# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rem463 _database_code_depnum_ccdc_archive 'CCDC 892941' #TrackingRef 'Hara_1353510871.Submissioncif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 N4 Na2 O2, C7 H8' _chemical_formula_sum 'C47 H58 N4 Na2 O2' _chemical_formula_weight 756.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.873(5) _cell_length_b 17.818(10) _cell_length_c 18.828(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.96(2) _cell_angle_gamma 90.00 _cell_volume 4496(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8552 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37051 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7791 _reflns_number_gt 3895 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution Bruker _computing_structure_refinement Bruker _computing_molecular_graphics 'Mercury 1.5' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Summary of restraints: Similarity of geometry (bond lengths and angles) for the two components of each of the 3 disordered groups (SHELXL SAME instructions) Similarity of anisotropic displacement parameters of atoms in positions close together (mainly disorder components; SHELXL SIMU instructions) Similarity of components of displacement of bonded atoms along the bonds joining them (so-called 'rigid bond' approximation), and also of atoms separated by 2 bonds (1-3 as well as 1-2 connections) (SHELXL DELU instructions) Approximate isotropic behaviour of anisotropically refined atoms (a relatively weak restraint; SHELXL ISOR instructions) Minor disorder component atoms of tmeda ligands were refined with isotropic rather than anisotropic displacement parameters because the occupancy factor <0.5 corresponds to a low electron density and hence high uncertainties for displacement parameters. ; _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^)+(0.0421P)^2^+5.3919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7791 _refine_ls_number_parameters 646 _refine_ls_number_restraints 1358 _refine_ls_R_factor_all 0.1695 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.06873(9) 0.81459(7) 0.16874(7) 0.0470(3) Uani 1 1 d U . . Na2 Na 0.21316(10) 0.79348(8) 0.06554(7) 0.0618(4) Uani 1 1 d U A . O1 O 0.04965(17) 0.81095(14) 0.04723(12) 0.0596(7) Uani 1 1 d U A . O2 O 0.22815(17) 0.78470(15) 0.18648(13) 0.0663(7) Uani 1 1 d U A . N1 N -0.0055(2) 0.74067(16) 0.24864(18) 0.0566(8) Uani 1 1 d U A . N2 N -0.0044(2) 0.91093(16) 0.23357(17) 0.0589(8) Uani 1 1 d U A . N3 N 0.3113(2) 0.87712(18) 0.00755(16) 0.0633(8) Uani 1 1 d U . . N4 N 0.3097(3) 0.70532(19) 0.01058(18) 0.0708(9) Uani 1 1 d U . . C1 C -0.0258(16) 0.7915(7) 0.0028(15) 0.038(2) Uani 0.55(2) 1 d PDU A 1 C2 C -0.0495(13) 0.7126(6) 0.0049(10) 0.042(2) Uani 0.55(2) 1 d PDU A 1 C3 C 0.0140(12) 0.6639(6) 0.0562(8) 0.053(3) Uani 0.55(2) 1 d PDU A 1 H3 H 0.0733 0.6826 0.0887 0.064 Uiso 0.55(2) 1 calc PR A 1 C4 C -0.0116(12) 0.5891(6) 0.0583(8) 0.065(3) Uani 0.55(2) 1 d PDU A 1 H4 H 0.0310 0.5566 0.0925 0.078 Uiso 0.55(2) 1 calc PR A 1 C5 C -0.0988(14) 0.5597(6) 0.0111(11) 0.071(4) Uani 0.55(2) 1 d PDU A 1 H5 H -0.1139 0.5079 0.0131 0.085 Uiso 0.55(2) 1 calc PR A 1 C6 C -0.1609(12) 0.6048(6) -0.0370(9) 0.068(3) Uani 0.55(2) 1 d PDU A 1 H6 H -0.2205 0.5844 -0.0677 0.081 Uiso 0.55(2) 1 calc PR A 1 C7 C -0.1394(13) 0.6839(6) -0.0431(10) 0.047(3) Uani 0.55(2) 1 d PDU A 1 C8 C -0.2022(15) 0.7309(9) -0.0939(11) 0.054(3) Uani 0.55(2) 1 d PDU A 1 H8 H -0.2593 0.7093 -0.1266 0.065 Uiso 0.55(2) 1 calc PR A 1 C1A C -0.0398(18) 0.7809(10) -0.0002(16) 0.038(3) Uani 0.45(2) 1 d PDU A 2 C2A C -0.0776(15) 0.7047(8) -0.0092(12) 0.043(3) Uani 0.45(2) 1 d PDU A 2 C3A C -0.0228(14) 0.6469(9) 0.0365(11) 0.064(4) Uani 0.45(2) 1 d PDU A 2 H3A H 0.0386 0.6585 0.0709 0.076 Uiso 0.45(2) 1 calc PR A 2 C4A C -0.0587(19) 0.5735(10) 0.0310(13) 0.079(5) Uani 0.45(2) 1 d PDU A 2 H4A H -0.0261 0.5364 0.0650 0.095 Uiso 0.45(2) 1 calc PR A 2 C5A C -0.1428(15) 0.5550(8) -0.0249(12) 0.076(4) Uani 0.45(2) 1 d PDU A 2 H5A H -0.1637 0.5040 -0.0308 0.091 Uiso 0.45(2) 1 calc PR A 2 C6A C -0.1953(13) 0.6070(6) -0.0705(11) 0.062(3) Uani 0.45(2) 1 d PDU A 2 H6A H -0.2539 0.5923 -0.1063 0.075 Uiso 0.45(2) 1 calc PR A 2 C7A C -0.1649(14) 0.6853(7) -0.0665(12) 0.044(3) Uani 0.45(2) 1 d PDU A 2 C8A C -0.2201(16) 0.7392(9) -0.1118(13) 0.042(3) Uani 0.45(2) 1 d PDU A 2 H8A H -0.2785 0.7272 -0.1492 0.050 Uiso 0.45(2) 1 calc PR A 2 C9 C -0.1857(2) 0.81085(18) -0.09963(17) 0.0411(8) Uani 1 1 d U . . C10 C -0.2449(2) 0.8655(2) -0.14769(18) 0.0543(9) Uani 1 1 d U A . H10 H -0.3038 0.8494 -0.1825 0.065 Uiso 1 1 calc R . . C11 C -0.2204(3) 0.9383(2) -0.1454(2) 0.0606(10) Uani 1 1 d U . . H11 H -0.2618 0.9727 -0.1781 0.073 Uiso 1 1 calc R A . C12 C -0.1336(3) 0.9641(2) -0.0948(2) 0.0577(10) Uani 1 1 d U A . H12 H -0.1168 1.0159 -0.0929 0.069 Uiso 1 1 calc R . . C13 C -0.0739(2) 0.91488(18) -0.04858(18) 0.0436(8) Uani 1 1 d U . . H13 H -0.0149 0.9329 -0.0152 0.052 Uiso 1 1 calc R A . C14 C -0.0967(2) 0.83739(17) -0.04863(15) 0.0341(7) Uani 1 1 d U A . C15 C 0.3102(3) 0.7637(2) 0.23355(18) 0.0497(8) Uani 1 1 d U . . C16 C 0.3399(3) 0.6859(2) 0.2468(2) 0.0623(10) Uani 1 1 d U A . C17 C 0.2759(4) 0.6282(3) 0.2104(3) 0.0908(13) Uani 1 1 d U . . H17 H 0.2129 0.6401 0.1782 0.109 Uiso 1 1 calc R A . C18 C 0.3083(5) 0.5493(3) 0.2230(3) 0.0972(15) Uani 1 1 d U A . H18 H 0.2672 0.5089 0.2001 0.117 Uiso 1 1 calc R . . C19 C 0.4007(5) 0.5376(3) 0.2694(3) 0.0992(16) Uani 1 1 d U . . H19 H 0.4232 0.4871 0.2759 0.119 Uiso 1 1 calc R A . C20 C 0.4625(4) 0.5902(3) 0.3065(3) 0.0898(14) Uani 1 1 d U A . H20 H 0.5245 0.5757 0.3385 0.108 Uiso 1 1 calc R . . C21 C 0.4363(3) 0.6676(2) 0.2984(2) 0.0576(10) Uani 1 1 d U . . C22 C 0.4944(3) 0.7236(3) 0.3359(2) 0.0667(11) Uani 1 1 d U A . H22 H 0.5559 0.7107 0.3694 0.080 Uiso 1 1 calc R . . C23 C 0.4683(3) 0.7969(2) 0.32748(19) 0.0576(9) Uani 1 1 d U . . C24 C 0.5297(3) 0.8579(3) 0.3695(2) 0.0653(11) Uani 1 1 d U A . H24 H 0.5910 0.8464 0.4040 0.078 Uiso 1 1 calc R . . C25 C 0.4990(4) 0.9294(3) 0.3590(3) 0.0919(14) Uani 1 1 d U . . H25 H 0.5385 0.9676 0.3877 0.110 Uiso 1 1 calc R A . C26 C 0.4129(4) 0.9492(3) 0.3084(3) 0.0901(14) Uani 1 1 d U A . H26 H 0.3945 1.0005 0.3009 0.108 Uiso 1 1 calc R . . C27 C 0.3543(3) 0.8949(2) 0.2693(2) 0.0656(10) Uani 1 1 d U . . H27 H 0.2940 0.9098 0.2352 0.079 Uiso 1 1 calc R A . C28 C 0.3769(2) 0.8180(2) 0.27577(17) 0.0459(8) Uani 1 1 d U A . C29 C -0.0967(6) 0.7081(6) 0.2174(5) 0.078(3) Uani 0.720(7) 1 d PDU A 1 H29A H -0.1446 0.7470 0.1944 0.117 Uiso 0.720(7) 1 calc PR A 1 H29B H -0.1208 0.6823 0.2555 0.117 Uiso 0.720(7) 1 calc PR A 1 H29C H -0.0895 0.6718 0.1800 0.117 Uiso 0.720(7) 1 calc PR A 1 C30 C 0.0676(5) 0.6790(4) 0.2867(4) 0.082(2) Uani 0.720(7) 1 d PDU A 1 H30A H 0.0438 0.6568 0.3267 0.123 Uiso 0.720(7) 1 calc PR A 1 H30B H 0.1338 0.7010 0.3068 0.123 Uiso 0.720(7) 1 calc PR A 1 H30C H 0.0717 0.6400 0.2509 0.123 Uiso 0.720(7) 1 calc PR A 1 C31 C -0.0075(4) 0.7955(3) 0.3089(3) 0.0588(16) Uani 0.720(7) 1 d PDU A 1 H31A H -0.0446 0.7732 0.3422 0.071 Uiso 0.720(7) 1 calc PR A 1 H31B H 0.0616 0.8054 0.3381 0.071 Uiso 0.720(7) 1 calc PR A 1 C32 C -0.0545(12) 0.8660(4) 0.2794(7) 0.080(3) Uani 0.720(7) 1 d PDU A 1 H32A H -0.0608 0.8976 0.3213 0.096 Uiso 0.720(7) 1 calc PR A 1 H32B H -0.1230 0.8547 0.2498 0.096 Uiso 0.720(7) 1 calc PR A 1 C33 C 0.0805(13) 0.9548(10) 0.2810(8) 0.084(3) Uani 0.720(7) 1 d PDU A 1 H33A H 0.0551 0.9885 0.3131 0.126 Uiso 0.720(7) 1 calc PR A 1 H33B H 0.1128 0.9844 0.2498 0.126 Uiso 0.720(7) 1 calc PR A 1 H33C H 0.1292 0.9202 0.3111 0.126 Uiso 0.720(7) 1 calc PR A 1 C34 C -0.0763(11) 0.9644(7) 0.1883(7) 0.089(4) Uani 0.720(7) 1 d PDU A 1 H34A H -0.1324 0.9367 0.1571 0.133 Uiso 0.720(7) 1 calc PR A 1 H34B H -0.0431 0.9936 0.1573 0.133 Uiso 0.720(7) 1 calc PR A 1 H34C H -0.1010 0.9985 0.2205 0.133 Uiso 0.720(7) 1 calc PR A 1 C29A C -0.0795(17) 0.6759(13) 0.2018(15) 0.080(7) Uani 0.280(7) 1 d PDU A 2 H29D H -0.1197 0.6541 0.2325 0.119 Uiso 0.280(7) 1 calc PR A 2 H29E H -0.0393 0.6364 0.1872 0.119 Uiso 0.280(7) 1 calc PR A 2 H29F H -0.1237 0.6984 0.1578 0.119 Uiso 0.280(7) 1 calc PR A 2 C30A C 0.0539(15) 0.7172(12) 0.3042(12) 0.089(7) Uiso 0.280(7) 1 d PDU A 2 H30D H 0.0179 0.7031 0.3406 0.134 Uiso 0.280(7) 1 calc PR A 2 H30E H 0.1025 0.7566 0.3245 0.134 Uiso 0.280(7) 1 calc PR A 2 H30F H 0.0887 0.6733 0.2917 0.134 Uiso 0.280(7) 1 calc PR A 2 C31A C -0.0942(11) 0.7968(7) 0.2556(8) 0.068(5) Uiso 0.280(7) 1 d PDU A 2 H31C H -0.1427 0.8009 0.2068 0.082 Uiso 0.280(7) 1 calc PR A 2 H31D H -0.1296 0.7744 0.2898 0.082 Uiso 0.280(7) 1 calc PR A 2 C32A C -0.062(3) 0.8722(11) 0.2813(17) 0.079(8) Uiso 0.280(7) 1 d PDU A 2 H32C H -0.0186 0.8690 0.3322 0.095 Uiso 0.280(7) 1 calc PR A 2 H32D H -0.1206 0.9028 0.2824 0.095 Uiso 0.280(7) 1 calc PR A 2 C33A C 0.060(4) 0.966(3) 0.273(3) 0.107(15) Uiso 0.280(7) 1 d PDU A 2 H33D H 0.0209 1.0031 0.2920 0.161 Uiso 0.280(7) 1 calc PR A 2 H33E H 0.0945 0.9908 0.2401 0.161 Uiso 0.280(7) 1 calc PR A 2 H33F H 0.1087 0.9425 0.3138 0.161 Uiso 0.280(7) 1 calc PR A 2 C34A C -0.081(3) 0.945(2) 0.1686(18) 0.082(8) Uani 0.280(7) 1 d PDU A 2 H34D H -0.1145 0.9052 0.1359 0.123 Uiso 0.280(7) 1 calc PR A 2 H34E H -0.0467 0.9788 0.1417 0.123 Uiso 0.280(7) 1 calc PR A 2 H34F H -0.1299 0.9738 0.1866 0.123 Uiso 0.280(7) 1 calc PR A 2 C35 C 0.3750(6) 0.9116(6) 0.0713(5) 0.075(2) Uani 0.560(8) 1 d PDU A 1 H35A H 0.4309 0.9362 0.0579 0.113 Uiso 0.560(8) 1 calc PR A 1 H35B H 0.4006 0.8732 0.1087 0.113 Uiso 0.560(8) 1 calc PR A 1 H35C H 0.3370 0.9489 0.0911 0.113 Uiso 0.560(8) 1 calc PR A 1 C36 C 0.2439(11) 0.9327(7) -0.0430(6) 0.092(4) Uani 0.560(8) 1 d PDU A 1 H36A H 0.2844 0.9665 -0.0644 0.138 Uiso 0.560(8) 1 calc PR A 1 H36B H 0.2068 0.9620 -0.0148 0.138 Uiso 0.560(8) 1 calc PR A 1 H36C H 0.1969 0.9055 -0.0823 0.138 Uiso 0.560(8) 1 calc PR A 1 C37 C 0.3572(6) 0.8306(4) -0.0360(5) 0.053(2) Uani 0.560(8) 1 d PDU A 1 H37A H 0.4122 0.8590 -0.0481 0.064 Uiso 0.560(8) 1 calc PR A 1 H37B H 0.3074 0.8192 -0.0828 0.064 Uiso 0.560(8) 1 calc PR A 1 C38 C 0.3997(6) 0.7551(4) 0.0013(5) 0.073(2) Uani 0.560(8) 1 d PDU A 1 H38A H 0.4460 0.7651 0.0499 0.087 Uiso 0.560(8) 1 calc PR A 1 H38B H 0.4368 0.7285 -0.0295 0.087 Uiso 0.560(8) 1 calc PR A 1 C39 C 0.3697(8) 0.6424(7) 0.0607(5) 0.075(3) Uani 0.560(8) 1 d PDU A 1 H39A H 0.4136 0.6172 0.0350 0.113 Uiso 0.560(8) 1 calc PR A 1 H39B H 0.3232 0.6059 0.0723 0.113 Uiso 0.560(8) 1 calc PR A 1 H39C H 0.4100 0.6648 0.1063 0.113 Uiso 0.560(8) 1 calc PR A 1 C40 C 0.2645(8) 0.6701(6) -0.0561(5) 0.097(3) Uani 0.560(8) 1 d PDU A 1 H40A H 0.3146 0.6414 -0.0730 0.145 Uiso 0.560(8) 1 calc PR A 1 H40B H 0.2350 0.7081 -0.0930 0.145 Uiso 0.560(8) 1 calc PR A 1 H40C H 0.2121 0.6361 -0.0492 0.145 Uiso 0.560(8) 1 calc PR A 1 C35A C 0.3795(10) 0.9410(7) 0.0505(7) 0.080(4) Uiso 0.440(8) 1 d PDU A 2 H35D H 0.4117 0.9675 0.0172 0.120 Uiso 0.440(8) 1 calc PR A 2 H35E H 0.4307 0.9191 0.0911 0.120 Uiso 0.440(8) 1 calc PR A 2 H35F H 0.3389 0.9764 0.0702 0.120 Uiso 0.440(8) 1 calc PR A 2 C36A C 0.2553(14) 0.9143(11) -0.0564(10) 0.096(6) Uiso 0.440(8) 1 d PDU A 2 H36D H 0.2209 0.9576 -0.0422 0.144 Uiso 0.440(8) 1 calc PR A 2 H36E H 0.2059 0.8795 -0.0857 0.144 Uiso 0.440(8) 1 calc PR A 2 H36F H 0.3002 0.9314 -0.0857 0.144 Uiso 0.440(8) 1 calc PR A 2 C37A C 0.3888(9) 0.8225(6) -0.0117(7) 0.063(4) Uiso 0.440(8) 1 d PDU A 2 H37C H 0.4392 0.8062 0.0331 0.076 Uiso 0.440(8) 1 calc PR A 2 H37D H 0.4231 0.8460 -0.0461 0.076 Uiso 0.440(8) 1 calc PR A 2 C38A C 0.3209(9) 0.7545(6) -0.0492(6) 0.088(4) Uiso 0.440(8) 1 d PDU A 2 H38C H 0.2550 0.7729 -0.0778 0.105 Uiso 0.440(8) 1 calc PR A 2 H38D H 0.3529 0.7271 -0.0828 0.105 Uiso 0.440(8) 1 calc PR A 2 C39A C 0.3823(13) 0.6738(9) 0.0548(10) 0.099(6) Uiso 0.440(8) 1 d PDU A 2 H39D H 0.3581 0.6453 0.0912 0.148 Uiso 0.440(8) 1 calc PR A 2 H39E H 0.4299 0.7119 0.0799 0.148 Uiso 0.440(8) 1 calc PR A 2 H39F H 0.4153 0.6397 0.0277 0.148 Uiso 0.440(8) 1 calc PR A 2 C40A C 0.2246(10) 0.6481(8) -0.0236(8) 0.105(4) Uiso 0.440(8) 1 d PDU A 2 H40D H 0.2443 0.6177 -0.0608 0.157 Uiso 0.440(8) 1 calc PR A 2 H40E H 0.1632 0.6755 -0.0464 0.157 Uiso 0.440(8) 1 calc PR A 2 H40F H 0.2130 0.6153 0.0152 0.157 Uiso 0.440(8) 1 calc PR A 2 C41 C -0.3371(4) 0.6320(3) 0.1007(3) 0.128(2) Uani 1 1 d U . . H41A H -0.3839 0.6167 0.0546 0.192 Uiso 1 1 calc R . . H41B H -0.3550 0.6074 0.1421 0.192 Uiso 1 1 calc R . . H41C H -0.2692 0.6175 0.1000 0.192 Uiso 1 1 calc R . . C42 C -0.3419(3) 0.7141(3) 0.1090(3) 0.0786(12) Uani 1 1 d U . . C43 C -0.3771(3) 0.7476(3) 0.1670(2) 0.0775(12) Uani 1 1 d U . . H43 H -0.3988 0.7167 0.2010 0.093 Uiso 1 1 calc R . . C44 C -0.3792(3) 0.8239(3) 0.1732(2) 0.0801(12) Uani 1 1 d U . . H44 H -0.4025 0.8452 0.2119 0.096 Uiso 1 1 calc R . . C45 C -0.3488(3) 0.8707(3) 0.1255(2) 0.0820(13) Uani 1 1 d U . . H45 H -0.3502 0.9236 0.1312 0.098 Uiso 1 1 calc R . . C46 C -0.3165(3) 0.8395(3) 0.0693(2) 0.0775(12) Uani 1 1 d U . . H46 H -0.2964 0.8711 0.0351 0.093 Uiso 1 1 calc R . . C47 C -0.3128(3) 0.7631(3) 0.0619(2) 0.0743(12) Uani 1 1 d U . . H47 H -0.2891 0.7432 0.0227 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0447(7) 0.0548(8) 0.0447(7) 0.0057(6) 0.0172(6) 0.0055(6) Na2 0.0459(8) 0.0886(11) 0.0557(9) 0.0208(8) 0.0216(7) 0.0173(7) O1 0.0422(13) 0.0881(19) 0.0445(13) 0.0027(13) 0.0040(11) 0.0196(13) O2 0.0426(13) 0.105(2) 0.0497(14) 0.0128(14) 0.0090(11) 0.0034(13) N1 0.0617(19) 0.0485(18) 0.069(2) 0.0025(15) 0.0341(17) 0.0005(15) N2 0.070(2) 0.0478(18) 0.070(2) 0.0088(15) 0.0379(17) 0.0078(15) N3 0.070(2) 0.074(2) 0.0500(18) 0.0010(16) 0.0231(16) 0.0019(17) N4 0.092(2) 0.071(2) 0.057(2) -0.0020(17) 0.0321(19) -0.0055(19) C1 0.039(5) 0.034(4) 0.051(4) -0.004(4) 0.027(4) -0.004(4) C2 0.043(7) 0.045(4) 0.047(6) 0.002(3) 0.026(4) 0.000(4) C3 0.075(8) 0.039(4) 0.052(6) 0.002(4) 0.027(5) 0.006(4) C4 0.087(8) 0.042(5) 0.081(8) 0.010(5) 0.049(5) 0.009(5) C5 0.103(13) 0.035(5) 0.088(12) -0.010(5) 0.050(8) -0.013(5) C6 0.082(8) 0.043(5) 0.088(9) -0.020(5) 0.042(6) -0.017(5) C7 0.062(9) 0.041(4) 0.050(10) -0.008(4) 0.037(5) -0.012(4) C8 0.046(7) 0.060(5) 0.053(9) -0.018(5) 0.007(5) -0.020(6) C1A 0.035(6) 0.055(6) 0.028(5) 0.003(6) 0.017(4) 0.007(5) C2A 0.046(10) 0.043(5) 0.048(9) 0.009(6) 0.027(5) 0.023(4) C3A 0.070(9) 0.058(7) 0.066(9) 0.012(7) 0.024(6) 0.023(6) C4A 0.102(15) 0.049(8) 0.092(13) 0.015(10) 0.036(8) 0.025(9) C5A 0.099(10) 0.043(6) 0.098(11) 0.000(6) 0.047(7) 0.015(6) C6A 0.070(8) 0.044(5) 0.085(11) -0.003(5) 0.042(6) 0.002(5) C7A 0.049(8) 0.045(4) 0.049(10) -0.010(5) 0.029(5) 0.002(5) C8A 0.034(7) 0.046(5) 0.049(9) -0.006(5) 0.019(5) 0.004(4) C9 0.0386(18) 0.0477(19) 0.0411(18) -0.0107(15) 0.0175(15) -0.0043(15) C10 0.0376(19) 0.081(3) 0.0389(19) -0.0083(19) 0.0007(16) 0.0007(19) C11 0.051(2) 0.069(3) 0.058(2) 0.016(2) 0.0093(19) 0.017(2) C12 0.062(2) 0.040(2) 0.074(3) 0.0067(18) 0.024(2) 0.0072(18) C13 0.0379(18) 0.0431(19) 0.049(2) -0.0094(16) 0.0104(15) -0.0040(16) C14 0.0324(16) 0.0401(18) 0.0320(16) -0.0034(13) 0.0120(13) 0.0019(14) C15 0.046(2) 0.069(2) 0.0411(19) 0.0133(17) 0.0232(16) 0.0090(18) C16 0.082(3) 0.065(2) 0.056(2) -0.0020(19) 0.048(2) -0.008(2) C17 0.116(4) 0.102(3) 0.074(3) -0.008(3) 0.061(3) -0.015(3) C18 0.134(4) 0.084(3) 0.098(4) -0.014(3) 0.074(3) -0.017(3) C19 0.127(4) 0.083(3) 0.110(4) -0.004(3) 0.070(3) -0.013(3) C20 0.103(4) 0.076(3) 0.108(4) 0.016(3) 0.059(3) 0.017(3) C21 0.074(3) 0.054(2) 0.062(2) 0.0300(18) 0.049(2) 0.0299(19) C22 0.058(2) 0.080(3) 0.070(3) 0.020(2) 0.031(2) 