# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Martyn Coles' 'Peter B Hitchcock' 'Majid S Khalaf' _publ_contact_author_name 'Martyn Coles' _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_section_title ; A structural and theoretical evaluation of the bicyclic guanidinate derived from 1,4,6-triazabicyclo[3.3.0]oct-4-ene ; _publ_requested_category FM # Attachment 'mpc-apr-2008.cif' data_(1a)-jul307 _database_code_depnum_ccdc_archive 'CCDC 685440' _audit_creation_date 2007-07-03T11:25:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H27 Li2 N9 S, C4 H8 O' _chemical_formula_sum 'C19 H35 Li2 N9 O S' _chemical_formula_weight 451.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1795(3) _cell_length_b 10.4390(3) _cell_length_c 12.4108(4) _cell_angle_alpha 78.589(2) _cell_angle_beta 67.596(2) _cell_angle_gamma 83.120(2) _cell_volume 1193.74(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15182 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.349492E-1 _diffrn_orient_matrix_ub_12 0.619154E-1 _diffrn_orient_matrix_ub_13 -0.764691E-1 _diffrn_orient_matrix_ub_21 0.464215E-1 _diffrn_orient_matrix_ub_22 0.506185E-1 _diffrn_orient_matrix_ub_23 0.350948E-1 _diffrn_orient_matrix_ub_31 0.89114E-1 _diffrn_orient_matrix_ub_32 -0.563705E-1 _diffrn_orient_matrix_ub_33 -0.270424E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_number 17634 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 4665 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atoms on N were refined. 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^)+(0.0517P)^2^+0.6619P] 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_number_reflns 4665 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.063 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.306 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.042 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.3043(3) 0.4782(3) 0.6189(3) 0.0314(7) Uani 1 1 d . . . Li2 Li 0.5363(3) 0.3208(3) 0.4862(3) 0.0342(7) Uani 1 1 d . . . S S 0.42946(5) 0.11913(5) 0.72575(5) 0.03868(16) Uani 1 1 d . . . N1 N 0.46777(15) 0.53266(15) 0.65540(13) 0.0298(3) Uani 1 1 d . . . N2 N 0.67032(15) 0.40735(15) 0.54207(13) 0.0303(3) Uani 1 1 d . . . N3 N 0.63760(16) 0.43674(16) 0.72986(13) 0.0337(4) Uani 1 1 d . . . N4 N 0.11134(16) 0.48871(16) 0.75270(14) 0.0369(4) Uani 1 1 d . . . N5 N 0.1417(2) 0.29530(19) 0.88496(16) 0.0457(5) Uani 1 1 d . . . H5X H 0.233(3) 0.267(2) 0.839(2) 0.056(7) Uiso 1 1 d . . . N6 N -0.07456(17) 0.37796(17) 0.89437(15) 0.0417(4) Uani 1 1 d . . . N7 N 0.31817(16) 0.28688(15) 0.58455(14) 0.0322(4) Uani 1 1 d . . . N8 N 0.21588(18) 0.09295(15) 0.65291(16) 0.0383(4) Uani 1 1 d . . . N9 N 0.37634(19) -0.15299(18) 0.58471(19) 0.0407(4) Uani 1 1 d . . . H9Y H 0.426(3) -0.134(3) 0.624(2) 0.065(8) Uiso 1 1 d . . . H9X H 0.398(3) -0.093(3) 0.519(3) 0.064(8) Uiso 1 1 d . . . C1 C 0.58899(18) 0.46199(17) 0.63537(15) 0.0280(4) Uani 1 1 d . . . C2 C 0.4247(2) 0.5552(2) 0.77878(17) 0.0381(5) Uani 1 1 d . . . H2B H 0.3212 0.5459 0.8217 0.046 Uiso 1 1 calc R . . H2A H 0.4487 0.6437 0.7805 0.046 Uiso 1 1 calc R . . C3 C 0.5094(2) 0.4497(2) 0.83352(17) 0.0427(5) Uani 1 1 d . . . H3B H 0.5304 0.4791 0.8961 0.051 Uiso 1 1 calc R . . H3A H 0.4593 0.3669 0.8661 0.051 Uiso 1 1 calc R . . C4 C 0.7290(2) 0.3181(2) 0.71276(18) 0.0397(5) Uani 1 1 d . . . H4B H 0.6744 0.2384 0.7512 0.048 Uiso 1 1 calc R . . H4A H 0.8068 0.3167 0.7424 0.048 Uiso 1 1 calc R . . C5 C 0.7851(2) 0.3328(2) 0.57768(18) 0.0398(5) Uani 1 1 d . . . H5B H 0.8738 0.381 0.5418 0.048 Uiso 1 1 calc R . . H5A H 0.8047 0.246 0.5525 0.048 Uiso 1 1 calc R . . C6 C 0.0702(2) 0.3899(2) 0.83564(17) 0.0355(4) Uani 1 1 d . . . C7 C -0.0240(2) 0.5611(2) 0.7532(2) 0.0449(5) Uani 1 1 d . . . H7B H -0.0485 0.5447 0.6874 0.054 Uiso 1 1 calc R . . H7A H -0.016 0.6564 0.7453 0.054 Uiso 1 1 calc R . . C8 C -0.1369(2) 0.5085(2) 0.8728(2) 0.0438(5) Uani 1 1 d . . . H8B H -0.1461 0.5602 0.9343 0.053 Uiso 1 1 calc R . . H8A H -0.2309 0.5061 0.867 0.053 Uiso 1 1 calc R . . C9 C -0.0972(2) 0.2920(3) 1.0060(2) 0.0549(6) Uani 1 1 d . . . H9B H -0.1835 0.2418 1.0314 0.066 Uiso 1 1 calc R . . H9A H -0.1042 0.3408 1.0688 0.066 Uiso 1 1 calc R . . C10 C 0.0383(3) 0.2036(3) 0.9730(2) 0.0582(6) Uani 1 1 d . . . H10B H 0.0657 0.1691 1.0422 0.07 Uiso 1 1 calc R . . H10A H 0.0277 0.1296 0.9383 0.07 Uiso 1 1 calc R . . C11 C 0.2065(2) 0.2911(2) 0.53452(19) 0.0399(5) Uani 1 1 d . . . H11A H 0.2496 0.297 0.4476 0.048 Uiso 1 1 calc R . . H11B H 0.1396 0.3677 0.5534 0.048 Uiso 1 1 calc R . . C12 C 0.1297(2) 0.1651(2) 0.5907(2) 0.0449(5) Uani 1 1 d . . . H12A H 0.0316 0.182 0.6456 0.054 Uiso 1 1 calc R . . H12B H 0.1263 0.118 0.5301 0.054 Uiso 1 1 calc R . . C13 C 0.31663(18) 0.17100(17) 0.65014(15) 0.0285(4) Uani 1 1 d . . . C14 C 0.1790(2) -0.03292(18) 0.72670(18) 0.0372(5) Uani 1 1 d . . . H14B H 0.0748 -0.0325 0.7702 0.045 Uiso 1 1 calc R . . H14A H 0.2252 -0.0475 0.7856 0.045 Uiso 1 1 calc R . . C15 C 0.2240(2) -0.14490(19) 0.65632(18) 0.0379(5) Uani 1 1 d . . . H15B H 0.1984 -0.2283 0.7118 0.046 Uiso 1 1 calc R . . H15A H 0.1698 -0.1349 0.6035 0.046 Uiso 1 1 calc R . . O O 0.8116(2) 0.9561(3) 0.81896(19) 0.1008(8) Uani 1 1 d . A 1 C16 C 0.6729(3) 0.9489(4) 0.9074(2) 0.0802(9) Uani 1 1 d . A 1 H16B H 0.6152 1.0306 0.8976 0.096 Uiso 1 1 calc R A 1 H16A H 0.6773 0.9341 0.9873 0.096 Uiso 1 1 calc R A 1 C17 C 0.6113(4) 0.8353(3) 0.8894(3) 0.0941(12) Uani 1 1 d . A 1 H17B H 0.5069 0.8488 0.9123 0.113 Uiso 1 1 calc R A 1 H17A H 0.6325 0.7532 0.9368 0.113 Uiso 1 1 calc R A 1 C18 C 0.6820(3) 0.8305(3) 0.7598(3) 0.0672(7) Uani 1 1 d . A 1 H18B H 0.7221 0.7414 0.746 0.081 Uiso 1 1 calc R A 1 H18A H 0.6141 0.8578 0.7189 0.081 Uiso 1 1 calc R A 1 C19 C 0.7973(3) 0.9254(3) 0.7189(2) 0.0645(7) Uani 1 1 d . A 1 H19B H 0.888 0.886 0.6689 0.077 Uiso 1 1 calc R A 1 H19A H 0.7725 1.0057 0.6715 0.077 Uiso 1 1 calc R A 1 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 0.0272(15) 0.0332(16) 0.0318(16) -0.0050(12) -0.0089(13) -0.0014(12) Li2 0.0292(16) 0.0314(16) 0.0394(17) -0.0070(13) -0.0100(13) 0.0015(13) S 0.0339(3) 0.0378(3) 0.0455(3) -0.0022(2) -0.0194(2) 0.0026(2) N1 0.0271(8) 0.0343(8) 0.0281(8) -0.0075(6) -0.0095(6) -0.0002(6) N2 0.0281(8) 0.0323(8) 0.0312(8) -0.0056(6) -0.0131(7) 0.0044(6) N3 0.0313(8) 0.0426(9) 0.0300(8) -0.0063(7) -0.0150(7) 0.0002(7) N4 0.0262(8) 0.0417(10) 0.0381(9) -0.0066(7) -0.0073(7) 0.0004(7) N5 0.0370(10) 0.0554(12) 0.0359(9) -0.0075(8) -0.0065(8) 0.0077(8) N6 0.0303(9) 0.0468(10) 0.0422(10) -0.0066(8) -0.0065(7) -0.0041(7) N7 0.0290(8) 0.0310(8) 0.0365(9) -0.0036(7) -0.0133(7) -0.0006(6) N8 0.0397(9) 0.0250(8) 0.0555(11) -0.0040(7) -0.0244(8) -0.0027(7) N9 0.0345(10) 0.0362(10) 0.0458(11) -0.0109(8) -0.0065(8) -0.0016(7) C1 0.0273(9) 0.0285(9) 0.0291(9) -0.0017(7) -0.0119(7) -0.0045(7) C2 0.0299(10) 0.0505(12) 0.0345(10) -0.0147(9) -0.0089(8) -0.0014(9) C3 0.0367(11) 0.0624(14) 0.0307(10) -0.0096(9) -0.0126(9) -0.0051(10) C4 0.0427(11) 0.0406(11) 0.0425(11) -0.0054(9) -0.0255(9) 0.0046(9) C5 0.0375(11) 0.0431(11) 0.0420(11) -0.0105(9) -0.0206(9) 0.0120(9) C6 0.0286(10) 0.0431(11) 0.0348(10) -0.0152(9) -0.0088(8) 0.0027(8) C7 0.0301(10) 0.0440(12) 0.0573(14) -0.0063(10) -0.0140(10) 0.0007(9) C8 0.0265(10) 0.0474(12) 0.0550(13) -0.0149(10) -0.0102(9) 0.0018(9) C9 0.0455(13) 0.0648(16) 0.0416(13) -0.0022(11) -0.0048(10) -0.0038(11) C10 0.0565(15) 0.0591(15) 0.0440(13) 0.0024(11) -0.0093(11) 0.0044(12) C11 0.0450(12) 0.0348(11) 0.0478(12) -0.0057(9) -0.0271(10) 0.0000(9) C12 0.0383(11) 0.0471(13) 0.0535(13) -0.0019(10) -0.0235(10) -0.0057(9) C13 0.0249(9) 0.0274(9) 0.0305(9) -0.0094(7) -0.0066(7) 0.0042(7) C14 0.0335(10) 0.0314(10) 0.0405(11) -0.0069(8) -0.0060(8) -0.0033(8) C15 0.0340(10) 0.0287(10) 0.0459(12) -0.0068(8) -0.0074(9) -0.0056(8) O 0.0509(12) 0.189(3) 0.0673(13) -0.0350(15) -0.0186(10) -0.0112(14) C16 0.0624(18) 0.122(3) 0.0491(16) -0.0167(16) -0.0175(13) 0.0164(18) C17 0.095(2) 0.0609(19) 0.078(2) 0.0026(16) 0.0132(18) -0.0017(17) C18 0.0614(16) 0.0593(16) 0.0764(19) -0.0065(13) -0.0269(14) 0.0119(13) C19 0.0583(16) 0.085(2) 0.0431(14) -0.0051(13) -0.0159(12) 0.0042(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N4 2.040(3) . ? Li1 N1 2.050(3) . ? Li1 N2 2.054(3) 2_666 ? Li1 N7 2.101(3) . ? Li2 N9 2.068(4) 2_656 ? Li2 N1 2.099(4) 2_666 ? Li2 N2 2.103(4) . ? Li2 N7 2.121(3) . ? S C13 1.7217(18) . ? N1 C1 1.323(2) . ? N1 C2 1.483(2) . ? N1 Li2 2.099(4) 2_666 ? N2 C1 1.330(2) . ? N2 C5 1.485(2) . ? N2 Li1 2.054(3) 2_666 ? N3 C1 1.407(2) . ? N3 C4 1.457(2) . ? N3 C3 1.457(2) . ? N4 C6 1.286(3) . ? N4 C7 1.488(2) . ? N5 C6 1.344(3) . ? N5 C10 1.472(3) . ? N5 H5X 0.93(3) . ? N6 C6 1.381(2) . ? N6 C9 1.446(3) . ? N6 C8 1.453(3) . ? N7 C13 1.316(2) . ? N7 C11 1.482(2) . ? N8 C13 1.371(2) . ? N8 C12 1.435(3) . ? N8 C14 1.444(2) . ? N9 C15 1.466(3) . ? N9 Li2 2.068(4) 2_656 ? N9 H9Y 0.88(3) . ? N9 H9X 0.90(3) . ? C2 C3 1.530(3) . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C3 H3B 0.99 . ? C3 H3A 0.99 . ? C4 C5 1.533(3) . ? C4 H4B 0.99 . ? C4 H4A 0.99 . ? C5 H5B 0.99 . ? C5 H5A 0.99 . ? C7 C8 1.534(3) . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 H8B 0.99 . ? C8 H8A 0.99 . ? C9 C10 1.529(3) . ? C9 H9B 0.99 . ? C9 H9A 0.99 . ? C10 H10B 0.99 . ? C10 H10A 0.99 . ? C11 C12 1.514(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C14 C15 1.520(3) . ? C14 H14B 0.99 . ? C14 H14A 0.99 . ? C15 H15B 0.99 . ? C15 H15A 0.99 . ? O C19 1.405(3) . ? O C16 1.420(3) . ? C16 C17 1.496(5) . ? C16 H16B 0.99 . ? C16 H16A 0.99 . ? C17 C18 1.500(4) . ? C17 H17B 0.99 . ? C17 H17A 0.99 . ? C18 C19 1.497(4) . ? C18 H18B 0.99 . ? C18 H18A 0.99 . ? C19 H19B 0.99 . ? C19 H19A 0.99 . ? 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 N4 Li1 N1 113.33(16) . . ? N4 Li1 N2 117.95(15) . 2_666 ? N1 Li1 N2 102.07(14) . 