso 1 1 calc R . . C8 C 0.31279(18) 0.70336(11) 0.30898(10) 0.0332(5) Uani 1 1 d . . . H8A H 0.3744 0.6678 0.2917 0.050 Uiso 1 1 calc R . . H8B H 0.2451 0.6709 0.3208 0.050 Uiso 1 1 calc R . . H8C H 0.3373 0.7325 0.3548 0.050 Uiso 1 1 calc R . . C9 C 0.38916(18) 0.81415(11) 0.22564(12) 0.0378(5) Uani 1 1 d . . . H9A H 0.3699 0.8520 0.1846 0.057 Uiso 1 1 calc R . . H9B H 0.4505 0.7782 0.2086 0.057 Uiso 1 1 calc R . . H9C H 0.4144 0.8444 0.2706 0.057 Uiso 1 1 calc R . . C10 C 0.02303(15) 0.77686(10) 0.01344(10) 0.0256(4) Uani 1 1 d . . . H10 H -0.0006 0.8276 0.0401 0.031 Uiso 1 1 calc R . . C11 C -0.08458(16) 0.72548(10) 0.00159(12) 0.0329(5) Uani 1 1 d . . . H11A H -0.1158 0.7098 0.0513 0.049 Uiso 1 1 calc R . . H11B H -0.0650 0.6769 -0.0275 0.049 Uiso 1 1 calc R . . H11C H -0.1416 0.7570 -0.0265 0.049 Uiso 1 1 calc R . . C12 C 0.07441(19) 0.80113(12) -0.06354(11) 0.0385(5) Uani 1 1 d . . . H12A H 0.0995 0.7526 -0.0908 0.058 Uiso 1 1 calc R . . H12B H 0.1399 0.8369 -0.0551 0.058 Uiso 1 1 calc R . . H12C H 0.0167 0.8294 -0.0939 0.058 Uiso 1 1 calc R . . C13 C 0.15869(15) 1.04804(9) 0.08087(10) 0.0229(4) Uani 1 1 d . . . C14 C 0.09363(15) 1.08306(9) 0.02124(10) 0.0246(4) Uani 1 1 d . . . C15 C 0.13229(16) 1.15265(10) -0.01450(11) 0.0282(4) Uani 1 1 d . . . H15 H 0.0871 1.1767 -0.0533 0.034 Uiso 1 1 calc R . . C16 C 0.23541(17) 1.18792(10) 0.00524(11) 0.0301(5) Uani 1 1 d . . . H16 H 0.2603 1.2360 -0.0193 0.036 Uiso 1 1 calc R . . C17 C 0.30100(16) 1.15237(10) 0.06071(10) 0.0292(4) Uani 1 1 d . . . H17 H 0.3728 1.1755 0.0731 0.035 Uiso 1 1 calc R . . C18 C 0.26527(15) 1.08319(9) 0.09953(10) 0.0253(4) Uani 1 1 d . . . C19 C -0.01785(15) 1.04548(10) -0.00565(11) 0.0285(4) Uani 1 1 d . . . H19 H -0.0264 0.9920 0.0202 0.034 Uiso 1 1 calc R . . C20 C -0.11906(18) 1.09745(12) 0.01673(15) 0.0500(6) Uani 1 1 d . . . H20A H -0.1141 1.1497 -0.0094 0.075 Uiso 1 1 calc R . . H20B H -0.1185 1.1061 0.0720 0.075 Uiso 1 1 calc R . . H20C H -0.1899 1.0702 0.0020 0.075 Uiso 1 1 calc R . . C21 C -0.01765(19) 1.03076(14) -0.09166(13) 0.0523(6) Uani 1 1 d . . . H21A H 0.0478 0.9969 -0.1053 0.078 Uiso 1 1 calc R . . H21B H -0.0122 1.0826 -0.1184 0.078 Uiso 1 1 calc R . . H21C H -0.0884 1.0034 -0.1064 0.078 Uiso 1 1 calc R . . C22 C 0.34142(16) 1.04861(11) 0.16159(11) 0.0322(4) Uani 1 1 d . . . H22 H 0.3002 1.0018 0.1849 0.039 Uiso 1 1 calc R . . C23 C 0.3639(2) 1.10987(12) 0.22504(12) 0.0436(5) Uani 1 1 d . . . H23A H 0.2912 1.1277 0.2469 0.065 Uiso 1 1 calc R . . H23B H 0.4046 1.1566 0.2040 0.065 Uiso 1 1 calc R . . H23C H 0.4105 1.0847 0.2649 0.065 Uiso 1 1 calc R . . C24 C 0.45346(18) 1.01652(12) 0.12860(13) 0.0441(6) Uani 1 1 d . . . H24A H 0.4960 1.0611 0.1053 0.066 Uiso 1 1 calc R . . H24B H 0.4369 0.9755 0.0899 0.066 Uiso 1 1 calc R . . H24C H 0.4991 0.9924 0.1695 0.066 Uiso 1 1 calc R . . C25 C 0.15132(14) 0.91013(9) 0.11183(10) 0.0219(4) Uani 1 1 d . . . H25 H 0.2034 0.9012 0.0712 0.026 Uiso 1 1 calc R . . C26 C 0.19585(16) 0.95638(11) 0.34271(12) 0.0345(5) Uani 1 1 d . . . H26A H 0.2227 0.9916 0.3839 0.052 Uiso 1 1 calc R . . H26B H 0.2386 0.9682 0.2960 0.052 Uiso 1 1 calc R . . H26C H 0.2078 0.8998 0.3571 0.052 Uiso 1 1 calc R . . C27 C 0.05684(19) 1.05748(10) 0.31645(12) 0.0384(5) Uani 1 1 d . . . H27A H 0.0936 1.0731 0.2685 0.058 Uiso 1 1 calc R . . H27B H 0.0908 1.0880 0.3586 0.058 Uiso 1 1 calc R . . H27C H -0.0250 1.0693 0.3135 0.058 Uiso 1 1 calc R . . C28 C 0.00782(17) 0.94247(11) 0.39574(11) 0.0342(5) Uani 1 1 d . . . H28A H -0.0688 0.9677 0.3951 0.041 Uiso 1 1 calc R . . H28B H 0.0469 0.9595 0.4432 0.041 Uiso 1 1 calc R . . C29 C -0.00484(18) 0.85086(11) 0.39533(11) 0.0349(5) Uani 1 1 d . . . H29A H 0.0711 0.8256 0.4017 0.042 Uiso 1 1 calc R . . H29B H -0.0531 0.8340 0.4388 0.042 Uiso 1 1 calc R . . C30 C -0.03040(19) 0.73649(10) 0.30996(13) 0.0416(5) Uani 1 1 d . . . H30A H -0.0623 0.7037 0.3513 0.062 Uiso 1 1 calc R . . H30B H 0.0525 0.7291 0.3081 0.062 Uiso 1 1 calc R . . H30C H -0.0640 0.7196 0.2613 0.062 Uiso 1 1 calc R . . C31 C -0.18185(16) 0.83425(12) 0.32470(11) 0.0358(5) Uani 1 1 d . . . H31A H -0.2004 0.8836 0.3541 0.043 Uiso 1 1 calc R . . H31B H -0.2186 0.7877 0.3503 0.043 Uiso 1 1 calc R . . C32 C -0.22781(18) 0.84215(11) 0.24500(11) 0.0373(5) Uani 1 1 d . . . H32A H -0.2165 0.7905 0.2176 0.045 Uiso 1 1 calc R . . H32B H -0.3109 0.8528 0.2474 0.045 Uiso 1 1 calc R . . C33 C -0.20152(19) 0.89934(12) 0.12220(11) 0.0415(5) Uani 