0.015(2) C23 0.049(2) 0.082(3) 0.049(2) 0.0225(19) 0.0246(17) 0.0123(19) C24 0.042(2) 0.101(3) 0.050(2) 0.006(2) 0.0073(17) -0.004(2) C25 0.098(4) 0.084(3) 0.097(4) 0.004(3) 0.030(3) -0.005(3) C26 0.104(4) 0.072(3) 0.098(4) 0.008(3) 0.032(3) 0.003(3) C27 0.070(3) 0.066(3) 0.064(3) 0.013(2) 0.021(2) 0.002(2) C28 0.0345(17) 0.067(2) 0.0381(18) 0.0199(17) 0.0131(14) 0.0117(17) C29 0.071(4) 0.105(8) 0.062(5) -0.017(4) 0.026(4) -0.024(4) C30 0.091(5) 0.074(5) 0.092(5) 0.031(4) 0.041(4) 0.023(4) C31 0.079(4) 0.055(3) 0.053(3) 0.006(2) 0.034(3) -0.006(3) C32 0.117(6) 0.052(4) 0.104(5) 0.010(3) 0.090(5) 0.015(3) C33 0.111(8) 0.080(6) 0.073(6) -0.019(5) 0.045(5) -0.019(7) C34 0.075(5) 0.071(7) 0.132(10) 0.030(6) 0.049(6) 0.020(5) C29A 0.076(12) 0.070(14) 0.108(17) -0.007(10) 0.052(11) -0.022(9) C34A 0.097(15) 0.071(13) 0.090(11) 0.022(11) 0.044(10) 0.039(13) C35 0.075(5) 0.086(6) 0.070(5) -0.009(4) 0.031(4) -0.006(4) C36 0.161(10) 0.071(7) 0.050(5) 0.017(5) 0.036(5) 0.032(6) C37 0.038(4) 0.083(5) 0.042(4) 0.005(3) 0.016(4) -0.008(3) C38 0.065(5) 0.084(5) 0.085(6) 0.003(4) 0.048(4) 0.017(3) C39 0.075(6) 0.090(7) 0.072(5) 0.019(5) 0.040(4) 0.034(5) C40 0.101(7) 0.118(8) 0.065(5) -0.007(5) 0.009(5) -0.001(5) C41 0.108(4) 0.104(4) 0.148(5) 0.006(4) -0.011(4) 0.004(3) C42 0.063(3) 0.089(3) 0.071(3) 0.001(2) -0.007(2) 0.010(2) C43 0.059(3) 0.113(3) 0.051(2) 0.023(2) -0.002(2) -0.007(3) C44 0.070(3) 0.111(4) 0.059(3) -0.005(3) 0.018(2) 0.002(3) C45 0.083(3) 0.098(3) 0.071(3) -0.005(2) 0.029(2) 0.000(3) C46 0.070(3) 0.099(3) 0.065(3) 0.000(2) 0.020(2) 0.004(3) C47 0.059(3) 0.115(3) 0.048(2) -0.005(2) 0.012(2) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O2 2.215(3) . ? Na1 O1 2.235(3) . ? Na1 N1 2.421(3) . ? Na1 N2 2.471(3) . ? Na2 O1 2.226(3) . ? Na2 O2 2.238(3) . ? Na2 N3 2.457(3) . ? Na2 N4 2.459(4) . ? O1 C1 1.210(16) . ? O1 C1A 1.433(17) . ? O2 C15 1.304(4) . ? N1 C30A 1.225(19) . ? N1 C29 1.377(8) . ? N1 C31 1.503(6) . ? N1 C30 1.542(7) . ? N1 C31A 1.617(14) . ? N1 C29A 1.642(19) . ? N2 C33A 1.40(4) . ? N2 C32 1.476(11) . ? N2 C34 1.480(11) . ? N2 C33 1.501(12) . ? N2 C32A 1.51(3) . ? N2 C34A 1.52(3) . ? N3 C36A 1.418(17) . ? N3 C37 1.427(7) . ? N3 C35 1.432(8) . ? N3 C36 1.517(10) . ? N3 C37A 1.560(12) . ? N3 C35A 1.565(12) . ? N4 C39A 1.261(16) . ? N4 C40 1.400(8) . ? N4 C38A 1.466(11) . ? N4 C39 1.560(9) . ? N4 C40A 1.567(12) . ? N4 C38 1.577(8) . ? C1 C14 1.443(17) . ? C1 C2 1.446(10) . ? C2 C3 1.422(9) . ? C2 C7 1.434(10) . ? C3 C4 1.383(10) . ? C4 C5 1.405(13) . ? C5 C6 1.343(13) . ? C6 C7 1.451(9) . ? C7 C8 1.394(10) . ? C8 C9 1.452(16) . ? C1A C14 1.448(19) . ? C1A C2A 1.449(11) . ? C2A C3A 1.430(11) . ? C2A C7A 1.440(11) . ? C3A C4A 1.393(14) . ? C4A C5A 1.394(15) . ? C5A C6A 1.343(13) . ? C6A C7A 1.453(11) . ? C7A C8A 1.379(12) . ? C8A C9 1.361(18) . ? C9 C14 1.434(4) . ? C9 C10 1.435(5) . ? C10 C11 1.339(5) . ? C11 C12 1.406(5) . ? C12 C13 1.356(4) . ? C13 C14 1.417(4) . ? C15 C28 1.429(5) . ? C15 C16 1.449(5) . ? C16 C17 1.414(6) . ? C16 C21 1.472(5) . ? C17 C18 1.476(7) . ? C18 C19 1.368(7) . ? C19 C20 1.338(7) . ? C20 C21 1.425(5) . ? C21 C22 1.360(5) . ? C22 C23 1.354(5) . ? C23 C28 1.435(5) . ? C23 C24 1.477(5) . ? C24 C25 1.343(6) . ? C25 C26 1.367(6) . ? C26 C27 1.353(6) . ? C27 C28 1.405(5) . ? C31 C32 1.459(11) . ? C31A C32A 1.459(17) . ? C37 C38 1.560(9) . ? C37A C38A 1.584(12) . ? C41 C42 1.474(7) . ? C42 C47 1.377(6) . ? C42 C43 1.435(6) . ? C43 C44 1.366(6) . ? C44 C45 1.369(6) . ? C45 C46 1.368(6) . ? C46 C47 1.370(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Na1 O1 89.84(10) . . ? O2 Na1 N1 110.13(11) . . ? O1 Na1 N1 131.56(12) . . ? O2 Na1 N2 127.88(12) . . ? O1 Na1 N2 124.79(11) . . ? N1 Na1 N2 77.06(11) . . ? O1 Na2 O2 89.46(10) . . ? O1 Na2 N3 120.40(11) . . ? O2 Na2 N3 125.31(12) . . ? O1 Na2 N4 131.91(13) . . ? O2 Na2 N4 117.76(12) . . ? N3 Na2 N4 77.04(12) . . ? C1 O1 Na2 137.0(15) . . ? C1A O1 Na2 136.7(14) . . ? C1 O1 Na1 124.7(15) . . ? C1A O1 Na1 120.2(14) . . ? Na2 O1 Na1 89.94(9) . . ? C15 O2 Na1 146.5(2) . . ? C15 O2 Na2 123.2(2) . . ? Na1 O2 Na2 90.17(10) . . ? C29 N1 C31 113.8(5) . . ? C29 N1 C30 108.6(5) . . ? C31 N1 C30 104.5(4) . . ? C30A N1 C31A 120.0(12) . . ? C30A N1 C29A 114.1(14) . . ? C31A N1 C29A 95.5(9) . . ? C30A N1 Na1 114.5(11) . . ? C29 N1 Na1 117.0(5) . . ? C31 N1 Na1 102.1(2) . . ? C30 N1 Na1 110.0(3) . . ? C31A N1 Na1 99.7(5) . . ? C29A N1 Na1 110.9(10) . . ? C32 N2 C34 109.7(8) . . ? C32 N2 C33 110.5(7) . . ? C34 N2 C33 108.4(9) . . ? C33A N2 C32A 111(2) . . ? C33A N2 C34A 111(2) . . ? C32A N2 C34A 107(2) . . ? C33A N2 Na1 117(3) . . ? C32 N2 Na1 103.2(4) . . ? C34 N2 Na1 117.7(5) . . ? C33 N2 Na1 107.2(8) . . ? C32A N2 Na1 108.8(10) . . ? C34A N2 Na1 99.9(11) . . ? C37 N3 C35 117.5(5) . . ? C37 N3 C36 108.3(6) . . ? C35 N3 C36 113.1(7) . . ? C36A N3 C37A 110.7(8) . . ? C36A N3 C35A 103.0(9) . . ? C37A N3 C35A 102.3(7) . . ? C36A N3 Na2 114.5(9) . . ? C37 N3 Na2 106.5(3) . . ? C35 N3 Na2 100.4(4) . . ? C36 N3 Na2 110.6(6) . . ? C37A N3 Na2 102.6(5) . . ? C35A N3 Na2 122.8(5) . . ? C39A N4 C40 119.3(10) . . ? C39A N4 C38A 123.3(9) . . ? C40 N4 C39 105.4(6) . . ? C39A N4 C40A 111.7(9) . . ? C38A N4 C40A 107.0(7) . . ? C40 N4 C38 109.7(6) . . ? C39 N4 C38 99.1(6) . . ? C39A N4 Na2 115.8(9) . . ? C40 N4 Na2 119.8(5) . . ? C38A N4 Na2 96.8(5) . . ? C39 N4 Na2 117.9(4) . . ? C40A N4 Na2 98.8(6) . . ? C38 N4 Na2 102.7(3) . . ? O1 C1 C14 128.3(9) . . ? O1 C1 C2 115.0(12) . . ? C14 C1 C2 116.7(10) . . ? C3 C2 C7 119.7(8) . . ? C3 C2 C1 120.4(9) . . ? C7 C2 C1 119.8(9) . . ? C4 C3 C2 119.3(9) . . ? C3 C4 C5 121.8(10) . . ? C6 C5 C4 120.1(10) . . ? C5 C6 C7 121.7(9) . . ? C8 C7 C2 120.4(8) . . ? C8 C7 C6 122.2(10) . . ? C2 C7 C6 117.4(8) . . ? C7 C8 C9 123.9(11) . . ? O1 C1A C14 112.1(11) . . ? O1 C1A C2A 130.7(14) . . ? C14 C1A C2A 117.1(11) . . ? C3A C2A C7A 119.4(10) . . ? C3A C2A C1A 119.0(11) . . ? C7A C2A C1A 121.4(10) . . ? C4A C3A C2A 120.4(11) . . ? C3A C4A C5A 119.5(13) . . ? C6A C5A C4A 121.9(12) . . ? C5A C6A C7A 121.9(11) . . ? C8A C7A C2A 121.4(11) . . ? C8A C7A C6A 122.0(11) . . ? C2A C7A C6A 116.5(10) . . ? C9 C8A C7A 115.7(13) . . ? C8A C9 C14 128.8(7) . . ? C8A C9 C10 114.2(7) . . ? C14 C9 C10 116.9(3) . . ? C14 C9 C8 113.5(6) . . ? C10 C9 C8 129.6(6) . . ? C11 C10 C9 122.5(3) . . ? C10 C11 C12 120.3(3) . . ? C13 C12 C11 119.9(3) . . ? C12 C13 C14 122.0(3) . . ? C13 C14 C9 118.4(3) . . ? C13 C14 C1 116.0(5) . . ? C9 C14 C1 125.6(5) . . ? C13 C14 C1A 126.3(7) . . ? C9 C14 C1A 115.3(7) . . ? O2 C15 C28 120.7(3) . . ? O2 C15 C16 123.4(4) . . ? C28 C15 C16 115.9(3) . . ? C17 C16 C15 119.8(4) . . ? C17 C16 C21 120.6(4) . . ? C15 C16 C21 119.7(3) . . ? C16 C17 C18 119.2(5) . . ? C19 C18 C17 116.4(5) . . ? C20 C19 C18 126.5(6) . . ? C19 C20 C21 120.7(5) . . ? C22 C21 C20 123.7(4) . . ? C22 C21 C16 119.7(3) . . ? C20 C21 C16 116.6(4) . . ? C23 C22 C21 122.9(4) . . ? C22 C23 C28 119.6(4) . . ? C22 C23 C24 123.2(4) . . ? C28 C23 C24 117.2(4) . . ? C25 C24 C23 120.2(4) . . ? C24 C25 C26 122.3(5) . . ? C27 C26 C25 119.3(5) . . ? C26 C27 C28 124.1(4) . . ? C27 C28 C15 121.0(3) . . ? C27 C28 C23 116.9(4) . . ? C15 C28 C23 122.1(3) . . ? C32 C31 N1 111.4(6) . . ? C31 C32 N2 117.2(9) . . ? C32A C31A N1 114.7(19) . . ? C31A C32A N2 113(2) . . ? N3 C37 C38 114.5(6) . . ? C37 C38 N4 108.5(5) . . ? N3 C37A C38A 102.4(8) . . ? N4 C38A C37A 106.5(9) . . ? C47 C42 C43 116.1(4) . . ? C47 C42 C41 122.1(5) . . ? C43 C42 C41 121.8(5) . . ? C44 C43 C42 119.8(4) . . ? C43 C44 C45 122.2(5) . . ? C46 C45 C44 118.5(5) . . ? C45 C46 C47 120.7(5) . . ? C46 C47 C42 122.6(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.588 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.042 data_jkcben5 _database_code_depnum_ccdc_archive 'CCDC 892942' #TrackingRef 'Hara_1353510871.Submissioncif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H58 Li2 N4 O2' _chemical_formula_weight 724.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2149(10) _cell_length_b 12.9366(12) _cell_length_c 15.0500(12) _cell_angle_alpha 66.429(8) _cell_angle_beta 81.568(7) _cell_angle_gamma 75.877(8) _cell_volume 2110.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9002 _cell_measurement_theta_min 2.7836 _cell_measurement_theta_max 30.9169 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_min 0.77705 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ALL organic fragments disordered over two sites. All C-C and C-N distances needed to be restrained. Also fixed equivalent atoms of the two disordered portions to have equal displacement parameters. C-C distances for anthracenolate portion based on those observed in equivalent K structure. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25300 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9215 _reflns_number_gt 5408 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysalisPro _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics XSEED _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9215 _refine_ls_number_parameters 647 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.3588(2) 0.6531(2) 0.24861(19) 0.0404(6) Uani 1 1 d . . . Li2 Li 0.2301(2) 0.8547(2) 0.19152(18) 0.0369(6) Uani 1 1 d . A . O1 O 0.33843(9) 0.77953(9) 0.28982(7) 0.0399(3) Uani 1 1 d . A . C71 C 0.1789(12) 0.7796(11) 0.4531(9) 0.056(2) Uani 0.514(6) 1 d PD A 2 H71 H 0.1574 0.7559 0.4072 0.067 Uiso 0.514(6) 1 calc PR A 2 C72 C 0.1079(8) 0.7820(7) 0.5316(6) 0.0684(16) Uani 0.514(6) 1 d PD A 2 H72 H 0.0385 0.7571 0.5411 0.082 Uiso 0.514(6) 1 calc PR A 2 C73 C 0.1358(10) 0.8206(9) 0.5984(7) 0.0696(19) Uani 0.514(6) 1 d PD A 2 H73 H 0.0837 0.8233 0.6512 0.083 Uiso 0.514(6) 1 calc PR A 2 C74 C 0.2342(10) 0.8539(15) 0.5900(10) 0.0551(18) Uani 0.514(6) 1 d PD A 2 H74 H 0.2510 0.8812 0.6354 0.066 Uiso 0.514(6) 1 calc PR A 2 C65 C 0.3132(8) 0.8474(13) 0.5108(9) 0.0349(17) Uani 0.514(6) 1 d PD A 2 C66 C 0.2839(14) 0.812(2) 0.4399(13) 0.0376(19) Uani 0.514(6) 1 d PD A 2 C61 C 0.3570(10) 0.8035(18) 0.3584(13) 0.0263(16) Uani 0.514(6) 1 d PD A 2 C64 C 0.4199(8) 0.8713(15) 0.5009(10) 0.0385(18) Uani 0.514(6) 1 d PD A 2 H64 H 0.4406 0.8974 0.5455 0.046 Uiso 0.514(6) 1 calc PR A 2 C63 C 0.4978(8) 0.8575(15) 0.4264(10) 0.0335(16) Uani 0.514(6) 1 d PD A 2 C70 C 0.6091(7) 0.8768(11) 0.4236(8) 0.0399(15) Uani 0.514(6) 1 d PD A 2 H70 H 0.6276 0.8986 0.4718 0.048 Uiso 0.514(6) 1 calc PR A 2 C69 C 0.6883(9) 0.8644(12) 0.3536(9) 0.0450(15) Uani 0.514(6) 1 d PD A 2 H69 H 0.7614 0.8789 0.3517 0.054 Uiso 0.514(6) 1 calc PR A 2 C68 C 0.6602(12) 0.830(2) 0.2833(13) 0.0449(15) Uani 0.514(6) 1 d PD A 2 H68 H 0.7162 0.8166 0.2358 0.054 Uiso 0.514(6) 1 calc PR A 2 C67 C 0.5544(15) 0.814(3) 0.283(2) 0.0396(16) Uani 0.514(6) 1 d PD A 2 H67 H 0.5376 0.7968 0.2317 0.048 Uiso 0.514(6) 1 calc PR A 2 C62 C 0.4666(8) 0.8235(11) 0.3549(8) 0.0226(17) Uani 0.514(6) 1 d PD A 2 O2 O 0.23898(9) 0.72153(8) 0.16259(7) 0.0393(3) Uani 1 1 d . A . C25 C 0.2338(4) 0.7124(4) -0.0231(3) 0.0366(8) Uani 0.738(3) 1 d PD A 1 H25 H 0.2940 0.7414 -0.0141 0.044 Uiso 0.738(3) 1 calc PR A 1 C26 C 0.2291(3) 0.7065(3) -0.1110(2) 0.0478(8) Uani 0.738(3) 1 d PD A 1 H26 H 0.2849 0.7303 -0.1616 0.057 Uiso 0.738(3) 1 calc PR A 1 C27 C 0.1405(3) 0.6648(3) -0.1253(2) 0.0535(10) Uani 0.738(3) 1 d PD A 1 H27 H 0.1370 0.6592 -0.1858 0.064 Uiso 0.738(3) 1 calc PR A 1 C28 C 0.0598(3) 0.6322(2) -0.0544(2) 0.0496(7) Uani 0.738(3) 1 d PD A 1 H28 H 0.0000 0.6054 -0.0667 0.059 Uiso 0.738(3) 1 calc PR A 1 C19 C 0.0618(3) 0.6367(3) 0.0387(2) 0.0381(7) Uani 0.738(3) 1 d PD A 1 C18 C -0.0215(2) 0.6028(3) 0.1127(3) 0.0483(8) Uani 0.738(3) 1 d PD A 1 H18 H -0.0828 0.5772 0.1013 0.058 Uiso 0.738(3) 1 calc PR A 1 C17 C -0.0147(2) 0.6065(3) 0.2029(2) 0.0439(7) Uani 0.738(3) 1 d PD A 1 C24 C -0.0975(3) 0.5716(3) 0.2798(3) 0.0642(10) Uani 0.738(3) 1 d PD A 1 H24 H -0.1576 0.5432 0.2700 0.077 Uiso 0.738(3) 1 calc PR A 1 C23 C -0.0922(3) 0.5780(3) 0.3664(2) 0.0692(10) Uani 0.738(3) 1 d PD A 1 H23 H -0.1483 0.5537 0.4166 0.083 Uiso 0.738(3) 1 calc PR A 1 C22 C -0.0044(3) 0.6202(3) 0.3831(2) 0.0620(8) Uani 0.738(3) 1 d PD A 1 H22 H -0.0027 0.6267 0.4436 0.074 Uiso 0.738(3) 1 calc PR A 1 C21 C 0.0778(3) 0.6517(3) 0.3123(2) 0.0466(7) Uani 0.738(3) 1 d PD A 1 H21 H 0.1377 0.6782 0.3247 0.056 Uiso 0.738(3) 1 calc PR A 1 C16 C 0.0761(3) 0.6460(4) 0.2201(2) 0.0368(7) Uani 0.738(3) 1 d PD A 1 C15 C 0.1621(5) 0.6823(8) 0.1471(3) 0.0289(9) Uani 0.738(3) 1 d PD A 1 C20 C 0.1534(5) 0.6773(6) 0.0556(3) 0.0290(8) Uani 0.738(3) 1 d PD A 1 N31 N 0.37116(13) 0.49036(13) 0.36674(11) 0.0560(4) Uani 1 1 d D B . N32 N 0.51574(12) 0.56899(12) 0.18931(11) 0.0506(4) Uani 1 1 d D B . C30 C 0.3531(5) 0.5125(9) 0.4563(5) 0.0662(16) Uani 0.686(2) 1 d PD B 1 H30A H 0.3724 0.4397 0.5118 0.099 Uiso 0.686(2) 1 calc PR B 1 H30B H 0.2736 0.5481 0.4641 0.099 Uiso 0.686(2) 1 calc PR B 1 H30C H 0.4013 0.5646 0.4531 0.099 Uiso 0.686(2) 1 calc PR B 1 C31 C 0.2980(10) 0.4157(13) 0.3743(13) 0.068(2) Uani 0.686(2) 1 d PD B 1 H31A H 0.3190 0.3422 0.4287 0.102 Uiso 0.686(2) 1 calc PR B 1 H31B H 0.3053 0.4021 0.3140 0.102 Uiso 0.686(2) 1 calc PR B 1 H31C H 0.2196 0.4517 0.3855 0.102 Uiso 0.686(2) 1 calc PR B 1 C32 C 0.4919(3) 0.4399(4) 0.3626(2) 0.0942(17) Uani 0.686(2) 1 d PD B 1 H32A H 0.5328 0.4755 0.3912 0.113 Uiso 0.686(2) 1 calc PR B 1 H32B H 0.5035 0.3566 0.4034 0.113 Uiso 0.686(2) 1 calc PR B 1 C33 C 0.5401(4) 0.4533(3) 0.2684(2) 0.0819(14) Uani 0.686(2) 1 d PD B 1 H33A H 0.5152 0.3988 0.2485 0.098 Uiso 0.686(2) 1 calc PR B 1 H33B H 0.6231 0.4292 0.2728 0.098 Uiso 0.686(2) 1 calc PR B 1 C34 C 0.4847(14) 0.5505(13) 0.1078(7) 0.076(3) Uani 0.686(2) 1 d PD B 1 H34A H 0.4769 0.6227 0.0507 0.114 Uiso 0.686(2) 1 calc PR B 1 H34B H 0.4126 0.5247 0.1244 0.114 Uiso 0.686(2) 1 calc PR B 1 H34C H 0.5436 0.4916 0.0937 0.114 Uiso 0.686(2) 1 calc PR B 1 C35 C 0.6184(4) 0.6157(6) 0.1585(6) 0.080(2) Uani 0.686(2) 1 d PD B 1 H35A H 0.6462 0.6216 0.2138 0.121 Uiso 0.686(2) 1 calc PR B 1 H35B H 0.6017 0.6923 0.1068 0.121 Uiso 0.686(2) 1 calc PR B 1 H35C H 0.6763 0.5646 0.1342 0.121 Uiso 0.686(2) 1 calc PR B 1 N41 N 0.0668(7) 0.9715(7) 0.1893(4) 0.0526(5) Uani 0.686(2) 1 d PD A 1 C40 C -0.0060(3) 0.9425(3) 0.1379(2) 0.0545(8) Uani 0.686(2) 1 d PD A 1 H41A H -0.0711 1.0062 0.1158 0.082 Uiso 0.686(2) 1 calc PR B 1 H41B H -0.0326 0.8726 0.1817 0.082 Uiso 0.686(2) 1 calc PR B 1 H41C H 0.0366 0.9291 0.0818 0.082 Uiso 0.686(2) 1 calc PR B 1 C41 C 0.0052(3) 0.9795(3) 0.2778(3) 0.0768(10) Uani 0.686(2) 1 d PD A 1 H41D H -0.0637 1.0394 0.2609 0.115 Uiso 0.686(2) 1 calc PR B 1 H41E H 0.0530 0.9991 0.3132 0.115 Uiso 0.686(2) 1 calc PR B 1 H41F H -0.0151 0.9053 0.3188 0.115 Uiso 0.686(2) 1 calc PR B 1 C42 C 0.0960(3) 1.0851(2) 0.1258(3) 0.0826(12) Uani 0.686(2) 1 d PD A 1 H42A H 0.1300 1.1134 0.1653 0.099 Uiso 0.686(2) 1 calc PR B 1 H42B H 0.0258 1.1414 0.1005 0.099 Uiso 0.686(2) 1 calc PR B 1 C43 C 0.1769(7) 1.0789(10) 0.0421(8) 0.0702(16) Uani 0.686(2) 1 d PD A 1 H43C H 0.1412 1.0567 -0.0007 0.084 Uiso 0.686(2) 1 calc PR B 1 H43D H 0.1951 1.1556 0.0037 0.084 Uiso 0.686(2) 1 calc PR B 1 N41A N 0.0718(14) 0.9735(15) 0.1820(8) 0.0526(5) Uani 0.314(2) 1 d PD A 2 C40A C -0.0331(6) 0.9324(6) 0.1940(5) 0.0545(8) Uani 0.314(2) 1 d PD A 2 H41G H -0.0955 0.9984 0.1691 0.082 Uiso 0.314(2) 1 calc PR B 2 H41H H -0.0493 0.8891 0.2630 0.082 Uiso 0.314(2) 1 calc PR B 2 H41I H -0.0247 0.8823 0.1579 0.082 Uiso 0.314(2) 1 calc PR B 2 C41A C 0.0781(6) 1.0381(7) 0.2424(6) 0.0768(10) Uani 0.314(2) 1 d PD A 2 H41J H 0.1531 1.0568 0.2323 