# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1-MIL-145(Li)[DMF] _database_code_depnum_ccdc_archive 'CCDC 895709' #TrackingRef '- MIL-145(Li)[DMF].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MIL-145 _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 Li4 N4 O10' _chemical_formula_sum 'C22 H20 Li4 N4 O10' _chemical_formula_weight 528.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.666(4) _cell_length_b 11.692(5) _cell_length_c 12.366(5) _cell_angle_alpha 72.750(9) _cell_angle_beta 67.912(8) _cell_angle_gamma 76.869(9) _cell_volume 1226.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2865 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 23.83 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9718 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6740 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4296 _reflns_number_gt 3057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1309P)^2^+0.4921P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4296 _refine_ls_number_parameters 384 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2383 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.171 _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 Li1 Li 0.4531(3) 0.6167(3) 0.9467(2) 0.0262(8) Uani 1 1 d . . . Li2 Li 0.4651(3) 0.9274(2) 0.6125(2) 0.0219(7) Uani 1 1 d . . . Li3 Li 1.2340(3) 1.1085(3) 0.5165(3) 0.0314(9) Uani 1 1 d . . . Li4 Li 0.4451(3) 0.6926(3) 0.6948(2) 0.0280(8) Uani 1 1 d . . . O1 O 0.65167(12) 0.87305(10) 0.65482(9) 0.0237(3) Uani 1 1 d . . . O2 O 0.56373(12) 0.71299(11) 0.79073(10) 0.0274(3) Uani 1 1 d . . . O3 O 1.29661(12) 0.83535(11) 0.69816(11) 0.0287(3) Uani 1 1 d . . . O4 O 1.14722(14) 0.96873(12) 0.61068(12) 0.0411(4) Uani 1 1 d . . . O5 O 0.42781(13) 0.09914(10) 0.55542(9) 0.0226(3) Uani 1 1 d . . . O6 O 0.26817(19) 0.70766(17) 1.01424(16) 0.0652(6) Uani 1 1 d . . . O7 O 1.1007(2) 1.25185(16) 0.53597(18) 0.0762(7) Uani 1 1 d . . . O8 O 0.45804(13) 0.45396(10) 0.92592(9) 0.0253(3) Uani 1 1 d . . . O9 O 0.39536(15) 0.53681(10) 0.76287(10) 0.0311(3) Uani 1 1 d . . . O10 O 0.46326(16) 0.29083(11) 0.48030(10) 0.0352(4) Uani 1 1 d . . . N1 N 0.95118(16) 0.50832(15) 0.97724(13) 0.0359(4) Uani 1 1 d . . . N2 N 0.48785(19) -0.00262(13) 0.95571(12) 0.0339(4) Uani 1 1 d . . . C1 C 0.66287(18) 0.78185(14) 0.73691(13) 