1 1 d . . . H33A H -0.1612 0.9406 0.0926 0.062 Uiso 1 1 calc R . . H33B H -0.2840 0.9063 0.1159 0.062 Uiso 1 1 calc R . . H33C H -0.1792 0.8456 0.1041 0.062 Uiso 1 1 calc R . . C34 C -0.21000(19) 0.98628(11) 0.22842(13) 0.0459(6) Uani 1 1 d . . . H34A H -0.2924 0.9914 0.2205 0.069 Uiso 1 1 calc R . . H34B H -0.1703 1.0286 0.1997 0.069 Uiso 1 1 calc R . . H34C H -0.1928 0.9920 0.2828 0.069 Uiso 1 1 calc R . . Li1 Li 0.0123(3) 0.89925(16) 0.23148(17) 0.0279(7) 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 N1 0.0201(8) 0.0184(7) 0.0256(8) 0.0005(6) 0.0015(7) 0.0004(6) N2 0.0237(8) 0.0188(7) 0.0280(8) 0.0020(6) 0.0035(7) 0.0018(6) N3 0.0254(9) 0.0272(8) 0.0292(9) -0.0022(7) 0.0021(7) -0.0002(6) N4 0.0242(9) 0.0302(8) 0.0356(10) 0.0022(7) 0.0000(8) 0.0003(7) N5 0.0265(9) 0.0286(7) 0.0294(9) -0.0008(7) 0.0023(7) 0.0021(7) C1 0.0192(9) 0.0198(8) 0.0223(9) 0.0009(7) 0.0060(8) -0.0016(7) C2 0.0188(9) 0.0223(8) 0.0218(9) 0.0011(7) 0.0026(8) -0.0015(7) C3 0.0198(9) 0.0244(8) 0.0255(9) 0.0031(8) 0.0005(8) 0.0009(8) C4 0.0231(10) 0.0195(8) 0.0306(10) -0.0017(8) 0.0041(9) 0.0023(7) C5 0.0240(10) 0.0259(9) 0.0234(9) -0.0040(7) 0.0009(8) -0.0022(8) C6 0.0170(9) 0.0227(8) 0.0230(9) 0.0013(7) 0.0030(8) -0.0011(7) C7 0.0250(11) 0.0256(9) 0.0261(10) -0.0025(8) -0.0009(8) 0.0020(8) C8 0.0357(12) 0.0365(10) 0.0274(10) -0.0014(8) -0.0047(9) 0.0011(9) C9 0.0368(12) 0.0379(10) 0.0387(11) -0.0052(9) -0.0050(10) -0.0087(9) C10 0.0230(10) 0.0266(9) 0.0273(10) -0.0008(8) -0.0032(8) 0.0024(8) C11 0.0248(11) 0.0306(10) 0.0434(12) -0.0020(9) -0.0102(9) 0.0009(8) C12 0.0374(13) 0.0455(11) 0.0324(12) 0.0096(9) -0.0051(10) 0.0015(9) C13 0.0234(10) 0.0192(8) 0.0260(9) -0.0039(7) 0.0062(8) 0.0003(7) C14 0.0254(10) 0.0201(8) 0.0283(10) -0.0008(7) 0.0037(8) 0.0015(7) C15 0.0304(11) 0.0226(8) 0.0317(10) 0.0048(8) 0.0016(9) 0.0007(8) C16 0.0368(12) 0.0219(9) 0.0314(11) 0.0013(8) 0.0078(10) -0.0066(8) C17 0.0273(11) 0.0294(9) 0.0310(11) -0.0052(8) 0.0029(9) -0.0059(8) C18 0.0270(11) 0.0222(8) 0.0268(10) -0.0029(7) 0.0030(9) -0.0005(8) C19 0.0246(10) 0.0241(8) 0.0367(11) 0.0046(8) 0.0039(9) -0.0026(8) C20 0.0322(13) 0.0431(11) 0.0746(16) -0.0088(11) 0.0007(12) 0.0033(10) C21 0.0436(14) 0.0689(15) 