2_666 ? N4 Li1 N7 103.34(14) . . ? N1 Li1 N7 116.98(15) . . ? N2 Li1 N7 103.39(14) 2_666 . ? N9 Li2 N1 106.54(16) 2_656 2_666 ? N9 Li2 N2 114.31(16) 2_656 . ? N1 Li2 N2 98.83(14) 2_666 . ? N9 Li2 N7 105.91(15) 2_656 . ? N1 Li2 N7 103.50(14) 2_666 . ? N2 Li2 N7 125.43(16) . . ? C1 N1 C2 104.63(14) . . ? C1 N1 Li1 121.59(15) . . ? C2 N1 Li1 113.33(14) . . ? C1 N1 Li2 114.56(14) . 2_666 ? C2 N1 Li2 124.08(15) . 2_666 ? Li1 N1 Li2 78.24(13) . 2_666 ? C1 N2 C5 104.50(14) . . ? C1 N2 Li1 114.99(14) . 2_666 ? C5 N2 Li1 126.18(15) . 2_666 ? C1 N2 Li2 107.91(14) . . ? C5 N2 Li2 123.14(15) . . ? Li1 N2 Li2 78.07(13) 2_666 . ? C1 N3 C4 105.12(14) . . ? C1 N3 C3 104.12(15) . . ? C4 N3 C3 124.60(17) . . ? C6 N4 C7 103.69(16) . . ? C6 N4 Li1 119.81(16) . . ? C7 N4 Li1 130.57(16) . . ? C6 N5 C10 108.21(18) . . ? C6 N5 H5X 119.6(15) . . ? C10 N5 H5X 122.0(15) . . ? C6 N6 C9 107.99(17) . . ? C6 N6 C8 104.90(16) . . ? C9 N6 C8 128.51(18) . . ? C13 N7 C11 106.97(15) . . ? C13 N7 Li1 132.76(15) . . ? C11 N7 Li1 102.66(14) . . ? C13 N7 Li2 105.25(14) . . ? C11 N7 Li2 125.82(15) . . ? Li1 N7 Li2 85.19(13) . . ? C13 N8 C12 109.97(15) . . ? C13 N8 C14 126.07(16) . . ? C12 N8 C14 122.76(16) . . ? C15 N9 Li2 119.14(16) . 2_656 ? C15 N9 H9Y 110.1(18) . . ? Li2 N9 H9Y 109.8(18) 2_656 . ? C15 N9 H9X 111.5(17) . . ? Li2 N9 H9X 100.1(17) 2_656 . ? H9Y N9 H9X 105(2) . . ? N1 C1 N2 130.69(16) . . ? N1 C1 N3 114.69(16) . . ? N2 C1 N3 114.58(15) . . ? N1 C2 C3 104.63(15) . . ? N1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? N1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? H2B C2 H2A 108.9 . . ? N3 C3 C2 100.11(15) . . ? N3 C3 H3B 111.8 . . ? C2 C3 H3B 111.8 . . ? N3 C3 H3A 111.8 . . ? C2 C3 H3A 111.8 . . ? H3B C3 H3A 109.5 . . ? N3 C4 C5 100.14(15) . . ? N3 C4 H4B 111.7 . . ? C5 C4 H4B 111.7 . . ? N3 C4 H4A 111.7 . . ? C5 C4 H4A 111.7 . . ? H4B C4 H4A 109.5 . . ? N2 C5 C4 105.38(15) . . ? N2 C5 H5B 110.7 . . ? C4 C5 H5B 110.7 . . ? N2 C5 H5A 110.7 . . ? C4 C5 H5A 110.7 . . ? H5B C5 H5A 108.8 . . ? N4 C6 N5 132.40(18) . . ? N4 C6 N6 117.34(18) . . ? N5 C6 N6 110.10(18) . . ? N4 C7 C8 105.33(17) . . ? N4 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? N4 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? H7B C7 H7A 108.8 . . ? N6 C8 C7 99.68(15) . . ? N6 C8 H8B 111.8 . . ? C7 C8 H8B 111.8 . . ? N6 C8 H8A 111.8 . . ? C7 C8 H8A 111.8 . . ? H8B C8 H8A 109.6 . . ? N6 C9 C10 100.56(17) . . ? N6 C9 H9B 111.7 . . ? C10 C9 H9B 111.7 . . ? N6 C9 H9A 111.7 . . ? C10 C9 H9A 111.7 . . ? H9B C9 H9A 109.4 . . ? N5 C10 C9 101.26(19) . . ? N5 C10 H10B 111.5 . . ? C9 C10 H10B 111.5 . . ? N5 C10 H10A 111.5 . . ? C9 C10 H10A 111.5 . . ? H10B C10 H10A 109.3 . . ? N7 C11 C12 106.11(15) . . ? N7 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? N7 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N8 C12 C11 102.62(16) . . ? N8 C12 H12A 111.2 . . ? C11 C12 H12A 111.2 . . ? N8 C12 H12B 111.2 . . ? C11 C12 H12B 111.2 . . ? H12A C12 H12B 109.2 . . ? N7 C13 N8 113.59(16) . . ? N7 C13 S 124.23(14) . . ? N8 C13 S 122.18(14) . . ? N8 C14 C15 112.63(16) . . ? N8 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? N8 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? H14B C14 H14A 107.8 . . ? N9 C15 C14 114.19(16) . . ? N9 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? N9 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? H15B C15 H15A 107.6 . . ? C19 O C16 105.2(2) . . ? O C16 C17 104.7(3) . . ? O C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? O C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? H16B C16 H16A 108.9 . . ? C16 C17 C18 104.8(2) . . ? C16 C17 H17B 110.8 . . ? C18 C17 H17B 110.8 . . ? C16 C17 H17A 110.8 . . ? C18 C17 H17A 110.8 . . ? H17B C17 H17A 108.9 . . ? C19 C18 C17 103.4(3) . . ? C19 C18 H18B 111.1 . . ? C17 C18 H18B 111.1 . . ? C19 C18 H18A 111.1 . . ? C17 C18 H18A 111.1 . . ? H18B C18 H18A 109 . . ? O C19 C18 108.2(2) . . ? O C19 H19B 110 . . ? C18 C19 H19B 110 . . ? O C19 H19A 110 . . ? C18 C19 H19A 110 . . ? H19B C19 H19A 108.4 . . ? #===END data_(1b)-jul1107 _database_code_depnum_ccdc_archive 'CCDC 685441' _audit_creation_date 2007-07-23T14:52:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C45 H75 Li6 N27, C4 H10 O' _chemical_formula_sum 'C49 H85 Li6 N27 O' _chemical_formula_weight 1110.08 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2908(2) _cell_length_b 15.0897(2) _cell_length_c 15.2485(2) _cell_angle_alpha 68.643(1) _cell_angle_beta 79.395(1) _cell_angle_gamma 88.720(1) _cell_volume 3006.54(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24635 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.427588E-1 _diffrn_orient_matrix_ub_12 0.504594E-1 _diffrn_orient_matrix_ub_13 -0.310028E-1 _diffrn_orient_matrix_ub_21 0.494642E-1 _diffrn_orient_matrix_ub_22 0.229607E-1 _diffrn_orient_matrix_ub_23 -0.600596E-1 _diffrn_orient_matrix_ub_31 -0.28377E-1 _diffrn_orient_matrix_ub_32 -0.44744E-1 _diffrn_orient_matrix_ub_33 -0.239488E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.03 _diffrn_reflns_number 47304 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 11783 _reflns_number_gt 9459 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atoms on N21,N23 and N26 were refined; others were in riding mode. 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^)+(0.0611P)^2^+2.1608P] 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_number_reflns 11783 _refine_ls_number_parameters 770 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.555 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.2849(2) 0.7077(2) 0.2106(2) 0.0302(6) Uani 1 1 d . . . Li2 Li 0.1559(2) 0.7626(2) 0.3579(2) 0.0300(6) Uani 1 1 d . . . Li3 Li 0.1398(2) 0.9254(2) 0.2214(2) 0.0297(6) Uani 1 1 d . . . Li4 Li 0.2680(2) 0.8672(2) 0.0737(2) 0.0291(6) Uani 1 1 d . B . Li5 Li 0.4715(2) 0.7156(2) 0.2946(2) 0.0361(7) Uani 1 1 d . . . Li6 Li 0.3323(2) 0.7683(2) 0.4437(2) 0.0358(7) Uani 1 1 d . . . N1 N 0.35833(10) 0.83747(10) 0.18073(10) 0.0266(3) Uani 1 1 d . . . N2 N 0.25494(10) 0.88017(10) 0.30197(11) 0.0279(3) Uani 1 1 d . . . N3 N 0.38975(10) 0.97176(10) 0.21004(10) 0.0250(3) Uani 1 1 d . . . N4 N 0.06905(10) 0.79825(11) 0.25288(11) 0.0280(3) Uani 1 1 d . . . N5 N 0.17238(10) 0.75308(10) 0.13334(11) 0.0282(3) Uani 1 1 d . . . N6 N 0.01027(10) 0.72529(11) 0.16462(12) 0.0315(3) Uani 1 1 d . . . N7 N 0.36923(12) 0.61826(12) 0.16551(13) 0.0380(4) Uani 1 1 d . . . N8 N 0.51651(11) 0.64011(11) 0.21203(12) 0.0339(4) Uani 1 1 d . . . N9 N 0.47853(12) 0.50209(12) 0.19337(14) 0.0408(4) Uani 1 1 d . . . N10 N 0.21648(11) 0.64133(11) 0.35105(12) 0.0321(4) Uani 1 1 d . . . N11 N 0.36091(10) 0.65287(10) 0.40628(11) 0.0286(3) Uani 1 1 d . . . N12 N 0.27771(14) 0.51068(13) 0.45227(17) 0.0607(6) Uani 1 1 d . . . N13 N 0.56633(11) 0.76628(11) 0.34758(11) 0.0325(4) Uani 1 1 d . . . N14 N 0.45424(11) 0.81241(12) 0.46035(12) 0.0370(4) Uani 1 1 d . . . N15 N 0.61494(11) 0.84519(13) 0.43615(12) 0.0383(4) Uani 1 1 d . . . N16 N 0.08152(11) 0.74695(13) 0.49045(12) 0.0388(4) Uani 1 1 d . . . N17 N 0.22402(11) 0.75502(12) 0.55079(12) 0.0366(4) Uani 1 1 d . . . N18 N 0.08801(13) 0.67291(13) 0.65013(12) 0.0438(4) Uani 1 1 d . . . N19 N 0.19819(10) 0.98801(10) 0.07314(10) 0.0275(3) Uani 1 1 d . . . N20 N 0.18889(11) 1.14493(11) -0.01918(11) 0.0338(4) Uani 1 1 d . . . N21 N 0.31136(12) 1.11257(11) 0.05667(12) 0.0353(4) Uani 1 1 d . . . H21X H 0.3434(17) 1.0809(17) 0.1013(17) 0.045(6) Uiso 1 1 d . . . N22 N 0.32094(11) 0.87444(12) -0.06135(11) 0.0338(4) Uani 1 1 d . . . N23 N 0.41916(17) 0.73891(17) -0.03189(16) 0.0617(6) Uani 1 1 d . . . H23X H 0.4047(19) 0.7109(19) 0.032(2) 0.061(8) Uiso 1 1 d . . . N25 N 0.04343(12) 1.01488(12) 0.25224(13) 0.0408(4) Uani 1 1 d . . . N26 N -0.01576(13) 0.92769(15) 0.42013(13) 0.0449(4) Uani 1 1 d . . . H26X H 0.0219(17) 0.8775(17) 0.4351(16) 0.044(6) Uiso 1 1 d . . . N27 N -0.10123(12) 1.03914(14) 0.33127(14) 0.0466(5) Uani 1 1 d . . . C1 C 0.32982(11) 0.89050(12) 0.23234(12) 0.0229(3) Uani 1 1 d . . . C2 C 0.45058(12) 0.88406(13) 0.11927(13) 0.0294(4) Uani 1 1 d . . . H2B H 0.4419 0.9218 0.0532 0.035 Uiso 1 1 calc R . . H2A H 0.4981 0.8358 0.1168 0.035 Uiso 1 1 calc R . . C3 C 0.48297(12) 0.94888(13) 0.16663(13) 0.0287(4) Uani 1 1 d . . . H3B H 0.5213 0.9149 0.2156 0.034 Uiso 1 1 calc R . . H3A H 0.5196 1.0066 0.1188 0.034 Uiso 1 1 calc R . . C4 C 0.37116(13) 0.99749(14) 0.29529(13) 0.0319(4) Uani 1 1 d . . . H4B H 0.3776 1.0672 0.2782 0.038 Uiso 1 1 calc R . . H4A H 0.4138 0.9654 0.3406 0.038 Uiso 1 1 calc R . . C5 C 0.26688(13) 0.95942(13) 0.33617(14) 0.0330(4) Uani 1 1 d . . . H5B H 0.2543 0.9358 0.4071 0.04 Uiso 1 1 calc R . . H5A H 0.2226 1.0102 0.3124 0.04 Uiso 1 1 calc R . . C6 C 0.08969(12) 0.76214(12) 0.18477(13) 0.0257(4) Uani 1 1 d . . . C7 C -0.03593(13) 0.78256(15) 0.28491(14) 0.0355(4) Uani 1 1 d . . . H7B H -0.0685 0.8419 0.2561 0.043 Uiso 1 1 calc R . . H7A H -0.0535 0.7612 0.3556 0.043 Uiso 1 1 calc R . . C8 C -0.06313(13) 0.70522(15) 0.25017(15) 0.0397(5) Uani 1 1 d . . . H8B H -0.0591 0.6405 0.2978 0.048 Uiso 1 1 calc R . . H8A H -0.1278 0.7127 0.2347 0.048 Uiso 1 1 calc R . . C9 C 0.04761(15) 0.65740(15) 0.12125(17) 0.0416(5) Uani 1 1 d . . . H9B H 0.0096 0.653 0.0747 0.05 Uiso 1 1 calc R . . H9A H 0.0512 0.5933 0.17 0.05 Uiso 1 1 calc R . . C10 C 0.14690(14) 0.70487(15) 0.07151(16) 0.0380(5) Uani 1 1 d . . . H10B H 0.1935 0.6566 0.0663 0.046 Uiso 1 1 calc R . . H10A H 0.1453 0.7515 0.0064 0.046 Uiso 1 1 calc R . . C11 C 0.45378(13) 0.59424(13) 0.18928(13) 0.0300(4) Uani 1 1 d . . . C12 C 0.32909(16) 0.53143(16) 0.1596(2) 0.0498(6) Uani 1 1 d . . . H12B H 0.3356 0.5371 0.092 0.06 Uiso 1 1 calc R . . H12A H 0.2608 0.5202 0.1902 0.06 Uiso 1 1 calc R . . C13 C 0.38797(17) 0.45045(16) 0.2138(2) 0.0546(6) Uani 1 1 d . . . H13B H 0.3614 0.4238 0.2834 0.066 Uiso 1 1 calc R . . H13A H 0.3931 0.3987 0.188 0.066 Uiso 1 1 calc R . . C14 C 0.54858(18) 0.47608(17) 0.2547(2) 0.0624(7) Uani 1 1 d . . . H14B H 0.5957 0.4338 0.2363 0.075 Uiso 1 1 calc R . . H14A H 0.5184 0.4449 0.323 0.075 Uiso 1 1 calc R . . C15 C 0.59342(16) 