0.0192(4) Uani 1 1 d . . . C2 C 1.17328(19) 0.87264(15) 0.68008(14) 0.0238(4) Uani 1 1 d . . . C3 C 0.80212(18) 0.75263(15) 0.77134(14) 0.0215(4) Uani 1 1 d . . . C4 C 0.91535(18) 0.82640(15) 0.71758(14) 0.0227(4) Uani 1 1 d . . . H4 H 0.9028 0.8981 0.6619 0.027 Uiso 1 1 calc R . . C5 C 1.04754(18) 0.79431(15) 0.74608(14) 0.0227(4) Uani 1 1 d . . . C6 C 1.06368(19) 0.69048(16) 0.83261(15) 0.0261(5) Uani 1 1 d . . . H6 H 1.1505 0.6694 0.8537 0.031 Uiso 1 1 calc R . . C7 C 0.94927(19) 0.61818(16) 0.88764(15) 0.0257(5) Uani 1 1 d . . . C8 C 0.82184(19) 0.64814(16) 0.85402(15) 0.0260(5) Uani 1 1 d . . . H8 H 0.7484 0.5965 0.8881 0.031 Uiso 1 1 calc R . . C9 C 0.44448(18) 0.20077(14) 0.56390(13) 0.0209(4) Uani 1 1 d . . . C10 C 0.42818(18) 0.44855(14) 0.83716(13) 0.0199(4) Uani 1 1 d . A . C11 C 0.44184(19) 0.20825(14) 0.68428(14) 0.0233(4) Uani 1 1 d . . . C12 C 0.43007(19) 0.31871(15) 0.70849(14) 0.0222(4) Uani 1 1 d . A . H12 H 0.4182 0.3893 0.6514 0.027 Uiso 1 1 calc R . . C13 C 0.43566(19) 0.32607(14) 0.81686(13) 0.0217(4) Uani 1 1 d . . . C14 C 0.4523(2) 0.22203(15) 0.90158(14) 0.0254(4) Uani 1 1 d . A . H14 H 0.4557 0.2261 0.9745 0.031 Uiso 1 1 calc R . . C15 C 0.4642(2) 0.11106(15) 0.87792(14) 0.0288(5) Uani 1 1 d . . . C16 C 0.4567(2) 0.10484(16) 0.77028(14) 0.0293(5) Uani 1 1 d . A . H16 H 0.4618 0.0300 0.7560 0.035 Uiso 1 1 calc R . . N3 N 0.8780(4) 1.3530(4) 0.5254(5) 0.204(2) Uani 1 1 d D . . C17 C 1.0270(5) 1.3312(3) 0.4851(3) 0.1147(14) Uani 1 1 d D . . H17 H 1.0781 1.3802 0.4127 0.138 Uiso 1 1 calc R . . C18 C 0.8156(12) 1.2362(8) 0.5866(8) 0.305(5) Uiso 1 1 d D . . H18A H 0.7430 1.2304 0.5534 0.458 Uiso 1 1 calc R . . H18B H 0.7680 1.2324 0.6709 0.458 Uiso 1 1 calc R . . H18C H 0.8958 1.1705 0.5750 0.458 Uiso 1 1 calc R . . C19 C 0.7932(7) 1.4367(5) 0.4599(5) 0.185(3) Uiso 1 1 d D . . H19A H 0.8593 1.4829 0.3891 0.278 Uiso 1 1 calc R . . H19B H 0.7244 1.4898 0.5083 0.278 Uiso 1 1 calc R . . H19C H 0.7377 1.3948 0.4371 0.278 Uiso 1 1 calc R . . N4 N 0.0734(3) 0.8286(2) 1.10738(19) 0.0687(7) Uani 1 1 d D . . C20A C 0.2171(4) 0.7997(4) 1.0381(4) 0.0395(12) Uani 0.50 1 d PD A 1 H20A H 0.2800 0.8596 1.0071 0.047 Uiso 0.50 1 calc PR A 1 C21A C 0.0216(9) 0.9377(6) 1.1428(6) 0.108(3) Uani 0.50 1 d P A 1 H21A H 0.0998 0.9889 1.1053 0.161 Uiso 0.50 1 calc PR A 1 H21B H -0.0060 0.9224 1.2285 