0.115 Uiso 0.314(2) 1 calc PR B 2 H41K H 0.0648 0.9908 0.3110 0.115 Uiso 0.314(2) 1 calc PR B 2 H41L H 0.0204 1.1094 0.2239 0.115 Uiso 0.314(2) 1 calc PR B 2 C42A C 0.0780(6) 1.0472(5) 0.0769(7) 0.0826(12) Uani 0.314(2) 1 d PD A 2 H42C H 0.0114 1.1116 0.0613 0.099 Uiso 0.314(2) 1 calc PR B 2 H42D H 0.0777 1.0013 0.0378 0.099 Uiso 0.314(2) 1 calc PR B 2 N42 N 0.2809(7) 0.9945(14) 0.0773(10) 0.0443(11) Uani 0.686(2) 1 d PD A 1 C44 C 0.3501(4) 1.0383(5) 0.1192(3) 0.0578(11) Uani 0.686(2) 1 d PD A 1 H44A H 0.4229 0.9845 0.1349 0.087 Uiso 0.686(2) 1 calc PR B 1 H44B H 0.3112 1.0464 0.1786 0.087 Uiso 0.686(2) 1 calc PR B 1 H44C H 0.3627 1.1136 0.0725 0.087 Uiso 0.686(2) 1 calc PR B 1 C45 C 0.3424(8) 0.9702(7) -0.0054(6) 0.0702(14) Uani 0.686(2) 1 d PD A 1 H45A H 0.3611 1.0413 -0.0551 0.105 Uiso 0.686(2) 1 calc PR B 1 H45B H 0.2952 0.9399 -0.0325 0.105 Uiso 0.686(2) 1 calc PR B 1 H45C H 0.4122 0.9131 0.0162 0.105 Uiso 0.686(2) 1 calc PR B 1 C32A C 0.4660(7) 0.4129(8) 0.3279(7) 0.0942(17) Uani 0.314(2) 1 d PD B 2 H32C H 0.4400 0.3978 0.2759 0.113 Uiso 0.314(2) 1 calc PR B 2 H32D H 0.4948 0.3387 0.3805 0.113 Uiso 0.314(2) 1 calc PR B 2 C30A C 0.3903(14) 0.510(2) 0.4511(12) 0.0662(16) Uani 0.314(2) 1 d PD B 2 H30D H 0.3283 0.5696 0.4610 0.099 Uiso 0.314(2) 1 calc PR B 2 H30E H 0.4619 0.5359 0.4407 0.099 Uiso 0.314(2) 1 calc PR B 2 H30F H 0.3936 0.4385 0.5086 0.099 Uiso 0.314(2) 1 calc PR B 2 C31A C 0.280(2) 0.427(3) 0.386(3) 0.068(2) Uani 0.314(2) 1 d PD B 2 H31D H 0.3000 0.3516 0.4391 0.102 Uiso 0.314(2) 1 calc PR B 2 H31E H 0.2695 0.4155 0.3276 0.102 Uiso 0.314(2) 1 calc PR B 2 H31F H 0.2096 0.4707 0.4050 0.102 Uiso 0.314(2) 1 calc PR B 2 C33A C 0.5589(8) 0.4904(7) 0.2872(6) 0.0819(14) Uani 0.314(2) 1 d PD B 2 H33C H 0.5608 0.5337 0.3281 0.098 Uiso 0.314(2) 1 calc PR B 2 H33D H 0.6351 0.4438 0.2818 0.098 Uiso 0.314(2) 1 calc PR B 2 C34A C 0.468(3) 0.530(3) 0.127(2) 0.076(3) Uani 0.314(2) 1 d PD B 2 H34D H 0.4407 0.5966 0.0683 0.114 Uiso 0.314(2) 1 calc PR B 2 H34E H 0.4048 0.4934 0.1620 0.114 Uiso 0.314(2) 1 calc PR B 2 H34F H 0.5264 0.4747 0.1076 0.114 Uiso 0.314(2) 1 calc PR B 2 N42A N 0.2830(16) 0.998(3) 0.066(2) 0.0443(11) Uani 0.314(2) 1 d PD A 2 C44A C 0.3802(11) 1.0286(13) 0.0892(9) 0.0578(11) Uani 0.314(2) 1 d PD A 2 H44D H 0.4025 1.0932 0.0334 0.087 Uiso 0.314(2) 1 calc PR B 2 H44E H 0.4435 0.9622 0.1045 0.087 Uiso 0.314(2) 1 calc PR B 2 H44F H 0.3592 1.0510 0.1454 0.087 Uiso 0.314(2) 1 calc PR B 2 C45A C 0.317(2) 0.9569(19) -0.0147(14) 0.0702(14) Uani 0.314(2) 1 d PD A 2 H45D H 0.2509 0.9394 -0.0321 0.105 Uiso 0.314(2) 1 calc PR B 2 H45E H 0.3760 0.8871 0.0058 0.105 Uiso 0.314(2) 1 calc PR B 2 H45F H 0.3450 1.0168 -0.0710 0.105 Uiso 0.314(2) 1 calc PR B 2 C35A C 0.5965(12) 0.6425(15) 0.1315(16) 0.080(2) Uani 0.314(2) 1 d PD B 2 H35D H 0.6289 0.6672 0.1738 0.121 Uiso 0.314(2) 1 calc PR B 2 H35E H 0.5571 0.7104 0.0802 0.121 Uiso 0.314(2) 1 calc PR B 2 H35F H 0.6571 0.5989 0.1023 0.121 Uiso 0.314(2) 1 calc PR B 2 C43A C 0.1845(16) 1.094(2) 0.0527(19) 0.0702(16) Uani 0.314(2) 1 d PD A 2 H43A H 0.1852 1.1499 -0.0153 0.084 Uiso 0.314(2) 1 calc PR B 2 H43B H 0.1879 1.1339 0.0958 0.084 Uiso 0.314(2) 1 calc PR B 2 C88 C 0.1011(11) 0.6567(12) -0.0955(8) 0.0496(7) Uani 0.262(3) 1 d PD A 2 H88 H 0.0509 0.6297 -0.1196 0.059 Uiso 0.262(3) 1 calc PR A 2 C87 C 0.1862(8) 0.7000(8) -0.1543(8) 0.0535(10) Uani 0.262(3) 1 d PD A 2 H87 H 0.1957 0.7038 -0.2193 0.064 Uiso 0.262(3) 1 calc PR A 2 C78 C -0.0046(9) 0.6099(10) 0.0655(7) 0.0483(8) Uani 0.262(3) 1 d PD A 2 H78 H -0.0589 0.5857 0.0431 0.058 Uiso 0.262(3) 1 calc PR A 2 C77 C -0.0166(8) 0.6039(10) 0.1607(7) 0.0439(7) Uani 0.262(3) 1 d PD A 2 C80 C 0.1649(17) 0.689(2) 0.0341(12) 0.0290(8) Uani 0.262(3) 1 d PD A 2 C83 C -0.1172(11) 0.5604(12) 0.3150(8) 0.0692(10) Uani 0.262(3) 1 d PD A 2 H83 H -0.1779 0.5313 0.3574 0.083 Uiso 0.262(3) 1 calc PR A 2 C81 C 0.0441(8) 0.6404(9) 0.2913(7) 0.0466(7) Uani 0.262(3) 1 d PD A 2 H81 H 0.0966 0.6660 0.3145 0.056 Uiso 0.262(3) 1 calc PR A 2 C79 C 0.0839(10) 0.6500(10) 0.0023(6) 0.0381(7) Uani 0.262(3) 1 d PD A 2 C86 C 0.2608(10) 0.7396(8) -0.1195(8) 0.0478(8) Uani 0.262(3) 1 d PD A 2 H86 H 0.3190 0.7722 -0.1630 0.057 Uiso 0.262(3) 1 calc PR A 2 C84 C -0.1075(7) 0.5595(8) 0.2244(7) 0.0642(10) Uani 0.262(3) 1 d PD A 2 H84 H -0.1593 0.5303 0.2041 0.077 Uiso 0.262(3) 1 calc PR A 2 C75 C 0.1511(18) 0.687(3) 0.1308(12) 0.0289(9) Uani 0.262(3) 1 d PD A 2 C76 C 0.0593(12) 0.6440(13) 0.1960(8) 0.0368(7) Uani 0.262(3) 1 d PD A 2 C82 C -0.0433(9) 0.6016(9) 0.3508(7) 0.0620(8) Uani 0.262(3) 1 d PD A 2 H82 H -0.0549 0.6020 0.4145 0.074 Uiso 0.262(3) 1 calc PR A 2 C85 C 0.2546(14) 0.7341(14) -0.0266(9) 0.0366(8) Uani 0.262(3) 1 d PD A 2 H85 H 0.3083 0.7591 -0.0043 0.044 Uiso 0.262(3) 1 calc PR A 2 C6 C 0.3074(15) 0.826(2) 0.4288(14) 0.0376(19) Uani 0.486(6) 1 d PD A 1 C11 C 0.1938(13) 0.8138(12) 0.4384(10) 0.056(2) Uani 0.486(6) 1 d PD A 1 H11 H 0.1686 0.7931 0.3921 0.067 Uiso 0.486(6) 1 calc PR A 1 C12 C 0.1182(9) 0.8301(7) 0.5100(6) 0.0684(16) Uani 0.486(6) 1 d PD A 1 H12 H 0.0423 0.8222 0.5130 0.082 Uiso 0.486(6) 1 calc PR A 1 C13 C 0.1556(11) 0.8590(10) 0.5797(7) 0.0696(19) Uani 0.486(6) 1 d PD A 1 H13 H 0.1048 0.8716 0.6303 0.083 Uiso 0.486(6) 1 calc PR A 1 C14 C 0.2650(11) 0.8688(16) 0.5739(11) 0.0551(18) Uani 0.486(6) 1 d PD A 1 H14 H 0.2887 0.8858 0.6230 0.066 Uiso 0.486(6) 1 calc PR A 1 C5 C 0.3470(9) 0.8552(14) 0.4988(10) 0.0349(17) Uani 0.486(6) 1 d PD A 1 C10 C 0.6453(7) 0.8690(12) 0.4077(9) 0.0399(15) Uani 0.486(6) 1 d PD A 1 H10 H 0.6735 0.8912 0.4515 0.048 Uiso 0.486(6) 1 calc PR A 1 C1 C 0.3854(11) 0.8113(19) 0.3522(14) 0.0263(16) Uani 0.486(6) 1 d PD A 1 C4 C 0.4559(8) 0.8700(16) 0.4957(11) 0.0385(18) Uani 0.486(6) 1 d PD A 1 H4A H 0.4788 0.8883 0.5443 0.046 Uiso 0.486(6) 1 calc PR A 1 C3 C 0.5314(8) 0.8576(16) 0.4203(11) 0.0335(16) Uani 0.486(6) 1 d PD A 1 C2 C 0.4979(9) 0.8272(12) 0.3489(9) 0.028(2) Uani 0.486(6) 1 d PD A 1 C7 C 0.5711(16) 0.806(3) 0.273(2) 0.0396(16) Uani 0.486(6) 1 d PD A 1 H7 H 0.5455 0.7819 0.2289 0.048 Uiso 0.486(6) 1 calc PR A 1 C8 C 0.6788(13) 0.820(2) 0.2657(14) 0.0449(15) Uani 0.486(6) 1 d PD A 1 H8 H 0.7292 0.8095 0.2140 0.054 Uiso 0.486(6) 1 calc PR A 1 C9 C 0.7158(9) 0.8495(13) 0.3350(10) 0.0450(15) Uani 0.486(6) 1 d PD A 1 H9 H 0.7923 0.8561 0.3307 0.054 Uiso 0.486(6) 1 calc PR A 1 C50 C 0.4975(3) 0.1644(3) 0.2178(3) 0.0606(8) Uani 0.6356(16) 1 d P C 1 H50A H 0.5131 0.0813 0.2330 0.091 Uiso 0.6356(16) 1 calc PR C 1 H50B H 0.5395 0.1800 0.2602 0.091 Uiso 0.6356(16) 1 calc PR C 1 H50C H 0.5211 0.2045 0.1498 0.091 Uiso 0.6356(16) 1 calc PR C 1 C51 C 0.37322(12) 0.20620(15) 0.23372(14) 0.0432(6) Uani 0.6356(16) 1 d PG C 1 C52 C 0.31569(16) 0.14497(14) 0.31781(13) 0.0460(6) Uani 0.6356(16) 1 d PG C 1 H52 H 0.3547 0.0759 0.3641 0.055 Uiso 0.6356(16) 1 calc PR C 1 C53 C 0.20114(16) 0.18480(16) 0.33413(12) 0.0512(7) Uani 0.6356(16) 1 d PG C 1 H53 H 0.1618 0.1430 0.3916 0.061 Uiso 0.6356(16) 1 calc PR C 1 C54 C 0.14413(12) 0.28585(17) 0.26635(15) 0.0577(7) Uani 0.6356(16) 1 d PG C 1 H54 H 0.0658 0.3131 0.2775 0.069 Uiso 0.6356(16) 1 calc PR C 1 C55 C 0.20166(15) 0.34708(14) 0.18225(13) 0.0576(7) Uani 0.6356(16) 1 d PG C 1 H55 H 0.1627 0.4161 0.1359 0.069 Uiso 0.6356(16) 1 calc PR C 1 C56 C 0.31620(15) 0.30725(15) 0.16594(11) 0.0481(7) Uani 0.6356(16) 1 d PG C 1 H56 H 0.3555 0.3491 0.1085 0.058 Uiso 0.6356(16) 1 calc PR C 1 C50A C 0.1387(5) 0.2216(5) 0.3455(4) 0.0606(8) Uani 0.3644(16) 1 d P C 2 H50D H 0.1512 0.1427 0.3943 0.091 Uiso 0.3644(16) 1 calc PR C 2 H50E H 0.0701 0.2367 0.3120 0.091 Uiso 0.3644(16) 1 calc PR C 2 H50F H 0.1299 0.2761 0.3775 0.091 Uiso 0.3644(16) 1 calc PR C 2 C51A C 0.2367(3) 0.2355(3) 0.2742(2) 0.0432(6) Uani 0.3644(16) 1 d PG C 2 C52A C 0.3399(3) 0.1588(3) 0.2958(2) 0.0460(6) Uani 0.3644(16) 1 d PG C 2 H52A H 0.3473 0.0945 0.3559 0.055 Uiso 0.3644(16) 1 calc PR C 2 C53A C 0.4323(3) 0.1760(3) 0.2297(3) 0.0512(7) Uani 0.3644(16) 1 d PG C 2 H53A H 0.5029 0.1236 0.2444 0.061 Uiso 0.3644(16) 1 calc PR C 2 C54A C 0.4216(2) 0.2701(3) 0.1418(2) 0.0577(7) Uani 0.3644(16) 1 d PG C 2 H54A H 0.4847 0.2819 0.0966 0.069 Uiso 0.3644(16) 1 calc PR C 2 C55A C 0.3184(3) 0.3469(3) 0.1202(2) 0.0576(7) Uani 0.3644(16) 1 d PG C 2 H55A H 0.3110 0.4112 0.0601 0.069 Uiso 0.3644(16) 1 calc PR C 2 C56A C 0.2260(2) 0.3296(3) 0.1864(3) 0.0481(7) Uani 0.3644(16) 1 d PG C 2 H56A H 0.1554 0.3821 0.1716 0.058 Uiso 0.3644(16) 1 calc PR 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 Li1 0.0419(15) 0.0383(14) 0.0440(15) -0.0203(12) -0.0096(12) -0.0011(11) Li2 0.0369(14) 0.0349(13) 0.0403(14) -0.0166(11) -0.0071(11) -0.0031(11) O1 0.0444(7) 0.0444(6) 0.0361(6) -0.0236(5) -0.0115(5) 0.0012(5) C71 0.047(3) 0.084(7) 0.052(3) -0.042(5) 0.0083(19) -0.017(3) C72 0.056(2) 0.091(6) 0.064(4) -0.041(4) 0.018(2) -0.020(3) C73 0.078(4) 0.084(6) 0.046(3) -0.036(4) 0.021(3) -0.012(3) C74 0.071(6) 0.064(4) 0.029(4) -0.024(4) 0.013(3) -0.010(4) C65 0.040(5) 0.0382(19) 0.026(3) -0.015(2) 0.005(3) -0.006(4) C66 0.036(6) 0.047(5) 0.032(3) -0.020(4) 0.001(3) -0.005(4) C61 0.021(5) 0.031(2) 0.031(2) -0.0143(19) -0.007(4) -0.003(4) C64 0.053(6) 0.0379(10) 0.0317(16) -0.0147(10) -0.014(4) -0.011(5) C63 0.036(5) 0.0316(8) 0.0356(17) -0.0075(12) -0.015(4) -0.013(4) C70 0.039(5) 0.0465(19) 0.037(3) -0.0130(18) -0.004(3) -0.017(4) C69 0.042(5) 0.050(3) 0.046(4) -0.020(2) -0.002(3) -0.010(3) C68 0.040(4) 0.054(3) 0.038(5) -0.019(3) 0.001(3) -0.003(3) C67 0.043(4) 0.040(5) 0.037(4) -0.020(2) -0.008(3) 0.004(5) C62 0.016(5) 0.033(2) 0.025(2) -0.0133(17) -0.005(3) -0.008(3) O2 0.0452(7) 0.0354(6) 0.0425(6) -0.0166(5) -0.0146(5) -0.0074(5) C25 0.038(2) 0.033(2) 0.0437(11) -0.0157(12) -0.0091(12) -0.0105(11) C26 0.058(2) 0.042(2) 0.0452(13) -0.0205(14) -0.0076(14) -0.0039(12) C27 0.069(3) 0.046(2) 0.055(2) -0.029(2) -0.0259(18) 0.0025(17) C28 0.056(2) 0.0473(16) 0.060(2) -0.0298(16) -0.0194(15) -0.0091(12) C19 0.044(2) 0.0283(12) 0.046(2) -0.0163(17) -0.0173(17) -0.0011(11) C18 0.0326(15) 0.0434(12) 0.074(3) -0.023(2) -0.006(2) -0.0135(10) C17 0.0339(11) 0.0368(10) 0.058(2) -0.0166(15) -0.0020(15) -0.0052(8) C24 0.0423(16) 0.0648(16) 0.081(3) -0.026(2) 0.0102(19) -0.0152(12) C23 0.0493(19) 0.0713(19) 0.067(2) -0.0134(17) 0.0169(18) -0.0109(14) C22 0.063(2) 0.0652(17) 0.0433(17) -0.0135(13) 0.0016(14) -0.0027(14) C21 0.0498(19) 0.0469(12) 0.0373(15) -0.0118(11) -0.0063(12) -0.0045(12) C16 0.0338(17) 0.0292(8) 0.043(2) -0.0093(14) -0.0079(14) -0.0025(10) C15 0.0303(17) 0.0210(11) 0.035(2) -0.008(2) -0.0146(16) -0.0006(13) C20 0.0331(16) 0.0217(19) 0.031(2) -0.008(2) -0.0082(16) -0.0033(8) N31 0.0538(10) 0.0483(9) 0.0529(9) -0.0090(7) -0.0152(7) 0.0022(7) N32 0.0456(9) 0.0540(9) 0.0567(9) -0.0307(7) -0.0096(7) 0.0028(7) C30 0.088(5) 0.0589(13) 0.0522(14) 0.0026(12) -0.042(3) -0.034(4) C31 0.103(4) 0.039(3) 0.066(5) -0.0173(18) -0.034(3) -0.009(4) C32 0.064(2) 0.106(3) 0.052(3) 0.011(2) -0.0193(17) 0.028(2) C33 0.092(2) 0.069(2) 0.067(2) -0.0409(16) -0.0215(17) 0.051(2) C34 0.061(5) 0.089(6) 0.106(5) -0.075(5) -0.014(4) 0.007(3) C35 0.044(3) 0.090(4) 0.134(5) -0.080(3) 0.003(3) -0.001(3) N41 0.0425(11) 0.0408(8) 0.0753(12) -0.0262(9) -0.0131(9) 0.0030(7) C40 0.0490(17) 0.0515(13) 0.059(2) -0.0205(17) -0.0191(16) 0.0066(12) C41 0.0474(18) 0.096(2) 0.112(3) -0.079(2) -0.0184(17) 0.0173(15) C42 0.0601(18) 0.0309(15) 0.143(4) -0.0208(16) -0.021(2) 0.0035(13) C43 0.0713(19) 0.036(3) 0.087(3) 0.0034(17) -0.0307(19) -0.0124(13) N41A 0.0425(11) 0.0408(8) 0.0753(12) -0.0262(9) -0.0131(9) 0.0030(7) C40A 0.0490(17) 0.0515(13) 0.059(2) -0.0205(17) -0.0191(16) 0.0066(12) C41A 0.0474(18) 0.096(2) 0.112(3) -0.079(2) -0.0184(17) 0.0173(15) C42A 0.0601(18) 0.0309(15) 0.143(4) -0.0208(16) -0.021(2) 0.0035(13) N42 0.0555(9) 0.0338(11) 0.043(3) -0.007(2) -0.0158(12) -0.0145(7) C44 0.069(3) 0.0522(16) 0.063(3) -0.0229(19) -0.014(2) -0.023(2) C45 0.106(5) 0.072(2) 0.0428(19) -0.0154(15) 0.005(2) -0.053(2) C32A 0.064(2) 0.106(3) 0.052(3) 0.011(2) -0.0193(17) 0.028(2) C30A 0.088(5) 0.0589(13) 0.0522(14) 0.0026(12) -0.042(3) -0.034(4) C31A 0.103(4) 0.039(3) 0.066(5) -0.0173(18) -0.034(3) -0.009(4) C33A 0.092(2) 0.069(2) 0.067(2) -0.0409(16) -0.0215(17) 0.051(2) C34A 0.061(5) 0.089(6) 0.106(5) -0.075(5) -0.014(4) 0.007(3) N42A 0.0555(9) 0.0338(11) 0.043(3) -0.007(2) -0.0158(12) -0.0145(7) C44A 0.069(3) 0.0522(16) 0.063(3) -0.0229(19) -0.014(2) -0.023(2) C45A 0.106(5) 0.072(2) 0.0428(19) -0.0154(15) 0.005(2) -0.053(2) C35A 0.044(3) 0.090(4) 0.134(5) -0.080(3) 0.003(3) -0.001(3) C43A 0.0713(19) 0.036(3) 0.087(3) 0.0034(17) -0.0307(19) -0.0124(13) C88 0.056(2) 0.0473(16) 0.060(2) -0.0298(16) -0.0194(15) -0.0091(12) C87 0.069(3) 0.046(2) 0.055(2) -0.029(2) -0.0259(18) 0.0025(17) C78 0.0326(15) 0.0434(12) 0.074(3) -0.023(2) -0.006(2) -0.0135(10) C77 0.0339(11) 0.0368(10) 0.058(2) -0.0166(15) -0.0020(15) -0.0052(8) C80 0.0331(16) 0.0217(19) 0.031(2) -0.008(2) -0.0082(16) -0.0033(8) C83 0.0493(19) 0.0713(19) 0.067(2) -0.0134(17) 0.0169(18) -0.0109(14) C81 0.0498(19) 0.0469(12) 0.0373(15) -0.0118(11) -0.0063(12) -0.0045(12) C79 0.044(2) 0.0283(12) 0.046(2) -0.0163(17) -0.0173(17) -0.0011(11) C86 0.058(2) 0.042(2) 0.0452(13) -0.0205(14) -0.0076(14) -0.0039(12) C84 0.0423(16) 0.0648(16) 0.081(3) -0.026(2) 0.0102(19) -0.0152(12) C75 0.0303(17) 0.0210(11) 0.035(2) -0.008(2) -0.0146(16) -0.0006(13) C76 0.0338(17) 0.0292(8) 0.043(2) -0.0093(14) -0.0079(14) -0.0025(10) C82 0.063(2) 0.0652(17) 0.0433(17) -0.0135(13) 0.0016(14) -0.0027(14) C85 0.038(2) 0.033(2) 0.0437(11) -0.0157(12) -0.0091(12) -0.0105(11) C6 0.036(6) 0.047(5) 0.032(3) -0.020(4) 0.001(3) -0.005(4) C11 0.047(3) 0.084(7) 0.052(3) -0.042(5) 0.0083(19) -0.017(3) C12 0.056(2) 0.091(6) 0.064(4) -0.041(4) 0.018(2) -0.020(3) C13 0.078(4) 0.084(6) 0.046(3) -0.036(4) 0.021(3) -0.012(3) C14 0.071(6) 0.064(4) 0.029(4) -0.024(4) 0.013(3) -0.010(4) C5 0.040(5) 0.0382(19) 0.026(3) -0.015(2) 0.005(3) -0.006(4) C10 0.039(5) 0.0465(19) 0.037(3) -0.0130(18) -0.004(3) -0.017(4) C1 0.021(5) 0.031(2) 0.031(2) -0.0143(19) -0.007(4) -0.003(4) C4 0.053(6) 0.0379(10) 0.0317(16) -0.0147(10) -0.014(4) -0.011(5) C3 0.036(5) 0.0316(8) 0.0356(17) -0.0075(12) -0.015(4) -0.013(4) C2 0.013(5) 0.029(2) 0.041(3) -0.005(2) -0.009(3) -0.008(3) C7 0.043(4) 0.040(5) 0.037(4) -0.020(2) -0.008(3) 0.004(5) C8 0.040(4) 0.054(3) 0.038(5) -0.019(3) 0.001(3) -0.003(3) C9 0.042(5) 0.050(3) 0.046(4) -0.020(2) -0.002(3) -0.010(3) C50 0.0593(19) 0.0650(17) 0.0647(18) -0.0314(15) -0.0033(15) -0.0139(15) C51 0.0503(15) 0.0426(13) 0.0427(13) -0.0186(11) -0.0102(12) -0.0117(11) C52 0.0605(16) 0.0369(10) 0.0408(14) -0.0113(10) -0.0149(12) -0.0091(10) C53 0.0569(19) 0.0483(15) 0.0499(16) -0.0173(13) -0.0079(15) -0.0131(14) C54 0.0518(16) 0.0611(16) 0.0644(18) -0.0277(15) -0.0094(13) -0.0088(13) C55 0.074(2) 0.0428(14) 0.0567(17) -0.0155(13) -0.0323(14) -0.0022(14) C56 0.0626(18) 0.0358(12) 0.0465(14) -0.0122(10) -0.0232(14) -0.0053(13) C50A 0.0593(19) 0.0650(17) 0.0647(18) -0.0314(15) -0.0033(15) -0.0139(15) C51A 0.0503(15) 0.0426(13) 0.0427(13) -0.0186(11) -0.0102(12) -0.0117(11) C52A 0.0605(16) 0.0369(10) 0.0408(14) -0.0113(10) -0.0149(12) -0.0091(10) C53A 0.0569(19) 0.0483(15) 0.0499(16) -0.0173(13) -0.0079(15) -0.0131(14) C54A 0.0518(16) 0.0611(16) 0.0644(18) -0.0277(15) -0.0094(13) -0.0088(13) C55A 0.074(2) 0.0428(14) 0.0567(17) -0.0155(13) -0.0323(14) -0.0022(14) C56A 0.0626(18) 0.0358(12) 0.0465(14) -0.0122(10) -0.0232(14) -0.0053(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.899(3) . ? Li1 