####################################################################### # # 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_s533bz _database_code_depnum_ccdc_archive 'CCDC 865606' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H50 Cu2 N4 Si2' _chemical_formula_weight 674.02 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 10.101(12) _cell_length_b 12.616(15) _cell_length_c 14.018(17) _cell_angle_alpha 96.910(17) _cell_angle_beta 98.657(19) _cell_angle_gamma 90.190(19) _cell_volume 1753(4) _cell_formula_units_Z 2 _cell_measurement_temperature 241(2) _cell_measurement_reflns_used 3444 _cell_measurement_theta_min 2.339 _cell_measurement_theta_max 23.818 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6951 _exptl_absorpt_correction_T_max 0.7800 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 241(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area scan' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.66 _diffrn_reflns_number 18587 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6180 _reflns_number_gt 4570 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.1267P] 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 6180 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Cu1 Cu 0.89968(4) 0.53347(3) -0.04832(3) 0.02684(12) Uani 1 1 d . . . N1 N 0.8603(2) 0.61535(19) 0.06613(18) 0.0279(6) Uani 1 1 d . . . C1 C 0.9395(3) 0.6083(2) 0.1522(2) 0.0256(7) Uani 1 1 d . . . C2 C 0.9001(3) 0.6683(3) 0.2431(2) 0.0302(8) Uani 1 1 d . . . C3 C 0.9531(4) 0.7703(3) 0.2782(2) 0.0414(9) Uani 1 1 d . . . H3A H 1.0149 0.8018 0.2457 0.050 Uiso 1 1 calc R . . C4 C 0.9148(5) 0.8250(3) 0.3607(3) 0.0602(12) Uani 1 1 d . . . H4A H 0.9503 0.8939 0.3836 0.072 Uiso 1 1 calc R . . C5 C 0.8253(5) 0.7799(4) 0.4098(3) 0.0710(15) Uani 1 1 d . . . H5A H 0.7987 0.8183 0.4652 0.085 Uiso 1 1 calc R . . C6 C 0.7746(4) 0.6778(4) 0.3773(3) 0.0675(14) Uani 1 1 d . . . H6A H 0.7146 0.6462 0.4112 0.081 Uiso 1 1 calc R . . C7 C 0.8125(4) 0.6220(3) 0.2942(2) 0.0465(10) Uani 1 1 d . . . H7A H 0.7785 0.5524 0.2725 0.056 Uiso 1 1 calc R . . C8 C 1.1308(3) 0.5436(3) 0.2549(2) 0.0326(8) Uani 1 1 d . . . H8A H 1.0943 0.5939 0.3038 0.039 Uiso 1 1 calc R . . C9 C 1.1199(4) 0.4321(3) 0.2829(3) 0.0481(10) Uani 1 1 d . . . H9A H 1.1462 0.3804 0.2314 0.058 Uiso 1 1 calc R . . H9B H 1.0265 0.4164 0.2884 0.058 Uiso 1 1 calc R . . C10 C 1.2084(5) 0.4190(4) 0.3792(3) 0.0684(13) Uani 1 1 d . . . H10A H 1.1765 0.4650 0.4321 0.082 Uiso 1 1 calc R . . H10B H 1.2025 0.3448 0.3927 0.082 Uiso 1 1 calc R . . C11 C 1.3533(5) 0.4484(4) 0.3748(3) 0.0768(15) Uani 1 1 d . . . H11A H 1.4079 0.4422 0.4378 0.092 Uiso 1 1 calc R . . H11B H 1.3873 0.3984 0.3256 0.092 Uiso 1 1 calc R . . C12 C 1.3660(4) 0.5611(4) 0.3500(3) 0.0673(13) Uani 1 1 d . . . H12A H 1.4596 0.5763 0.3444 0.081 Uiso 1 1 calc R . . H12B H 1.3409 0.6116 0.4027 0.081 Uiso 1 1 calc R . . C13 C 1.2763(3) 0.5770(3) 0.2540(3) 0.0469(10) Uani 1 1 d . . . H13A H 1.2802 