0.161 Uiso 0.50 1 calc PR A 1 H21C H -0.0647 0.9769 1.1191 0.161 Uiso 0.50 1 calc PR A 1 C22A C -0.0254(8) 0.7386(7) 1.1440(7) 0.122(3) Uani 0.50 1 d P A 1 H22A H 0.0158 0.6838 1.0918 0.183 Uiso 0.50 1 calc PR A 1 H22B H -0.1226 0.7773 1.1396 0.183 Uiso 0.50 1 calc PR A 1 H22C H -0.0352 0.6947 1.2250 0.183 Uiso 0.50 1 calc PR A 1 C20B C 0.1526(8) 0.7433(6) 1.0552(5) 0.093(2) Uani 0.50 1 d PD A 2 H20B H 0.0888 0.6969 1.0516 0.111 Uiso 0.50 1 calc PR A 2 C21B C 0.1407(11) 0.9109(9) 1.1395(9) 0.179(4) Uani 0.50 1 d P A 2 H21D H 0.1085 0.8977 1.2253 0.268 Uiso 0.50 1 calc PR A 2 H21E H 0.1085 0.9932 1.1056 0.268 Uiso 0.50 1 calc PR A 2 H21F H 0.2485 0.8950 1.1084 0.268 Uiso 0.50 1 calc PR A 2 C22B C -0.0857(9) 0.8454(14) 1.1602(8) 0.187(6) Uani 0.50 1 d P A 2 H22D H -0.1232 0.7692 1.1844 0.281 Uiso 0.50 1 calc PR A 2 H22E H -0.1291 0.9004 1.1029 0.281 Uiso 0.50 1 calc PR A 2 H22F H -0.1126 0.8781 1.2292 0.281 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0298(14) 0.0213(13) 0.0266(12) -0.0028(11) -0.0094(11) -0.0052(12) Li2 0.0209(12) 0.0200(13) 0.0243(12) 0.0015(10) -0.0096(10) -0.0067(11) Li3 0.0316(15) 0.0260(15) 0.0310(14) 0.0012(12) -0.0098(12) -0.0043(13) Li4 0.0359(14) 0.0225(14) 0.0269(12) -0.0011(11) -0.0150(11) -0.0045(12) O1 0.0265(5) 0.0221(6) 0.0222(5) 0.0037(4) -0.0148(4) -0.0029(5) O2 0.0246(5) 0.0290(6) 0.0306(5) 0.0055(5) -0.0159(4) -0.0123(5) O3 0.0207(5) 0.0252(6) 0.0384(6) 0.0033(5) -0.0135(4) -0.0073(5) O4 0.0339(6) 0.0323(7) 0.0498(7) 0.0222(6) -0.0242(5) -0.0152(6) O5 0.0347(6) 0.0153(5) 0.0220(5) -0.0034(4) -0.0151(4) -0.0025(5) O6 0.0382(9) 0.0748(11) 0.0681(9) -0.0243(8) -0.0077(7) 0.0135(8) O7 0.0776(11) 0.0459(9) 0.0993(12) -0.0225(9) -0.0367(9) 0.0231(9) O8 0.0405(6) 0.0189(5) 0.0222(5) -0.0042(4) -0.0154(4) -0.0069(5) O9 0.0529(6) 0.0158(5) 0.0302(5) 0.0019(4) -0.0246(5) -0.0061(5) O10 0.0686(8) 0.0217(6) 0.0190(5) 0.0012(4) -0.0194(5) -0.0123(6) N1 0.0332(6) 0.0351(8) 0.0379(7) 0.0164(7) -0.0230(5) -0.0154(7) N2 0.0658(9) 0.0182(7) 0.0258(5) -0.0013(5) -0.0288(5) -0.0024(7) C1 0.0204(7) 0.0198(7) 0.0186(6) -0.0024(6) -0.0096(5) -0.0022(6) C2 0.0221(7) 0.0234(8) 0.0259(7) 0.0000(6) -0.0096(6) -0.0080(7) C3 0.0214(7) 0.0224(8) 0.0206(7) 0.0010(6) -0.0107(6) -0.0041(7) C4 0.0254(8) 0.0197(8) 0.0221(7) 0.0020(6) -0.0111(6) -0.0046(7) C5 0.0232(7) 0.0210(8) 