0.57343(15) 0.23415(19) 0.0470(5) Uani 1 1 d . . . H15B H 0.6171 0.5748 0.2907 0.056 Uiso 1 1 calc R . . H15A H 0.6473 0.59 0.179 0.056 Uiso 1 1 calc R . . C16 C 0.28586(13) 0.60873(13) 0.39914(14) 0.0319(4) Uani 1 1 d . . . C17 C 0.15115(16) 0.55755(15) 0.37593(18) 0.0492(6) Uani 1 1 d . . . H17B H 0.152 0.5398 0.3194 0.059 Uiso 1 1 calc R . . H17A H 0.0851 0.5713 0.399 0.059 Uiso 1 1 calc R . . C18 C 0.18731(19) 0.47834(18) 0.4542(2) 0.0715(9) Uani 1 1 d . . . H18B H 0.1458 0.4667 0.5173 0.086 Uiso 1 1 calc R . . H18A H 0.1898 0.4186 0.4411 0.086 Uiso 1 1 calc R . . C19 C 0.34194(18) 0.49155(17) 0.5134(2) 0.0648(8) Uani 1 1 d . . . H19B H 0.3767 0.4339 0.514 0.078 Uiso 1 1 calc R . . H19A H 0.309 0.4817 0.5796 0.078 Uiso 1 1 calc R . . C20 C 0.40876(15) 0.57770(14) 0.47413(16) 0.0416(5) Uani 1 1 d . . . H20B H 0.4207 0.5977 0.5263 0.05 Uiso 1 1 calc R . . H20A H 0.4704 0.5643 0.4406 0.05 Uiso 1 1 calc R . . C21 C 0.53914(13) 0.80534(13) 0.41229(13) 0.0299(4) Uani 1 1 d . . . C22 C 0.67081(14) 0.77554(16) 0.32770(15) 0.0392(5) Uani 1 1 d . . . H22B H 0.6943 0.8287 0.2664 0.047 Uiso 1 1 calc R . . H22A H 0.6985 0.716 0.3238 0.047 Uiso 1 1 calc R . . C23 C 0.69751(15) 0.79538(19) 0.41172(18) 0.0497(6) Uani 1 1 d . . . H23B H 0.7044 0.7357 0.4655 0.06 Uiso 1 1 calc R . . H23A H 0.7569 0.836 0.3919 0.06 Uiso 1 1 calc R . . C24 C 0.57794(17) 0.84446(19) 0.53151(17) 0.0506(6) Uani 1 1 d . . . H24B H 0.6069 0.8972 0.543 0.061 Uiso 1 1 calc R . . H24A H 0.5874 0.783 0.5818 0.061 Uiso 1 1 calc R . . C25 C 0.47268(16) 0.85858(18) 0.52565(17) 0.0463(5) Uani 1 1 d . . . H25B H 0.4318 0.8285 0.5897 0.056 Uiso 1 1 calc R . . H25A H 0.4602 0.9272 0.5001 0.056 Uiso 1 1 calc R . . C26 C 0.13505(13) 0.73020(13) 0.55684(13) 0.0311(4) Uani 1 1 d . . . C27 C -0.00633(17) 0.68663(19) 0.54017(16) 0.0539(6) Uani 1 1 d . . . H27B H -0.0237 0.6518 0.5011 0.065 Uiso 1 1 calc R . . H27A H -0.0599 0.7259 0.5523 0.065 Uiso 1 1 calc R . . C28 C 0.01600(19) 0.61703(19) 0.63449(18) 0.0606(7) Uani 1 1 d . . . H28B H -0.0407 0.6011 0.6867 0.073 Uiso 1 1 calc R . . H28A H 0.0414 0.5577 0.628 0.073 Uiso 1 1 calc R . . C29 C 0.1646(2) 0.6311(2) 0.70056(18) 0.0649(7) Uani 1 1 d . . . H29B H 0.1831 0.5705 0.6926 0.078 Uiso 1 1 calc R . . H29A H 0.1473 0.6203 0.7697 0.078 Uiso 1 1 calc R . . C30 C 0.24337(16) 0.70992(18) 0.64848(15) 0.0487(6) Uani 1 1 d . . . H30B H 0.2406 0.7567 0.6805 0.058 Uiso 1 1 calc R . . H30A H 0.3071 0.6827 0.6472 0.058 Uiso 1 1 calc R . . C31 C 0.23409(12) 1.07529(13) 0.04243(12) 0.0275(4) Uani 1 1 d . . . C32 C 0.11781(13) 0.99625(14) 0.02116(14) 0.0326(4) Uani 1 1 d . . . H32B H 0.0559 0.9901 0.0651 0.039 Uiso 1 1 calc R . . H32A H 0.1193 0.9459 -0.0063 0.039 Uiso 1 1 calc R . . C33 C 0.13178(14) 1.09564(14) -0.05906(14) 0.0370(4) Uani 1 1 d . . . H33B H 0.1665 1.0931 -0.1205 0.044 Uiso 1 1 calc R . . H33A H 0.0702 1.1256 -0.0685 0.044 Uiso 1 1 calc R . . C34 C 0.25646(15) 1.22580(14) -0.07089(15) 0.0401(5) Uani 1 1 d . . . H34B H 0.2241 1.2868 -0.0864 0.048 Uiso 1 1 calc R . . H34A H 0.293 1.2211 -0.1307 0.048 Uiso 1 1 calc R . . C35 C 0.32035(14) 1.21563(13) 0.00202(14) 0.0357(4) Uani 1 1 d . . . H35B H 0.3871 1.2369 -0.03 0.043 Uiso 1 1 calc R . . H35A H 0.2971 1.252 0.0435 0.043 Uiso 1 1 calc R . . C36 C 0.37394(17) 0.81338(17) -0.08288(15) 0.0479(5) Uani 1 1 d . B . C41 C -0.01761(14) 0.99046(15) 0.33178(15) 0.0375(5) Uani 1 1 d . . . C42 C -0.00326(19) 1.09351(18) 0.18521(18) 0.0567(6) Uani 1 1 d . . . H42B H -0.0342 1.0698 0.1444 0.068 Uiso 1 1 calc R . . H42A H 0.044 1.1456 0.1434 0.068 Uiso 1 1 calc R . . C43 C -0.07740(17) 1.12827(18) 0.24988(18) 0.0526(6) Uani 1 1 d . . . H43B H -0.0499 1.1775 0.2677 0.063 Uiso 1 1 calc R . . H43A H -0.1332 1.1531 0.22 0.063 Uiso 1 1 calc R . . C44 C -0.13938(17) 1.0294(2) 0.42955(18) 0.0552(6) Uani 1 1 d . . . H44B H -0.2099 1.0291 0.442 0.066 Uiso 1 1 calc R . . H44A H -0.1137 1.0809 0.4455 0.066 Uiso 1 1 calc R . . C45 C -0.10385(16) 0.93318(19) 0.48454(17) 0.0524(6) Uani 1 1 d . . . H45B H -0.0908 0.9306 0.5469 0.063 Uiso 1 1 calc R . . H45A H -0.1505 0.8809 0.4957 0.063 Uiso 1 1 calc R . . O O 0.18534(15) 1.34352(15) 0.1432(2) 0.0819(6) Uani 1 1 d . A 1 C46 C 0.1679(3) 1.2621(4) 0.2270(3) 0.1287(19) Uani 1 1 d . A 1 H46B H 0.1127 1.2735 0.2707 0.154 Uiso 1 1 calc R A 1 H46A H 0.1486 1.2089 0.2098 0.154 Uiso 1 1 calc R A 1 C47 C 0.2408(2) 1.2322(2) 0.2779(3) 0.1019(13) Uani 1 1 d . A 1 H47C H 0.2964 1.2198 0.2364 0.153 Uiso 1 1 calc R A 1 H47B H 0.2196 1.1737 0.3334 0.153 Uiso 1 1 calc R A 1 H47A H 0.2581 1.282 0.2999 0.153 Uiso 1 1 calc R A 1 C48 C 0.1177(3) 1.3771(6) 0.0912(4) 0.161(3) Uani 1 1 d . A 1 H48B H 0.0633 1.3942 0.1315 0.194 Uiso 1 1 calc R A 1 H48A H 0.0946 1.3256 0.0735 0.194 Uiso 1 1 calc R A 1 C49 C 0.1494(4) 1.4620(3) 0.0017(4) 0.1217(16) Uani 1 1 d . A 1 H49C H 0.1695 1.5146 0.0185 0.183 Uiso 1 1 calc R A 1 H49B H 0.0965 1.4814 -0.033 0.183 Uiso 1 1 calc R A 1 H49A H 0.203 1.4458 -0.0391 0.183 Uiso 1 1 calc R A 1 C37 C 0.29688(14) 0.93819(16) -0.15323(14) 0.0396(5) Uani 0.505(11) 1 d P B 1 H37A H 0.3169 1.005 -0.1668 0.048 Uiso 0.505(11) 1 calc PR B 1 H37B H 0.2273 0.9345 -0.151 0.048 Uiso 0.505(11) 1 calc PR B 1 C38 C 0.35116(16) 0.90344(17) -0.23065(15) 0.0455(5) Uani 0.505(11) 1 d P B 1 H38A H 0.3118 0.9053 -0.2783 0.055 Uiso 0.505(11) 1 calc PR B 1 H38B H 0.4115 0.9415 -0.2641 0.055 Uiso 0.505(11) 1 calc PR B 1 C39 C 0.45156(18) 0.75308(19) -0.19172(18) 0.0545(6) Uani 0.505(11) 1 d P B 1 H39A H 0.5078 0.7965 -0.2286 0.065 Uiso 0.505(11) 1 calc PR B 1 H39B H 0.4384 0.7135 -0.2279 0.065 Uiso 0.505(11) 1 calc PR B 1 C40 C 0.4683(3) 0.6911(3) -0.0932(2) 0.1012(14) Uani 0.505(11) 1 d P B 1 H40A H 0.4409 0.6256 -0.0739 0.121 Uiso 0.505(11) 1 calc PR B 1 H40B H 0.5372 0.6883 -0.0912 0.121 Uiso 0.505(11) 1 calc PR B 1 N24 N 0.3685(5) 0.8072(3) -0.1737(3) 0.0400(15) Uani 0.505(11) 1 d P B 1 C37A C 0.29688(14) 0.93819(16) -0.15323(14) 0.0396(5) Uani 0.495(11) 1 d P B 2 H37C H 0.3169 1.005 -0.1668 0.048 Uiso 0.495(11) 1 calc PR B 2 H37D H 0.2273 0.9345 -0.151 0.048 Uiso 0.495(11) 1 calc PR B 2 C38A C 0.35116(16) 0.90344(17) -0.23065(15) 0.0455(5) Uani 0.495(11) 1 d P B 2 H38C H 0.308 0.8677 -0.2512 0.055 Uiso 0.495(11) 1 calc PR B 2 H38D H 0.3836 0.9573 -0.2873 0.055 Uiso 0.495(11) 1 calc PR B 2 C39A C 0.45156(18) 0.75308(19) -0.19172(18) 0.0545(6) Uani 0.495(11) 1 d P B 2 H39C H 0.5111 0.7646 -0.24 0.065 Uiso 0.495(11) 1 calc PR B 2 H39D H 0.4024 0.7229 -0.2113 0.065 Uiso 0.495(11) 1 calc PR B 2 C40A C 0.4683(3) 0.6911(3) -0.0932(2) 0.1012(14) Uani 0.495(11) 1 d P B 2 H40C H 0.4409 0.6256 -0.0739 0.121 Uiso 0.495(11) 1 calc PR B 2 H40D H 0.5372 0.6883 -0.0912 0.121 Uiso 0.495(11) 1 calc PR B 2 N24A N 0.4191(4) 0.8423(4) -0.1814(3) 0.0396(16) Uani 0.495(11) 1 d P B 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 0.0254(15) 0.0270(15) 0.0390(17) -0.0124(13) -0.0074(13) 0.0008(12) Li2 0.0260(15) 0.0299(16) 0.0295(15) -0.0059(13) -0.0040(12) -0.0032(12) Li3 0.0284(15) 0.0285(15) 0.0288(15) -0.0084(13) -0.0012(12) 0.0016(12) Li4 0.0280(15) 0.0291(15) 0.0295(15) -0.0112(13) -0.0024(12) 0.0005(12) Li5 0.0363(17) 0.0361(17) 0.0379(18) -0.0171(15) -0.0040(14) -0.0030(14) Li6 0.0292(16) 0.0393(18) 0.0389(18) -0.0165(15) -0.0016(13) -0.0013(13) N1 0.0230(7) 0.0268(8) 0.0290(8) -0.0114(6) 0.0005(6) -0.0023(6) N2 0.0257(7) 0.0276(8) 0.0296(8) -0.0130(6) 0.0022(6) -0.0026(6) N3 0.0236(7) 0.0240(7) 0.0268(7) -0.0087(6) -0.0043(6) -0.0033(6) N4 0.0222(7) 0.0304(8) 0.0288(8) -0.0080(6) -0.0047(6) 0.0010(6) N5 0.0246(7) 0.0284(8) 0.0336(8) -0.0132(7) -0.0068(6) 0.0008(6) N6 0.0241(8) 0.0318(8) 0.0401(9) -0.0132(7) -0.0092(7) -0.0017(6) N7 0.0348(9) 0.0330(9) 0.0545(11) -0.0234(8) -0.0141(8) 0.0076(7) N8 0.0344(9) 0.0316(8) 0.0396(9) -0.0164(7) -0.0101(7) 0.0056(7) N9 0.0372(9) 0.0297(9) 0.0630(12) -0.0241(8) -0.0135(8) 0.0080(7) N10 0.0267(8) 0.0272(8) 0.0401(9) -0.0065(7) -0.0122(7) -0.0019(6) N11 0.0257(8) 0.0242(8) 0.0332(8) -0.0049(6) -0.0109(6) 0.0020(6) N12 0.0523(12) 0.0261(9) 0.0877(16) 0.0115(10) -0.0405(11) -0.0101(8) N13 0.0289(8) 0.0367(9) 0.0322(8) -0.0138(7) -0.0039(6) -0.0028(7) N14 0.0309(9) 0.0448(10) 0.0423(9) -0.0245(8) -0.0057(7) 0.0002(7) N15 0.0313(9) 0.0467(10) 0.0433(10) -0.0221(8) -0.0101(7) -0.0037(7) N16 0.0304(9) 0.0473(10) 0.0306(9) -0.0066(8) -0.0011(7) -0.0093(7) N17 0.0294(8) 0.0451(10) 0.0321(9) -0.0113(8) -0.0045(7) 0.0052(7) N18 0.0447(10) 0.0480(11) 0.0280(9) -0.0035(8) -0.0012(7) -0.0074(8) N19 0.0259(7) 0.0272(8) 0.0277(8) -0.0082(6) -0.0047(6) 0.0010(6) N20 0.0333(8) 0.0289(8) 0.0333(8) -0.0032(7) -0.0094(7) 0.0024(6) N21 0.0360(9) 0.0276(8) 0.0379(9) -0.0037(7) -0.0131(7) -0.0030(7) N22 0.0319(8) 0.0395(9) 0.0316(8) -0.0171(7) -0.0014(7) -0.0007(7) N23 0.0769(15) 0.0659(14) 0.0391(11) -0.0210(11) -0.0028(10) 0.0308(12) N25 0.0382(9) 0.0399(10) 0.0419(10) -0.0161(8) -0.0006(8) 0.0099(7) N26 0.0419(10) 0.0515(12) 0.0409(10) -0.0208(9) 0.0014(8) 0.0050(9) N27 0.0339(9) 0.0628(12) 0.0538(11) -0.0363(10) -0.0049(8) 0.0125(8) C1 0.0217(8) 0.0214(8) 0.0240(8) -0.0056(7) -0.0055(6) -0.0009(6) C2 0.0241(9) 0.0330(10) 0.0277(9) -0.0101(8) 0.0017(7) -0.0028(7) C3 0.0214(8) 0.0326(10) 0.0280(9) -0.0071(8) -0.0025(7) -0.0046(7) C4 0.0353(10) 0.0312(10) 0.0335(10) -0.0163(8) -0.0075(8) -0.0015(8) C5 0.0348(10) 0.0317(10) 0.0349(10) -0.0177(8) -0.0013(8) 0.0003(8) C6 0.0248(9) 0.0192(8) 0.0298(9) -0.0028(7) -0.0096(7) -0.0002(6) C7 0.0233(9) 0.0458(11) 0.0328(10) -0.0098(9) -0.0038(8) 0.0010(8) C8 0.0243(9) 0.0436(12) 0.0451(12) -0.0088(10) -0.0064(8) -0.0042(8) C9 0.0374(11) 0.0395(11) 0.0565(13) -0.0247(10) -0.0147(10) -0.0018(9) C10 0.0338(10) 0.0403(11) 0.0487(12) -0.0252(10) -0.0108(9) 0.0015(8) C11 0.0339(10) 0.0266(9) 0.0307(9) -0.0132(8) -0.0037(8) 0.0053(7) C12 0.0383(12) 0.0431(12) 0.0819(17) -0.0365(12) -0.0173(11) 0.0040(9) C13 0.0464(13) 0.0345(12) 0.0883(19) -0.0291(12) -0.0122(12) 0.0014(10) C14 0.0551(15) 0.0357(12) 0.101(2) -0.0207(13) -0.0358(15) 