O1 1.921(3) . ? Li1 N31 2.132(3) . ? Li1 N32 2.216(3) . ? Li1 Li2 2.572(3) . ? Li1 C33A 2.770(8) . ? Li2 O2 1.915(3) . ? Li2 O1 1.918(3) . ? Li2 N42 2.088(17) . ? Li2 N41A 2.14(2) . ? Li2 N41 2.184(9) . ? Li2 N42A 2.20(4) . ? O1 C61 1.254(16) . ? O1 C1 1.400(16) . ? C71 C72 1.366(7) . ? C71 C66 1.407(7) . ? C71 H71 0.9500 . ? C72 C73 1.400(7) . ? C72 H72 0.9500 . ? C73 C74 1.346(8) . ? C73 H73 0.9500 . ? C74 C65 1.436(7) . ? C74 H74 0.9500 . ? C65 C64 1.385(7) . ? C65 C66 1.435(7) . ? C66 C61 1.433(7) . ? C61 C62 1.415(7) . ? C64 C63 1.399(7) . ? C64 H64 0.9500 . ? C63 C70 1.432(7) . ? C63 C62 1.442(7) . ? C70 C69 1.354(6) . ? C70 H70 0.9500 . ? C69 C68 1.416(7) . ? C69 H69 0.9500 . ? C68 C67 1.354(8) . ? C68 H68 0.9500 . ? C67 C62 1.426(8) . ? C67 H67 0.9500 . ? O2 C15 1.259(6) . ? O2 C75 1.46(2) . ? C25 C26 1.366(4) . ? C25 C20 1.421(4) . ? C25 H25 0.9500 . ? C26 C27 1.397(4) . ? C26 H26 0.9500 . ? C27 C28 1.350(4) . ? C27 H27 0.9500 . ? C28 C19 1.430(4) . ? C28 H28 0.9500 . ? C19 C18 1.401(4) . ? C19 C20 1.439(4) . ? C18 C17 1.392(4) . ? C18 H18 0.9500 . ? C17 C16 1.424(4) . ? C17 C24 1.424(4) . ? C24 C23 1.350(4) . ? C24 H24 0.9500 . ? C23 C22 1.410(4) . ? C23 H23 0.9500 . ? C22 C21 1.359(4) . ? C22 H22 0.9500 . ? C21 C16 1.422(3) . ? C21 H21 0.9500 . ? C16 C15 1.421(4) . ? C15 C20 1.424(4) . ? N31 C31 1.431(5) . ? N31 C30A 1.453(9) . ? N31 C30 1.462(5) . ? N31 C32 1.463(4) . ? N31 C31A 1.471(10) . ? N31 C32A 1.546(8) . ? N32 C34 1.456(6) . ? N32 C35 1.459(5) . ? N32 C34A 1.474(10) . ? N32 C35A 1.476(10) . ? N32 C33 1.485(4) . ? N32 C33A 1.500(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.413(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N41 C40 1.459(5) . ? N41 C41 1.460(6) . ? N41 C42 1.494(6) . ? C40 H41A 0.9800 . ? C40 H41B 0.9800 . ? C40 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C42 C43 1.499(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N42 1.464(6) . ? C43 H43C 0.9900 . ? C43 H43D 0.9900 . ? N41A C40A 1.465(10) . ? N41A C41A 1.479(10) . ? N41A C42A 1.487(10) . ? C40A H41G 0.9800 . ? C40A H41H 0.9800 . ? C40A H41I 0.9800 . ? C41A H41J 0.9800 . ? C41A H41K 0.9800 . ? C41A H41L 0.9800 . ? C42A C43A 1.502(10) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? N42 C44 1.453(5) . ? N42 C45 1.461(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C32A C33A 1.590(9) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? N42A C44A 1.470(10) . ? N42A C45A 1.472(10) . ? N42A C43A 1.473(10) . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C88 C87 1.339(9) . ? C88 C79 1.427(9) . ? C88 H88 0.9500 . ? C87 C86 1.396(8) . ? C87 H87 0.9500 . ? C78 C79 1.386(8) . ? C78 C77 1.390(8) . ? C78 H78 0.9500 . ? C77 C76 1.418(9) . ? C77 C84 1.428(9) . ? C80 C85 1.401(9) . ? C80 C75 1.428(10) . ? C80 C79 1.431(9) . ? C83 C84 1.356(9) . ? C83 C82 1.413(9) . ? C83 H83 0.9500 . ? C81 C82 1.347(9) . ? C81 C76 1.403(8) . ? C81 H81 0.9500 . ? C86 C85 1.362(9) . ? C86 H86 0.9500 . ? C84 H84 0.9500 . ? C75 C76 1.439(10) . ? C82 H82 0.9500 . ? C85 H85 0.9500 . ? C6 C11 1.414(8) . ? C6 C1 1.427(8) . ? C6 C5 1.432(8) . ? C11 C12 1.362(8) . ? C11 H11 0.9500 . ? C12 C13 1.409(8) . ? C12 H12 0.9500 . ? C13 C14 1.360(8) . ? C13 H13 0.9500 . ? C14 C5 1.433(7) . ? C14 H14 0.9500 . ? C5 C4 1.381(7) . ? C10 C9 1.357(7) . ? C10 C3 1.413(7) . ? C10 H10 0.9500 . ? C1 C2 1.429(7) . ? C4 C3 1.390(8) . ? C4 H4A 0.9500 . ? C3 C2 1.422(8) . ? C2 C7 1.421(8) . ? C7 C8 1.354(8) . ? C7 H7 0.9500 . ? C8 C9 1.410(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C50 C51 1.500(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C50A C51A 1.481(6) . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51A C52A 1.3900 . ? C51A C56A 1.3900 . ? C52A C53A 1.3900 . ? C52A H52A 0.9500 . ? C53A C54A 1.3900 . ? C53A H53A 0.9500 . ? C54A C55A 1.3900 . ? C54A H54A 0.9500 . ? C55A C56A 1.3900 . ? C55A H55A 0.9500 . ? C56A H56A 0.9500 . ? 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 O2 Li1 O1 95.36(12) . . ? O2 Li1 N31 124.52(15) . . ? O1 Li1 N31 113.00(13) . . ? O2 Li1 N32 114.36(13) . . ? O1 Li1 N32 128.05(15) . . ? N31 Li1 N32 84.83(10) . . ? O2 Li1 Li2 47.84(9) . . ? O1 Li1 Li2 47.89(8) . . ? N31 Li1 Li2 140.06(14) . . ? N32 Li1 Li2 135.11(14) . . ? O2 Li1 C33A 143.1(2) . . ? O1 Li1 C33A 118.4(2) . . ? N31 Li1 C33A 57.6(2) . . ? N32 Li1 C33A 32.69(17) . . ? Li2 Li1 C33A 157.5(3) . . ? O2 Li2 O1 94.96(11) . . ? O2 Li2 N42 115.3(3) . . ? O1 Li2 N42 112.1(3) . . ? O2 Li2 N41A 119.1(3) . . ? O1 Li2 N41A 132.9(3) . . ? N42 Li2 N41A 83.3(4) . . ? O2 Li2 N41 119.17(18) . . ? O1 Li2 N41 130.65(18) . . ? N42 Li2 N41 85.7(3) . . ? N41A Li2 N41 2.8(4) . . ? O2 Li2 N42A 112.4(5) . . ? O1 Li2 N42A 113.7(5) . . ? N42 Li2 N42A 3.1(7) . . ? N41A Li2 N42A 84.0(7) . . ? N41 Li2 N42A 86.5(6) . . ? O2 Li2 Li1 47.34(8) . . ? O1 Li2 Li1 47.99(8) . . ? N42 Li2 Li1 121.8(3) . . ? N41A Li2 Li1 154.1(3) . . ? N41 Li2 Li1 152.0(2) . . ? N42A Li2 Li1 120.6(6) . . ? C61 O1 C1 14.9(9) . . ? C61 O1 Li2 131.8(9) . . ? C1 O1 Li2 135.9(9) . . ? C61 O1 Li1 142.0(10) . . ? C1 O1 Li1 139.6(9) . . ? Li2 O1 Li1 84.12(11) . . ? C72 C71 C66 120.3(12) . . ? C72 C71 H71 119.8 . . ? C66 C71 H71 119.8 . . ? C71 C72 C73 120.9(9) . . ? C71 C72 H72 119.6 . . ? C73 C72 H72 119.6 . . ? C74 C73 C72 122.1(11) . . ? C74 C73 H73 119.0 . . ? C72 C73 H73 119.0 . . ? C73 C74 C65 118.5(11) . . ? C73 C74 H74 120.8 . . ? C65 C74 H74 120.8 . . ? C64 C65 C66 117.6(10) . . ? C64 C65 C74 122.4(10) . . ? C66 C65 C74 120.0(9) . . ? C71 C66 C61 117.9(10) . . ? C71 C66 C65 118.1(11) . . ? C61 C66 C65 123.9(11) . . ? O1 C61 C62 114.8(10) . . ? O1 C61 C66 129.4(9) . . ? C62 C61 C66 115.7(12) . . ? C65 C64 C63 121.3(10) . . ? C65 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C64 C63 C70 118.6(8) . . ? C64 C63 C62 120.5(8) . . ? C70 C63 C62 121.0(9) . . ? C69 C70 C63 121.3(11) . . ? C69 C70 H70 119.3 . . ? C63 C70 H70 119.3 . . ? C70 C69 C68 118.7(10) . . ? C70 C69 H69 120.6 . . ? C68 C69 H69 120.6 . . ? C67 C68 C69 120.7(11) . . ? C67 C68 H68 119.7 . . ? C69 C68 H68 119.7 . . ? C68 C67 C62 124.2(14) . . ? C68 C67 H67 117.9 . . ? C62 C67 H67 117.9 . . ? C61 C62 C67 125.2(11) . . ? C61 C62 C63 120.8(9) . . ? C67 C62 C63 113.9(10) . . ? C15 O2 C75 7.8(10) . . ? C15 O2 Li1 132.4(4) . . ? C75 O2 Li1 138.7(11) . . ? C15 O2 Li2 130.4(4) . . ? C75 O2 Li2 129.3(12) . . ? Li1 O2 Li2 84.82(11) . . ? C26 C25 C20 123.3(3) . . ? C26 C25 H25 118.3 . . ? C20 C25 H25 118.3 . . ? C25 C26 C27 118.8(3) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 121.1(3) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C19 121.9(3) . . ? C27 C28 H28 119.1 . . ? C19 C28 H28 119.1 . . ? C18 C19 C28 122.2(3) . . ? C18 C19 C20 119.9(3) . . ? C28 C19 C20 117.9(3) . . ? C17 C18 C19 120.1(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C17 C16 120.3(2) . . ? C18 C17 C24 121.4(3) . . ? C16 C17 C24 118.3(3) . . ? C23 C24 C17 121.3(3) . . ? C23 C24 H24 119.4 . . ? C17 C24 H24 119.4 . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C21 C22 C23 119.6(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C21 C16 121.6(3) . . ? C22 C21 H21 119.2 . . ? C16 C21 H21 119.2 . . ? C15 C16 C21 120.0(3) . . ? C15 C16 C17 121.7(3) . . ? C21 C16 C17 118.3(3) . . ? O2 C15 C16 120.6(4) . . ? O2 C15 C20 122.4(4) . . ? C16 C15 C20 116.9(4) . . ? C25 C20 C15 121.9(4) . . ? C25 C20 C19 116.9(3) . . ? C15 C20 C19 121.1(4) . . ? C31 N31 C30A 120.8(11) . . ? C31 N31 C30 107.4(7) . . ? C30A N31 C30 17.5(8) . . ? C31 N31 C32 114.6(7) . . ? C30A N31 C32 87.6(7) . . ? C30 N31 C32 104.1(3) . . ? C31 N31 C31A 12.1(17) . . ? C30A N31 C31A 112.0(17) . . ? C30 N31 C31A 97.2(14) . . ? C32 N31 C31A 124.7(15) . . ? C31 N31 C32A 87.8(6) . . ? C30A N31 C32A 118.9(8) . . ? C30 N31 C32A 133.4(4) . . ? C32 N31 C32A 33.1(4) . . ? C31A N31 C32A 99.6(14) . . ? C31 N31 Li1 119.7(8) . . ? C30A N31 Li1 105.8(10) . . ? C30 N31 Li1 107.3(4) . . ? C32 N31 Li1 102.5(2) . . ? C31A N31 Li1 118.8(19) . . ? C32A N31 Li1 101.9(4) . . ? C34 N32 C35 107.3(7) . . ? C34 N32 C34A 14.7(18) . . ? C35 N32 C34A 121.0(15) . . ? C34 N32 C35A 95.2(11) . . ? C35 N32 C35A 18.8(9) . . ? C34A N32 C35A 109.8(17) . . ? C34 N32 C33 105.9(6) . . ? C35 N32 C33 109.8(3) . . ? C34A N32 C33 94.9(14) . . ? C35A N32 C33 128.0(7) . . ? C34 N32 C33A 134.1(7) . . ? C35 N32 C33A 92.4(5) . . ? C34A N32 C33A 123.5(14) . . ? C35A N32 C33A 110.9(9) . . ? C33 N32 C33A 28.6(3) . . ? C34 N32 Li1 106.9(7) . . ? C35 N32 Li1 123.9(4) . . ? C34A N32 Li1 100.4(17) . . ? C35A N32 Li1 116.9(9) . . ? C33 N32 Li1 101.71(17) . . ? C33A N32 Li1 94.4(4) . . ? N31 C30 H30A 109.5 . . ? N31 C30 H30B 109.5 . . ? N31 C30 H30C 109.5 . . ? N31 C31 H31A 109.5 . . ? N31 C31 H31B 109.5 . . ? N31 C31 H31C 109.5 . . ? C33 C32 N31 114.8(3) . . ? C33 C32 H32A 108.6 . . ? N31 C32 H32A 108.6 . . ? C33 C32 H32B 108.6 . . ? N31 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C32 C33 N32 118.6(3) . . ? C32 C33 H33A 107.7 . . ? N32 C33 H33A 107.7 . . ? C32 C33 H33B 107.7 . . ? N32 C33 H33B 107.7 . . ? H33A C33 H33B 107.1 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? N32 C35 H35A 109.5 . . ? N32 C35 H35B 109.5 . . ? N32 C35 H35C 109.5 . . ? C40 N41 C41 108.4(4) . . ? C40 N41 C42 109.0(5) . . ? C41 N41 C42 109.6(5) . . ? C40 N41 Li2 105.6(4) . . ? C41 N41 Li2 122.3(5) . . ? C42 N41 Li2 101.3(4) . . ? N41 C42 C43 112.9(5) . . ? N41 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N41 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? N42 C43 C42 110.3(8) . . ? N42 C43 H43C 109.6 . . ? C42 C43 H43C 109.6 . . ? N42 C43 H43D 109.6 . . ? C42 C43 H43D 109.6 . . ? H43C C43 H43D 108.1 . . ? C40A N41A C41A 116.0(11) . . ? C40A N41A C42A 103.0(9) . . ? C41A N41A C42A 111.1(11) . . ? C40A N41A Li2 119.1(10) . . ? C41A N41A Li2 106.4(9) . . ? C42A N41A Li2 99.8(8) . . ? N41A C40A H41G 109.5 . . ? N41A C40A H41H 109.5 . . ? H41G C40A H41H 109.5 . . ? N41A C40A H41I 109.5 . . ? H41G C40A H41I 109.5 . . ? H41H C40A H41I 109.5 . . ? N41A C41A H41J 109.5 . . ? N41A C41A H41K 109.5 . . ? H41J C41A H41K 109.5 . . ? N41A C41A H41L 109.5 . . ? H41J C41A H41L 109.5 . . ? H41K C41A H41L 109.5 . . ? N41A C42A C43A 109.2(13) . . ? N41A C42A H42C 109.8 . . ? C43A C42A H42C 109.8 . . ? N41A C42A H42D 109.8 . . ? C43A C42A H42D 109.8 . . ? H42C C42A H42D 108.3 . . ? C44 N42 C45 110.3(6) . . ? C44 N42 C43 111.1(8) . . ? C45 N42 C43 107.6(10) . . ? C44 N42 Li2 105.9(8) . . ? C45 N42 Li2 115.9(8) . . ? C43 N42 Li2 106.0(6) . . ? N31 C32A C33A 101.4(7) . . ? N31 C32A H32C 111.5 . . ? C33A C32A H32C 111.5 . . ? N31 C32A H32D 111.5 . . ? C33A C32A H32D 111.5 . . ? H32C C32A H32D 109.3 . . ? N31 C30A H30D 109.5 . . ? N31 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? N31 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? N31 C31A H31D 109.5 . . ? N31 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? N31 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? N32 C33A C32A 100.6(6) . . ? N32 C33A Li1 52.9(3) . . ? C32A C33A Li1 77.5(5) . . ? N32 C33A H33C 111.6 . . ? C32A C33A H33C 111.6 . . ? Li1 C33A H33C 77.2 . . ? N32 C33A H33D 111.6 . . ? C32A C33A H33D 111.6 . . ? Li1 C33A H33D 164.2 . . ? H33C C33A H33D 109.4 . . ? N32 C34A H34D 109.5 . . ? N32 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? N32 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C44A N42A C45A 109.6(13) . . ? C44A N42A C43A 109.2(18) . . ? C45A N42A C43A 117(2) . . ? C44A N42A Li2 109.7(19) . . ? C45A N42A Li2 107.1(18) . . ? C43A N42A Li2 103.7(15) . . ? N42A C44A H44D 109.5 . . ? N42A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? N42A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? N42A C45A H45D 109.5 . . ? N42A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? N42A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? N32 C35A H35D 109.5 . . ? N32 C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? N32 C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? N42A C43A C42A 109.3(14) . . ? N42A C43A H43A 109.8 . . ? C42A C43A H43A 109.8 . . ? N42A C43A H43B 109.8 . . ? C42A C43A H43B 109.8 . . ? H43A C43A H43B 108.3 . . ? C87 C88 C79 121.8(11) . . ? C87 C88 H88 119.1 . . ? C79 C88 H88 119.1 . . ? C88 C87 C86 119.5(11) . . ? C88 C87 H87 120.2 . . ? C86 C87 H87 120.2 . . ? C79 C78 C77 122.2(9) . . ? C79 C78 H78 118.9 . . ? C77 C78 H78 118.9 . . ? C78 C77 C76 120.9(9) . . ? C78 C77 C84 120.6(9) . . ? C76 C77 C84 118.5(10) . . ? C85 C80 C75 118.8(12) . . ? C85 C80 C79 122.8(13) . . ? C75 C80 C79 118.4(14) . . ? C84 C83 C82 124.5(10) . . ? C84 C83 H83 117.8 . . ? C82 C83 H83 117.8 . . ? C82 C81 C76 121.4(10) . . ? C82 C81 H81 119.3 . . ? C76 C81 H81 119.3 . . ? C78 C79 C88 124.6(10) . . ? C78 C79 C80 119.6(9) . . ? C88 C79 C80 115.8(11) . . ? C85 C86 C87 123.7(10) . . ? C85 C86 H86 118.2 . . ? C87 C86 H86 118.2 . . ? C83 C84 C77 117.7(9) . . ? C83 C84 H84 121.2 . . ? C77 C84 H84 121.2 . . ? C80 C75 C76 121.4(16) . . ? C80 C75 O2 116.8(12) . . ? C76 C75 O2 121.6(13) . . ? C81 C76 C77 120.2(11) . . ? C81 C76 C75 122.4(11) . . ? C77 C76 C75 117.4(12) . . ? C81 C82 C83 117.6(9) . . ? C81 C82 H82 121.2 . . ? C83 C82 H82 121.2 . . ? C86 C85 C80 116.3(12) . . ? C86 C85 H85 121.8 . . ? C80 C85 H85 121.8 . . ? C11 C6 C1 123.6(11) . . ? C11 C6 C5 118.7(13) . . ? C1 C6 C5 117.6(12) . . ? C12 C11 C6 123.9(13) . . ? C12 C11 H11 118.1 . . ? C6 C11 H11 118.1 . . ? C11 C12 C13 118.2(11) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 119.4(12) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C5 124.5(13) . . ? C13 C14 H14 117.7 . . ? C5 C14 H14 117.7 . . ? C4 C5 C6 123.4(11) . . ? C4 C5 C14 121.4(11) . . ? C6 C5 C14 115.2(11) . . ? C9 C10 C3 122.2(12) . . ? C9 C10 H10 118.9 . . ? C3 C10 H10 118.9 . . ? O1 C1 C6 112.6(9) . . ? O1 C1 C2 128.6(12) . . ? C6 C1 C2 118.8(13) . . ? C5 C4 C3 118.9(11) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C4 C3 C10 125.5(9) . . ? C4 C3 C2 120.5(9) . . ? C10 C3 C2 113.9(10) . . ? C7 C2 C3 124.4(11) . . ? C7 C2 C1 114.9(12) . . ? C3 C2 C1 120.7(11) . . ? C8 C7 C2 117.8(14) . . ? C8 C7 H7 121.1 . . ? C2 C7 H7 121.1 . . ? C7 C8 C9 119.7(13) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 121.9(11) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 C50 119.71(18) . . ? C56 C51 C50 120.27(18) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C51A C50A H50D 109.5 . . ? C51A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C51A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C52A C51A C56A 120.0 . . ? C52A C51A C50A 120.8(3) . . ? C56A C51A C50A 119.1(3) . . ? C53A C52A C51A 120.0 . . ? C53A C52A H52A 120.0 . . ? C51A C52A H52A 120.0 . . ? C52A C53A C54A 120.0 . . ? C52A C53A H53A 120.0 . . ? C54A C53A H53A 120.0 . . ? C55A C54A C53A 120.0 . . ? C55A C54A H54A 120.0 . . ? C53A C54A H54A 120.0 . . ? C56A C55A C54A 120.0 . . ? C56A C55A H55A 120.0 . . ? C54A C55A H55A 120.0 . . ? C55A C56A C51A 120.0 . . ? C55A C56A H56A 120.0 . . ? C51A C56A H56A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Li1 Li2 O2 -171.26(17) . . . . ? N31 Li1 Li2 O2 -96.3(2) . . . . ? N32 Li1 Li2 O2 83.09(19) . . . . ? C33A Li1 Li2 O2 129.3(5) . . . . ? O2 Li1 Li2 O1 171.26(17) . . . . ? N31 Li1 Li2 O1 75.0(2) . . . . ? N32 Li1 Li2 O1 -105.7(2) . . . . ? C33A Li1 Li2 O1 -59.5(5) . . . . ? O2 Li1 Li2 N42 -96.5(3) . . . . ? O1 Li1 Li2 N42 92.2(3) . . . . ? N31 Li1 Li2 N42 167.2(3) . . . . ? N32 Li1 Li2 N42 -13.5(4) . . . . ? C33A Li1 Li2 N42 32.7(6) . . . . ? O2 Li1 Li2 N41A 67.3(7) . . . . ? O1 