0.0235(7) 0.0005(6) -0.0100(6) -0.0060(7) C6 0.0205(7) 0.0262(9) 0.0295(8) 0.0032(7) -0.0128(6) -0.0042(7) C7 0.0260(8) 0.0226(8) 0.0268(7) 0.0077(7) -0.0145(6) -0.0078(7) C8 0.0219(7) 0.0282(9) 0.0279(7) 0.0059(7) -0.0125(6) -0.0127(7) C9 0.0307(8) 0.0155(7) 0.0195(6) -0.0016(6) -0.0141(6) -0.0018(7) C10 0.0248(7) 0.0168(7) 0.0193(7) -0.0023(6) -0.0083(6) -0.0059(6) C11 0.0342(8) 0.0182(7) 0.0210(7) -0.0041(6) -0.0126(6) -0.0048(7) C12 0.0309(8) 0.0155(7) 0.0203(7) 0.0012(6) -0.0120(6) -0.0044(7) C13 0.0309(8) 0.0158(7) 0.0205(7) -0.0030(6) -0.0106(6) -0.0050(7) C14 0.0423(9) 0.0197(8) 0.0184(6) -0.0034(6) -0.0150(6) -0.0048(7) C15 0.0494(9) 0.0176(8) 0.0230(7) -0.0003(6) -0.0189(7) -0.0053(8) C16 0.0523(9) 0.0159(7) 0.0273(7) -0.0040(6) -0.0222(7) -0.0046(7) N3 0.091(2) 0.148(3) 0.303(5) 0.063(3) -0.095(2) 0.013(2) C17 0.155(3) 0.0789(19) 0.134(2) -0.0588(16) -0.080(2) 0.041(2) N4 0.0561(12) 0.0754(13) 0.0761(12) -0.0412(10) -0.0165(10) 0.0102(11) C20A 0.0269(18) 0.037(2) 0.059(2) -0.0181(17) -0.0125(16) -0.0058(17) C21A 0.093(5) 0.106(4) 0.111(4) -0.069(3) -0.013(4) 0.034(4) C22A 0.061(4) 0.154(5) 0.133(5) -0.092(4) 0.049(4) -0.041(4) C20B 0.104(4) 0.109(5) 0.072(3) -0.033(3) -0.046(3) 0.017(4) C21B 0.174(7) 0.198(6) 0.163(7) -0.099(5) 0.049(6) -0.127(5) C22B 0.048(4) 0.390(17) 0.117(6) -0.087(8) -0.005(4) -0.017(7) _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 Li1 O6 1.888(3) . ? Li1 O8 1.956(3) 2_667 ? Li1 O2 1.960(3) . ? Li1 O8 1.982(3) . ? Li1 Li1 2.765(5) 2_667 ? Li1 Li4 3.001(4) . ? Li2 O5 1.919(3) 1_565 ? Li2 O3 1.938(3) 1_455 ? Li2 O1 1.980(3) . ? Li2 O5 2.025(3) 2_666 ? Li2 Li4 2.655(4) . ? Li2 Li2 2.718(5) 2_676 ? Li2 Li3 2.745(4) 2_776 ? Li2 C9 2.771(4) 2_666 ? Li2 Li3 3.040(4) 1_455 ? Li3 O4 1.868(3) . ? Li3 O7 1.885(3) . ? Li3 O1 1.958(3) 2_776 ? Li3 O5 2.075(4) 1_665 ? Li3 Li2 2.745(4) 2_776 ? Li3 Li2 3.040(4) 1_655 ? Li4 O9 1.855(3) . ? Li4 O3 1.938(3) 1_455 ? Li4 O10 1.974(3) 2_666 ? Li4 O2 2.023(4) . ? O1 C1 1.2519(18) . ? O1 Li3 1.958(3) 2_776 ? O2 C1 1.250(2) . ? O3 C2 1.252(2) . ? O3 Li2 1.938(3) 1_655 ? O3 Li4 1.938(3) 1_655 ? O4 C2 1.235(2) . ? O5 C9 1.274(2) . ? O5 Li2 1.919(3) 1_545 ? O5 Li2 2.025(3) 2_666 ? O5 Li3 2.075(4) 1_445 ? O6 C20B 1.080(7) . ? O6 C20A 1.151(5) . ? O7 C17 1.206(4) . ? O8 C10 1.257(2) . ? O8 Li1 1.956(3) 2_667 ? O9 C10 1.2319(19) . ? O10 C9 1.2290(18) . ? O10 Li4 1.974(3) 2_666 ? N1 N1 1.223(3) 2_767 ? N1 C7 1.428(2) . ? N2 N2 1.224(3) 2_657 ? N2 C15 1.419(2) . ? C1 C3 1.498(3) . ? C2 C5 1.516(2) . ? C3 C8 1.369(2) . ? C3 C4 1.388(2) . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 C6 1.383(2) . ? C6 C7 1.385(3) . ? C6 H6 0.9300 . ? C7 C8 1.384(3) . ? C8 H8 0.9300 . ? C9 C11 1.507(3) . ? C9 Li2 2.771(4) 2_666 ? C10 C13 1.507(2) . ? C11 C16 1.374(2) . ? C11 C12 1.381(3) . ? C12 C13 1.390(3) . ? C12 H12 0.9300 . ? C13 C14 1.373(2) . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.384(3) . ? C16 H16 0.9300 . ? N3 C17 1.325(5) . ? N3 C19 1.397(7) . ? N3 C18 1.490(10) . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N4 C20B 1.288(7) . ? N4 C20A 1.357(4) . ? N4 C21A 1.395(8) . ? N4 C22B 1.419(8) . ? N4 C22A 1.439(9) . ? N4 C21B 1.488(12) . ? C20A H20A 0.9300 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C20B H20B 0.9300 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? 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 O6 Li1 O8 106.57(15) . 2_667 ? O6 Li1 O2 109.27(15) . . ? O8 Li1 O2 121.83(17) 2_667 . ? O6 Li1 O8 120.60(18) . . ? O8 Li1 O8 90.79(13) 2_667 . ? O2 Li1 O8 107.69(15) . . ? O6 Li1 Li1 124.51(17) . 2_667 ? O8 Li1 Li1 45.78(10) 2_667 2_667 ? O2 Li1 Li1 126.21(17) . 2_667 ? O8 Li1 Li1 45.00(10) . 2_667 ? O6 Li1 Li4 96.00(14) . . ? O8 Li1 Li4 156.73(14) 2_667 . ? O2 Li1 Li4 41.91(10) . . ? O8 Li1 Li4 82.33(13) . . ? Li1 Li1 Li4 123.64(18) 2_667 . ? O5 Li2 O3 119.50(14) 1_565 1_455 ? O5 Li2 O1 113.68(16) 1_565 . ? O3 Li2 O1 119.23(14) 1_455 . ? O5 Li2 O5 92.90(11) 1_565 2_666 ? O3 Li2 O5 111.53(16) 1_455 2_666 ? O1 Li2 O5 92.30(11) . 2_666 ? O5 Li2 Li4 165.46(17) 1_565 . ? O3 Li2 Li4 46.78(9) 1_455 . ? O1 Li2 Li4 80.52(12) . . ? O5 Li2 Li4 89.46(13) 2_666 . ? O5 Li2 Li2 48.07(9) 1_565 2_676 ? O3 Li2 Li2 128.4(2) 1_455 2_676 ? O1 Li2 Li2 108.27(16) . 2_676 ? O5 Li2 Li2 44.83(9) 2_666 2_676 ? Li4 Li2 Li2 132.56(19) . 2_676 ? O5 Li2 Li3 98.98(12) 1_565 2_776 ? O3 Li2 Li3 139.05(15) 1_455 2_776 ? O1 Li2 Li3 45.48(9) . 2_776 ? O5 Li2 Li3 48.76(10) 2_666 2_776 ? Li4 Li2 Li3 93.36(12) . 2_776 ? Li2 Li2 Li3 67.61(12) 2_676 2_776 ? O5 Li2 C9 114.24(12) 1_565 2_666 ? O3 Li2 C9 88.61(13) 1_455 2_666 ? O1 Li2 C9 95.04(11) . 2_666 ? O5 Li2 C9 25.17(6) 2_666 2_666 ? Li4 Li2 C9 65.39(10) . 