0.0152(11) C15 0.0424(12) 0.0412(12) 0.0649(15) -0.0230(11) -0.0222(11) 0.0123(9) C16 0.0311(10) 0.0225(9) 0.0371(10) -0.0030(8) -0.0101(8) -0.0008(7) C17 0.0397(12) 0.0345(11) 0.0676(15) -0.0051(11) -0.0232(11) -0.0085(9) C18 0.0523(15) 0.0372(13) 0.105(2) 0.0088(14) -0.0376(15) -0.0143(11) C19 0.0518(14) 0.0385(13) 0.0829(19) 0.0143(12) -0.0364(14) -0.0047(11) C20 0.0380(11) 0.0315(10) 0.0491(12) -0.0017(9) -0.0208(9) 0.0026(8) C21 0.0300(9) 0.0283(9) 0.0308(9) -0.0084(8) -0.0090(8) -0.0029(7) C22 0.0303(10) 0.0435(12) 0.0401(11) -0.0146(9) 0.0016(8) -0.0058(8) C23 0.0293(11) 0.0686(16) 0.0600(14) -0.0321(13) -0.0118(10) 0.0011(10) C24 0.0497(13) 0.0681(16) 0.0497(13) -0.0354(12) -0.0189(11) 0.0045(11) C25 0.0442(12) 0.0568(14) 0.0498(13) -0.0332(11) -0.0090(10) 0.0025(10) C26 0.0326(10) 0.0298(9) 0.0273(9) -0.0095(8) 0.0011(7) 0.0012(7) C27 0.0449(13) 0.0632(15) 0.0414(12) -0.0062(11) -0.0023(10) -0.0239(11) C28 0.0644(16) 0.0543(15) 0.0456(14) -0.0002(12) -0.0022(12) -0.0253(12) C29 0.0697(17) 0.0693(18) 0.0394(13) 0.0019(12) -0.0161(12) 0.0024(14) C30 0.0420(12) 0.0649(15) 0.0377(12) -0.0154(11) -0.0121(9) 0.0109(11) C31 0.0264(9) 0.0290(9) 0.0234(8) -0.0070(7) -0.0018(7) 0.0039(7) C32 0.0281(9) 0.0352(10) 0.0346(10) -0.0115(8) -0.0086(8) 0.0018(8) C33 0.0361(11) 0.0389(11) 0.0357(10) -0.0098(9) -0.0140(8) 0.0055(8) C34 0.0491(12) 0.0271(10) 0.0353(11) -0.0012(8) -0.0078(9) -0.0013(9) C35 0.0362(10) 0.0283(10) 0.0367(10) -0.0074(8) -0.0015(8) -0.0026(8) C36 0.0564(14) 0.0566(14) 0.0320(11) -0.0209(10) -0.0029(10) 0.0109(11) C41 0.0326(10) 0.0429(11) 0.0442(12) -0.0253(10) -0.0055(9) 0.0054(8) C42 0.0611(15) 0.0541(14) 0.0522(14) -0.0197(12) -0.0064(12) 0.0260(12) C43 0.0484(13) 0.0540(14) 0.0638(15) -0.0311(13) -0.0138(11) 0.0213(11) C44 0.0379(12) 0.0810(18) 0.0617(15) -0.0484(14) -0.0002(11) 0.0073(12) C45 0.0428(13) 0.0746(17) 0.0467(13) -0.0362(13) 0.0052(10) -0.0089(11) O 0.0681(13) 0.0608(12) 0.129(2) -0.0484(14) -0.0203(13) 0.0088(10) C46 0.061(2) 0.226(6) 0.063(2) -0.021(3) 0.0130(18) -0.016(3) C47 0.070(2) 0.063(2) 0.132(3) -0.003(2) 0.011(2) -0.0054(16) C48 0.081(3) 0.290(8) 0.097(3) -0.049(4) -0.028(3) 0.036(4) C49 0.166(4) 0.080(3) 0.153(4) -0.059(3) -0.082(4) 0.031(3) C37 0.0308(10) 0.0528(13) 0.0360(11) -0.0178(10) -0.0046(8) 0.0008(9) C38 0.0439(12) 0.0599(14) 0.0343(11) -0.0203(11) -0.0044(9) -0.0015(10) C39 0.0598(15) 0.0610(15) 0.0508(14) -0.0362(12) 0.0023(11) 0.0057(12) C40 0.147(3) 0.103(3) 0.0533(17) -0.0374(18) -0.0054(19) 0.072(3) N24 0.042(3) 0.047(2) 0.0342(19) -0.0238(17) 0.0048(17) -0.009(2) C37A 0.0308(10) 0.0528(13) 0.0360(11) -0.0178(10) -0.0046(8) 0.0008(9) C38A 0.0439(12) 0.0599(14) 0.0343(11) -0.0203(11) -0.0044(9) -0.0015(10) C39A 0.0598(15) 0.0610(15) 0.0508(14) -0.0362(12) 0.0023(11) 0.0057(12) C40A 0.147(3) 0.103(3) 0.0533(17) -0.0374(18) -0.0054(19) 0.072(3) N24A 0.034(3) 0.056(3) 0.0320(19) -0.0228(18) -0.0012(16) 0.001(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N7 2.010(3) . ? Li1 N10 2.063(4) . ? Li1 N1 2.100(3) . ? Li1 N5 2.122(3) . ? Li1 Li4 2.591(4) . ? Li1 C16 2.717(4) . ? Li1 Li2 2.982(4) . ? Li1 Li5 3.185(4) . ? Li2 N10 2.035(3) . ? Li2 N16 2.036(3) . ? Li2 N2 2.108(3) . ? Li2 N4 2.114(3) . ? Li2 Li3 2.617(4) . ? Li2 Li6 3.062(4) . ? Li3 N25 2.020(3) . ? Li3 N4 2.043(3) . ? Li3 N19 2.118(3) . ? Li3 N2 2.183(3) . ? Li3 C1 2.778(3) . ? Li3 Li4 3.008(4) . ? Li4 N22 2.023(3) . ? Li4 N5 2.042(3) . ? Li4 N19 2.056(3) . ? Li4 N1 2.179(3) . ? Li5 N13 1.994(4) . ? Li5 N8 2.002(4) . ? Li5 N11 2.049(4) . ? Li5 C20 2.768(4) . ? Li5 Li6 3.057(5) . ? Li6 N14 1.971(4) . ? Li6 N17 1.987(4) . ? Li6 N11 2.032(4) . ? Li6 N2 2.624(4) . ? N1 C1 1.324(2) . ? N1 C2 1.489(2) . ? N2 C1 1.329(2) . ? N2 C5 1.492(2) . ? N3 C1 1.410(2) . ? N3 C4 1.465(2) . ? N3 C3 1.467(2) . ? N4 C6 1.325(2) . ? N4 C7 1.486(2) . ? N5 C6 1.327(2) . ? N5 C10 1.479(2) . ? N6 C6 1.405(2) . ? N6 C9 1.453(3) . ? N6 C8 1.455(3) . ? N7 C11 1.330(2) . ? N7 C12 1.481(3) . ? N8 C11 1.312(2) . ? N8 C15 1.474(3) . ? N9 C11 1.409(2) . ? N9 C14 1.445(3) . ? N9 C13 1.449(3) . ? N10 C16 1.321(2) . ? N10 C17 1.479(2) . ? N11 C16 1.316(2) . ? N11 C20 1.482(2) . ? N12 C19 1.379(3) . ? N12 C18 1.383(3) . ? N12 C16 1.400(2) . ? N13 C21 1.321(2) . ? N13 C22 1.467(2) . ? N14 C21 1.321(2) . ? N14 C25 1.468(3) . ? N15 C21 1.415(2) . ? N15 C23 1.449(3) . ? N15 C24 1.449(3) . ? N16 C26 1.328(3) . ? N16 C27 1.476(3) . ? N17 C26 1.311(2) . ? N17 C30 1.471(3) . ? N18 C26 1.415(2) . ? N18 C28 1.450(3) . ? N18 C29 1.453(3) . ? N19 C31 1.308(2) . ? N19 C32 1.490(2) . ? N20 C31 1.370(2) . ? N20 C34 1.454(3) . ? N20 C33 1.459(3) . ? N21 C31 1.337(2) . ? N21 C35 1.468(2) . ? N21 H21X 0.88(2) . ? N22 C36 1.276(3) . ? N22 C37 1.479(3) . ? N23 C36 1.342(3) . ? N23 C40 1.454(3) . ? N23 H23X 0.89(3) . ? N25 C41 1.291(3) . ? N25 C42 1.493(3) . ? N26 C41 1.340(3) . ? N26 C45 1.468(3) . ? N26 H26X 0.90(2) . ? N27 C41 1.388(3) . ? N27 C44 1.452(3) . ? N27 C43 1.454(3) . ? C2 C3 1.533(3) . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C3 H3B 0.99 . ? C3 H3A 0.99 . ? C4 C5 1.541(3) . ? C4 H4B 0.99 . ? C4 H4A 0.99 . ? C5 H5B 0.99 . ? C5 H5A 0.99 . ? C7 C8 1.530(3) . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 H8B 0.99 . ? C8 H8A 0.99 . ? C9 C10 1.535(3) . ? C9 H9B 0.99 . ? C9 H9A 0.99 . ? C10 H10B 0.99 . ? C10 H10A 0.99 . ? C12 C13 1.536(3) . ? C12 H12B 0.99 . ? C12 H12A 0.99 . ? C13 H13B 0.99 . ? C13 H13A 0.99 . ? C14 C15 1.517(3) . ? C14 H14B 0.99 . ? C14 H14A 0.99 . ? C15 H15B 0.99 . ? C15 H15A 0.99 . ? C17 C18 1.510(3) . ? C17 H17B 0.99 . ? C17 H17A 0.99 . ? C18 H18B 0.99 . ? C18 H18A 0.99 . ? C19 C20 1.496(3) . ? C19 H19B 0.99 . ? C19 H19A 0.99 . ? C20 H20B 0.99 . ? C20 H20A 0.99 . ? C22 C23 1.530(3) . ? C22 H22B 0.99 . ? C22 H22A 0.99 . ? C23 H23B 0.99 . ? C23 H23A 0.99 . ? C24 C25 1.529(3) . ? C24 H24B 0.99 . ? C24 H24A 0.99 . ? C25 H25B 0.99 . ? C25 H25A 0.99 . ? C27 C28 1.525(3) . ? C27 H27B 0.99 . ? C27 H27A 0.99 . ? C28 H28B 0.99 . ? C28 H28A 0.99 . ? C29 C30 1.535(4) . ? C29 H29B 0.99 . ? C29 H29A 0.99 . ? C30 H30B 0.99 . ? C30 H30A 0.99 . ? C32 C33 1.540(3) . ? C32 H32B 0.99 . ? C32 H32A 0.99 . ? C33 H33B 0.99 . ? C33 H33A 0.99 . ? C34 C35 1.528(3) . ? C34 H34B 0.99 . ? C34 H34A 0.99 . ? C35 H35B 0.99 . ? C35 H35A 0.99 . ? C36 N24A 1.428(4) . ? C36 N24 1.438(4) . ? C42 C43 1.529(3) . ? C42 H42B 0.99 . ? C42 H42A 0.99 . ? C43 H43B 0.99 . ? C43 H43A 0.99 . ? C44 C45 1.519(4) . ? C44 H44B 0.99 . ? C44 H44A 0.99 . ? C45 H45B 0.99 . ? C45 H45A 0.99 . ? O C48 1.337(5) . ? O C46 1.399(5) . ? C46 C47 1.383(5) . ? C46 H46B 0.99 . ? C46 H46A 0.99 . ? C47 H47C 0.98 . ? C47 H47B 0.98 . ? C47 H47A 0.98 . ? C48 C49 1.495(7) . ? C48 H48B 0.99 . ? C48 H48A 0.99 . ? C49 H49C 0.98 . ? C49 H49B 0.98 . ? C49 H49A 0.98 . ? C37 C38 1.538(3) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 N24 1.438(5) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 N24 1.467(5) . ? C39 C40 1.513(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? 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 N7 Li1 N10 111.21(15) . . ? N7 Li1 N1 111.47(15) . . ? N10 Li1 N1 115.11(15) . . ? N7 Li1 N5 112.55(16) . . ? N10 Li1 N5 104.17(14) . . ? N1 Li1 N5 101.77(14) . . ? N7 Li1 Li4 113.09(16) . . ? N10 Li1 Li4 134.88(16) . . ? N1 Li1 Li4 54.14(10) . . ? N5 Li1 Li4 50.13(10) . . ? N7 Li1 C16 94.09(13) . . ? N10 Li1 C16 28.07(7) . . ? N1 Li1 C16 104.21(13) . . ? N5 Li1 C16 132.19(14) . . ? Li4 Li1 C16 149.54(15) . . ? N7 Li1 Li2 153.90(16) . . ? N10 Li1 Li2 42.93(9) . . ? N1 Li1 Li2 83.97(12) . . ? N5 Li1 Li2 83.02(12) . . ? Li4 Li1 Li2 93.00(12) . . ? C16 Li1 Li2 60.94(10) . . ? N7 Li1 Li5 77.54(12) . . ? N10 Li1 Li5 86.51(12) . . ? N1 Li1 Li5 58.61(10) . . ? N5 Li1 Li5 160.38(15) . . ? Li4 Li1 Li5 110.86(13) . . ? C16 Li1 Li5 60.26(9) . . ? Li2 Li1 Li5 94.49(12) . . ? N10 Li2 N16 113.58(16) . . ? N10 Li2 N2 112.17(15) . . ? N16 Li2 N2 112.24(16) . . ? N10 Li2 N4 103.65(15) . . ? N16 Li2 N4 112.74(15) . . ? N2 Li2 N4 101.53(14) . . ? N10 Li2 Li3 130.42(16) . . ? N16 Li2 Li3 115.44(16) . . ? N2 Li2 Li3 53.72(10) . . ? N4 Li2 Li3 49.77(10) . . ? N10 Li2 Li1 43.68(9) . . ? N16 Li2 Li1 156.97(16) . . ? N2 Li2 Li1 80.54(11) . . ? N4 Li2 Li1 81.60(12) . . ? Li3 Li2 Li1 87.59(12) . . ? N10 Li2 Li6 80.11(12) . . ? N16 Li2 Li6 84.85(12) . . ? N2 Li2 Li6 57.50(10) . . ? N4 Li2 Li6 157.59(15) . . ? Li3 Li2 Li6 110.98(13) . . ? Li1 Li2 Li6 86.67(11) . . ? N25 Li3 N4 107.55(15) . . ? N25 Li3 N19 106.92(15) . . ? N4 Li3 N19 111.12(15) . . ? N25 Li3 N2 120.25(16) . . ? N4 Li3 N2 101.39(14) . . ? N19 Li3 N2 109.45(14) . . ? N25 Li3 Li2 117.95(15) . . ? N4 Li3 Li2 52.21(10) . . ? N19 Li3 Li2 134.90(16) . . ? N2 Li3 Li2 51.13(10) . . ? N25 Li3 C1 136.79(15) . . ? N4 Li3 C1 108.06(13) . . ? N19 Li3 C1 81.94(11) . . ? N2 Li3 C1 27.92(6) . . ? Li2 Li3 C1 68.93(10) . . ? N25 Li3 Li4 149.06(16) . . ? N4 Li3 Li4 83.52(12) . . ? N19 Li3 Li4 43.07(9) . . ? N2 Li3 Li4 84.02(11) . . ? Li2 Li3 Li4 91.88(13) . . ? C1 Li3 Li4 59.08(9) . . ? N22 Li4 N5 106.24(15) . . ? N22 Li4 N19 111.17(15) . . ? N5 Li4 N19 108.87(14) . . ? N22 Li4 N1 121.42(15) . . ? N5 Li4 N1 101.77(14) . . ? N19 Li4 N1 106.52(14) . . ? N22 Li4 Li1 116.39(15) . . ? N5 Li4 Li1 52.93(10) . . ? N19 Li4 Li1 132.14(16) . . ? N1 Li4 Li1 51.35(10) . . ? N22 Li4 Li3 154.24(16) . . ? N5 Li4 Li3 79.80(11) . . ? N19 Li4 Li3 44.71(9) . . ? N1 Li4 Li3 80.34(11) . . ? Li1 Li4 Li3 87.52(12) . . ? N13 Li5 N8 119.16(18) . . ? N13 Li5 N11 106.48(16) . . ? N8 Li5 N11 115.44(17) . . ? N13 Li5 C20 89.71(13) . . ? N8 Li5 C20 103.69(15) . . ? N11 Li5 C20 31.57(8) . . ? N13 Li5 Li6 81.70(13) . . ? N8 Li5 Li6 155.38(17) . . ? N11 Li5 Li6 41.30(10) . . ? C20 Li5 Li6 60.82(10) . . ? N13 Li5 Li1 158.20(17) . . ? N8 Li5 Li1 79.61(12) . . ? N11 Li5 Li1 71.14(11) . . ? C20 Li5 Li1 96.66(12) . . ? Li6 Li5 Li1 83.29(11) . . ? N14 Li6 N17 114.40(18) . . ? N14 Li6 N11 106.20(16) . . ? N17 Li6 N11 117.54(17) . . ? N14 Li6 N2 117.83(16) . . ? N17 Li6 N2 