Li1 Li2 N41A -103.9(7) . . . . ? N31 Li1 Li2 N41A -29.0(8) . . . . ? N32 Li1 Li2 N41A 150.4(6) . . . . ? C33A Li1 Li2 N41A -163.4(8) . . . . ? O2 Li1 Li2 N41 71.3(4) . . . . ? O1 Li1 Li2 N41 -100.0(4) . . . . ? N31 Li1 Li2 N41 -25.0(5) . . . . ? N32 Li1 Li2 N41 154.4(3) . . . . ? C33A Li1 Li2 N41 -159.5(5) . . . . ? O2 Li1 Li2 N42A -93.2(5) . . . . ? O1 Li1 Li2 N42A 95.5(5) . . . . ? N31 Li1 Li2 N42A 170.5(5) . . . . ? N32 Li1 Li2 N42A -10.1(6) . . . . ? C33A Li1 Li2 N42A 36.1(7) . . . . ? O2 Li2 O1 C61 -159.6(8) . . . . ? N42 Li2 O1 C61 80.5(9) . . . . ? N41A Li2 O1 C61 -21.4(9) . . . . ? N41 Li2 O1 C61 -23.6(9) . . . . ? N42A Li2 O1 C61 83.3(10) . . . . ? Li1 Li2 O1 C61 -166.0(8) . . . . ? O2 Li2 O1 C1 -179.5(8) . . . . ? N42 Li2 O1 C1 60.5(8) . . . . ? N41A Li2 O1 C1 -41.3(9) . . . . ? N41 Li2 O1 C1 -43.5(8) . . . . ? N42A Li2 O1 C1 63.4(10) . . . . ? Li1 Li2 O1 C1 174.0(8) . . . . ? O2 Li2 O1 Li1 6.44(12) . . . . ? N42 Li2 O1 Li1 -113.5(3) . . . . ? N41A Li2 O1 Li1 144.6(4) . . . . ? N41 Li2 O1 Li1 142.4(3) . . . . ? N42A Li2 O1 Li1 -110.7(6) . . . . ? O2 Li1 O1 C61 156.5(7) . . . . ? N31 Li1 O1 C61 25.3(8) . . . . ? N32 Li1 O1 C61 -76.7(8) . . . . ? Li2 Li1 O1 C61 163.0(8) . . . . ? C33A Li1 O1 C61 -39.0(8) . . . . ? O2 Li1 O1 C1 179.9(9) . . . . ? N31 Li1 O1 C1 48.8(9) . . . . ? N32 Li1 O1 C1 -53.2(9) . . . . ? Li2 Li1 O1 C1 -173.6(9) . . . . ? C33A Li1 O1 C1 -15.6(10) . . . . ? O2 Li1 O1 Li2 -6.49(12) . . . . ? N31 Li1 O1 Li2 -137.65(15) . . . . ? N32 Li1 O1 Li2 120.35(18) . . . . ? C33A Li1 O1 Li2 158.0(3) . . . . ? C66 C71 C72 C73 2(2) . . . . ? C71 C72 C73 C74 -1.8(17) . . . . ? C72 C73 C74 C65 -1(2) . . . . ? C73 C74 C65 C64 -174.8(14) . . . . ? C73 C74 C65 C66 3(2) . . . . ? C72 C71 C66 C61 177.5(18) . . . . ? C72 C71 C66 C65 0(3) . . . . ? C64 C65 C66 C71 175.5(17) . . . . ? C74 C65 C66 C71 -3(3) . . . . ? C64 C65 C66 C61 -2(3) . . . . ? C74 C65 C66 C61 180(2) . . . . ? C1 O1 C61 C62 -7(6) . . . . ? Li2 O1 C61 C62 -119.4(11) . . . . ? Li1 O1 C61 C62 83.6(16) . . . . ? C1 O1 C61 C66 174(9) . . . . ? Li2 O1 C61 C66 61(3) . . . . ? Li1 O1 C61 C66 -96(2) . . . . ? C71 C66 C61 O1 7(4) . . . . ? C65 C66 C61 O1 -175.9(19) . . . . ? C71 C66 C61 C62 -172.6(17) . . . . ? C65 C66 C61 C62 5(3) . . . . ? C66 C65 C64 C63 -2(3) . . . . ? C74 C65 C64 C63 176.1(16) . . . . ? C65 C64 C63 C70 -176.2(15) . . . . ? C65 C64 C63 C62 3(3) . . . . ? C64 C63 C70 C69 179.7(16) . . . . ? C62 C63 C70 C69 0(2) . . . . ? C63 C70 C69 C68 -1(2) . . . . ? C70 C69 C68 C67 3(3) . . . . ? C69 C68 C67 C62 -5(5) . . . . ? O1 C61 C62 C67 -2(3) . . . . ? C66 C61 C62 C67 177(3) . . . . ? O1 C61 C62 C63 176.8(15) . . . . ? C66 C61 C62 C63 -4(3) . . . . ? C68 C67 C62 C61 -177(3) . . . . ? C68 C67 C62 C63 4(4) . . . . ? C64 C63 C62 C61 0(2) . . . . ? C70 C63 C62 C61 179.4(15) . . . . ? C64 C63 C62 C67 179(2) . . . . ? C70 C63 C62 C67 -1(3) . . . . ? O1 Li1 O2 C15 -136.5(4) . . . . ? N31 Li1 O2 C15 -13.7(5) . . . . ? N32 Li1 O2 C15 87.3(5) . . . . ? Li2 Li1 O2 C15 -143.0(5) . . . . ? C33A Li1 O2 C15 66.7(6) . . . . ? O1 Li1 O2 C75 -143.0(12) . . . . ? N31 Li1 O2 C75 -20.3(12) . . . . ? N32 Li1 O2 C75 80.8(12) . . . . ? Li2 Li1 O2 C75 -149.5(12) . . . . ? C33A Li1 O2 C75 60.1(12) . . . . ? O1 Li1 O2 Li2 6.50(12) . . . . ? N31 Li1 O2 Li2 129.24(17) . . . . ? N32 Li1 O2 Li2 -129.73(15) . . . . ? C33A Li1 O2 Li2 -150.4(4) . . . . ? O1 Li2 O2 C15 137.8(3) . . . . ? N42 Li2 O2 C15 -104.9(4) . . . . ? N41A Li2 O2 C15 -8.3(5) . . . . ? N41 Li2 O2 C15 -5.1(4) . . . . ? N42A Li2 O2 C15 -104.0(7) . . . . ? Li1 Li2 O2 C15 144.3(3) . . . . ? O1 Li2 O2 C75 147.9(8) . . . . ? N42 Li2 O2 C75 -94.8(9) . . . . ? N41A Li2 O2 C75 1.8(9) . . . . ? N41 Li2 O2 C75 5.0(9) . . . . ? N42A Li2 O2 C75 -93.9(10) . . . . ? Li1 Li2 O2 C75 154.4(8) . . . . ? O1 Li2 O2 Li1 -6.50(12) . . . . ? N42 Li2 O2 Li1 110.8(3) . . . . ? N41A Li2 O2 Li1 -152.5(4) . . . . ? N41 Li2 O2 Li1 -149.4(2) . . . . ? N42A Li2 O2 Li1 111.7(6) . . . . ? C20 C25 C26 C27 0.5(7) . . . . ? C25 C26 C27 C28 0.9(5) . . . . ? C26 C27 C28 C19 -1.1(4) . . . . ? C27 C28 C19 C18 -179.9(3) . . . . ? C27 C28 C19 C20 -0.1(6) . . . . ? C28 C19 C18 C17 178.6(3) . . . . ? C20 C19 C18 C17 -1.1(6) . . . . ? C19 C18 C17 C16 0.8(5) . . . . ? C19 C18 C17 C24 -179.4(3) . . . . ? C18 C17 C24 C23 -178.3(3) . . . . ? C16 C17 C24 C23 1.5(5) . . . . ? C17 C24 C23 C22 0.4(5) . . . . ? C24 C23 C22 C21 -2.0(4) . . . . ? C23 C22 C21 C16 1.6(5) . . . . ? C22 C21 C16 C15 178.5(5) . . . . ? C22 C21 C16 C17 0.2(6) . . . . ? C18 C17 C16 C15 -0.2(7) . . . . ? C24 C17 C16 C15 180.0(6) . . . . ? C18 C17 C16 C21 178.0(3) . . . . ? C24 C17 C16 C21 -1.7(5) . . . . ? C75 O2 C15 C16 -147(12) . . . . ? Li1 O2 C15 C16 66.2(10) . . . . ? Li2 O2 C15 C16 -61.8(9) . . . . ? C75 O2 C15 C20 29(11) . . . . ? Li1 O2 C15 C20 -117.0(7) . . . . ? Li2 O2 C15 C20 115.0(7) . . . . ? C21 C16 C15 O2 -1.3(11) . . . . ? C17 C16 C15 O2 177.0(6) . . . . ? C21 C16 C15 C20 -178.2(6) . . . . ? C17 C16 C15 C20 0.0(10) . . . . ? C26 C25 C20 C15 178.7(7) . . . . ? C26 C25 C20 C19 -1.6(9) . . . . ? O2 C15 C20 C25 2.5(13) . . . . ? C16 C15 C20 C25 179.4(7) . . . . ? O2 C15 C20 C19 -177.2(7) . . . . ? C16 C15 C20 C19 -0.3(12) . . . . ? C18 C19 C20 C25 -178.9(5) . . . . ? C28 C19 C20 C25 1.4(8) . . . . ? C18 C19 C20 C15 0.8(9) . . . . ? C28 C19 C20 C15 -178.9(6) . . . . ? O2 Li1 N31 C31 11.8(6) . . . . ? O1 Li1 N31 C31 126.4(6) . . . . ? N32 Li1 N31 C31 -104.3(6) . . . . ? Li2 Li1 N31 C31 75.3(6) . . . . ? C33A Li1 N31 C31 -123.6(6) . . . . ? O2 Li1 N31 C30A -128.9(7) . . . . ? O1 Li1 N31 C30A -14.3(7) . . . . ? N32 Li1 N31 C30A 115.0(7) . . . . ? Li2 Li1 N31 C30A -65.5(7) . . . . ? C33A Li1 N31 C30A 95.6(7) . . . . ? O2 Li1 N31 C30 -110.6(3) . . . . ? O1 Li1 N31 C30 3.9(3) . . . . ? N32 Li1 N31 C30 133.2(2) . . . . ? Li2 Li1 N31 C30 -47.2(3) . . . . ? C33A Li1 N31 C30 113.9(3) . . . . ? O2 Li1 N31 C32 140.0(3) . . . . ? O1 Li1 N31 C32 -105.4(3) . . . . ? N32 Li1 N31 C32 23.9(2) . . . . ? Li2 Li1 N31 C32 -156.6(3) . . . . ? C33A Li1 N31 C32 4.5(3) . . . . ? O2 Li1 N31 C31A -1.9(14) . . . . ? O1 Li1 N31 C31A 112.6(14) . . . . ? N32 Li1 N31 C31A -118.1(14) . . . . ? Li2 Li1 N31 C31A 61.5(14) . . . . ? C33A Li1 N31 C31A -137.4(14) . . . . ? O2 Li1 N31 C32A 106.1(4) . . . . ? O1 Li1 N31 C32A -139.3(4) . . . . ? N32 Li1 N31 C32A -10.0(4) . . . . ? Li2 Li1 N31 C32A 169.6(4) . . . . ? C33A Li1 N31 C32A -29.4(4) . . . . ? O2 Li1 N32 C34 -18.1(6) . . . . ? O1 Li1 N32 C34 -137.1(5) . . . . ? N31 Li1 N32 C34 107.6(5) . . . . ? Li2 Li1 N32 C34 -72.0(6) . . . . ? C33A Li1 N32 C34 138.8(7) . . . . ? O2 Li1 N32 C35 107.3(4) . . . . ? O1 Li1 N32 C35 -11.7(4) . . . . ? N31 Li1 N32 C35 -127.0(4) . . . . ? Li2 Li1 N32 C35 53.4(4) . . . . ? C33A Li1 N32 C35 -95.8(5) . . . . ? O2 Li1 N32 C34A -31.7(14) . . . . ? O1 Li1 N32 C34A -150.7(14) . . . . ? N31 Li1 N32 C34A 94.0(14) . . . . ? Li2 Li1 N32 C34A -85.6(14) . . . . ? C33A Li1 N32 C34A 125.2(14) . . . . ? O2 Li1 N32 C35A 87.0(10) . . . . ? O1 Li1 N32 C35A -32.0(10) . . . . ? N31 Li1 N32 C35A -147.3(10) . . . . ? Li2 Li1 N32 C35A 33.1(10) . . . . ? C33A Li1 N32 C35A -116.1(11) . . . . ? O2 Li1 N32 C33 -129.0(2) . . . . ? O1 Li1 N32 C33 112.0(3) . . . . ? N31 Li1 N32 C33 -3.3(2) . . . . ? Li2 Li1 N32 C33 177.2(3) . . . . ? C33A Li1 N32 C33 27.9(4) . . . . ? O2 Li1 N32 C33A -156.9(4) . . . . ? O1 Li1 N32 C33A 84.1(4) . . . . ? N31 Li1 N32 C33A -31.2(4) . . . . ? Li2 Li1 N32 C33A 149.2(4) . . . . ? C31 N31 C32 C33 87.5(9) . . . . ? C30A N31 C32 C33 -149.5(11) . . . . ? C30 N31 C32 C33 -155.5(6) . . . . ? C31A N31 C32 C33 95(2) . . . . ? C32A N31 C32 C33 49.0(7) . . . . ? Li1 N31 C32 C33 -43.8(5) . . . . ? N31 C32 C33 N32 47.5(7) . . . . ? C34 N32 C33 C32 -132.7(8) . . . . ? C35 N32 C33 C32 111.8(6) . . . . ? C34A N32 C33 C32 -122.8(17) . . . . ? C35A N32 C33 C32 117.4(14) . . . . ? C33A N32 C33 C32 56.4(8) . . . . ? Li1 N32 C33 C32 -21.1(5) . . . . ? O2 Li2 N41 C40 -15.7(4) . . . . ? O1 Li2 N41 C40 -143.3(3) . . . . ? N42 Li2 N41 C40 101.0(4) . . . . ? N41A Li2 N41 C40 73(8) . . . . ? N42A Li2 N41 C40 98.0(5) . . . . ? Li1 Li2 N41 C40 -68.6(5) . . . . ? O2 Li2 N41 C41 108.7(4) . . . . ? O1 Li2 N41 C41 -18.9(5) . . . . ? N42 Li2 N41 C41 -134.6(4) . . . . ? N41A Li2 N41 C41 -163(8) . . . . ? N42A Li2 N41 C41 -137.6(6) . . . . ? Li1 Li2 N41 C41 55.8(6) . . . . ? O2 Li2 N41 C42 -129.3(3) . . . . ? O1 Li2 N41 C42 103.1(3) . . . . ? N42 Li2 N41 C42 -12.6(4) . . . . ? N41A Li2 N41 C42 -41(8) . . . . ? N42A Li2 N41 C42 -15.6(5) . . . . ? Li1 Li2 N41 C42 177.8(3) . . . . ? C40 N41 C42 C43 -71.8(7) . . . . ? C41 N41 C42 C43 169.7(6) . . . . ? Li2 N41 C42 C43 39.3(6) . . . . ? N41 C42 C43 N42 -57.6(7) . . . . ? O2 Li2 N41A C40A 25.2(9) . . . . ? O1 Li2 N41A C40A -105.4(7) . . . . ? N42 Li2 N41A C40A 140.5(8) . . . . ? N41 Li2 N41A C40A -68(8) . . . . ? N42A Li2 N41A C40A 137.5(9) . . . . ? Li1 Li2 N41A C40A -25.7(12) . . . . ? O2 Li2 N41A C41A 158.6(6) . . . . ? O1 Li2 N41A C41A 28.0(9) . . . . ? N42 Li2 N41A C41A -86.1(7) . . . . ? N41 Li2 N41A C41A 65(8) . . . . ? N42A Li2 N41A C41A -89.1(8) . . . . ? Li1 Li2 N41A C41A 107.7(8) . . . . ? O2 Li2 N41A C42A -85.8(6) . . . . ? O1 Li2 N41A C42A 143.6(5) . . . . ? N42 Li2 N41A C42A 29.5(6) . . . . ? N41 Li2 N41A C42A -179(100) . . . . ? N42A Li2 N41A C42A 26.5(7) . . . . ? Li1 Li2 N41A C42A -136.7(7) . . . . ? C40A N41A C42A C43A -178.5(13) . . . . ? C41A N41A C42A C43A 56.5(18) . . . . ? Li2 N41A C42A C43A -55.4(13) . . . . ? C42 C43 N42 C44 -73.8(10) . . . . ? C42 C43 N42 C45 165.4(7) . . . . ? C42 C43 N42 Li2 40.8(6) . . . . ? O2 Li2 N42 C44 -136.4(5) . . . . ? O1 Li2 N42 C44 -29.2(6) . . . . ? N41A Li2 N42 C44 104.5(6) . . . . ? N41 Li2 N42 C44 103.2(6) . . . . ? N42A Li2 N42 C44 -152(17) . . . . ? Li1 Li2 N42 C44 -82.5(6) . . . . ? O2 Li2 N42 C45 -13.8(7) . . . . ? O1 Li2 N42 C45 93.4(6) . . . . ? N41A Li2 N42 C45 -132.9(7) . . . . ? N41 Li2 N42 C45 -134.2(6) . . . . ? N42A Li2 N42 C45 -29(16) . . . . ? Li1 Li2 N42 C45 40.1(7) . . . . ? O2 Li2 N42 C43 105.4(5) . . . . ? O1 Li2 N42 C43 -147.4(5) . . . . ? N41A Li2 N42 C43 -13.6(5) . . . . ? N41 Li2 N42 C43 -14.9(5) . . . . ? N42A Li2 N42 C43 90(16) . . . . ? Li1 Li2 N42 C43 159.4(4) . . . . ? C31 N31 C32A C33A 167.2(9) . . . . ? C30A N31 C32A C33A -68.4(12) . . . . ? C30 N31 C32A C33A -80.8(8) . . . . ? C32 N31 C32A C33A -47.3(7) . . . . ? C31A N31 C32A C33A 169.7(19) . . . . ? Li1 N31 C32A C33A 47.4(5) . . . . ? C34 N32 C33A C32A -53.3(12) . . . . ? C35 N32 C33A C32A -170.4(6) . . . . ? C34A N32 C33A C32A -40(2) . . . . ? C35A N32 C33A C32A -173.6(11) . . . . ? C33 N32 C33A C32A -41.1(7) . . . . ? Li1 N32 C33A C32A 65.4(5) . . . . ? C34 N32 C33A Li1 -118.7(10) . . . . ? C35 N32 C33A Li1 124.2(4) . . . . ? C34A N32 C33A Li1 -106(2) . . . . ? C35A N32 C33A Li1 121.0(10) . . . . ? C33 N32 C33A Li1 -106.5(9) . . . . ? N31 C32A C33A N32 -82.5(6) . . . . ? N31 C32A C33A Li1 -34.6(4) . . . . ? O2 Li1 C33A N32 36.5(6) . . . . ? O1 Li1 C33A N32 -117.1(3) . . . . ? N31 Li1 C33A N32 142.3(4) . . . . ? Li2 Li1 C33A N32 -70.5(6) . . . . ? O2 Li1 C33A C32A -77.3(6) . . . . ? O1 Li1 C33A C32A 129.1(4) . . . . ? N31 Li1 C33A C32A 28.5(4) . . . . ? N32 Li1 C33A C32A -113.8(6) . . . . ? Li2 Li1 C33A C32A 175.7(5) . . . . ? O2 Li2 N42A C44A -120.0(11) . . . . ? O1 Li2 N42A C44A -13.5(15) . . . . ? N42 Li2 N42A C44A 45(15) . . . . ? N41A Li2 N42A C44A 121.0(13) . . . . ? N41 Li2 N42A C44A 119.8(12) . . . . ? Li1 Li2 N42A C44A -67.4(13) . . . . ? O2 Li2 N42A C45A -1.1(15) . . . . ? O1 Li2 N42A C45A 105.3(13) . . . . ? N42 Li2 N42A C45A 164(17) . . . . ? N41A Li2 N42A C45A -120.2(14) . . . . ? N41 Li2 N42A C45A -121.3(14) . . . . ? Li1 Li2 N42A C45A 51.4(15) . . . . ? O2 Li2 N42A C43A 123.5(11) . . . . ? O1 Li2 N42A C43A -130.1(11) . . . . ? N42 Li2 N42A C43A -72(16) . . . . ? N41A Li2 N42A C43A 4.5(11) . . . . ? N41 Li2 N42A C43A 3.3(11) . . . . ? Li1 Li2 N42A C43A 176.0(10) . . . . ? C44A N42A C43A C42A -153(2) . . . . ? C45A N42A C43A C42A 82(3) . . . . ? Li2 N42A C43A C42A -35.7(18) . . . . ? N41A C42A C43A N42A 66(2) . . . . ? C79 C88 C87 C86 0(2) . . . . ? C79 C78 C77 C76 3(2) . . . . ? C79 C78 C77 C84 -178.5(10) . . . . ? C77 C78 C79 C88 179.2(13) . . . . ? C77 C78 C79 C80 -2(2) . . . . ? C87 C88 C79 C78 177.6(13) . . . . ? C87 C88 C79 C80 -2(2) . . . . ? C85 C80 C79 C78 -178.2(18) . . . . ? C75 C80 C79 C78 0(3) . . . . ? C85 C80 C79 C88 1(3) . . . . ? C75 C80 C79 C88 179(2) . . . . ? C88 C87 C86 C85 2(2) . . . . ? C82 C83 C84 C77 0(2) . . . . ? C78 C77 C84 C83 -177.3(13) . . . . ? C76 C77 C84 C83 1.3(17) . . . . ? C85 C80 C75 C76 179(2) . . . . ? C79 C80 C75 C76 1(4) . . . . ? C85 C80 C75 O2 -6(4) . . . . ? C79 C80 C75 O2 176.6(19) . . . . ? C15 O2 C75 C80 -147(13) . . . . ? Li1 O2 C75 C80 -109(2) . . . . ? Li2 O2 C75 C80 112(2) . . . . ? C15 O2 C75 C76 29(9) . . . . ? Li1 O2 C75 C76 67(3) . . . . ? Li2 O2 C75 C76 -72(3) . . . . ? C82 C81 C76 C77 -1(2) . . . . ? C82 C81 C76 C75 179.0(18) . . . . ? C78 C77 C76 C81 178.1(13) . . . . ? C84 C77 C76 C81 -0.5(19) . . . . ? C78 C77 C76 C75 -2(2) . . . . ? C84 C77 C76 C75 179.1(17) . . . . ? C80 C75 C76 C81 180(2) . . . . ? O2 C75 C76 C81 4(3) . . . . ? C80 C75 C76 C77 0(3) . . . . ? O2 C75 C76 C77 -175.1(18) . . . . ? C76 C81 C82 C83 2.3(18) . . . . ? C84 C83 C82 C81 -1(2) . . . . ? C87 C86 C85 C80 -2(2) . . . . ? C75 C80 C85 C86 -177(2) . . . . ? C79 C80 C85 C86 1(3) . . . . ? C1 C6 C11 C12 -178(2) . . . . ? C5 C6 C11 C12 1(3) . . . . ? C6 C11 C12 C13 -1(2) . . . . ? C11 C12 C13 C14 -0.5(17) . . . . ? C12 C13 C14 C5 2(2) . . . . ? C11 C6 C5 C4 -179.4(19) . . . . ? C1 C6 C5 C4 0(3) . . . . ? C11 C6 C5 C14 1(3) . . . . ? C1 C6 C5 C14 180(2) . . . . ? C13 C14 C5 C4 177.9(16) . . . . ? C13 C14 C5 C6 -2(3) . . . . ? C61 O1 C1 C6 -9(6) . . . . ? Li2 O1 C1 C6 73(2) . . . . ? Li1 O1 C1 C6 -116.6(16) . . . . ? C61 O1 C1 C2 170(9) . . . . ? Li2 O1 C1 C2 -109.0(17) . . . . ? Li1 O1 C1 C2 62(2) . . . . ? C11 C6 C1 O1 -2(3) . . . . ? C5 C6 C1 O1 178.3(18) . . . . ? C11 C6 C1 C2 179.1(19) . . . . ? C5 C6 C1 C2 0(3) . . . . ? C6 C5 C4 C3 1(3) . . . . ? C14 C5 C4 C3 -178.9(18) . . . . ? C5 C4 C3 C10 -179.4(17) . . . . ? C5 C4 C3 C2 -2(3) . . . . ? C9 C10 C3 C4 176.3(18) . . . . ? C9 C10 C3 C2 -2(2) . . . . ? C4 C3 C2 C7 -176(3) . . . . ? C10 C3 C2 C7 2(3) . . . . ? C4 C3 C2 C1 1(3) . . . . ? C10 C3 C2 C1 179.4(15) . . . . ? O1 C1 C2 C7 -1(3) . . . . ? C6 C1 C2 C7 177(3) . . . . ? O1 C1 C2 C3 -178.7(18) . . . . ? C6 C1 C2 C3 0(3) . . . . ? C3 C2 C7 C8 -3(5) . . . . ? C1 C2 C7 C8 180(3) . . . . ? C2 C7 C8 C9 3(5) . . . . ? C3 C10 C9 C8 2(3) . . . . ? C7 C8 C9 C10 -3(4) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C50 C51 C52 C53 178.4(2) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C50 C51 C56 C55 -178.4(2) . . . . ? C56A C51A C52A C53A 0.0 . . . . ? C50A C51A C52A C53A -177.2(4) . . . . ? C51A C52A C53A C54A 0.0 . . . . ? C52A C53A C54A C55A 0.0 . . . . ? C53A C54A C55A C56A 0.0 . . . . ? C54A C55A C56A C51A 0.0 . . . . ? C52A C51A C56A C55A 0.0 . . . . ? C50A C51A C56A C55A 177.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.364 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.035 data_pgabf1 _database_code_depnum_ccdc_archive 'CCDC 892943' #TrackingRef 'Hara_1353510871.Submissioncif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 K2 N6 O2' _chemical_formula_weight 811.