0.6523 0.2436 0.056 Uiso 1 1 calc R . . H13B H 1.3102 0.5346 0.1999 0.056 Uiso 1 1 calc R . . C14 C 0.5757(4) 0.6512(4) 0.1106(3) 0.0673(13) Uani 1 1 d . . . H14A H 0.6042 0.6556 0.1803 0.101 Uiso 1 1 calc R . . H14B H 0.5495 0.5781 0.0849 0.101 Uiso 1 1 calc R . . H14C H 0.5002 0.6973 0.0976 0.101 Uiso 1 1 calc R . . C15 C 0.7569(4) 0.8391(3) 0.0887(3) 0.0681(13) Uani 1 1 d . . . H15A H 0.8303 0.8604 0.0573 0.102 Uiso 1 1 calc R . . H15B H 0.7825 0.8517 0.1587 0.102 Uiso 1 1 calc R . . H15C H 0.6788 0.8805 0.0696 0.102 Uiso 1 1 calc R . . C16 C 0.6506(4) 0.6822(4) -0.0817(3) 0.0620(12) Uani 1 1 d . . . H16A H 0.7200 0.7036 -0.1168 0.093 Uiso 1 1 calc R . . H16B H 0.5741 0.7279 -0.0926 0.093 Uiso 1 1 calc R . . H16C H 0.6234 0.6086 -0.1047 0.093 Uiso 1 1 calc R . . Cu2 Cu 0.58096(4) 0.03836(3) -0.04555(3) 0.02680(12) Uani 1 1 d . . . N3 N 0.6660(2) 0.11559(19) 0.07275(18) 0.0265(6) Uani 1 1 d . . . C17 C 0.6197(3) 0.1027(2) 0.1562(2) 0.0263(7) Uani 1 1 d . . . C18 C 0.6938(3) 0.1595(2) 0.2509(2) 0.0285(7) Uani 1 1 d . . . C19 C 0.6569(4) 0.2603(3) 0.2887(3) 0.0460(10) Uani 1 1 d . . . H19A H 0.5853 0.2946 0.2549 0.055 Uiso 1 1 calc R . . C20 C 0.7256(4) 0.3107(3) 0.3765(3) 0.0595(12) Uani 1 1 d . . . H20A H 0.6995 0.3786 0.4016 0.071 Uiso 1 1 calc R . . C21 C 0.8307(4) 0.2618(4) 0.4261(3) 0.0638(12) Uani 1 1 d . . . H21A H 0.8777 0.2964 0.4846 0.077 Uiso 1 1 calc R . . C22 C 0.8670(4) 0.1617(4) 0.3897(3) 0.0575(11) Uani 1 1 d . . . H22A H 0.9383 0.1274 0.4239 0.069 Uiso 1 1 calc R . . C23 C 0.7983(3) 0.1111(3) 0.3021(2) 0.0433(9) Uani 1 1 d . . . H23A H 0.8240 0.0428 0.2778 0.052 Uiso 1 1 calc R . . C24 C 0.4684(3) 0.0305(3) 0.2541(2) 0.0343(8) Uani 1 1 d . . . H24A H 0.5273 0.0766 0.3056 0.041 Uiso 1 1 calc R . . C25 C 0.4835(4) -0.0842(3) 0.2759(2) 0.0479(10) Uani 1 1 d . . . H25A H 0.5779 -0.1035 0.2798 0.057 Uiso 1 1 calc R . . H25B H 0.4319 -0.1318 0.2228 0.057 Uiso 1 1 calc R . . C26 C 0.4349(6) -0.0998(4) 0.3715(3) 0.0765(15) Uani 1 1 d . . . H26A H 0.4396 -0.1755 0.3807 0.092 Uiso 1 1 calc R . . H26B H 0.4942 -0.0595 0.4256 0.092 Uiso 1 1 calc R . . C27 C 0.2927(6) -0.0631(5) 0.3731(4) 0.096(2) Uani 1 1 d . . . H27A H 0.2680 -0.0686 0.4373 0.116 Uiso 1 1 calc R . . H27B H 0.2316 -0.1100 0.3250 0.116 Uiso 1 1 calc R . . C28 C 0.2772(5) 0.0515(5) 0.3506(3) 0.0836(17) Uani 1 1 d . . . H28A H 0.3285 0.0993 0.4036 0.100 Uiso 1 1 calc R . . H28B H 0.1827 0.0705 0.3467 0.100 Uiso 1 1 calc R . . C29 C 0.3258(4) 0.0676(4) 0.2544(3) 0.0550(11) Uani 1 1 d . . . H29A H 0.2668 0.0273 0.2002 0.066 Uiso 1 1 calc R . . H29B H 0.3214 0.1434 0.2453 0.066 Uiso 1 1 calc R . . C30 C 0.8239(4) 0.1866(4) -0.0681(3) 0.0687(14) Uani 1 1 d . . . H30A H 0.8377 0.1127 -0.0921 0.103 Uiso 1 1 calc R . . H30B H 0.9003 0.2300 -0.0755 0.103 Uiso 1 1 calc R . . H30C H 0.7435 0.2118 -0.1048 0.103 Uiso 1 1 calc R . . C31 C 0.7808(5) 0.3405(3) 0.1030(4) 0.0718(14) Uani 1 1 d . . . H31A H 0.7706 0.3500 0.1712 0.108 Uiso 1 1 