98.43(14) . . ? N11 Li6 N2 102.21(14) . . ? N14 Li6 Li5 79.51(12) . . ? N17 Li6 Li5 159.19(17) . . ? N11 Li6 Li5 41.70(10) . . ? N2 Li6 Li5 87.38(12) . . ? N14 Li6 Li2 160.42(18) . . ? N17 Li6 Li2 76.16(12) . . ? N11 Li6 Li2 80.97(12) . . ? N2 Li6 Li2 42.66(8) . . ? Li5 Li6 Li2 95.54(13) . . ? C1 N1 C2 104.86(14) . . ? C1 N1 Li1 120.18(14) . . ? C2 N1 Li1 134.30(14) . . ? C1 N1 Li4 106.89(13) . . ? C2 N1 Li4 100.80(13) . . ? Li1 N1 Li4 74.50(12) . . ? C1 N2 C5 105.17(14) . . ? C1 N2 Li2 123.96(14) . . ? C5 N2 Li2 130.37(14) . . ? C1 N2 Li3 101.81(13) . . ? C5 N2 Li3 103.28(14) . . ? Li2 N2 Li3 75.15(12) . . ? C1 N2 Li6 97.02(12) . . ? C5 N2 Li6 88.33(13) . . ? Li2 N2 Li6 79.84(12) . . ? Li3 N2 Li6 154.28(12) . . ? C1 N3 C4 105.74(13) . . ? C1 N3 C3 104.90(13) . . ? C4 N3 C3 125.24(14) . . ? C6 N4 C7 104.66(14) . . ? C6 N4 Li3 113.95(14) . . ? C7 N4 Li3 123.38(15) . . ? C6 N4 Li2 117.35(14) . . ? C7 N4 Li2 118.65(14) . . ? Li3 N4 Li2 78.02(13) . . ? C6 N5 C10 104.54(14) . . ? C6 N5 Li4 118.49(14) . . ? C10 N5 Li4 118.81(15) . . ? C6 N5 Li1 115.43(14) . . ? C10 N5 Li1 121.77(14) . . ? Li4 N5 Li1 76.94(13) . . ? C6 N6 C9 105.43(14) . . ? C6 N6 C8 105.20(15) . . ? C9 N6 C8 126.24(16) . . ? C11 N7 C12 104.74(15) . . ? C11 N7 Li1 123.85(15) . . ? C12 N7 Li1 121.28(16) . . ? C11 N8 C15 104.58(15) . . ? C11 N8 Li5 119.39(16) . . ? C15 N8 Li5 120.37(16) . . ? C11 N9 C14 104.62(16) . . ? C11 N9 C13 104.44(16) . . ? C14 N9 C13 124.3(2) . . ? C16 N10 C17 105.00(15) . . ? C16 N10 Li2 117.91(15) . . ? C17 N10 Li2 116.71(15) . . ? C16 N10 Li1 104.65(15) . . ? C17 N10 Li1 119.00(16) . . ? Li2 N10 Li1 93.38(13) . . ? C16 N11 C20 104.78(14) . . ? C16 N11 Li6 115.00(15) . . ? C20 N11 Li6 113.75(16) . . ? C16 N11 Li5 123.93(16) . . ? C20 N11 Li5 102.04(15) . . ? Li6 N11 Li5 97.00(14) . . ? C19 N12 C18 137.5(2) . . ? C19 N12 C16 107.33(18) . . ? C18 N12 C16 107.67(17) . . ? C21 N13 C22 104.97(15) . . ? C21 N13 Li5 121.35(16) . . ? C22 N13 Li5 133.62(16) . . ? C21 N14 C25 105.07(16) . . ? C21 N14 Li6 125.33(16) . . ? C25 N14 Li6 129.60(16) . . ? C21 N15 C23 104.47(16) . . ? C21 N15 C24 104.52(16) . . ? C23 N15 C24 124.64(18) . . ? C26 N16 C27 104.90(16) . . ? C26 N16 Li2 114.18(15) . . ? C27 N16 Li2 125.86(17) . . ? C26 N17 C30 105.40(16) . . ? C26 N17 Li6 127.18(17) . . ? C30 N17 Li6 116.60(16) . . ? C26 N18 C28 104.46(17) . . ? C26 N18 C29 104.49(17) . . ? C28 N18 C29 123.3(2) . . ? C31 N19 C32 103.78(14) . . ? C31 N19 Li4 127.98(14) . . ? C32 N19 Li4 108.07(14) . . ? C31 N19 Li3 116.48(14) . . ? C32 N19 Li3 106.77(14) . . ? Li4 N19 Li3 92.22(13) . . ? C31 N20 C34 107.89(15) . . ? C31 N20 C33 105.78(15) . . ? C34 N20 C33 127.82(16) . . ? C31 N21 C35 109.77(16) . . ? C31 N21 H21X 122.9(15) . . ? C35 N21 H21X 126.2(15) . . ? C36 N22 C37 104.83(16) . . ? C36 N22 Li4 125.01(17) . . ? C37 N22 Li4 129.50(15) . . ? C36 N23 C40 110.3(2) . . ? C36 N23 H23X 123.7(18) . . ? C40 N23 H23X 122.7(18) . . ? C41 N25 C42 103.07(17) . . ? C41 N25 Li3 122.71(17) . . ? C42 N25 Li3 128.69(16) . . ? C41 N26 C45 108.76(19) . . ? C41 N26 H26X 126.0(15) . . ? C45 N26 H26X 122.5(15) . . ? C41 N27 C44 107.31(19) . . ? C41 N27 C43 104.25(17) . . ? C44 N27 C43 126.02(19) . . ? N1 C1 N2 131.24(15) . . ? N1 C1 N3 114.39(14) . . ? N2 C1 N3 114.38(15) . . ? N1 C1 Li3 106.83(12) . . ? N2 C1 Li3 50.27(11) . . ? N3 C1 Li3 115.45(12) . . ? N1 C2 C3 105.33(14) . . ? N1 C2 H2B 110.7 . . ? C3 C2 H2B 110.7 . . ? N1 C2 H2A 110.7 . . ? C3 C2 H2A 110.7 . . ? H2B C2 H2A 108.8 . . ? N3 C3 C2 99.71(13) . . ? N3 C3 H3B 111.8 . . ? C2 C3 H3B 111.8 . . ? N3 C3 H3A 111.8 . . ? C2 C3 H3A 111.8 . . ? H3B C3 H3A 109.6 . . ? N3 C4 C5 100.28(14) . . ? N3 C4 H4B 111.7 . . ? C5 C4 H4B 111.7 . . ? N3 C4 H4A 111.7 . . ? C5 C4 H4A 111.7 . . ? H4B C4 H4A 109.5 . . ? N2 C5 C4 105.62(14) . . ? N2 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? N2 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? H5B C5 H5A 108.7 . . ? N4 C6 N5 131.36(16) . . ? N4 C6 N6 114.41(15) . . ? N5 C6 N6 114.22(16) . . ? N4 C7 C8 105.08(15) . . ? N4 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? N4 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? H7B C7 H7A 108.8 . . ? N6 C8 C7 100.01(15) . . ? N6 C8 H8B 111.8 . . ? C7 C8 H8B 111.8 . . ? N6 C8 H8A 111.8 . . ? C7 C8 H8A 111.8 . . ? H8B C8 H8A 109.5 . . ? N6 C9 C10 99.41(15) . . ? N6 C9 H9B 111.9 . . ? C10 C9 H9B 111.9 . . ? N6 C9 H9A 111.9 . . ? C10 C9 H9A 111.9 . . ? H9B C9 H9A 109.6 . . ? N5 C10 C9 105.11(16) . . ? N5 C10 H10B 110.7 . . ? C9 C10 H10B 110.7 . . ? N5 C10 H10A 110.7 . . ? C9 C10 H10A 110.7 . . ? H10B C10 H10A 108.8 . . ? N8 C11 N7 131.34(17) . . ? N8 C11 N9 114.72(16) . . ? N7 C11 N9 113.90(16) . . ? N7 C12 C13 104.77(17) . . ? N7 C12 H12B 110.8 . . ? C13 C12 H12B 110.8 . . ? N7 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? H12B C12 H12A 108.9 . . ? N9 C13 C12 99.84(18) . . ? N9 C13 H13B 111.8 . . ? C12 C13 H13B 111.8 . . ? N9 C13 H13A 111.8 . . ? C12 C13 H13A 111.8 . . ? H13B C13 H13A 109.5 . . ? N9 C14 C15 100.43(18) . . ? N9 C14 H14B 111.7 . . ? C15 C14 H14B 111.7 . . ? N9 C14 H14A 111.7 . . ? C15 C14 H14A 111.7 . . ? H14B C14 H14A 109.5 . . ? N8 C15 C14 105.19(17) . . ? N8 C15 H15B 110.7 . . ? C14 C15 H15B 110.7 . . ? N8 C15 H15A 110.7 . . ? C14 C15 H15A 110.7 . . ? H15B C15 H15A 108.8 . . ? N11 C16 N10 131.01(17) . . ? N11 C16 N12 114.49(16) . . ? N10 C16 N12 114.49(16) . . ? N11 C16 Li1 98.09(13) . . ? N10 C16 Li1 47.28(11) . . ? N12 C16 Li1 130.91(17) . . ? N10 C17 C18 105.81(17) . . ? N10 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? N10 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? H17B C17 H17A 108.7 . . ? N12 C18 C17 104.60(18) . . ? N12 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? N12 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? H18B C18 H18A 108.9 . . ? N12 C19 C20 104.89(18) . . ? N12 C19 H19B 110.8 . . ? C20 C19 H19B 110.8 . . ? N12 C19 H19A 110.8 . . ? C20 C19 H19A 110.8 . . ? H19B C19 H19A 108.8 . . ? N11 C20 C19 105.75(16) . . ? N11 C20 Li5 46.38(11) . . ? C19 C20 Li5 135.27(18) . . ? N11 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? Li5 C20 H20B 112.3 . . ? N11 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? Li5 C20 H20A 66.5 . . ? H20B C20 H20A 108.7 . . ? N13 C21 N14 131.84(17) . . ? N13 C21 N15 114.22(16) . . ? N14 C21 N15 113.92(16) . . ? N13 C22 C23 105.43(16) . . ? N13 C22 H22B 110.7 . . ? C23 C22 H22B 110.7 . . ? N13 C22 H22A 110.7 . . ? C23 C22 H22A 110.7 . . ? H22B C22 H22A 108.8 . . ? N15 C23 C22 100.13(16) . . ? N15 C23 H23B 111.7 . . ? C22 C23 H23B 111.7 . . ? N15 C23 H23A 111.7 . . ? C22 C23 H23A 111.7 . . ? H23B C23 H23A 109.5 . . ? N15 C24 C25 99.88(16) . . ? N15 C24 H24B 111.8 . . ? C25 C24 H24B 111.8 . . ? N15 C24 H24A 111.8 . . ? C25 C24 H24A 111.8 . . ? H24B C24 H24A 109.5 . . ? N14 C25 C24 105.09(17) . . ? N14 C25 H25B 110.7 . . ? C24 C25 H25B 110.7 . . ? N14 C25 H25A 110.7 . . ? C24 C25 H25A 110.7 . . ? H25B C25 H25A 108.8 . . ? N17 C26 N16 131.53(17) . . ? N17 C26 N18 114.62(17) . . ? N16 C26 N18 113.81(17) . . ? N16 C27 C28 105.83(18) . . ? N16 C27 H27B 110.6 . . ? C28 C27 H27B 110.6 . . ? N16 C27 H27A 110.6 . . ? C28 C27 H27A 110.6 . . ? H27B C27 H27A 108.7 . . ? N18 C28 C27 100.54(18) . . ? N18 C28 H28B 111.7 . . ? C27 C28 H28B 111.7 . . ? N18 C28 H28A 111.7 . . ? C27 C28 H28A 111.7 . . ? H28B C28 H28A 109.4 . . ? N18 C29 C30 100.31(18) . . ? N18 C29 H29B 111.7 . . ? C30 C29 H29B 111.7 . . ? N18 C29 H29A 111.7 . . ? C30 C29 H29A 111.7 . . ? H29B C29 H29A 109.5 . . ? N17 C30 C29 104.89(18) . . ? N17 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? N17 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? H30B C30 H30A 108.8 . . ? N19 C31 N21 132.37(17) . . ? N19 C31 N20 117.34(16) . . ? N21 C31 N20 110.25(16) . . ? N19 C32 C33 105.93(15) . . ? N19 C32 H32B 110.5 . . ? C33 C32 H32B 110.5 . . ? N19 C32 H32A 110.5 . . ? C33 C32 H32A 110.5 . . ? H32B C32 H32A 108.7 . . ? N20 C33 C32 100.37(14) . . ? N20 C33 H33B 111.7 . . ? C32 C33 H33B 111.7 . . ? N20 C33 H33A 111.7 . . ? C32 C33 H33A 111.7 . . ? H33B C33 H33A 109.5 . . ? N20 C34 C35 101.49(15) . . ? N20 C34 H34B 111.5 . . ? C35 C34 H34B 111.5 . . ? N20 C34 H34A 111.5 . . ? C35 C34 H34A 111.5 . . ? H34B C34 H34A 109.3 . . ? N21 C35 C34 101.67(15) . . ? N21 C35 H35B 111.4 . . ? C34 C35 H35B 111.4 . . ? N21 C35 H35A 111.4 . . ? C34 C35 H35A 111.4 . . ? H35B C35 H35A 109.3 . . ? N22 C36 N23 133.6(2) . . ? N22 C36 N24A 115.2(2) . . ? N23 C36 N24A 108.2(2) . . ? N22 C36 N24 114.8(2) . . ? N23 C36 N24 109.9(2) . . ? N25 C41 N26 132.49(19) . . ? N25 C41 N27 117.1(2) . . ? N26 C41 N27 110.30(18) . . ? N25 C42 C43 105.10(19) . . ? N25 C42 H42B 110.7 . . ? C43 C42 H42B 110.7 . . ? N25 C42 H42A 110.7 . . ? C43 C42 H42A 110.7 . . ? H42B C42 H42A 108.8 . . ? N27 C43 C42 99.25(18) . . ? N27 C43 H43B 111.9 . . ? C42 C43 H43B 111.9 . . ? N27 C43 H43A 111.9 . . ? C42 C43 H43A 111.9 . . ? H43B C43 H43A 109.6 . . ? N27 C44 C45 101.16(18) . . ? N27 C44 H44B 111.5 . . ? C45 C44 H44B 111.5 . . ? N27 C44 H44A 111.5 . . ? C45 C44 H44A 111.5 . . ? H44B C44 H44A 109.4 . . ? N26 C45 C44 102.71(19) . . ? N26 C45 H45B 111.2 . . ? C44 C45 H45B 111.2 . . ? N26 C45 H45A 111.2 . . ? C44 C45 H45A 111.2 . . ? H45B C45 H45A 109.1 . . ? C48 O C46 121.3(4) . . ? C47 C46 O 118.2(3) . . ? C47 C46 H46B 107.8 . . ? O C46 H46B 107.8 . . ? C47 C46 H46A 107.8 . . ? O C46 H46A 107.8 . . ? H46B C46 H46A 107.1 . . ? C46 C47 H47C 109.5 . . ? C46 C47 H47B 109.5 . . ? H47C C47 H47B 109.5 . . ? C46 C47 H47A 109.5 . . ? H47C C47 H47A 109.5 . . ? H47B C47 H47A 109.5 . . ? O C48 C49 114.3(4) . . ? O C48 H48B 108.7 . . ? C49 C48 H48B 108.7 . . ? O C48 H48A 108.7 . . ? C49 C48 H48A 108.7 . . ? H48B C48 H48A 107.6 . . ? C48 C49 H49C 109.5 . . ? C48 C49 H49B 109.5 . . ? H49C C49 H49B 109.5 . . ? C48 C49 H49A 109.5 . . ? H49C C49 H49A 109.5 . . ? H49B C49 H49A 109.5 . . ? N22 C37 C38 106.14(17) . . ? N22 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? N22 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? N24 C38 C37 101.2(2) . . ? N24 C38 H38A 111.5 . . ? C37 C38 H38A 111.5 . . ? N24 C38 H38B 111.5 . . ? C37 C38 H38B 111.5 . . ? H38A C38 H38B 109.3 . . ? N24 C39 C40 104.9(2) . . ? N24 C39 H39A 110.8 . . ? C40 C39 H39A 110.8 . . ? N24 C39 H39B 110.8 . . ? C40 C39 H39B 110.8 . . ? H39A C39 H39B 108.8 . . ? N23 C40 C39 103.2(2) . . ? N23 C40 H40A 111.1 . . ? C39 C40 H40A 111.1 . . ? N23 C40 H40B 111.1 . . ? C39 C40 H40B 111.1 . . ? H40A C40 H40B 109.1 . . ? C38 N24 C36 102.8(3) . . ? C38 N24 C39 126.8(4) . . ? C36 N24 C39 103.3(4) . . ? #===END data_(2)-aug807 _database_code_depnum_ccdc_archive 'CCDC 685442' _audit_creation_date 2007-08-10T14:02:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H28 Al2 N6' _chemical_formula_sum 'C14 H28 Al2 N6' _chemical_formula_weight 334.