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4500(3) _cell_length_b 17.6550(4) _cell_length_c 13.5543(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.112(3) _cell_angle_gamma 90.00 _cell_volume 2332.84(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6390 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 30.68 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_T_min 0.98061 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14911 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.50 _reflns_number_total 5899 _reflns_number_gt 4025 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysalisPro _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics XSEED _computing_publication_material SHELXL _refine_special_details ; Part of the PMDETA chelate was modelled as disordered over two sites (refined occupancy 86.6 : 13.6). DFIX commands were used to give a sensible geometry (C-C 1.53 & N-C 1.47 A) and the atoms of each major and minor disordered "pair" were forced to have equivalent thermal parameters. 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^ > 2\s(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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5899 _refine_ls_number_parameters 277 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.07850(4) 0.41639(2) 0.10253(3) 0.02585(11) Uani 1 1 d . . . O1 O -0.00650(11) 0.43774(6) -0.09820(8) 0.0262(3) Uani 1 1 d . . . N1 N 0.34778(15) 0.34304(9) 0.20173(11) 0.0344(4) Uani 1 1 d . A . N2 N 0.10754(15) 0.31105(8) 0.27115(11) 0.0335(3) Uani 1 1 d D . . N3 N -0.14801(15) 0.32170(9) 0.08271(13) 0.0409(4) Uani 1 1 d D . . C1 C 0.3484(3) 0.27959(13) 0.13368(18) 0.0585(6) Uani 1 1 d . . . H1A H 0.3495 0.2986 0.0661 0.088 Uiso 1 1 calc R . . H1B H 0.2659 0.2488 0.1211 0.088 Uiso 1 1 calc R . . H1C H 0.4300 0.2485 0.1680 0.088 Uiso 1 1 calc R . . C2 C 0.4613(2) 0.39381(13) 0.21124(16) 0.0480(5) Uani 1 1 d . . . H2A H 0.5483 0.3669 0.2447 0.072 Uiso 1 1 calc R . . H2B H 0.4578 0.4376 0.2546 0.072 Uiso 1 1 calc R . . H2C H 0.4543 0.4111 0.1408 0.072 Uiso 1 1 calc R . . C3 C 0.35948(19) 0.31820(12) 0.30764(14) 0.0423(5) Uani 1 1 d . . . H3A H 0.3684 0.3635 0.3527 0.051 Uiso 1 1 calc R A . H3B H 0.4446 0.2881 0.3385 0.051 Uiso 1 1 calc R . . C4 C 0.24036(19) 0.27143(10) 0.31074(14) 0.0394(4) Uani 1 1 d D A . H4A H 0.2337 0.2251 0.2680 0.047 Uiso 1 1 calc R . . H4B H 0.2590 0.2554 0.3846 0.047 Uiso 1 1 calc R . . C5 C 0.0936(4) 0.3658(2) 0.3477(3) 0.0438(8) Uani 0.866(3) 1 d PD A 1 H5A H 0.0078 0.3941 0.3159 0.066 Uiso 0.866(3) 1 calc PR A 1 H5B H 0.1712 0.4011 0.3677 0.066 Uiso 0.866(3) 1 calc PR A 1 H5C H 0.0926 0.3390 0.4107 0.066 Uiso 0.866(3) 1 calc PR A 1 C6 C -0.0004(2) 0.25296(12) 0.24563(16) 0.0312(5) Uani 0.866(3) 1 d PD A 1 H6A H -0.0018 0.2306 0.3122 0.037 Uiso 0.866(3) 1 calc PR A 1 H6B H 0.0219 0.2120 0.2045 0.037 Uiso 0.866(3) 1 calc PR A 1 C7 C -0.1418(2) 0.28397(13) 0.18268(18) 0.0376(6) Uani 0.866(3) 1 d PD A 1 H7A H -0.2090 0.2419 0.1655 0.045 Uiso 0.866(3) 1 calc PR A 1 H7B H -0.1684 0.3209 0.2268 0.045 Uiso 0.866(3) 1 calc PR A 1 C6A C -0.0375(10) 0.2866(8) 0.2586(9) 0.0312(5) Uani 0.134(3) 1 d PD A 2 H6A1 H -0.0339 0.2485 0.3131 0.037 Uiso 0.134(3) 1 calc PR A 2 H6A2 H -0.0903 0.3308 0.2680 0.037 Uiso 0.134(3) 1 calc PR A 2 C7A C -0.1073(14) 0.2531(6) 0.1492(9) 0.0376(6) Uani 0.134(3) 1 d PD A 2 H7A1 H -0.0433 0.2213 0.1282 0.045 Uiso 0.134(3) 1 calc PR A 2 H7A2 H -0.1882 0.2224 0.1455 0.045 Uiso 0.134(3) 1 calc PR A 2 C8 C -0.1295(3) 0.27020(16) 0.0076(2) 0.0489(7) Uani 0.866(3) 1 d PD A 1 H8A H -0.0379 0.2475 0.0371 0.073 Uiso 0.866(3) 1 calc PR A 1 H8B H -0.1387 0.2975 -0.0575 0.073 Uiso 0.866(3) 1 calc PR A 1 H8C H -0.1990 0.2302 -0.0082 0.073 Uiso 0.866(3) 1 calc PR A 1 C9 C -0.2803(4) 0.3597(3) 0.0355(3) 0.0520(10) Uani 0.866(3) 1 d PD A 1 H9A H -0.2826 0.3873 -0.0279 0.078 Uiso 0.866(3) 1 calc PR A 1 H9B H -0.2930 0.3954 0.0866 0.078 Uiso 0.866(3) 1 calc PR A 1 H9C H -0.3540 0.3220 0.0160 0.078 Uiso 0.866(3) 1 calc PR A 1 C10 C 0.00796(15) 0.43564(8) -0.18859(11) 0.0203(3) Uani 1 1 d . . . C11 C 0.14120(15) 0.43427(8) -0.19709(11) 0.0204(3) Uani 1 1 d . . . C12 C 0.26139(16) 0.43423(9) -0.10449(12) 0.0260(4) Uani 1 1 d . . . H12 H 0.2526 0.4376 -0.0373 0.031 Uiso 1 1 calc R . . C13 C 0.38851(16) 0.42943(10) -0.10956(13) 0.0317(4) Uani 1 1 d . . . H13 H 0.4672 0.4292 -0.0464 0.038 Uiso 1 1 calc R . . C14 C 0.40371(17) 0.42475(10) -0.20864(14) 0.0319(4) Uani 1 1 d . . . H14 H 0.4928 0.4205 -0.2119 0.038 Uiso 1 1 calc R . . C15 C 0.29126(16) 0.42624(9) -0.30004(13) 0.0279(4) Uani 1 1 d . . . H15 H 0.3034 0.4239 -0.3661 0.034 Uiso 1 1 calc R . . C16 C 0.15564(15) 0.43126(8) -0.29804(12) 0.0217(3) Uani 1 1 d . . . C17 C 0.03916(16) 0.43174(9) -0.39124(11) 0.0230(3) Uani 1 1 d . . . H17 H 0.0495 0.4303 -0.4580 0.028 Uiso 1 1 calc R . . C18 C -0.09173(15) 0.43434(8) -0.38608(11) 0.0204(3) Uani 1 1 d . . . C19 C -0.21306(17) 0.43539(9) -0.47959(12) 0.0270(4) Uani 1 1 d . . . H19 H -0.2044 0.4354 -0.5470 0.032 Uiso 1 1 calc R . . C20 C -0.33994(17) 0.43633(10) -0.47380(13) 0.0321(4) Uani 1 1 d . . . H20 H -0.4186 0.4375 -0.5370 0.038 Uiso 1 1 calc R . . C21 C -0.35636(17) 0.43565(10) -0.37518(14) 0.0321(4) Uani 1 1 d . . . H21 H -0.4457 0.4357 -0.3720 0.039 Uiso 1 1 calc R . . C22 C -0.24381(16) 0.43488(9) -0.28409(12) 0.0257(4) Uani 1 1 d . . . H22 H -0.2560 0.4342 -0.2179 0.031 Uiso 1 1 calc R . . C23 C -0.10913(15) 0.43514(8) -0.28604(11) 0.0200(3) Uani 1 1 d . . . C5A C 0.134(3) 0.3735(16) 0.352(2) 0.0438(8) Uani 0.134(3) 1 d PD A 2 H5A1 H 0.0510 0.4048 0.3360 0.066 Uiso 0.134(3) 1 calc PR A 2 H5A2 H 0.2100 0.4051 0.3508 0.066 Uiso 0.134(3) 1 calc PR A 2 H5A3 H 0.1566 0.3513 0.4228 0.066 Uiso 0.134(3) 1 calc PR A 2 C8A C -0.168(2) 0.2835(12) -0.0229(10) 0.0489(7) Uani 0.134(3) 1 d PD A 2 H8A1 H -0.1623 0.3216 -0.0737 0.073 Uiso 0.134(3) 1 calc PR A 2 H8A2 H -0.2581 0.2590 -0.0499 0.073 Uiso 0.134(3) 1 calc PR A 2 H8A3 H -0.0961 0.2454 -0.0128 0.073 Uiso 0.134(3) 1 calc PR A 2 C9A C -0.270(3) 0.369(2) 0.066(3) 0.0520(10) Uani 0.134(3) 1 d PD A 2 H9A1 H -0.2884 0.3995 0.0015 0.078 Uiso 0.134(3) 1 calc PR A 2 H9A2 H -0.2533 0.4029 0.1265 0.078 Uiso 0.134(3) 1 calc PR A 2 H9A3 H -0.3491 0.3368 0.0577 0.078 Uiso 0.134(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.03440(19) 0.02396(18) 0.01916(15) 0.00500(14) 0.00959(12) 0.00330(17) O1 0.0323(6) 0.0309(6) 0.0167(5) 0.0006(4) 0.0105(4) 0.0054(5) N1 0.0431(8) 0.0326(8) 0.0245(7) 0.0028(6) 0.0085(6) 0.0018(7) N2 0.0470(9) 0.0282(8) 0.0250(7) 0.0039(6) 0.0126(6) -0.0048(7) N3 0.0342(8) 0.0339(9) 0.0514(10) 0.0123(7) 0.0115(7) 0.0027(7) C1 0.0902(17) 0.0410(13) 0.0491(13) -0.0067(10) 0.0306(12) -0.0022(13) C2 0.0425(11) 0.0593(14) 0.0393(11) -0.0008(9) 0.0110(8) -0.0093(10) C3 0.0440(11) 0.0477(12) 0.0285(9) 0.0092(8) 0.0049(8) 0.0040(9) C4 0.0600(12) 0.0271(9) 0.0279(9) 0.0069(7) 0.0120(8) 0.0053(9) C5 0.070(3) 0.0265(13) 0.0444(12) -0.0010(9) 0.0324(17) -0.0040(15) C6 0.0439(12) 0.0204(11) 0.0348(10) 0.0045(8) 0.0209(9) 0.0027(9) C7 0.0371(11) 0.0289(12) 0.0549(14) 0.0052(10) 0.0262(10) 0.0019(10) C6A 0.0439(12) 0.0204(11) 0.0348(10) 0.0045(8) 0.0209(9) 0.0027(9) C7A 0.0371(11) 0.0289(12) 0.0549(14) 0.0052(10) 0.0262(10) 0.0019(10) C8 0.0529(18) 0.0379(15) 0.0546(16) 0.0131(12) 0.0178(13) 0.0121(12) C9 0.0492(14) 0.0399(18) 0.064(3) 0.0038(18) 0.0168(15) 0.0106(14) C10 0.0270(8) 0.0152(7) 0.0184(7) 0.0006(5) 0.0079(6) 0.0029(6) C11 0.0242(7) 0.0149(7) 0.0209(7) 0.0007(5) 0.0067(6) 0.0007(6) C12 0.0286(8) 0.0251(9) 0.0211(7) -0.0013(6) 0.0049(6) 0.0004(7) C13 0.0241(8) 0.0324(10) 0.0311(9) 0.0006(7) 0.0010(7) -0.0004(7) C14 0.0225(8) 0.0322(10) 0.0416(10) 0.0043(7) 0.0123(7) -0.0017(7) C15 0.0299(8) 0.0272(9) 0.0309(8) 0.0048(7) 0.0160(7) 0.0000(7) C16 0.0253(8) 0.0171(8) 0.0238(7) 0.0026(6) 0.0104(6) 0.0006(6) C17 0.0312(8) 0.0224(8) 0.0174(7) 0.0007(6) 0.0111(6) 0.0017(7) C18 0.0266(8) 0.0157(7) 0.0180(7) 0.0015(5) 0.0070(6) 0.0026(6) C19 0.0332(9) 0.0277(9) 0.0174(7) 0.0012(6) 0.0058(6) 0.0019(7) C20 0.0266(8) 0.0370(10) 0.0247(8) 0.0003(7) -0.0003(6) 0.0024(8) C21 0.0206(8) 0.0397(11) 0.0347(9) 0.0006(7) 0.0082(7) 0.0042(7) C22 0.0265(8) 0.0286(9) 0.0236(8) 0.0004(6) 0.0108(6) 0.0030(7) C23 0.0244(7) 0.0163(7) 0.0192(7) 0.0007(5) 0.0078(6) 0.0026(6) C5A 0.070(3) 0.0265(13) 0.0444(12) -0.0010(9) 0.0324(17) -0.0040(15) C8A 0.0529(18) 0.0379(15) 0.0546(16) 0.0131(12) 0.0178(13) 0.0121(12) C9A 0.0492(14) 0.0399(18) 0.064(3) 0.0038(18) 0.0168(15) 0.0106(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 K1 O1 2.5676(10) . ? K1 O1 2.6777(12) 3_565 ? K1 N3 2.8306(16) . ? K1 N2 2.8767(14) . ? K1 N1 2.9457(15) . ? K1 C10 3.1243(15) 3_565 ? K1 K1 3.9809(7) 3_565 ? O1 C10 1.2879(17) . ? O1 K1 2.6777(12) 3_565 ? N1 C1 1.453(3) . ? N1 C2 1.455(3) . ? N1 C3 1.463(2) . ? N2 C5 1.463(3) . ? N2 C6 1.471(2) . ? N2 C4 1.472(2) . ? N2 C5A 1.512(10) . ? N2 C6A 1.525(8) . ? N3 C8 1.429(3) . ? N3 C9 1.461(3) . ? N3 C9A 1.472(10) . ? N3 C7A 1.478(8) . ? N3 C7 1.490(3) . ? N3 C8A 1.527(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.507(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.517(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C6A C7A 1.517(9) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.438(2) . ? C10 C23 1.4414(19) . ? C10 K1 3.1243(15) 3_565 ? C11 C12 1.420(2) . ? C11 C16 1.431(2) . ? C12 C13 1.357(2) . ? C12 H12 0.9500 . ? C13 C14 1.410(2) . ? C13 H13 0.9500 . ? C14 C15 1.367(2) . ? C14 H14 0.9500 . ? C15 C16 1.430(2) . ? C15 H15 0.9500 . ? C16 C17 1.404(2) . ? C17 C18 1.395(2) . ? C17 H17 0.9500 . ? C18 C23 1.432(2) . ? C18 C19 1.434(2) . ? C19 C20 1.356(2) . ? C19 H19 0.9500 . ? C20 C21 1.408(2) . ? C20 H20 0.9500 . ? C21 C22 1.364(2) . ? C21 H21 0.9500 . ? C22 C23 1.417(2) . ? C22 H22 0.9500 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? 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 O1 K1 O1 81.28(4) . 3_565 ? O1 K1 N3 91.60(4) . . ? O1 K1 N3 110.31(4) 3_565 . ? O1 K1 N2 146.52(4) . . ? O1 K1 N2 125.99(4) 3_565 . ? N3 K1 N2 62.54(4) . . ? O1 K1 N1 117.21(4) . . ? O1 K1 N1 130.35(4) 3_565 . ? N3 K1 N1 114.35(4) . . ? N2 K1 N1 62.81(4) . . ? O1 K1 C10 103.69(4) . 3_565 ? O1 K1 C10 24.11(3) 3_565 3_565 ? N3 K1 C10 100.65(5) . 3_565 ? N2 K1 C10 101.88(4) . 3_565 ? N1 K1 C10 123.66(4) . 3_565 ? O1 K1 K1 41.67(3) . 3_565 ? O1 K1 K1 39.61(2) 3_565 3_565 ? N3 K1 K1 104.56(3) . 3_565 ? N2 K1 K1 158.94(4) . 3_565 ? N1 K1 K1 136.92(3) . 3_565 ? C10 K1 K1 62.53(3) 3_565 3_565 ? C10 O1 K1 152.80(10) . . ? C10 O1 K1 97.77(9) . 3_565 ? K1 O1 K1 98.72(4) . 3_565 ? C1 N1 C2 109.98(17) . . ? C1 N1 C3 111.95(16) . . ? C2 N1 C3 108.68(14) . . ? C1 N1 K1 105.72(12) . . ? C2 N1 K1 112.58(12) . . ? C3 N1 K1 107.95(11) . . ? C5 N2 C6 111.35(17) . . ? C5 N2 C4 112.1(2) . . ? C6 N2 C4 107.29(15) . . ? C5 N2 C5A 16.2(10) . . ? C6 N2 C5A 127.0(10) . . ? C4 N2 C5A 100.5(13) . . ? C5 N2 C6A 85.3(5) . . ? C6 N2 C6A 29.4(5) . . ? C4 N2 C6A 132.4(6) . . ? C5A N2 C6A 101.5(9) . . ? C5 N2 K1 97.3(2) . . ? C6 N2 K1 114.30(10) . . ? C4 N2 K1 114.37(10) . . ? C5A N2 K1 92.6(15) . . ? C6A N2 K1 106.1(5) . . ? C8 N3 C9 109.26(18) . . ? C8 N3 C9A 125.6(12) . . ? C9 N3 C9A 16.4(13) . . ? C8 N3 C7A 80.2(5) . . ? C9 N3 C7A 131.5(6) . . ? C9A N3 C7A 127.2(19) . . ? C8 N3 C7 112.99(18) . . ? C9 N3 C7 109.2(2) . . ? C9A N3 C7 98.6(16) . . ? C7A N3 C7 34.0(5) . . ? C8 N3 C8A 19.8(7) . . ? C9 N3 C8A 90.2(8) . . ? C9A N3 C8A 106.7(14) . . ? C7A N3 C8A 97.0(9) . . ? C7 N3 C8A 127.0(9) . . ? C8 N3 K1 96.89(16) . . ? C9 N3 K1 113.4(2) . . ? C9A N3 K1 109.0(18) . . ? C7A N3 K1 112.3(5) . . ? C7 N3 K1 114.62(11) . . ? C8A N3 K1 100.2(10) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 114.43(15) . . ? N1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N2 C4 C3 114.17(15) . . ? N2 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? N2 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? N2 C6 C7 112.94(17) . . ? N2 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N3 C7 C6 112.79(17) . . ? N3 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N3 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7A C6A N2 109.2(9) . . ? C7A C6A H6A1 109.8 . . ? N2 C6A H6A1 109.8 . . ? C7A C6A H6A2 109.8 . . ? N2 C6A H6A2 109.8 . . ? H6A1 C6A H6A2 108.3 . . ? N3 C7A C6A 102.0(9) . . ? N3 C7A H7A1 111.4 . . ? C6A C7A H7A1 111.4 . . ? N3 C7A H7A2 111.4 . . ? C6A C7A H7A2 111.4 . . ? H7A1 C7A H7A2 109.2 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? O1 C10 C11 121.70(13) . . ? O1 C10 C23 121.34(14) . . ? C11 C10 C23 116.95(13) . . ? O1 C10 K1 58.12(8) . 3_565 ? C11 C10 K1 117.55(9) . 3_565 ? C23 C10 K1 94.76(9) . 3_565 ? C12 C11 C16 118.74(14) . . ? C12 C11 C10 120.18(14) . . ? C16 C11 C10 121.07(13) . . ? C13 C12 C11 121.69(15) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 119.99(14) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.47(16) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 121.22(15) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 121.83(14) . . ? C17 C16 C11 120.31(14) . . ? C15 C16 C11 117.85(13) . . ? C18 C17 C16 120.20(14) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C23 120.60(13) . . ? C17 C18 C19 121.78(14) . . ? C23 C18 C19 117.61(14) . . ? C20 C19 C18 121.37(15) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 120.72(14) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.94(15) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.42(15) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 118.91(13) . . ? C22 C23 C10 120.25(13) . . ? C18 C23 C10 120.83(13) . . ? N2 C5A H5A1 109.5 . . ? N2 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? N2 C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? N3 C8A H8A1 109.5 . . ? N3 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? N3 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N3 C9A H9A1 109.5 . . ? N3 C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? N3 C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 K1 O1 C10 126.7(2) 3_565 . . . ? N3 K1 O1 C10 -123.0(2) . . . . ? N2 K1 O1 C10 -85.5(2) . . . . ? N1 K1 O1 C10 -4.4(2) . . . . ? C10 K1 O1 C10 135.7(2) 3_565 . . . ? K1 K1 O1 C10 126.7(2) 3_565 . . . ? O1 K1 O1 K1 0.0 3_565 . . 3_565 ? N3 K1 O1 K1 110.31(4) . . . 3_565 ? N2 K1 O1 K1 147.74(7) . . . 3_565 ? N1 K1 O1 K1 -131.12(4) . . . 3_565 ? C10 K1 O1 K1 8.94(4) 3_565 . . 