2_666 ? Li2 Li2 C9 67.40(12) 2_676 2_666 ? Li3 Li2 C9 61.33(10) 2_776 2_666 ? O5 Li2 Li3 42.39(10) 1_565 1_455 ? O3 Li2 Li3 82.72(12) 1_455 1_455 ? O1 Li2 Li3 155.97(15) . 1_455 ? O5 Li2 Li3 87.77(12) 2_666 1_455 ? Li4 Li2 Li3 123.50(15) . 1_455 ? Li2 Li2 Li3 56.60(11) 2_676 1_455 ? Li3 Li2 Li3 124.22(11) 2_776 1_455 ? C9 Li2 Li3 95.14(12) 2_666 1_455 ? O4 Li3 O7 113.37(16) . . ? O4 Li3 O1 122.10(19) . 2_776 ? O7 Li3 O1 107.77(15) . 2_776 ? O4 Li3 O5 106.62(15) . 1_665 ? O7 Li3 O5 113.7(2) . 1_665 ? O1 Li3 O5 91.43(13) 2_776 1_665 ? O4 Li3 Li2 115.48(15) . 2_776 ? O7 Li3 Li2 130.98(17) . 2_776 ? O1 Li3 Li2 46.14(9) 2_776 2_776 ? O5 Li3 Li2 47.21(10) 1_665 2_776 ? O4 Li3 Li2 71.08(11) . 1_655 ? O7 Li3 Li2 143.5(2) . 1_655 ? O1 Li3 Li2 97.78(12) 2_776 1_655 ? O5 Li3 Li2 38.57(8) 1_665 1_655 ? Li2 Li3 Li2 55.78(11) 2_776 1_655 ? O9 Li4 O3 123.24(17) . 1_455 ? O9 Li4 O10 107.48(16) . 2_666 ? O3 Li4 O10 99.80(13) 1_455 2_666 ? O9 Li4 O2 104.21(14) . . ? O3 Li4 O2 102.87(16) 1_455 . ? O10 Li4 O2 120.58(16) 2_666 . ? O9 Li4 Li2 170.00(17) . . ? O3 Li4 Li2 46.77(9) 1_455 . ? O10 Li4 Li2 77.32(11) 2_666 . ? O2 Li4 Li2 79.95(13) . . ? O9 Li4 Li1 70.89(11) . . ? O3 Li4 Li1 102.84(13) 1_455 . ? O10 Li4 Li1 153.47(16) 2_666 . ? O2 Li4 Li1 40.31(9) . . ? Li2 Li4 Li1 108.90(14) . . ? C1 O1 Li3 126.35(13) . 2_776 ? C1 O1 Li2 121.74(13) . . ? Li3 O1 Li2 88.37(13) 2_776 . ? C1 O2 Li1 145.16(16) . . ? C1 O2 Li4 116.79(13) . . ? Li1 O2 Li4 97.78(14) . . ? C2 O3 Li2 120.63(13) . 1_655 ? C2 O3 Li4 139.03(17) . 1_655 ? Li2 O3 Li4 86.45(13) 1_655 1_655 ? C2 O4 Li3 140.52(17) . . ? C9 O5 Li2 144.36(15) . 1_545 ? C9 O5 Li2 112.28(12) . 2_666 ? Li2 O5 Li2 87.10(11) 1_545 2_666 ? C9 O5 Li3 112.06(13) . 1_445 ? Li2 O5 Li3 99.04(14) 1_545 1_445 ? Li2 O5 Li3 84.03(13) 2_666 1_445 ? C20B O6 C20A 49.4(5) . . ? C20B O6 Li1 168.2(5) . . ? C20A O6 Li1 142.4(3) . . ? C17 O7 Li3 141.2(3) . . ? C10 O8 Li1 151.92(14) . 2_667 ? C10 O8 Li1 117.37(13) . . ? Li1 O8 Li1 89.22(13) 2_667 . ? C10 O9 Li4 136.66(17) . . ? C9 O10 Li4 131.12(14) . 