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5214(2) _cell_length_b 10.1796(3) _cell_length_c 12.2236(2) _cell_angle_alpha 99.825(2) _cell_angle_beta 103.853(2) _cell_angle_gamma 114.523(1) _cell_volume 891.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9271 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.169 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.29314E-2 _diffrn_orient_matrix_ub_12 0.669751E-1 _diffrn_orient_matrix_ub_13 -0.514131E-1 _diffrn_orient_matrix_ub_21 -0.135901 _diffrn_orient_matrix_ub_22 -0.408178E-1 _diffrn_orient_matrix_ub_23 -0.216849E-1 _diffrn_orient_matrix_ub_31 0.205933E-1 _diffrn_orient_matrix_ub_32 0.819066E-1 _diffrn_orient_matrix_ub_33 0.68687E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0229 _diffrn_reflns_number 13658 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 3495 _reflns_number_gt 3242 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The lower occupancy site for the disordered N6 was left isotropic. 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^)+(0.0455P)^2^+0.4610P] 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_number_reflns 3495 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.238 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' 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 Al1 Al 0.27049(6) 0.41408(5) 0.73962(4) 0.02574(13) Uani 1 1 d . . . Al2 Al 0.20906(6) 0.05078(5) 0.84411(4) 0.02260(13) Uani 1 1 d . . . N1 N 0.47094(17) 0.37263(14) 0.75091(11) 0.0265(3) Uani 1 1 d . . . N2 N 0.42871(16) 0.14717(14) 0.80948(11) 0.0236(3) Uani 1 1 d . . . N3 N 0.68548(17) 0.29254(15) 0.77431(11) 0.0276(3) Uani 1 1 d . . . N4 N 0.04917(19) 0.23350(16) 0.64118(11) 0.0291(3) Uani 1 1 d . C . N5 N 0.00199(17) 0.01993(14) 0.71753(11) 0.0269(3) Uani 1 1 d . C . C1 C 0.51469(19) 0.26816(16) 0.77777(12) 0.0224(3) Uani 1 1 d . . . C2 C 0.6344(2) 0.48463(19) 0.73127(16) 0.0355(4) Uani 1 1 d . . . H2A H 0.663 0.5898 0.7693 0.043 Uiso 1 1 calc R . . H2B H 0.6126 0.4691 0.6457 0.043 Uiso 1 1 calc R . . C3 C 0.7901(2) 0.45357(19) 0.78841(16) 0.0357(4) Uani 1 1 d . . . H3A H 0.8788 0.4726 0.7459 0.043 Uiso 1 1 calc R . . H3B H 0.8559 0.5147 0.8728 0.043 Uiso 1 1 calc R . . C4 C 0.7450(2) 0.2128(2) 0.84915(15) 0.0324(4) Uani 1 1 d . . . H4A H 0.8126 0.2774 0.9326 0.039 Uiso 1 1 calc R . . H4B H 0.8221 0.1749 0.8203 0.039 Uiso 1 1 calc R . . C5 C 0.5585(2) 0.08320(19) 0.83374(15) 0.0308(3) Uani 1 1 d . . . H5A H 0.5218 -0.0059 0.7667 0.037 Uiso 1 1 calc R . . H5B H 0.5619 0.0525 0.9065 0.037 Uiso 1 1 calc R . . C6 C -0.0440(2) 0.09694(18) 0.65058(13) 0.0278(3) Uani 1 1 d . . . C7 C -0.0815(3) 0.2472(2) 0.54319(16) 0.0459(5) Uani 1 1 d . . . H7A H -0.0223 0.2846 0.4864 0.055 Uiso 1 1 calc R A 1 H7B H -0.1233 0.318 0.575 0.055 Uiso 1 1 calc R A 1 C10 C -0.1680(2) -0.1299(2) 0.68156(17) 0.0416(4) Uani 1 1 d . . . H10A H -0.2279 -0.1344 0.742 0.05 Uiso 1 1 calc R B 1 H10B H -0.1381 -0.2143 0.671 0.05 Uiso 1 1 calc R B 1 C11 C 0.2553(2) 0.4851(2) 0.89433(15) 0.0332(4) Uani 1 1 d . . . H11A H 0.1604 0.4012 0.9086 0.05 Uiso 1 1 calc R . . H11B H 0.2239 0.5675 0.8954 0.05 Uiso 1 1 calc R . . H11C H 0.3742 0.5222 0.9563 0.05 Uiso 1 1 calc R . . C12 C 0.3026(3) 0.5581(2) 0.64624(19) 0.0485(5) Uani 1 1 d . . . H12A H 0.4129 0.655 0.6924 0.073 Uiso 1 1 calc R . . H12B H 0.1949 0.5743 0.6274 0.073 Uiso 1 1 calc R . . H12C H 0.316 0.5165 0.5727 0.073 Uiso 1 1 calc R . . C13 C 0.2333(3) 0.1644(2) 0.99966(15) 0.0377(4) Uani 1 1 d . . . H13A H 0.2963 0.1355 1.0616 0.057 Uiso 1 1 calc R . . H13B H 0.1109 0.1409 1.0026 0.057 Uiso 1 1 calc R . . H13C H 0.3047 0.2733 1.0124 0.057 Uiso 1 1 calc R . . C14 C 0.1693(3) -0.15708(19) 0.83357(16) 0.0366(4) Uani 1 1 d . . . H14A H 0.147 -0.2106 0.7522 0.055 Uiso 1 1 calc R . . H14B H 0.0626 -0.2113 0.856 0.055 Uiso 1 1 calc R . . H14C H 0.2785 -0.1525 0.8873 0.055 Uiso 1 1 calc R . . C8 C -0.2413(3) 0.0885(3) 0.48411(16) 0.0457(5) Uani 0.866(10) 1 d P C 1 H8A H -0.3596 0.0903 0.4596 0.055 Uiso 0.866(10) 1 calc PR C 1 H8B H -0.2275 0.0357 0.414 0.055 Uiso 0.866(10) 1 calc PR C 1 C9 C -0.2919(2) -0.1388(2) 0.56558(17) 0.0439(5) Uani 0.866(10) 1 d P C 1 H9A H -0.2742 -0.1907 0.497 0.053 Uiso 0.866(10) 1 calc PR C 1 H9B H -0.4231 -0.1913 0.5579 0.053 Uiso 0.866(10) 1 calc PR C 1 N6 N -0.2294(3) 0.0165(2) 0.5771(2) 0.0327(7) Uani 0.866(10) 1 d P C 1 C8A C -0.2413(3) 0.0885(3) 0.48411(16) 0.0457(5) Uani 0.134(10) 1 d P C 2 H8A1 H -0.3559 0.0806 0.4952 0.055 Uiso 0.134(10) 1 calc PR C 2 H8A2 H -0.2629 0.0522 0.3987 0.055 Uiso 0.134(10) 1 calc PR C 2 C9A C -0.2919(2) -0.1388(2) 0.56558(17) 0.0439(5) Uani 0.134(10) 1 d P C 2 H9A1 H -0.4101 -0.1493 0.5717 0.053 Uiso 0.134(10) 1 calc PR C 2 H9A2 H -0.3172 -0.2259 0.5008 0.053 Uiso 0.134(10) 1 calc PR C 2 N6B N -0.1768(18) 0.0202(11) 0.5428(12) 0.020(3) Uiso 0.134(10) 1 d P C 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 Al1 0.0309(3) 0.0263(2) 0.0266(2) 0.01213(19) 0.01214(19) 0.0168(2) Al2 0.0240(2) 0.0223(2) 0.0205(2) 0.00793(17) 0.00824(17) 0.00931(18) N1 0.0260(6) 0.0251(6) 0.0313(7) 0.0114(5) 0.0149(5) 0.0110(5) N2 0.0212(6) 0.0269(6) 0.0243(6) 0.0089(5) 0.0071(5) 0.0128(5) N3 0.0213(6) 0.0325(7) 0.0292(7) 0.0066(5) 0.0118(5) 0.0122(5) N4 0.0326(7) 0.0366(7) 0.0207(6) 0.0092(5) 0.0049(5) 0.0209(6) N5 0.0221(6) 0.0269(7) 0.0261(6) 0.0062(5) 0.0064(5) 0.0085(5) C1 0.0217(7) 0.0260(7) 0.0181(6) 0.0035(5) 0.0078(5) 0.0108(6) C2 0.0341(9) 0.0302(8) 0.0439(10) 0.0156(7) 0.0229(8) 0.0101(7) C3 0.0267(8) 0.0343(9) 0.0410(9) 0.0084(7) 0.0186(7) 0.0074(7) C4 0.0253(8) 0.0419(9) 0.0309(8) 0.0063(7) 0.0080(6) 0.0197(7) C5 0.0271(8) 0.0357(9) 0.0316(8) 0.0103(7) 0.0058(6) 0.0192(7) C6 0.0271(8) 0.0310(8) 0.0199(7) -0.0001(6) 0.0030(6) 0.0148(7) C7 0.0544(12) 0.0543(12) 0.0275(9) 0.0097(8) -0.0023(8) 0.0345(10) C10 0.0275(8) 0.0314(9) 0.0467(10) 0.0060(8) 0.0044(8) 0.0037(7) C11 0.0298(8) 0.0359(9) 0.0319(8) 0.0044(7) 0.0100(7) 0.0165(7) C12 0.0651(13) 0.0470(11) 0.0536(12) 0.0322(10) 0.0274(10) 0.0346(10) C13 0.0410(10) 0.0398(9) 0.0270(8) 0.0067(7) 0.0145(7) 0.0142(8) C14 0.0418(9) 0.0278(8) 0.0377(9) 0.0130(7) 0.0115(8) 0.0143(7) C8 0.0347(10) 0.0742(14) 0.0278(9) 0.0149(9) 0.0051(7) 0.0289(10) C9 0.0229(8) 0.0485(11) 0.0407(10) 0.0051(8) 0.0063(7) 0.0053(8) N6 0.0237(10) 0.0423(10) 0.0228(10) 0.0014(7) 0.0020(8) 0.0141(7) C8A 0.0347(10) 0.0742(14) 0.0278(9) 0.0149(9) 0.0051(7) 0.0289(10) C9A 0.0229(8) 0.0485(11) 0.0407(10) 0.0051(8) 0.0063(7) 0.0053(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al1 N1 1.9026(14) . ? Al1 N4 1.9143(15) . ? Al1 C11 1.9605(17) . ? Al1 C12 1.9790(18) . ? Al2 N2 1.9084(13) . ? Al2 N5 1.9166(13) . ? Al2 C13 1.9644(17) . ? Al2 C14 1.9747(17) . ? N1 C1 1.329(2) . ? N1 C2 1.4942(19) . ? N2 C1 1.3244(19) . ? N2 C5 1.4973(19) . ? N3 C1 1.3837(19) . ? N3 C4 1.458(2) . ? N3 C3 1.459(2) . ? N4 C6 1.326(2) . ? N4 C7 1.497(2) . ? N5 C6 1.326(2) . ? N5 C10 1.500(2) . ? C2 C3 1.526(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.527(2) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 N6B 1.352(10) . ? C6 N6 1.403(2) . ? C7 C8 1.513(3) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C10 C9 1.514(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C8 N6 1.460(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 N6 1.411(3) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N4 108.04(6) . . ? N1 Al1 C11 112.88(7) . . ? N4 Al1 C11 110.85(7) . . ? N1 Al1 C12 104.76(8) . . ? N4 Al1 C12 104.92(8) . . ? C11 Al1 C12 114.82(9) . . ? N2 Al2 N5 109.86(6) . . ? N2 Al2 C13 110.83(7) . . ? N5 Al2 C13 113.62(7) . . ? N2 Al2 C14 105.10(7) . . ? N5 Al2 C14 103.40(7) . . ? C13 Al2 C14 113.48(8) . . ? C1 N1 C2 105.45(13) . . ? C1 N1 Al1 137.08(10) . . ? C2 N1 Al1 117.40(10) . . ? C1 N2 C5 105.47(12) . . ? C1 N2 Al2 138.42(10) . . ? C5 N2 Al2 115.80(10) . . ? C1 N3 C4 106.64(12) . . ? C1 N3 C3 106.34(13) . . ? C4 N3 C3 124.81(13) . . ? C6 N4 C7 105.44(14) . . ? C6 N4 Al1 134.98(11) . . ? C7 N4 Al1 117.77(12) . . ? C6 N5 C10 105.27(13) . . ? C6 N5 Al2 138.61(11) . . ? C10 N5 Al2 116.03(11) . . ? N2 C1 N1 132.68(13) . . ? N2 C1 N3 113.70(13) . . ? N1 C1 N3 113.61(13) . . ? N1 C2 C3 104.45(13) . . ? N1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? N1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? N3 C3 C2 100.12(13) . . ? N3 C3 H3A 111.7 . . ? C2 C3 H3A 111.7 . . ? N3 C3 H3B 111.7 . . ? C2 C3 H3B 111.7 . . ? H3A C3 H3B 109.5 . . ? N3 C4 C5 99.98(12) . . ? N3 C4 H4A 111.8 . . ? C5 C4 H4A 111.8 . . ? N3 C4 H4B 111.8 . . ? C5 C4 H4B 111.8 . . ? H4A C4 H4B 109.5 . . ? N2 C5 C4 104.43(13) . . ? N2 C5 H5A 110.9 . . ? C4 C5 H5A 110.9 . . ? N2 C5 H5B 110.9 . . ? C4 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? N5 C6 N4 132.83(14) . . ? N5 C6 N6B 119.1(4) . . ? N4 C6 N6B 103.1(5) . . ? N5 C6 N6 112.26(15) . . ? N4 C6 N6 114.91(15) . . ? N4 C7 C8 105.14(15) . . ? N4 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? N4 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? N5 C10 C9 105.07(15) . . ? N5 C10 H10A 110.7 . . ? C9 C10 H10A 110.7 . . ? N5 C10 H10B 110.7 . . ? C9 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? Al1 C11 H11A 109.5 . . ? Al1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Al1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C12 H12A 109.5 . . ? Al1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Al1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Al2 C13 H13A 109.5 . . ? Al2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al2 C14 H14A 109.5 . . ? Al2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Al2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N6 C8 C7 102.83(14) . . ? N6 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? N6 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? N6 C9 C10 101.00(15) . . ? N6 C9 H9A 111.6 . . ? C10 C9 H9A 111.6 . . ? N6 C9 H9B 111.6 . . ? C10 C9 H9B 111.6 . . ? H9A C9 H9B 109.4 . . ? C6 N6 C9 108.09(15) . . ? C6 N6 C8 104.9(2) . . ? C9 N6 C8 128.65(19) . . ? #===END data_(3)-sep307 _database_code_depnum_ccdc_archive 'CCDC 685443' _audit_creation_date 2007-09-19T15:30:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H38 N12 Zn3, 2(C7 H8)' _chemical_formula_sum 'C36 H54 N12 Zn3' _chemical_formula_weight 851.02 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' _symmetry_space_group_name_Hall 'I -4' _symmetry_Int_Tables_number 82 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 20.5807(8) _cell_length_b 20.5807(8) _cell_length_c 20.3647(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8625.