3_565 ? O1 K1 N1 C1 -45.07(13) . . . . ? O1 K1 N1 C1 -147.37(12) 3_565 . . . ? N3 K1 N1 C1 60.42(13) . . . . ? N2 K1 N1 C1 97.13(13) . . . . ? C10 K1 N1 C1 -176.54(12) 3_565 . . . ? K1 K1 N1 C1 -92.24(13) 3_565 . . . ? O1 K1 N1 C2 75.02(13) . . . . ? O1 K1 N1 C2 -27.28(14) 3_565 . . . ? N3 K1 N1 C2 -179.49(12) . . . . ? N2 K1 N1 C2 -142.77(13) . . . . ? C10 K1 N1 C2 -56.44(13) 3_565 . . . ? K1 K1 N1 C2 27.86(14) 3_565 . . . ? O1 K1 N1 C3 -165.03(11) . . . . ? O1 K1 N1 C3 92.67(12) 3_565 . . . ? N3 K1 N1 C3 -59.54(12) . . . . ? N2 K1 N1 C3 -22.82(11) . . . . ? C10 K1 N1 C3 63.51(13) 3_565 . . . ? K1 K1 N1 C3 147.81(10) 3_565 . . . ? O1 K1 N2 C5 -147.89(14) . . . . ? O1 K1 N2 C5 -8.59(16) 3_565 . . . ? N3 K1 N2 C5 -104.68(15) . . . . ? N1 K1 N2 C5 113.18(15) . . . . ? C10 K1 N2 C5 -8.74(15) 3_565 . . . ? K1 K1 N2 C5 -48.80(19) 3_565 . . . ? O1 K1 N2 C6 -30.48(16) . . . . ? O1 K1 N2 C6 108.83(13) 3_565 . . . ? N3 K1 N2 C6 12.73(13) . . . . ? N1 K1 N2 C6 -129.40(14) . . . . ? C10 K1 N2 C6 108.68(13) 3_565 . . . ? K1 K1 N2 C6 68.62(17) 3_565 . . . ? O1 K1 N2 C4 93.75(13) . . . . ? O1 K1 N2 C4 -126.95(11) 3_565 . . . ? N3 K1 N2 C4 136.96(12) . . . . ? N1 K1 N2 C4 -5.18(11) . . . . ? C10 K1 N2 C4 -127.10(11) 3_565 . . . ? K1 K1 N2 C4 -167.16(9) 3_565 . . . ? O1 K1 N2 C5A -163.5(10) . . . . ? O1 K1 N2 C5A -24.2(10) 3_565 . . . ? N3 K1 N2 C5A -120.2(10) . . . . ? N1 K1 N2 C5A 97.6(10) . . . . ? C10 K1 N2 C5A -24.3(10) 3_565 . . . ? K1 K1 N2 C5A -64.4(10) 3_565 . . . ? O1 K1 N2 C6A -60.7(5) . . . . ? O1 K1 N2 C6A 78.6(5) 3_565 . . . ? N3 K1 N2 C6A -17.5(5) . . . . ? N1 K1 N2 C6A -159.6(5) . . . . ? C10 K1 N2 C6A 78.4(5) 3_565 . . . ? K1 K1 N2 C6A 38.4(6) 3_565 . . . ? O1 K1 N3 C8 54.19(13) . . . . ? O1 K1 N3 C8 135.48(13) 3_565 . . . ? N2 K1 N3 C8 -103.61(13) . . . . ? N1 K1 N3 C8 -66.79(13) . . . . ? C10 K1 N3 C8 158.44(13) 3_565 . . . ? K1 K1 N3 C8 94.30(13) 3_565 . . . ? O1 K1 N3 C9 -60.29(17) . . . . ? O1 K1 N3 C9 20.99(18) 3_565 . . . ? N2 K1 N3 C9 141.91(18) . . . . ? N1 K1 N3 C9 178.73(17) . . . . ? C10 K1 N3 C9 43.96(18) 3_565 . . . ? K1 K1 N3 C9 -20.19(18) 3_565 . . . ? O1 K1 N3 C9A -77.3(14) . . . . ? O1 K1 N3 C9A 4.0(14) 3_565 . . . ? N2 K1 N3 C9A 124.9(14) . . . . ? N1 K1 N3 C9A 161.8(14) . . . . ? C10 K1 N3 C9A 27.0(14) 3_565 . . . ? K1 K1 N3 C9A -37.2(14) 3_565 . . . ? O1 K1 N3 C7A 136.4(6) . . . . ? O1 K1 N3 C7A -142.3(6) 3_565 . . . ? N2 K1 N3 C7A -21.4(6) . . . . ? N1 K1 N3 C7A 15.4(6) . . . . ? C10 K1 N3 C7A -119.4(6) 3_565 . . . ? K1 K1 N3 C7A 176.5(6) 3_565 . . . ? O1 K1 N3 C7 173.41(13) . . . . ? O1 K1 N3 C7 -105.31(13) 3_565 . . . ? N2 K1 N3 C7 15.61(13) . . . . ? N1 K1 N3 C7 52.43(14) . . . . ? C10 K1 N3 C7 -82.34(13) 3_565 . . . ? K1 K1 N3 C7 -146.49(13) 3_565 . . . ? O1 K1 N3 C8A 34.4(8) . . . . ? O1 K1 N3 C8A 115.7(8) 3_565 . . . ? N2 K1 N3 C8A -123.4(8) . . . . ? N1 K1 N3 C8A -86.5(8) . . . . ? C10 K1 N3 C8A 138.7(8) 3_565 . . . ? K1 K1 N3 C8A 74.5(8) 3_565 . . . ? C1 N1 C3 C4 -64.2(2) . . . . ? C2 N1 C3 C4 174.09(17) . . . . ? K1 N1 C3 C4 51.71(19) . . . . ? C5 N2 C4 C3 -76.1(2) . . . . ? C6 N2 C4 C3 161.32(16) . . . . ? C5A N2 C4 C3 -64.4(13) . . . . ? C6A N2 C4 C3 179.3(6) . . . . ? K1 N2 C4 C3 33.44(18) . . . . ? N1 C3 C4 N2 -60.9(2) . . . . ? C5 N2 C6 C7 69.0(3) . . . . ? C4 N2 C6 C7 -167.91(17) . . . . ? C5A N2 C6 C7 74(2) . . . . ? C6A N2 C6 C7 39.7(9) . . . . ? K1 N2 C6 C7 -40.0(2) . . . . ? C8 N3 C7 C6 66.8(3) . . . . ? C9 N3 C7 C6 -171.4(2) . . . . ? C9A N3 C7 C6 -158.5(15) . . . . ? C7A N3 C7 C6 50.8(9) . . . . ? C8A N3 C7 C6 83.1(11) . . . . ? K1 N3 C7 C6 -43.0(2) . . . . ? N2 C6 C7 N3 56.4(3) . . . . ? C5 N2 C6A C7A 153.4(10) . . . . ? C6 N2 C6A C7A -53.8(8) . . . . ? C4 N2 C6A C7A -90.6(10) . . . . ? C5A N2 C6A C7A 153.4(19) . . . . ? K1 N2 C6A C7A 57.2(10) . . . . ? C8 N3 C7A C6A 150.5(9) . . . . ? C9 N3 C7A C6A -102.4(9) . . . . ? C9A N3 C7A C6A -81.9(19) . . . . ? C7 N3 C7A C6A -44.4(6) . . . . ? C8A N3 C7A C6A 161.0(13) . . . . ? K1 N3 C7A C6A 57.0(10) . . . . ? N2 C6A C7A N3 -79.0(12) . . . . ? K1 O1 C10 C11 -22.1(3) . . . . ? K1 O1 C10 C11 104.83(13) 3_565 . . . ? K1 O1 C10 C23 158.42(15) . . . . ? K1 O1 C10 C23 -74.67(14) 3_565 . . . ? K1 O1 C10 K1 -126.9(2) . . . 3_565 ? O1 C10 C11 C12 0.8(2) . . . . ? C23 C10 C11 C12 -179.65(13) . . . . ? K1 C10 C11 C12 68.62(16) 3_565 . . . ? O1 C10 C11 C16 179.44(14) . . . . ? C23 C10 C11 C16 -1.0(2) . . . . ? K1 C10 C11 C16 -112.76(13) 3_565 . . . ? C16 C11 C12 C13 -1.7(2) . . . . ? C10 C11 C12 C13 176.91(15) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C12 C13 C14 C15 1.1(3) . . . . ? C13 C14 C15 C16 -1.1(3) . . . . ? C14 C15 C16 C17 -179.07(15) . . . . ? C14 C15 C16 C11 -0.3(2) . . . . ? C12 C11 C16 C17 -179.55(14) . . . . ? C10 C11 C16 C17 1.8(2) . . . . ? C12 C11 C16 C15 1.7(2) . . . . ? C10 C11 C16 C15 -176.95(14) . . . . ? C15 C16 C17 C18 178.01(14) . . . . ? C11 C16 C17 C18 -0.7(2) . . . . ? C16 C17 C18 C23 -1.1(2) . . . . ? C16 C17 C18 C19 179.60(14) . . . . ? C17 C18 C19 C20 178.61(16) . . . . ? C23 C18 C19 C20 -0.7(2) . . . . ? C18 C19 C20 C21 -0.5(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C20 C21 C22 C23 0.3(3) . . . . ? C21 C22 C23 C18 -1.5(2) . . . . ? C21 C22 C23 C10 178.93(15) . . . . ? C17 C18 C23 C22 -177.62(14) . . . . ? C19 C18 C23 C22 1.7(2) . . . . ? C17 C18 C23 C10 1.9(2) . . . . ? C19 C18 C23 C10 -178.80(13) . . . . ? O1 C10 C23 C22 -1.7(2) . . . . ? C11 C10 C23 C22 178.73(14) . . . . ? K1 C10 C23 C22 -57.01(14) 3_565 . . . ? O1 C10 C23 C18 178.73(14) . . . . ? C11 C10 C23 C18 -0.8(2) . . . . ? K1 C10 C23 C18 123.47(13) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.399 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.047 data_jkcben6a _database_code_depnum_ccdc_archive 'CCDC 892944' #TrackingRef 'Hara_1353510871.Submissioncif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Mg N2 O' _chemical_formula_weight 390.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6935(8) _cell_length_b 12.3086(6) _cell_length_c 12.5596(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.338(4) _cell_angle_gamma 90.00 _cell_volume 2234.61(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2577 _cell_measurement_theta_min 4.7147 _cell_measurement_theta_max 44.9989 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81096 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; Very weak diffraction at higher angles. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3571 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.72 _diffrn_reflns_theta_max 45.04 _reflns_number_total 1791 _reflns_number_gt 1460 _reflns_threshold_expression I>2sigma(I) _computing_data_collection CrysalisPro _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics XSEED _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+1.8068P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1791 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.28630(11) 0.03288(13) 0.10006(11) 0.0419(6) Uani 1 1 d . . . O1 O 0.1965(2) 0.0715(3) 0.1838(3) 0.0498(11) Uani 1 1 d . . . C11 C 0.0461(4) 0.2159(4) 0.1863(4) 0.0435(15) Uani 1 1 d . . . H11A H 0.0718 0.2132 0.1222 0.052 Uiso 1 1 calc R . . C12 C -0.0243(4) 0.2851(4) 0.1911(4) 0.0447(15) Uani 1 1 d . . . H12A H -0.0474 0.3296 0.1304 0.054 Uiso 1 1 calc R . . C13 C -0.0642(4) 0.2921(4) 0.2856(4) 0.0452(15) Uani 1 1 d . . . H13A H -0.1130 0.3418 0.2892 0.054 Uiso 1 1 calc R . . C14 C -0.0316(4) 0.2269(4) 0.3709(4) 0.0434(14) Uani 1 1 d . . . H14A H -0.0592 0.2309 0.4336 0.052 Uiso 1 1 calc R . . C15 C 0.0418(3) 0.1533(4) 0.3696(4) 0.0392(14) Uani 1 1 d . . . C16 C 0.0777(4) 0.0893(4) 0.4593(4) 0.0431(14) Uani 1 1 d . . . H16A H 0.0510 0.0943 0.5226 0.052 Uiso 1 1 calc R . . C17 C 0.1515(4) 0.0182(4) 0.4586(4) 0.0417(14) Uani 1 1 d . . . C18 C 0.1893(4) -0.0464(4) 0.5493(4) 0.0478(15) Uani 1 1 d . . . H18A H 0.1625 -0.0428 0.6126 0.057 Uiso 1 1 calc R . . C19 C 0.2624(4) -0.1129(4) 0.5486(4) 0.0503(15) Uani 1 1 d . . . H19A H 0.2859 -0.1551 0.6107 0.060 Uiso 1 1 calc R . . C110 C 0.3038(4) -0.1198(4) 0.4558(4) 0.0513(15) Uani 1 1 d . . . H11B H 0.3551 -0.1667 0.4554 0.062 Uiso 1 1 calc R . . C111 C 0.2700(4) -0.0590(4) 0.3668(4) 0.0489(15) Uani 1 1 d . . . H11C H 0.2986 -0.0646 0.3049 0.059 Uiso 1 1 calc R . . C112 C 0.1938(4) 0.0124(4) 0.3633(4) 0.0421(14) Uani 1 1 d . . . C113 C 0.1585(4) 0.0754(4) 0.2711(4) 0.0412(14) Uani 1 1 d . . . C114 C 0.0828(3) 0.1472(4) 0.2741(4) 0.0370(14) Uani 1 1 d . . . N31 N 0.3196(3) 0.1892(3) 0.0345(3) 0.0449(12) Uani 1 1 d . . . C311 C 0.3041(4) 0.2828(5) 0.1036(4) 0.0626(17) Uani 1 1 d . . . H31A H 0.3091 0.3507 0.0643 0.094 Uiso 1 1 calc R . . H31B H 0.3508 0.2821 0.1700 0.094 Uiso 1 1 calc R . . H31C H 0.2423 0.2775 0.1222 0.094 Uiso 1 1 calc R . . C312 C 0.4157(4) 0.1942(5) 0.0169(5) 0.0682(18) Uani 1 1 d . . . H31D H 0.4265 0.2640 -0.0162 0.102 Uiso 1 1 calc R . . H31E H 0.4269 0.1349 -0.0312 0.102 Uiso 1 1 calc R . . H31F H 0.4579 0.1871 0.0865 0.102 Uiso 1 1 calc R . . C32 C 0.2523(4) 0.1978(5) -0.0691(4) 0.0626(17) Uani 1 1 d . . . H32A H 0.1920 0.2228 -0.0536 0.075 Uiso 1 1 calc R . . H32B H 0.2747 0.2529 -0.1158 0.075 Uiso 1 1 calc R . . C33 C 0.2391(5) 0.0941(5) -0.1277(4) 0.0698(19) Uani 1 1 d . . . H33A H 0.2984 0.0719 -0.1483 0.084 Uiso 1 1 calc R . . H33B H 0.1934 0.1043 -0.1951 0.084 Uiso 1 1 calc R . . N34 N 0.2069(3) 0.0067(3) -0.0631(3) 0.0464(12) Uani 1 1 d . . . C341 C 0.1065(4) 0.0121(5) -0.0640(5) 0.0706(19) Uani 1 1 d . . . H34A H 0.0729 0.0024 -0.1382 0.106 Uiso 1 1 calc R . . H34B H 0.0910 0.0831 -0.0366 0.106 Uiso 1 1 calc R . . H34C H 0.0888 -0.0454 -0.0178 0.106 Uiso 1 1 calc R . . C342 C 0.2273(4) -0.1001(5) -0.1092(4) 0.0622(17) Uani 1 1 d . . . H34D H 0.1936 -0.1059 -0.1838 0.093 Uiso 1 1 calc R . . H34E H 0.2078 -0.1588 -0.0655 0.093 Uiso 1 1 calc R . . H34F H 0.2939 -0.1060 -0.1087 0.093 Uiso 1 1 calc R . . C22 C 0.4753(4) -0.0945(5) 0.2187(4) 0.0591(17) Uani 1 1 d . . . H22A H 0.4508 -0.1210 0.2824 0.071 Uiso 1 1 calc R . . H22B H 0.5182 -0.1506 0.2002 0.071 Uiso 1 1 calc R . . C23 C 0.5292(4) 0.0063(5) 0.2501(5) 0.0679(18) Uani 1 1 d . . . H23A H 0.5419 0.0419 0.1837 0.082 Uiso 1 1 calc R . . H23B H 0.5895 -0.0142 0.2943 0.082 Uiso 1 1 calc R . . C21 C 0.3949(3) -0.0841(4) 0.1243(4) 0.0504(15) Uani 1 1 d . . . H21A H 0.3633 -0.1555 0.1197 0.060 Uiso 1 1 calc R . . H21B H 0.4238 -0.0791 0.0591 0.060 Uiso 1 1 calc R . . C24 C 0.4831(4) 0.0877(5) 0.3129(5) 0.0781(19) Uani 1 1 d . . . H24A H 0.5218 0.1528 0.3266 0.117 Uiso 1 1 calc R . . H24B H 0.4749 0.0556 0.3820 0.117 Uiso 1 1 calc R . . H24C H 0.4226 0.1074 0.2709 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0543(12) 0.0494(12) 0.0226(11) 0.0002(8) 0.0084(8) 0.0038(8) O1 0.060(2) 0.069(3) 0.022(2) 0.0032(17) 0.0135(18) 0.0111(18) C11 0.056(4) 0.054(4) 0.021(3) 0.000(3) 0.009(3) -0.003(3) C12 0.055(4) 0.058(4) 0.021(3) 0.005(3) 0.007(3) 0.002(3) C13 0.056(4) 0.052(4) 0.029(4) -0.001(3) 0.009(3) 0.001(3) C14 0.057(4) 0.053(4) 0.024(3) -0.005(3) 0.015(3) -0.004(3) C15 0.047(3) 0.051(4) 0.020(3) -0.003(3) 0.007(3) -0.008(3) C16 0.064(4) 0.043(3) 0.025(3) 0.000(3) 0.016(3) -0.008(3) C17 0.056(4) 0.046(3) 0.022(4) -0.005(3) 0.004(3) -0.008(3) C18 0.068(4) 0.057(4) 0.020(3) 0.002(3) 0.009(3) -0.009(3) C19 0.071(4) 0.049(4) 0.030(4) 0.011(3) 0.008(3) 0.003(3) C110 0.064(4) 0.049(4) 0.041(4) 0.007(3) 0.010(3) 0.000(3) C111 0.061(4) 0.054(4) 0.031(4) 0.003(3) 0.009(3) -0.003(3) C112 0.055(4) 0.048(4) 0.022(4) -0.004(3) 0.004(3) -0.004(3) C113 0.055(4) 0.052(4) 0.016(4) -0.006(3) 0.006(3) -0.005(3) C114 0.050(3) 0.042(3) 0.019(3) 0.000(3) 0.008(3) -0.004(3) N31 0.056(3) 0.047(3) 0.030(3) 0.000(2) 0.004(2) 0.006(2) C311 0.074(4) 0.056(4) 0.054(4) -0.007(3) 0.002(3) 0.002(3) C312 0.066(4) 0.070(4) 0.075(4) 0.016(3) 0.028(3) 0.004(3) C32 0.095(5) 0.057(4) 0.032(4) 0.008(3) 0.000(3) 0.005(3) C33 0.107(5) 0.062(4) 0.035(4) 0.004(4) -0.003(3) 0.000(4) N34 0.061(3) 0.048(3) 0.029(3) 0.003(2) 0.006(2) 0.000(2) C341 0.059(4) 0.090(5) 0.057(4) -0.019(3) -0.006(3) 0.011(3) C342 0.075(4) 0.076(5) 0.033(3) -0.010(3) 0.004(3) 0.002(3) C22 0.066(4) 0.068(5) 0.041(4) -0.008(3) 0.004(3) 0.012(3) C23 0.078(4) 0.068(4) 0.054(4) 0.000(3) 0.003(3) 0.010(4) C21 0.061(4) 0.054(4) 0.034(3) 0.000(3) 0.004(3) 0.000(3) C24 0.087(5) 0.082(5) 0.063(4) -0.011(4) 0.005(4) 0.004(4) _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 Mg1 O1 1.890(4) . ? Mg1 C21 2.130(5) . ? Mg1 N31 2.183(4) . ? Mg1 N34 2.193(4) . ? O1 C113 1.318(6) . ? C11 C12 1.349(7) . ? C11 C114 1.418(7) . ? C11 H11A 0.9500 . ? C12 C13 1.418(7) . ? C12 H12A 0.9500 . ? C13 C14 1.354(7) . ? C13 H13A 0.9500 . ? C14 C15 1.411(7) . ? C14 H14A 0.9500 . ? C15 C16 1.398(7) . ? C15 C114 1.437(7) . ? C16 C17 1.394(7) . ? C16 H16A 0.9500 . ? C17 C18 1.418(7) . ? C17 C112 1.447(7) . ? C18 C19 1.350(7) . ? C18 H18A 0.9500 . ? C19 C110 1.411(7) . ? C19 H19A 0.9500 . ? C110 C111 1.363(7) . ? C110 H11B 0.9500 . ? C111 C112 1.418(7) . ? C111 H11C 0.9500 . ? C112 C113 1.413(7) . ? C113 C114 1.426(7) . ? N31 C312 1.469(6) . ? N31 C311 1.485(6) . ? N31 C32 1.490(6) . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C32 C33 1.469(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N34 1.475(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? N34 C341 1.476(7) . ? N34 C342 1.488(7) . ? C341 H34A 0.9800 . ? C341 H34B 0.9800 . ? C341 H34C 0.9800 . ? C342 H34D 0.9800 . ? C342 H34E 0.9800 . ? C342 H34F 0.9800 . ? C22 C23 1.487(8) . ? C22 C21 1.522(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.509(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 O1 Mg1 C21 132.08(18) . . ? O1 Mg1 N31 102.39(16) . . ? C21 Mg1 N31 115.93(19) . . ? O1 Mg1 N34 104.46(17) . . ? C21 Mg1 N34 107.06(18) . . ? N31 Mg1 N34 83.95(15) . . ? C113 O1 Mg1 156.2(3) . . ? C12 C11 C114 122.0(5) . . ? C12 C11 H11A 119.0 . . ? C114 C11 H11A 119.0 . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 119.1(5) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 122.3(5) . . ? C13 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C16 C15 C14 122.1(5) . . ? C16 C15 C114 119.2(5) . . ? C14 C15 C114 118.6(5) . . ? C17 C16 C15 122.0(5) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C16 C17 C18 122.7(5) . . ? C16 C17 C112 119.1(5) . . ? C18 C17 C112 118.2(5) . . ? C19 C18 C17 122.1(5) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C18 C19 C110 120.2(5) . . ? C18 C19 H19A 119.9 . . ? C110 C19 H19A 119.9 . . ? C111 C110 C19 119.8(5) . . ? C111 C110 H11B 120.1 . . ? C19 C110 H11B 120.1 . . ? C110 C111 C112 122.3(5) . . ? C110 C111 H11C 118.8 . . ? C112 C111 H11C 118.8 . . ? C113 C112 C111 122.5(5) . . ? C113 C112 C17 120.1(5) . . ? C111 C112 C17 117.4(5) . . ? O1 C113 C112 120.9(5) . . ? O1 C113 C114 119.6(4) . . ? C112 C113 C114 119.5(5) . . ? C11 C114 C113 122.6(5) . . ? C11 C114 C15 117.4(5) . . ? C113 C114 C15 120.0(5) . . ? C312 N31 C311 107.9(4) . . ? C312 N31 C32 111.8(4) . . ? C311 N31 C32 108.0(4) . . ? C312 N31 Mg1 112.3(3) . . ? C311 N31 Mg1 113.3(3) . . ? C32 N31 Mg1 103.5(3) . . ? N31 C311 H31A 109.5 . . ? N31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? N31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? N31 C312 H31D 109.5 . . ? N31 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? N31 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? C33 C32 N31 112.6(4) . . ? C33 C32 H32A 109.1 . . ? N31 C32 H32A 109.1 . . ? C33 C32 H32B 109.1 . . ? N31 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C32 C33 N34 112.6(5) . . ? C32 C33 H33A 109.1 . . ? N34 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? N34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C33 N34 C341 112.5(4) . . ? C33 N34 C342 108.9(4) . . ? C341 N34 C342 108.0(4) . . ? C33 N34 Mg1 103.7(3) . . ? C341 N34 Mg1 111.3(3) . . ? C342 N34 Mg1 112.5(3) . . ? N34 C341 H34A 109.5 . . ? N34 C341 H34B 109.5 . . ? H34A C341 H34B 109.5 . . ? N34 C341 H34C 109.5 . . ? H34A C341 H34C 109.5 . . ? H34B C341 H34C 109.5 . . ? N34 C342 H34D 109.5 . . ? N34 C342 H34E 109.5 . . ? H34D C342 H34E 109.5 . . ? N34 C342 H34F 109.5 . . ? H34D C342 H34F 109.5 . . ? H34E C342 H34F 109.5 . . ? C23 C22 C21 116.1(5) . . ? C23 C22 H22A 108.3 . . ? C21 C22 H22A 108.3 . . ? C23 C22 H22B 108.3 . . ? C21 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 C24 115.1(5) . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C22 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C22 C21 Mg1 128.7(4) . . ? C22 C21 H21A 105.1 . . ? Mg1 C21 H21A 105.1 . . ? C22 C21 H21B 105.1 . . ? Mg1 C21 H21B 105.1 . . ? H21A C21 H21B 105.