2_666 ? N1 N1 C7 114.8(2) 2_767 . ? N2 N2 C15 114.6(2) 2_657 . ? O2 C1 O1 122.95(16) . . ? O2 C1 C3 118.33(14) . . ? O1 C1 C3 118.71(14) . . ? O4 C2 O3 124.40(16) . . ? O4 C2 C5 117.39(16) . . ? O3 C2 C5 118.21(14) . . ? C8 C3 C4 118.82(16) . . ? C8 C3 C1 119.53(15) . . ? C4 C3 C1 121.59(14) . . ? C3 C4 C5 120.72(15) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.73(16) . . ? C6 C5 C2 120.77(16) . . ? C4 C5 C2 119.49(14) . . ? C5 C6 C7 119.35(17) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.20(15) . . ? C8 C7 N1 114.36(16) . . ? C6 C7 N1 125.40(17) . . ? C3 C8 C7 121.05(16) . . ? C3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? O10 C9 O5 123.87(16) . . ? O10 C9 C11 119.23(16) . . ? O5 C9 C11 116.90(13) . . ? O10 C9 Li2 85.40(12) . 2_666 ? O5 C9 Li2 42.54(9) . 2_666 ? C11 C9 Li2 149.07(12) . 2_666 ? O9 C10 O8 124.79(17) . . ? O9 C10 C13 116.62(16) . . ? O8 C10 C13 118.58(14) . . ? C16 C11 C12 118.85(17) . . ? C16 C11 C9 120.40(16) . . ? C12 C11 C9 120.71(14) . . ? C11 C12 C13 121.03(14) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 119.58(16) . . ? C14 C13 C10 121.37(16) . . ? C12 C13 C10 119.02(14) . . ? C13 C14 C15 119.69(17) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.24(15) . . ? C16 C15 N2 114.66(16) . . ? C14 C15 N2 125.09(17) . . ? C11 C16 C15 120.58(17) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C17 N3 C19 123.7(4) . . ? C17 N3 C18 109.0(5) . . ? C19 N3 C18 113.7(6) . . ? O7 C17 N3 124.3(4) . . ? O7 C17 H17 117.9 . . ? N3 C17 H17 117.9 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20B N4 C20A 41.3(4) . . ? C20B N4 C21A 164.1(5) . . ? C20A N4 C21A 123.3(4) . . ? C20B N4 C22B 126.3(8) . . ? C20A N4 C22B 165.1(6) . . ? C21A N4 C22B 68.2(7) . . ? C20B N4 C22A 74.7(5) . . ? C20A N4 C22A 115.9(4) . . ? C21A N4 C22A 120.9(5) . . ? C22B N4 C22A 53.7(7) . . ? C20B N4 C21B 123.0(6) . . ? C20A N4 C21B 84.2(4) . . ? C21A N4 C21B 45.2(5) . . ? C22B N4 C21B 109.9(7) . . ? C22A N4 C21B 149.5(5) . . ? O6 C20A N4 125.8(4) . . ? O6 C20A H20A 117.1 . . ? N4 C20A H20A 117.1 . . ? N4 C21A H21A 109.5 . . ? N4 C21A H21B 109.5 . . ? N4 C21A H21C 109.5 . . ? N4 C22A H22A 109.5 . . ? N4 C22A H22B 109.5 . . ? N4 C22A H22C 109.5 . . ? O6 C20B N4 141.2(8) . . ? O6 C20B H20B 109.4 . . ? N4 C20B H20B 109.4 . . ? N4 C21B H21D 109.5 . . ? N4 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? N4 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? N4 C22B H22D 109.5 . . ? N4 C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N4 C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.789 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.082