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30828 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7104 _exptl_absorpt_correction_T_max 0.7835 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.15583E-1 _diffrn_orient_matrix_ub_12 -0.33644E-2 _diffrn_orient_matrix_ub_13 -0.463863E-1 _diffrn_orient_matrix_ub_21 0.424439E-1 _diffrn_orient_matrix_ub_22 0.197857E-1 _diffrn_orient_matrix_ub_23 0.130971E-1 _diffrn_orient_matrix_ub_31 0.177931E-1 _diffrn_orient_matrix_ub_32 -0.442506E-1 _diffrn_orient_matrix_ub_33 0.93828E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_unetI/netI 0.0744 _diffrn_reflns_number 19504 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 8306 _reflns_number_gt 6048 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The two poorly defined toluene solvate molecules were included with isotropic C atoms. 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^)+(0.0844P)^2^+16.9627P] 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_number_reflns 8306 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_diff_density_max 0.534 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn1 Zn 0.36387(4) 0.25368(4) 0.12806(4) 0.0446(2) Uani 1 1 d . . . Zn2 Zn 0.48632(4) 0.33537(4) 0.18642(4) 0.0483(2) Uani 1 1 d . . . Zn3 Zn 0.47521(5) 0.16213(4) 0.06126(5) 0.0524(3) Uani 1 1 d . . . N1 N 0.3183(3) 0.3348(3) 0.1493(3) 0.0505(16) Uani 1 1 d . . . N2 N 0.4106(3) 0.3966(3) 0.1890(3) 0.0530(16) Uani 1 1 d . . . N3 N 0.3081(3) 0.4405(3) 0.1796(3) 0.0560(17) Uani 1 1 d . . . N4 N 0.3109(3) 0.1768(3) 0.1103(3) 0.0541(17) Uani 1 1 d . . . N5 N 0.3933(4) 0.1077(3) 0.0645(4) 0.065(2) Uani 1 1 d . . . N6 N 0.2878(4) 0.0749(3) 0.0756(4) 0.067(2) Uani 1 1 d . . . N7 N 0.4288(3) 0.2465(3) 0.2026(3) 0.0423(14) Uani 1 1 d . . . N8 N 0.5042(3) 0.1686(3) 0.1552(3) 0.0502(16) Uani 1 1 d . . . N9 N 0.4820(3) 0.1694(3) 0.2643(3) 0.0493(15) Uani 1 1 d . . . N10 N 0.4245(3) 0.2549(3) 0.0479(3) 0.0471(15) Uani 1 1 d . . . N11 N 0.5059(3) 0.3274(3) 0.0896(3) 0.0497(16) Uani 1 1 d . . . N12 N 0.4750(3) 0.3296(3) -0.0177(3) 0.0502(15) Uani 1 1 d . . . C1 C 0.3499(4) 0.3871(4) 0.1714(4) 0.0475(18) Uani 1 1 d . . . C2 C 0.2491(4) 0.3537(4) 0.1436(5) 0.060(2) Uani 1 1 d . . . H2A H 0.2204 0.3191 0.1609 0.072 Uiso 1 1 calc R . . H2B H 0.2374 0.3625 0.0973 0.072 Uiso 1 1 calc R . . C3 C 0.2438(4) 0.4158(4) 0.1855(5) 0.067(2) Uani 1 1 d . . . H3A H 0.2114 0.4464 0.1673 0.081 Uiso 1 1 calc R . . H3B H 0.2328 0.4057 0.2317 0.081 Uiso 1 1 calc R . . C4 C 0.3427(5) 0.4816(4) 0.2265(4) 0.063(2) Uani 1 1 d . . . H4A H 0.3304 0.4708 0.2723 0.076 Uiso 1 1 calc R . . H4B H 0.3339 0.5282 0.2184 0.076 Uiso 1 1 calc R . . C5 C 0.4123(5) 0.4653(4) 0.2134(5) 0.061(2) Uani 1 1 d . . . H5A H 0.4385 0.4686 0.254 0.073 Uiso 1 1 calc R . . H5B H 0.4309 0.4947 0.1798 0.073 Uiso 1 1 calc R . . C6 C 0.3348(5) 0.1225(4) 0.0850(4) 0.054(2) Uani 1 1 d . . . C7 C 0.2398(5) 0.1677(4) 0.1174(5) 0.068(2) Uani 1 1 d . . . H7A H 0.2157 0.2063 0.1014 0.082 Uiso 1 1 calc R . . H7B H 0.2277 0.1592 0.1636 0.082 Uiso 1 1 calc R . . C8 C 0.2268(5) 0.1090(5) 0.0745(6) 0.085(3) Uani 1 1 d . . . H8A H 0.1914 0.0819 0.0929 0.102 Uiso 1 1 calc R . . H8B H 0.2151 0.1221 0.0292 0.102 Uiso 1 1 calc R . . C9 C 0.3148(6) 0.0336(5) 0.0249(5) 0.088(3) Uani 1 1 d . . . H9A H 0.3021 0.049 -0.0194 0.105 Uiso 1 1 calc R . . H9B H 0.3004 -0.012 0.0304 0.105 Uiso 1 1 calc R . . C10 C 0.3871(6) 0.0401(5) 0.0355(5) 0.082(3) Uani 1 1 d . . . H10A H 0.4111 0.0365 -0.0064 0.099 Uiso 1 1 calc R . . H10B H 0.4033 0.0066 0.0664 0.099 Uiso 1 1 calc R . . C11 C 0.4716(4) 0.1948(4) 0.2028(4) 0.0453(18) Uani 1 1 d . . . C12 C 0.4037(4) 0.2493(4) 0.2710(4) 0.0522(19) Uani 1 1 d . . . H12A H 0.3623 0.2252 0.2751 0.063 Uiso 1 1 calc R . . H12B H 0.3966 0.2949 0.285 0.063 Uiso 1 1 calc R . . C13 C 0.4586(4) 0.2165(4) 0.3128(4) 0.0522(18) Uani 1 1 d . . . H13A H 0.4929 0.2479 0.3255 0.063 Uiso 1 1 calc R . . H13B H 0.4412 0.195 0.3525 0.063 Uiso 1 1 calc R . . C14 C 0.5452(4) 0.1365(5) 0.2604(5) 0.065(2) Uani 1 1 d . . . H14A H 0.5468 0.0975 0.2889 0.078 Uiso 1 1 calc R . . H14B H 0.5814 0.166 0.2719 0.078 Uiso 1 1 calc R . . C15 C 0.5457(4) 0.1188(4) 0.1886(5) 0.059(2) Uani 1 1 d . . . H15A H 0.5905 0.1199 0.171 0.071 Uiso 1 1 calc R . . H15B H 0.5276 0.0747 0.1819 0.071 Uiso 1 1 calc R . . C16 C 0.4681(4) 0.3035(4) 0.0441(4) 0.0448(17) Uani 1 1 d . . . C17 C 0.3948(4) 0.2540(4) -0.0192(4) 0.053(2) Uani 1 1 d . . . H17A H 0.3546 0.2803 -0.0205 0.064 Uiso 1 1 calc R . . H17B H 0.3844 0.209 -0.0329 0.064 Uiso 1 1 calc R . . C18 C 0.4470(4) 0.2833(4) -0.0632(4) 0.0491(18) Uani 1 1 d . . . H18A H 0.4791 0.2504 -0.0775 0.059 Uiso 1 1 calc R . . H18B H 0.4281 0.305 -0.1022 0.059 Uiso 1 1 calc R . . C19 C 0.5395(4) 0.3598(4) -0.0168(4) 0.059(2) Uani 1 1 d . . . H19A H 0.5409 0.3992 -0.0447 0.07 Uiso 1 1 calc R . . H19B H 0.5736 0.3291 -0.0314 0.07 Uiso 1 1 calc R . . C20 C 0.5468(4) 0.3766(4) 0.0552(5) 0.065(2) Uani 1 1 d . . . H20A H 0.5928 0.3733 0.0692 0.077 Uiso 1 1 calc R . . H20B H 0.5311 0.4212 0.0642 0.077 Uiso 1 1 calc R . . C21 C 0.5573(5) 0.3528(5) 0.2491(5) 0.070(3) Uani 1 1 d . . . H21A H 0.5921 0.3766 0.2269 0.105 Uiso 1 1 calc R . . H21B H 0.5743 0.3115 0.2659 0.105 Uiso 1 1 calc R . . H21C H 0.5406 0.3788 0.2857 0.105 Uiso 1 1 calc R . . C22 C 0.5353(6) 0.1390(5) -0.0102(5) 0.083(3) Uani 1 1 d . . . H22A H 0.527 0.167 -0.0483 0.125 Uiso 1 1 calc R . . H22B H 0.5286 0.0935 -0.0226 0.125 Uiso 1 1 calc R . . H22C H 0.5802 0.1451 0.0046 0.125 Uiso 1 1 calc R . . C1S C 0.0861(8) 0.3549(8) 0.2615(9) 0.125(5) Uiso 1 1 d . A 1 C2S C 0.0742(8) 0.3915(10) 0.2057(9) 0.140(6) Uiso 1 1 d . A 1 H2S H 0.0704 0.4374 0.2082 0.168 Uiso 1 1 calc R A 1 C3S C 0.0682(9) 0.3612(10) 0.1491(10) 0.144(6) Uiso 1 1 d . A 1 H3S H 0.0582 0.3887 0.113 0.172 Uiso 1 1 calc R A 1 C4S C 0.0737(10) 0.2998(12) 0.1344(13) 0.180(8) Uiso 1 1 d . A 1 H4S H 0.0689 0.2846 0.0906 0.216 Uiso 1 1 calc R A 1 C5S C 0.0871(10) 0.2577(12) 0.1866(12) 0.176(8) Uiso 1 1 d . A 1 H5S H 0.0914 0.2121 0.1811 0.211 Uiso 1 1 calc R A 1 C6S C 0.0939(8) 0.2891(9) 0.2492(9) 0.136(5) Uiso 1 1 d . A 1 H6S H 0.1047 0.2623 0.2856 0.164 Uiso 1 1 calc R A 1 C7S C 0.0920(10) 0.3826(10) 0.3240(10) 0.172(7) Uiso 1 1 d . A 1 H7S1 H 0.1012 0.3485 0.3563 0.257 Uiso 0.5 1 calc PR A 1 H7S2 H 0.0513 0.4046 0.3356 0.257 Uiso 0.5 1 calc PR A 1 H7S3 H 0.1276 0.4143 0.3239 0.257 Uiso 0.5 1 calc PR A 1 H7S4 H 0.0855 0.4297 0.3209 0.257 Uiso 0.5 1 calc PR A 1 H7S5 H 0.1354 0.3736 0.3416 0.257 Uiso 0.5 1 calc PR A 1 H7S6 H 0.0591 0.364 0.3533 0.257 Uiso 0.5 1 calc PR A 1 C8S C 0.2740(7) 0.2863(7) 0.3841(8) 0.117(4) Uiso 1 1 d . B 1 C9S C 0.3130(9) 0.2592(9) 0.4363(9) 0.142(6) Uiso 1 1 d . B 1 H9S H 0.3428 0.2855 0.46 0.171 Uiso 1 1 calc R B 1 C10S C 0.3063(9) 0.1984(9) 0.4499(10) 0.146(6) Uiso 1 1 d . B 1 H10S H 0.3253 0.1801 0.4882 0.175 Uiso 1 1 calc R B 1 C11S C 0.2713(8) 0.1616(8) 0.4078(8) 0.121(5) Uiso 1 1 d . B 1 H11S H 0.2696 0.1161 0.4153 0.145 Uiso 1 1 calc R B 1 C12S C 0.2413(9) 0.1838(9) 0.3599(9) 0.140(6) Uiso 1 1 d . B 1 H12S H 0.219 0.154 0.3324 0.168 Uiso 1 1 calc R B 1 C13S C 0.2378(10) 0.2571(10) 0.3421(9) 0.153(6) Uiso 1 1 d . B 1 H13S H 0.2138 0.2763 0.3073 0.183 Uiso 1 1 calc R B 1 C14S C 0.2874(14) 0.3600(14) 0.3725(14) 0.245(12) Uiso 1 1 d . B 1 H14C H 0.316 0.3765 0.4073 0.367 Uiso 0.5 1 calc PR B 1 H14D H 0.2463 0.384 0.3732 0.367 Uiso 0.5 1 calc PR B 1 H14E H 0.3085 0.3659 0.3298 0.367 Uiso 0.5 1 calc PR B 1 H14F H 0.2646 0.3744 0.3329 0.367 Uiso 0.5 1 calc PR B 1 H14G H 0.3342 0.3669 0.367 0.367 Uiso 0.5 1 calc PR B 1 H14H H 0.272 0.385 0.4104 0.367 Uiso 0.5 1 calc PR B 1 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 Zn1 0.0436(5) 0.0414(5) 0.0490(5) 0.0042(4) -0.0012(4) -0.0010(4) Zn2 0.0493(5) 0.0455(5) 0.0502(5) 0.0040(4) -0.0065(4) -0.0023(4) Zn3 0.0609(6) 0.0463(5) 0.0501(5) 0.0041(4) 0.0044(5) 0.0054(4) N1 0.041(3) 0.053(4) 0.058(4) 0.001(3) -0.001(3) 0.008(3) N2 0.056(4) 0.045(4) 0.057(4) -0.003(3) -0.002(4) 0.004(3) N3 0.059(4) 0.049(4) 0.060(4) 0.007(3) 0.004(4) 0.012(3) N4 0.053(4) 0.051(4) 0.058(4) 0.004(3) -0.006(3) -0.016(3) N5 0.094(6) 0.041(4) 0.060(4) -0.006(3) 0.007(4) -0.015(4) N6 0.082(6) 0.054(4) 0.064(5) 0.005(4) -0.009(4) -0.024(4) N7 0.049(3) 0.039(3) 0.038(3) 0.003(3) -0.005(3) 0.003(3) N8 0.049(4) 0.049(4) 0.053(4) 0.006(3) 0.000(3) 0.008(3) N9 0.056(4) 0.044(4) 0.049(4) 0.005(3) -0.004(3) 0.001(3) N10 0.053(4) 0.042(3) 0.046(4) 0.005(3) -0.004(3) -0.002(3) N11 0.052(4) 0.049(4) 0.049(4) 