0.0444(14) -0.0122(12) 0.0018(12) -0.0244(12) C22 0.0277(11) 0.0351(10) 0.0337(11) 0.0029(9) -0.0003(9) -0.0044(9) C23 0.0441(14) 0.0488(12) 0.0380(12) -0.0007(10) -0.0068(11) -0.0123(10) C24 0.0310(12) 0.0465(12) 0.0547(15) 0.0061(11) -0.0034(11) 0.0034(10) C25 0.0192(10) 0.0254(9) 0.0210(9) -0.0041(7) -0.0004(8) 0.0004(7) C26 0.0300(11) 0.0361(10) 0.0375(11) -0.0026(9) 0.0008(10) -0.0005(9) C27 0.0412(12) 0.0280(10) 0.0459(13) -0.0043(9) -0.0017(10) 0.0007(9) C28 0.0359(12) 0.0425(11) 0.0243(10) -0.0050(8) -0.0002(9) -0.0017(9) C29 0.0358(12) 0.0406(11) 0.0283(10) 0.0070(9) 0.0020(10) -0.0026(9) C30 0.0395(13) 0.0287(10) 0.0567(15) 0.0029(10) -0.0009(11) -0.0031(9) C31 0.0261(11) 0.0457(11) 0.0355(12) 0.0075(9) 0.0050(9) -0.0032(9) C32 0.0275(11) 0.0425(11) 0.0419(12) 0.0025(10) 0.0037(10) -0.0054(9) C33 0.0419(14) 0.0487(12) 0.0340(11) -0.0027(9) 0.0032(10) -0.0040(10) C34 0.0457(14) 0.0390(11) 0.0531(14) -0.0099(10) -0.0137(12) 0.0120(10) Li1 0.0254(17) 0.0265(14) 0.0319(17) -0.0049(13) -0.0019(14) 0.0046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C25 1.327(2) . ? N1 C1 1.420(2) . ? N1 Li1 2.029(3) . ? N2 C25 1.313(2) . ? N2 C13 1.414(2) . ? N2 Li1 2.626(3) . ? N3 C27 1.468(2) . ? N3 C28 1.471(2) . ? N3 C26 1.472(2) . ? N3 Li1 2.206(3) . ? N4 C29 1.473(2) . ? N4 C30 1.475(2) . ? N4 C31 1.480(2) . ? N4 Li1 2.210(3) . ? N5 C33 1.449(2) . ? N5 C34 1.454(2) . ? N5 C32 1.470(2) . ? N5 Li1 2.226(3) . ? C1 C6 1.411(2) . ? C1 C2 1.417(2) . ? C2 C3 1.392(2) . ? C2 C7 1.513(2) . ? C3 C4 1.382(2) . ? C4 C5 1.376(2) . ? C5 C6 1.390(2) . ? C6 C10 1.517(2) . ? C7 C8 1.529(2) . ? C7 C9 1.529(3) . ? C10 C12 1.532(3) . ? C10 C11 1.535(2) . ? C13 C18 1.416(2) . ? C13 C14 1.418(2) . ? C14 C15 1.387(2) . ? C14 C19 1.522(2) . ? C15 C16 1.386(3) . ? C16 C17 1.372(3) . ? C17 C18 1.396(2) . ? C18 C22 1.519(3) . ? C19 C20 1.517(3) . ? C19 C21 1.528(3) . ? C22 C23 1.528(3) . ? C22 C24 1.530(3) . ? C25 Li1 2.663(4) . ? C28 C29 1.523(3) . ? C31 C32 1.504(3) . ? 