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Mg1 O1 C113 15.3(9) . . . . ? N31 Mg1 O1 C113 -127.9(8) . . . . ? N34 Mg1 O1 C113 145.2(8) . . . . ? C114 C11 C12 C13 0.4(7) . . . . ? C11 C12 C13 C14 -1.1(7) . . . . ? C12 C13 C14 C15 1.1(7) . . . . ? C13 C14 C15 C16 177.4(4) . . . . ? C13 C14 C15 C114 -0.4(7) . . . . ? C14 C15 C16 C17 -178.7(4) . . . . ? C114 C15 C16 C17 -0.9(7) . . . . ? C15 C16 C17 C18 179.3(4) . . . . ? C15 C16 C17 C112 1.6(7) . . . . ? C16 C17 C18 C19 -178.3(5) . . . . ? C112 C17 C18 C19 -0.5(7) . . . . ? C17 C18 C19 C110 0.1(8) . . . . ? C18 C19 C110 C111 0.2(8) . . . . ? C19 C110 C111 C112 0.1(8) . . . . ? C110 C111 C112 C113 -179.9(5) . . . . ? C110 C111 C112 C17 -0.5(7) . . . . ? C16 C17 C112 C113 -2.1(7) . . . . ? C18 C17 C112 C113 -179.9(4) . . . . ? C16 C17 C112 C111 178.5(4) . . . . ? C18 C17 C112 C111 0.7(7) . . . . ? Mg1 O1 C113 C112 -8.8(11) . . . . ? Mg1 O1 C113 C114 168.9(6) . . . . ? C111 C112 C113 O1 -1.0(7) . . . . ? C17 C112 C113 O1 179.7(4) . . . . ? C111 C112 C113 C114 -178.7(4) . . . . ? C17 C112 C113 C114 2.0(7) . . . . ? C12 C11 C114 C113 -178.6(5) . . . . ? C12 C11 C114 C15 0.3(7) . . . . ? O1 C113 C114 C11 -0.2(7) . . . . ? C112 C113 C114 C11 177.5(4) . . . . ? O1 C113 C114 C15 -179.0(4) . . . . ? C112 C113 C114 C15 -1.3(7) . . . . ? C16 C15 C114 C11 -178.1(4) . . . . ? C14 C15 C114 C11 -0.3(7) . . . . ? C16 C15 C114 C113 0.8(7) . . . . ? C14 C15 C114 C113 178.6(4) . . . . ? O1 Mg1 N31 C312 149.4(3) . . . . ? C21 Mg1 N31 C312 -1.1(4) . . . . ? N34 Mg1 N31 C312 -107.1(4) . . . . ? O1 Mg1 N31 C311 26.8(3) . . . . ? C21 Mg1 N31 C311 -123.6(3) . . . . ? N34 Mg1 N31 C311 130.3(3) . . . . ? O1 Mg1 N31 C32 -89.9(3) . . . . ? C21 Mg1 N31 C32 119.7(3) . . . . ? N34 Mg1 N31 C32 13.6(3) . . . . ? C312 N31 C32 C33 80.8(6) . . . . ? C311 N31 C32 C33 -160.6(5) . . . . ? Mg1 N31 C32 C33 -40.3(5) . . . . ? N31 C32 C33 N34 58.0(7) . . . . ? C32 C33 N34 C341 80.5(6) . . . . ? C32 C33 N34 C342 -159.9(5) . . . . ? C32 C33 N34 Mg1 -39.9(5) . . . . ? O1 Mg1 N34 C33 114.4(3) . . . . ? C21 Mg1 N34 C33 -102.2(4) . . . . ? N31 Mg1 N34 C33 13.1(3) . . . . ? O1 Mg1 N34 C341 -6.8(4) . . . . ? C21 Mg1 N34 C341 136.7(4) . . . . ? N31 Mg1 N34 C341 -108.0(4) . . . . ? O1 Mg1 N34 C342 -128.1(3) . . . . ? C21 Mg1 N34 C342 15.3(4) . . . . ? N31 Mg1 N34 C342 130.6(4) . . . . ? C21 C22 C23 C24 76.2(7) . . . . ? C23 C22 C21 Mg1 -49.9(7) . . . . ? O1 Mg1 C21 C22 -57.8(6) . . . . ? N31 Mg1 C21 C22 81.7(5) . . . . ? N34 Mg1 C21 C22 173.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 45.04 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.371 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.060 data_jkcben7 _database_code_depnum_ccdc_archive 'CCDC 892945' #TrackingRef 'Hara_1353510871.Submissioncif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 N2 O Zn' _chemical_formula_weight 403.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2484(9) _cell_length_b 13.6732(7) _cell_length_c 12.7425(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.087(8) _cell_angle_gamma 90.00 _cell_volume 2028.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8043 _cell_measurement_theta_min 2.7720 _cell_measurement_theta_max 30.8647 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81696 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21632 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 28.99 _reflns_number_total 5387 _reflns_number_gt 3820 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysalisPro _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics XSEED _computing_publication_material SHELXL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5387 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.695553(17) 0.053924(13) 0.400276(15) 0.02080(6) Uani 1 1 d . . . O1 O 0.80923(11) 0.10036(9) 0.33657(10) 0.0367(3) Uani 1 1 d . . . C11 C 1.00387(15) 0.21193(12) 0.35485(13) 0.0239(4) Uani 1 1 d . . . H11A H 0.9708 0.2147 0.4131 0.029 Uiso 1 1 calc R . . C12 C 1.10017(15) 0.26532(12) 0.36261(14) 0.0257(4) Uani 1 1 d . . . H12A H 1.1331 0.3051 0.4256 0.031 Uiso 1 1 calc R . . C13 C 1.15094(15) 0.26162(12) 0.27768(14) 0.0265(4) Uani 1 1 d . . . H13A H 1.2186 0.2983 0.2841 0.032 Uiso 1 1 calc R . . C14 C 1.10384(15) 0.20594(12) 0.18661(14) 0.0241(4) Uani 1 1 d . . . H14A H 1.1395 0.2040 0.1302 0.029 Uiso 1 1 calc R . . C15 C 1.00212(14) 0.15031(11) 0.17376(12) 0.0183(3) Uani 1 1 d . . . C16 C 0.94880(14) 0.09730(11) 0.07755(13) 0.0209(3) Uani 1 1 d . . . H16A H 0.9825 0.0956 0.0197 0.025 Uiso 1 1 calc R . . C17 C 0.84690(14) 0.04703(11) 0.06581(12) 0.0191(3) Uani 1 1 d . . . C18 C 0.78854(16) -0.00417(12) -0.03355(13) 0.0250(4) Uani 1 1 d . . . H18A H 0.8211 -0.0052 -0.0922 0.030 Uiso 1 1 calc R . . C19 C 0.68776(16) -0.05144(12) -0.04641(14) 0.0292(4) Uani 1 1 d . . . H19A H 0.6511 -0.0849 -0.1135 0.035 Uiso 1 1 calc R . . C110 C 0.63730(15) -0.05129(12) 0.03875(14) 0.0282(4) Uani 1 1 d . . . H11B H 0.5664 -0.0841 0.0289 0.034 Uiso 1 1 calc R . . C111 C 0.68993(15) -0.00414(12) 0.13549(14) 0.0244(4) Uani 1 1 d . . . H11C H 0.6551 -0.0051 0.1925 0.029 Uiso 1 1 calc R . . C112 C 0.79575(13) 0.04656(11) 0.15331(13) 0.0185(3) Uani 1 1 d . . . C113 C 0.84974(14) 0.09824(11) 0.25270(13) 0.0207(3) Uani 1 1 d . . . C114 C 0.95200(14) 0.15210(11) 0.26123(12) 0.0183(3) Uani 1 1 d . . . C21 C 0.58645(15) -0.05753(12) 0.37748(15) 0.0238(4) Uani 1 1 d . . . C22 C 0.64114(17) -0.15986(13) 0.39588(16) 0.0337(4) Uani 1 1 d . . . H22A H 0.5809 -0.2093 0.3865 0.051 Uiso 1 1 calc R . . H22B H 0.6952 -0.1641 0.4708 0.051 Uiso 1 1 calc R . . H22C H 0.6822 -0.1714 0.3421 0.051 Uiso 1 1 calc R . . N31 N 0.79450(12) 0.08067(10) 0.56878(11) 0.0219(3) Uani 1 1 d . . . C311 C 0.75423(18) 0.01924(14) 0.64432(15) 0.0362(5) Uani 1 1 d . . . H31A H 0.7934 0.0389 0.7207 0.054 Uiso 1 1 calc R . . H31B H 0.7714 -0.0495 0.6343 0.054 Uiso 1 1 calc R . . H31C H 0.6712 0.0275 0.6282 0.054 Uiso 1 1 calc R . . C312 C 0.91895(16) 0.06380(14) 0.59239(16) 0.0372(5) Uani 1 1 d . . . H31D H 0.9595 0.0828 0.6687 0.056 Uiso 1 1 calc R . . H31E H 0.9472 0.1030 0.5419 0.056 Uiso 1 1 calc R . . H31F H 0.9327 -0.0057 0.5822 0.056 Uiso 1 1 calc R . . C32 C 0.77474(16) 0.18572(12) 0.58510(14) 0.0284(4) Uani 1 1 d . . . H32A H 0.8247 0.2257 0.5540 0.034 Uiso 1 1 calc R . . H32B H 0.7959 0.1998 0.6651 0.034 Uiso 1 1 calc R . . C33 C 0.65073(16) 0.21400(13) 0.53023(14) 0.0300(4) Uani 1 1 d . . . H33A H 0.6009 0.1765 0.5638 0.036 Uiso 1 1 calc R . . H33B H 0.6406 0.2844 0.5426 0.036 Uiso 1 1 calc R . . N34 N 0.61584(12) 0.19418(9) 0.41018(11) 0.0231(3) Uani 1 1 d . . . C341 C 0.65566(18) 0.27277(13) 0.35142(17) 0.0419(5) Uani 1 1 d . . . H34A H 0.6201 0.3348 0.3615 0.063 Uiso 1 1 calc R . . H34B H 0.6339 0.2571 0.2726 0.063 Uiso 1 1 calc R . . H34C H 0.7394 0.2786 0.3812 0.063 Uiso 1 1 calc R . . C342 C 0.48941(16) 0.18815(13) 0.36626(15) 0.0327(4) Uani 1 1 d . . . H34D H 0.4559 0.2510 0.3772 0.049 Uiso 1 1 calc R . . H34E H 0.4619 0.1366 0.4052 0.049 Uiso 1 1 calc R . . H34F H 0.4665 0.1729 0.2872 0.049 Uiso 1 1 calc R . . H21A H 0.5459(15) -0.0481(11) 0.4292(14) 0.021(4) Uiso 1 1 d . . . H21B H 0.5334(19) -0.0526(14) 0.3067(18) 0.051(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02083(10) 0.02342(10) 0.02013(10) -0.00388(9) 0.00923(7) -0.00593(9) O1 0.0374(8) 0.0519(8) 0.0296(7) -0.0192(6) 0.0231(6) -0.0223(7) C11 0.0258(10) 0.0268(9) 0.0214(9) -0.0028(7) 0.0106(7) -0.0041(7) C12 0.0278(10) 0.0251(9) 0.0233(9) -0.0047(7) 0.0067(8) -0.0053(7) C13 0.0219(9) 0.0257(9) 0.0330(10) 0.0012(8) 0.0101(8) -0.0056(7) C14 0.0252(9) 0.0264(9) 0.0249(9) 0.0016(7) 0.0142(7) -0.0006(7) C15 0.0191(8) 0.0169(8) 0.0196(8) 0.0031(6) 0.0069(7) 0.0034(6) C16 0.0253(9) 0.0219(8) 0.0184(8) 0.0024(7) 0.0110(7) 0.0032(7) C17 0.0227(8) 0.0157(7) 0.0169(7) 0.0028(7) 0.0033(6) 0.0043(7) C18 0.0327(10) 0.0229(9) 0.0183(8) 0.0009(7) 0.0063(7) 0.0027(8) C19 0.0347(10) 0.0244(9) 0.0212(9) -0.0041(8) -0.0022(7) -0.0006(8) C110 0.0232(9) 0.0240(8) 0.0329(9) 0.0008(8) 0.0019(7) -0.0026(8) C111 0.0232(9) 0.0236(9) 0.0266(9) 0.0002(7) 0.0080(7) -0.0016(7) C112 0.0168(8) 0.0167(7) 0.0205(8) 0.0019(7) 0.0038(6) 0.0020(7) C113 0.0216(9) 0.0221(8) 0.0204(8) 0.0003(7) 0.0092(7) 0.0003(7) C114 0.0194(8) 0.0175(7) 0.0181(8) 0.0012(6) 0.0061(7) 0.0009(6) C21 0.0224(9) 0.0248(8) 0.0259(9) -0.0065(8) 0.0100(7) -0.0051(8) C22 0.0355(11) 0.0270(9) 0.0425(11) -0.0093(8) 0.0181(9) -0.0041(8) N31 0.0215(7) 0.0241(7) 0.0193(7) 0.0019(5) 0.0054(6) -0.0017(6) C311 0.0395(12) 0.0425(11) 0.0238(10) 0.0066(8) 0.0059(9) -0.0127(9) C312 0.0219(9) 0.0464(12) 0.0384(11) 0.0077(9) 0.0021(8) 0.0027(9) C32 0.0308(10) 0.0271(9) 0.0244(9) -0.0050(7) 0.0041(8) -0.0053(7) C33 0.0327(11) 0.0250(9) 0.0306(10) -0.0088(8) 0.0075(8) 0.0007(8) N34 0.0238(8) 0.0199(7) 0.0230(7) 0.0032(6) 0.0036(6) -0.0037(6) C341 0.0399(12) 0.0321(10) 0.0489(12) 0.0184(9) 0.0067(10) -0.0073(9) C342 0.0262(10) 0.0299(10) 0.0378(11) 0.0020(8) 0.0040(8) 0.0000(8) _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 O1 1.9242(12) . ? Zn1 C21 1.9878(17) . ? Zn1 N31 2.1440(13) . ? Zn1 N34 2.1734(13) . ? O1 C113 1.3110(18) . ? C11 C12 1.364(2) . ? C11 C114 1.423(2) . ? C11 H11A 0.9500 . ? C12 C13 1.407(2) . ? C12 H12A 0.9500 . ? C13 C14 1.358(2) . ? C13 H13A 0.9500 . ? C14 C15 1.425(2) . ? C14 H14A 0.9500 . ? C15 C16 1.399(2) . ? C15 C114 1.430(2) . ? C16 C17 1.392(2) . ? C16 H16A 0.9500 . ? C17 C18 1.429(2) . ? C17 C112 1.439(2) . ? C18 C19 1.357(2) . ? C18 H18A 0.9500 . ? C19 C110 1.406(2) . ? C19 H19A 0.9500 . ? C110 C111 1.363(2) . ? C110 H11B 0.9500 . ? C111 C112 1.424(2) . ? C111 H11C 0.9500 . ? C112 C113 1.421(2) . ? C113 C114 1.428(2) . ? C21 C22 1.538(2) . ? C21 H21A 0.949(17) . ? C21 H21B 0.94(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N31 C311 1.473(2) . ? N31 C312 1.477(2) . ? N31 C32 1.482(2) . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C32 C33 1.512(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N34 1.480(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? N34 C341 1.476(2) . ? N34 C342 1.476(2) . ? C341 H34A 0.9800 . ? C341 H34B 0.9800 . ? C341 H34C 0.9800 . ? C342 H34D 0.9800 . ? C342 H34E 0.9800 . ? C342 H34F 0.9800 . ? 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 O1 Zn1 C21 137.14(6) . . ? O1 Zn1 N31 96.21(5) . . ? C21 Zn1 N31 114.99(6) . . ? O1 Zn1 N34 97.48(5) . . ? C21 Zn1 N34 113.03(6) . . ? N31 Zn1 N34 85.17(5) . . ? C113 O1 Zn1 147.48(11) . . ? C12 C11 C114 121.28(15) . . ? C12 C11 H11A 119.4 . . ? C114 C11 H11A 119.4 . . ? C11 C12 C13 120.25(16) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 120.38(16) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 121.45(15) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 122.06(14) . . ? C16 C15 C114 119.69(14) . . ? C14 C15 C114 118.22(14) . . ? C17 C16 C15 120.61(14) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 121.50(15) . . ? C16 C17 C112 120.71(14) . . ? C18 C17 C112 117.78(15) . . ? C19 C18 C17 121.75(16) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C110 120.49(16) . . ? C18 C19 H19A 119.8 . . ? C110 C19 H19A 119.8 . . ? C111 C110 C19 120.07(16) . . ? C111 C110 H11B 120.0 . . ? C19 C110 H11B 120.0 . . ? C110 C111 C112 121.72(16) . . ? C110 C111 H11C 119.1 . . ? C112 C111 H11C 119.1 . . ? C113 C112 C111 122.18(14) . . ? C113 C112 C17 119.62(14) . . ? C111 C112 C17 118.18(15) . . ? O1 C113 C112 123.24(15) . . ? O1 C113 C114 118.14(14) . . ? C112 C113 C114 118.60(14) . . ? C11 C114 C113 120.87(14) . . ? C11 C114 C15 118.38(14) . . ? C113 C114 C15 120.70(14) . . ? C22 C21 Zn1 115.73(12) . . ? C22 C21 H21A 108.4(9) . . ? Zn1 C21 H21A 105.5(10) . . ? C22 C21 H21B 110.6(12) . . ? Zn1 C21 H21B 108.6(12) . . ? H21A C21 H21B 107.6(16) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C311 N31 C312 108.14(14) . . ? C311 N31 C32 111.01(14) . . ? C312 N31 C32 109.02(14) . . ? C311 N31 Zn1 110.94(11) . . ? C312 N31 Zn1 113.83(11) . . ? C32 N31 Zn1 103.87(9) . . ? N31 C311 H31A 109.5 . . ? N31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? N31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? N31 C312 H31D 109.5 . . ? N31 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? N31 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? N31 C32 C33 111.55(14) . . ? N31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? N31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? N34 C33 C32 110.94(14) . . ? N34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? N34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.0 . . ? C341 N34 C342 108.73(14) . . ? C341 N34 C33 110.86(14) . . ? C342 N34 C33 109.54(14) . . ? C341 N34 Zn1 112.81(12) . . ? C342 N34 Zn1 111.47(10) . . ? C33 N34 Zn1 103.35(10) . . ? N34 C341 H34A 109.5 . . ? N34 C341 H34B 109.5 . . ? H34A C341 H34B 109.5 . . ? N34 C341 H34C 109.5 . . ? H34A C341 H34C 109.5 . . ? H34B C341 H34C 109.5 . . ? N34 C342 H34D 109.5 . . ? N34 C342 H34E 109.5 . . ? H34D C342 H34E 109.5 . . ? N34 C342 H34F 109.5 . . ? H34D C342 H34F 109.5 . . ? H34E C342 H34F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Zn1 O1 C113 18.5(3) . . . . ? N31 Zn1 O1 C113 156.4(2) . . . . ? N34 Zn1 O1 C113 -117.7(2) . . . . ? C114 C11 C12 C13 -0.5(3) . . . . ? C11 C12 C13 C14 0.9(3) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C13 C14 C15 C16 176.09(16) . . . . ? C13 C14 C15 C114 -1.8(2) . . . . ? C14 C15 C16 C17 -177.30(15) . . . . ? C114 C15 C16 C17 0.6(2) . . . . ? C15 C16 C17 C18 177.35(15) . . . . ? C15 C16 C17 C112 -1.5(2) . . . . ? C16 C17 C18 C19 -178.46(16) . . . . ? C112 C17 C18 C19 0.4(2) . . . . ? C17 C18 C19 C110 0.0(3) . . . . ? C18 C19 C110 C111 -0.5(3) . . . . ? C19 C110 C111 C112 0.5(3) . . . . ? C110 C111 C112 C113 178.22(16) . . . . ? C110 C111 C112 C17 0.0(2) . . . . ? C16 C17 C112 C113 0.2(2) . . . . ? C18 C17 C112 C113 -178.73(14) . . . . ? C16 C17 C112 C111 178.47(14) . . . . ? C18 C17 C112 C111 -0.4(2) . . . . ? Zn1 O1 C113 C112 5.0(3) . . . . ? Zn1 O1 C113 C114 -176.21(16) . . . . ? C111 C112 C113 O1 2.6(3) . . . . ? C17 C112 C113 O1 -179.18(15) . . . . ? C111 C112 C113 C114 -176.19(15) . . . . ? C17 C112 C113 C114 2.0(2) . . . . ? C12 C11 C114 C113 -178.55(16) . . . . ? C12 C11 C114 C15 -1.1(2) . . . . ? O1 C113 C114 C11 -4.4(2) . . . . ? C112 C113 C114 C11 174.49(15) . . . . ? O1 C113 C114 C15 178.19(14) . . . . ? C112 C113 C114 C15 -3.0(2) . . . . ? C16 C15 C114 C11 -175.82(15) . . . . ? C14 C15 C114 C11 2.1(2) . . . . ? C16 C15 C114 C113 1.7(2) . . . . ? C14 C15 C114 C113 179.65(15) . . . . ? O1 Zn1 C21 C22 61.59(17) . . . . ? N31 Zn1 C21 C22 -71.07(14) . . . . ? N34 Zn1 C21 C22 -166.64(12) . . . . ? O1 Zn1 N31 C311 -157.54(12) . . . . ? C21 Zn1 N31 C311 -7.75(14) . . . . ? N34 Zn1 N31 C311 105.43(12) . . . . ? O1 Zn1 N31 C312 -35.30(12) . . . . ? C21 Zn1 N31 C312 114.49(12) . . . . ? N34 Zn1 N31 C312 -132.32(12) . . . . ? O1 Zn1 N31 C32 83.13(11) . . . . ? C21 Zn1 N31 C32 -127.08(11) . . . . ? N34 Zn1 N31 C32 -13.90(10) . . . . ? C311 N31 C32 C33 -78.32(17) . . . . ? C312 N31 C32 C33 162.65(15) . . . . ? Zn1 N31 C32 C33 40.96(15) . . . . ? N31 C32 C33 N34 -59.06(18) . . . . ? C32 C33 N34 C341 -80.15(18) . . . . ? C32 C33 N34 C342 159.86(14) . . . . ? C32 C33 N34 Zn1 40.96(15) . . . . ? O1 Zn1 N34 C341 9.72(12) . . . . ? C21 Zn1 N34 C341 -139.50(12) . . . . ? N31 Zn1 N34 C341 105.36(12) . . . . ? O1 Zn1 N34 C342 132.38(11) . . . . ? C21 Zn1 N34 C342 -16.84(13) . . . . ? N31 Zn1 N34 C342 -131.98(11) . . . . ? O1 Zn1 N34 C33 -110.06(11) . . . . ? C21 Zn1 N34 C33 100.71(12) . . . . ? N31 Zn1 N34 C33 -14.42(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.390 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.055 #===END