0.003(3) 0.004(3) -0.015(3) N12 0.053(4) 0.049(4) 0.049(4) 0.008(3) 0.002(3) -0.006(3) C1 0.059(5) 0.041(4) 0.042(4) 0.001(3) 0.005(4) 0.004(4) C2 0.041(4) 0.071(6) 0.069(6) 0.010(5) -0.002(4) 0.004(4) C3 0.061(5) 0.065(5) 0.077(6) 0.008(5) 0.009(5) 0.019(4) C4 0.082(6) 0.058(5) 0.051(5) -0.009(4) -0.003(5) 0.013(5) C5 0.073(6) 0.039(4) 0.072(6) -0.004(4) -0.001(5) -0.007(4) C6 0.073(6) 0.044(5) 0.046(4) 0.008(4) -0.011(4) -0.015(4) C7 0.079(6) 0.045(5) 0.081(7) 0.003(4) 0.009(5) -0.014(4) C8 0.079(7) 0.090(7) 0.084(7) 0.010(6) -0.017(6) -0.032(6) C9 0.121(10) 0.068(6) 0.074(7) -0.001(5) -0.017(6) -0.039(7) C10 0.124(10) 0.052(5) 0.071(7) -0.009(5) -0.005(6) -0.025(6) C11 0.043(4) 0.045(4) 0.049(5) 0.010(3) -0.001(3) 0.002(3) C12 0.054(5) 0.049(4) 0.053(5) 0.008(4) -0.003(4) -0.003(4) C13 0.055(4) 0.052(4) 0.049(4) 0.000(4) -0.004(4) 0.002(4) C14 0.058(5) 0.067(6) 0.070(6) 0.024(5) -0.005(4) 0.002(4) C15 0.056(5) 0.057(5) 0.064(5) 0.009(4) -0.002(4) 0.008(4) C16 0.044(4) 0.044(4) 0.047(4) 0.001(3) 0.001(3) 0.003(3) C17 0.059(5) 0.054(5) 0.046(5) 0.009(4) -0.009(4) 0.002(4) C18 0.057(5) 0.046(4) 0.044(4) 0.005(4) 0.008(4) 0.001(4) C19 0.055(5) 0.055(5) 0.066(6) 0.005(4) 0.006(4) -0.007(4) C20 0.058(5) 0.066(5) 0.069(6) 0.018(5) 0.013(5) -0.002(4) C21 0.062(5) 0.069(6) 0.078(6) 0.006(5) -0.023(5) -0.015(5) C22 0.104(8) 0.085(7) 0.060(6) 0.000(5) 0.003(6) 0.037(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn1 N4 1.956(6) . ? Zn1 N1 1.963(6) . ? Zn1 N7 2.027(6) . ? Zn1 N10 2.056(7) . ? Zn2 C21 1.972(8) . ? Zn2 N2 2.006(6) . ? Zn2 N11 2.019(6) . ? Zn2 N7 2.204(6) . ? Zn3 C22 1.969(10) . ? Zn3 N8 2.009(7) . ? Zn3 N5 2.025(8) . ? Zn3 N10 2.193(6) . ? N1 C1 1.336(10) . ? N1 C2 1.481(10) . ? N2 C1 1.314(10) . ? N2 C5 1.498(10) . ? N3 C1 1.406(10) . ? N3 C3 1.422(11) . ? N3 C4 1.460(11) . ? N4 C6 1.324(11) . ? N4 C7 1.483(11) . ? N5 C6 1.310(12) . ? N5 C10 1.518(11) . ? N6 C6 1.390(11) . ? N6 C8 1.438(13) . ? N6 C9 1.448(14) . ? N7 C11 1.381(9) . ? N7 C12 1.488(10) . ? N8 C11 1.297(10) . ? N8 C15 1.496(10) . ? N9 C11 1.373(9) . ? N9 C13 1.466(10) . ? N9 C14 1.468(11) . ? N10 C16 1.345(10) . ? N10 C17 1.497(10) . ? N11 C16 1.305(10) . ? N11 C20 1.493(10) . ? N12 C16 1.376(10) . ? N12 C18 1.449(10) . ? N12 C19 1.467(10) . ? C2 C3 1.541(13) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.497(13) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C7 C8 1.516(14) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.510(16) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C12 C13 1.569(11) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.508(13) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C17 C18 1.524(11) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.514(13) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C1S C2S 1.39(2) . ? C1S C6S 1.39(2) . ? C1S C7S 1.40(2) . ? C2S C3S 1.32(2) . ? C2S H2S 0.95 . ? C3S C4S 1.30(2) . ? C3S H3S 0.95 . ? C4S C5S 1.40(3) . ? C4S H4S 0.95 . ? C5S C6S 1.44(3) . ? C5S H5S 0.95 . ? C6S H6S 0.95 . ? C7S H7S1 0.98 . ? C7S H7S2 0.98 . ? C7S H7S3 0.98 . ? C7S H7S4 0.98 . ? C7S H7S5 0.98 . ? C7S H7S6 0.98 . ? C8S C13S 1.28(2) . ? C8S C9S 1.44(2) . ? C8S C14S 1.56(3) . ? C9S C10S 1.29(2) . ? C9S H9S 0.95 . ? C10S C11S 1.35(2) . ? C10S H10S 0.95 . ? C11S C12S 1.24(2) . ? C11S H11S 0.95 . ? C12S C13S 1.55(2) . ? C12S H12S 0.95 . ? C13S H13S 0.95 . ? C14S H14C 0.98 . ? C14S H14D 0.98 . ? C14S H14E 0.98 . ? C14S H14F 0.98 . ? C14S H14G 0.98 . ? C14S H14H 0.98 . ? 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 N4 Zn1 N1 117.6(3) . . ? N4 Zn1 N7 116.5(3) . . ? N1 Zn1 N7 102.2(3) . . ? N4 Zn1 N10 101.6(3) . . ? N1 Zn1 N10 117.0(3) . . ? N7 Zn1 N10 101.3(2) . . ? C21 Zn2 N2 116.4(4) . . ? C21 Zn2 N11 120.0(4) . . ? N2 Zn2 N11 103.4(3) . . ? C21 Zn2 N7 116.9(3) . . ? N2 Zn2 N7 95.7(2) . . ? N11 Zn2 N7 100.7(2) . . ? C22 Zn3 N8 122.2(4) . . ? C22 Zn3 N5 114.4(4) . . ? N8 Zn3 N5 104.6(3) . . ? C22 Zn3 N10 114.7(4) . . ? N8 Zn3 N10 101.7(2) . . ? N5 Zn3 N10 95.2(3) . . ? C1 N1 C2 106.4(7) . . ? C1 N1 Zn1 121.9(5) . . ? C2 N1 Zn1 131.7(5) . . ? C1 N2 C5 104.7(6) . . ? C1 N2 Zn2 129.7(5) . . ? C5 N2 Zn2 125.6(5) . . ? C1 N3 C3 107.4(6) . . ? C1 N3 C4 103.4(6) . . ? C3 N3 C4 127.3(8) . . ? C6 N4 C7 107.4(7) . . ? C6 N4 Zn1 123.2(6) . . ? C7 N4 Zn1 129.3(6) . . ? C6 N5 C10 105.0(8) . . ? C6 N5 Zn3 130.3(5) . . ? C10 N5 Zn3 124.4(7) . . ? C6 N6 C8 105.5(7) . . ? C6 N6 C9 104.2(8) . . ? C8 N6 C9 127.5(8) . . ? C11 N7 C12 104.4(6) . . ? C11 N7 Zn1 118.7(5) . . ? C12 N7 Zn1 118.0(5) . . ? C11 N7 Zn2 107.3(5) . . ? C12 N7 Zn2 107.1(4) . . ? Zn1 N7 Zn2 100.5(2) . . ? C11 N8 C15 104.0(6) . . ? C11 N8 Zn3 125.8(5) . . ? C15 N8 Zn3 123.8(5) . . ? C11 N9 C13 108.1(6) . . ? C11 N9 C14 105.4(6) . . ? C13 N9 C14 129.2(7) . . ? C16 N10 C17 103.4(6) . . ? C16 N10 Zn1 117.3(5) . . ? C17 N10 Zn1 118.5(5) . . ? C16 N10 Zn3 109.6(5) . . ? C17 N10 Zn3 107.2(5) . . ? Zn1 N10 Zn3 100.3(3) . . ? C16 N11 C20 105.0(7) . . ? C16 N11 Zn2 127.2(5) . . ? C20 N11 Zn2 121.0(5) . . ? C16 N12 C18 106.7(6) . . ? C16 N12 C19 104.3(6) . . ? C18 N12 C19 130.3(6) . . ? N2 C1 N1 132.4(7) . . ? N2 C1 N3 115.6(7) . . ? N1 C1 N3 111.9(7) . . ? N1 C2 C3 104.0(7) . . ? N1 C2 H2A 111 . . ? C3 C2 H2A 111 . . ? N1 C2 H2B 111 . . ? C3 C2 H2B 111 . . ? H2A C2 H2B 109 . . ? N3 C3 C2 100.7(7) . . ? N3 C3 H3A 111.6 . . ? C2 C3 H3A 111.6 . . ? N3 C3 H3B 111.6 . . ? C2 C3 H3B 111.6 . . ? H3A C3 H3B 109.4 . . ? N3 C4 C5 102.7(7) . . ? N3 C4 H4A 111.2 . . ? C5 C4 H4A 111.2 . . ? N3 C4 H4B 111.2 . . ? C5 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? C4 C5 N2 104.3(7) . . ? C4 C5 H5A 110.9 . . ? N2 C5 H5A 110.9 . . ? C4 C5 H5B 110.9 . . ? N2 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? N5 C6 N4 131.4(7) . . ? N5 C6 N6 115.6(8) . . ? N4 C6 N6 112.9(8) . . ? N4 C7 C8 102.6(8) . . ? N4 C7 H7A 111.3 . . ? C8 C7 H7A 111.3 . . ? N4 C7 H7B 111.3 . . ? C8 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? N6 C8 C7 103.0(8) . . ? N6 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? N6 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? N6 C9 C10 102.9(8) . . ? N6 C9 H9A 111.2 . . ? C10 C9 H9A 111.2 . . ? N6 C9 H9B 111.2 . . ? C10 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? C9 C10 N5 102.7(9) . . ? C9 C10 H10A 111.2 . . ? N5 C10 H10A 111.2 . . ? C9 C10 H10B 111.2 . . ? N5 C10 H10B 111.2 . . ? H10A C10 H10B 109.1 . . ? N8 C11 N9 116.2(6) . . ? N8 C11 N7 130.4(7) . . ? N9 C11 N7 113.4(7) . . ? N7 C12 C13 103.9(6) . . ? N7 C12 H12A 111 . . ? C13 C12 H12A 111 . . ? N7 C12 H12B 111 . . ? C13 C12 H12B 111 . . ? H12A C12 H12B 109 . . ? N9 C13 C12 99.0(6) . . ? N9 C13 H13A 112 . . ? C12 C13 H13A 112 . . ? N9 C13 H13B 112 . . ? C12 C13 H13B 112 . . ? H13A C13 H13B 109.7 . . ? N9 C14 C15 99.7(6) . . ? N9 C14 H14A 111.8 . . ? C15 C14 H14A 111.8 . . ? N9 C14 H14B 111.8 . . ? C15 C14 H14B 111.8 . . ? H14A C14 H14B 109.6 . . ? N8 C15 C14 105.7(7) . . ? N8 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? N8 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? N11 C16 N10 129.6(7) . . ? N11 C16 N12 116.1(7) . . ? N10 C16 N12 114.2(7) . . ? N10 C17 C18 104.0(6) . . ? N10 C17 H17A 110.9 . . ? C18 C17 H17A 110.9 . . ? N10 C17 H17B 110.9 . . ? C18 C17 H17B 110.9 . . ? H17A C17 H17B 109 . . ? N12 C18 C17 99.5(6) . . ? N12 C18 H18A 111.9 . . ? C17 C18 H18A 111.9 . . ? N12 C18 H18B 111.9 . . ? C17 C18 H18B 111.9 . . ? H18A C18 H18B 109.6 . . ? N12 C19 C20 101.4(6) . . ? N12 C19 H19A 111.5 . . ? C20 C19 H19A 111.5 . . ? N12 C19 H19B 111.5 . . ? C20 C19 H19B 111.5 . . ? H19A C19 H19B 109.3 . . ? N11 C20 C19 104.1(7) . . ? N11 C20 H20A 110.9 . . ? C19 C20 H20A 110.9 . . ? N11 C20 H20B 110.9 . . ? C19 C20 H20B 110.9 . . ? H20A C20 H20B 109 . . ? Zn2 C21 H21A 109.5 . . ? Zn2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Zn2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Zn3 C22 H22A 109.5 . . ? Zn3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Zn3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2S C1S C6S 113.8(18) . . ? C2S C1S C7S 122.6(18) . . ? C6S C1S C7S 123.5(18) . . ? C3S C2S C1S 118.5(19) . . ? C3S C2S H2S 120.7 . . ? C1S C2S H2S 120.7 . . ? C4S C3S C2S 131(2) . . ? C4S C3S H3S 114.6 . . ? C2S C3S H3S 114.6 . . ? C3S C4S C5S 116(2) . . ? C3S C4S H4S 121.9 . . ? C5S C4S H4S 121.9 . . ? C4S C5S C6S 115(2) . . ? C4S C5S H5S 122.7 . . ? C6S C5S H5S 122.7 . . ? C1S C6S C5S 126.0(19) . . ? C1S C6S H6S 117 . . ? C5S C6S H6S 117 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C1S C7S H7S4 109.5 . . ? H7S1 C7S H7S4 141.1 . . ? H7S2 C7S H7S4 56.3 . . ? H7S3 C7S H7S4 56.3 . . ? C1S C7S H7S5 109.5 . . ? H7S1 C7S H7S5 56.3 . . ? H7S2 C7S H7S5 141.1 . . ? H7S3 C7S H7S5 56.3 . . ? H7S4 C7S H7S5 109.5 . . ? C1S C7S H7S6 109.5 . . ? H7S1 C7S H7S6 56.3 . . ? H7S2 C7S H7S6 56.3 . . ? H7S3 C7S H7S6 141.1 . . ? H7S4 C7S H7S6 109.5 . . ? H7S5 C7S H7S6 109.5 . . ? C13S C8S C9S 129.2(18) . . ? C13S C8S C14S 117.3(19) . . ? C9S C8S C14S 112.8(18) . . ? C10S C9S C8S 118.3(19) . . ? C10S C9S H9S 120.9 . . ? C8S C9S H9S 120.9 . . ? C9S C10S C11S 118(2) . . ? C9S C10S H10S 121.1 . . ? C11S C10S H10S 121.1 . . ? C12S C11S C10S 123.8(19) . . ? C12S C11S H11S 118.1 . . ? C10S C11S H11S 118.1 . . ? C11S C12S C13S 124(2) . . ? C11S C12S H12S 117.8 . . ? C13S C12S H12S 117.8 . . ? C8S C13S C12S 105.8(18) . . ? C8S C13S H13S 127.1 . . ? C12S C13S H13S 127.1 . . ? C8S C14S H14C 109.5 . . ? C8S C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? C8S C14S H14E 109.5 . . ? H14C C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? C8S C14S H14F 109.5 . . ? H14C C14S H14F 141.1 . . ? H14D C14S H14F 56.3 . . ? H14E C14S H14F 56.3 . . ? C8S C14S H14G 109.5 . . ? H14C C14S H14G 56.3 . . ? H14D C14S H14G 141.1 . . ? H14E C14S H14G 56.3 . . ? H14F C14S H14G 109.5 . . ? C8S C14S H14H 109.5 . . ? H14C C14S H14H 56.3 . . ? H14D C14S H14H 56.3 . . ? H14E C14S H14H 141.1 . . ? H14F C14S H14H 109.5 . . ? H14G C14S H14H 109.5 . . ? #===END