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 C25 N1 C1 116.81(14) . . ? C25 N1 Li1 103.02(13) . . ? C1 N1 Li1 139.40(13) . . ? C25 N2 C13 118.84(14) . . ? C25 N2 Li1 77.18(11) . . ? C13 N2 Li1 162.70(12) . . ? C27 N3 C28 111.33(15) . . ? C27 N3 C26 108.15(14) . . ? C28 N3 C26 109.52(15) . . ? C27 N3 Li1 111.11(14) . . ? C28 N3 Li1 105.99(13) . . ? C26 N3 Li1 110.74(13) . . ? C29 N4 C30 111.18(15) . . ? C29 N4 C31 110.84(16) . . ? C30 N4 C31 109.66(15) . . ? C29 N4 Li1 106.82(13) . . ? C30 N4 Li1 111.06(14) . . ? C31 N4 Li1 107.16(14) . . ? C33 N5 C34 108.52(16) . . ? C33 N5 C32 108.76(15) . . ? C34 N5 C32 111.21(16) . . ? C33 N5 Li1 116.68(14) . . ? C34 N5 Li1 106.11(14) . . ? C32 N5 Li1 105.53(14) . . ? C6 C1 C2 119.23(14) . . ? C6 C1 N1 121.62(15) . . ? C2 C1 N1 119.09(14) . . ? C3 C2 C1 119.20(15) . . ? C3 C2 C7 120.96(15) . . ? C1 C2 C7 119.75(14) . . ? C4 C3 C2 121.23(16) . . ? C5 C4 C3 119.49(15) . . ? C4 C5 C6 121.60(16) . . ? C5 C6 C1 119.19(16) . . ? C5 C6 C10 118.25(15) . . ? C1 C6 C10 122.56(14) . . ? C2 C7 C8 113.83(13) . . ? C2 C7 C9 110.69(15) . . ? C8 C7 C9 110.29(15) . . ? C6 C10 C12 111.78(15) . . ? C6 C10 C11 111.82(13) . . ? C12 C10 C11 110.42(16) . . ? N2 C13 C18 121.68(16) . . ? N2 C13 C14 119.67(15) . . ? C18 C13 C14 118.47(15) . . ? C15 C14 C13 119.79(16) . . ? C15 C14 C19 118.66(16) . . ? C13 C14 C19 121.54(15) . . ? C16 C15 C14 121.44(17) . . ? C17 C16 C15 119.01(16) . . ? C16 C17 C18 121.95(17) . . ? C17 C18 C13 119.25(16) . . ? C17 C18 C22 118.81(16) . . ? C13 C18 C22 121.93(15) . . ? C20 C19 C14 111.06(15) . . ? C20 C19 C21 110.31(18) . . ? C14 C19 C21 111.70(15) . . ? C18 C22 C23 111.91(15) . . ? C18 C22 C24 111.34(16) . . ? C23 C22 C24 110.94(16) . . ? N2 C25 N1 122.01(15) . . ? N2 C25 Li1 74.09(11) . . ? N1 C25 Li1 47.92(10) . . ? N3 C28 C29 111.29(15) . . ? N4 C29 C28 111.25(15) . . ? N4 C31 C32 110.80(16) . . ? N5 C32 C31 112.39(16) . . ? N1 Li1 N3 122.47(15) . . ? N1 Li1 N4 118.11(13) . . ? N3 Li1 N4 81.80(12) . . ? N1 Li1 N5 118.47(15) . . ? N3 Li1 N5 117.63(14) . . ? N4 Li1 N5 81.35(12) . . ? N1 Li1 N2 57.79(9) . . ? N3 Li1 N2 97.51(11) . . ? N4 Li1 N2 174.61(15) . . ? N5 Li1 N2 103.62(12) . . ? N1 Li1 C25 29.06(7) . . ? N3 Li1 C25 112.24(13) . . ? N4 Li1 C25 147.05(13) . . ? N5 Li1 C25 114.05(13) . . ? N2 Li1 C25 28.73(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.215 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.048 #===END