calc R . . H31B H 0.7011 0.3647 0.0646 0.108 Uiso 1 1 calc R . . H31C H 0.8581 0.3818 0.0938 0.108 Uiso 1 1 calc R . . C32 C 0.9682(4) 0.1539(4) 0.1262(3) 0.0733(14) Uani 1 1 d . . . H32A H 0.9651 0.1571 0.1953 0.110 Uiso 1 1 calc R . . H32B H 1.0394 0.2011 0.1159 0.110 Uiso 1 1 calc R . . H32C H 0.9852 0.0814 0.1001 0.110 Uiso 1 1 calc R . . Si1 Si 0.71694(9) 0.69472(7) 0.05136(7) 0.0330(2) Uani 1 1 d . . . Si2 Si 0.80505(9) 0.19678(8) 0.06339(7) 0.0345(2) Uani 1 1 d . . . N2 N 1.0501(2) 0.5509(2) 0.15902(17) 0.0277(6) Uani 1 1 d . . . N4 N 0.5125(2) 0.0423(2) 0.15964(17) 0.0278(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0267(2) 0.0295(2) 0.0229(2) 0.00054(16) 0.00115(16) 0.00701(16) N1 0.0286(15) 0.0268(14) 0.0270(15) 0.0009(11) 0.0021(12) 0.0034(11) C1 0.0296(18) 0.0200(16) 0.0268(17) -0.0001(13) 0.0052(14) -0.0027(13) C2 0.0268(18) 0.0371(19) 0.0253(17) -0.0003(14) 0.0026(14) 0.0112(15) C3 0.052(2) 0.039(2) 0.031(2) -0.0016(16) 0.0020(17) 0.0083(17) C4 0.081(3) 0.050(3) 0.039(2) -0.016(2) -0.007(2) 0.020(2) C5 0.064(3) 0.111(4) 0.030(2) -0.020(3) 0.003(2) 0.042(3) C6 0.048(3) 0.126(4) 0.029(2) 0.003(3) 0.0101(19) 0.007(3) C7 0.044(2) 0.067(3) 0.029(2) 0.0049(18) 0.0071(17) -0.0021(19) C8 0.0300(18) 0.042(2) 0.0238(17) -0.0010(15) -0.0004(14) 0.0077(15) C9 0.050(2) 0.055(2) 0.039(2) 0.0130(19) 0.0007(18) 0.0036(19) C10 0.087(4) 0.068(3) 0.048(3) 0.022(2) -0.010(2) 0.011(3) C11 0.075(4) 0.097(4) 0.050(3) 0.012(3) -0.021(2) 0.036(3) C12 0.039(2) 0.106(4) 0.047(3) -0.002(3) -0.015(2) -0.005(2) C13 0.037(2) 0.057(3) 0.041(2) -0.0002(19) -0.0068(17) -0.0009(18) C14 0.033(2) 0.099(4) 0.076(3) 0.026(3) 0.014(2) 0.015(2) C15 0.065(3) 0.044(2) 0.089(3) 0.003(2) -0.008(3) 0.022(2) C16 0.062(3) 0.078(3) 0.041(2) 0.000(2) -0.003(2) 0.036(2) Cu2 0.0273(2) 0.0298(2) 0.0226(2) 0.00008(16) 0.00432(16) -0.00564(17) N3 0.0272(15) 0.0264(14) 0.0253(14) 0.0027(11) 0.0028(11) -0.0039(11) C17 0.0269(17) 0.0229(16) 0.0272(17) -0.0008(13) 0.0010(14) 0.0038(13) C18 0.0273(18) 0.0320(18) 0.0244(17) -0.0014(14) 0.0023(14) -0.0050(14) C19 0.057(2) 0.038(2) 0.037(2) -0.0072(17) -0.0017(18) 0.0065(18) C20 0.080(3) 0.048(3) 0.042(2) -0.017(2) -0.001(2) 0.001(2) C21 0.068(3) 0.078(3) 0.035(2) -0.013(2) -0.010(2) -0.013(3) C22 0.049(3) 0.081(3) 0.036(2) -0.001(2) -0.0101(19) 0.007(2) C23 0.041(2) 0.050(2) 0.035(2) -0.0016(17) -0.0036(17) 0.0023(18) C24 0.036(2) 0.043(2) 0.0234(18) -0.0013(15) 0.0057(15) -0.0072(16) C25 0.061(3) 0.054(2) 0.029(2) 0.0105(17) 0.0054(18) -0.008(2) C26 0.114(4) 0.080(3) 0.040(3) 0.020(2) 0.016(3) -0.028(3) C27 0.095(4) 0.147(6) 0.054(3) 0.013(3) 0.034(3) -0.053(4) C28 0.056(3) 0.150(5) 0.049(3) -0.001(3) 0.031(2) 0.006(3) C29 0.049(2) 0.076(3) 0.042(2) -0.001(2) 0.0217(19) 0.009(2) C30 0.063(3) 0.097(4) 0.047(3) 0.005(2) 0.013(2) -0.042(3) C31 0.078(3) 0.039(2) 0.101(4) 0.001(2) 0.025(3) -0.021(2) C32 0.032(2) 0.097(4) 0.095(4) 0.034(3) 0.007(2) -0.001(2) Si1 0.0298(5) 0.0362(5) 0.0318(5) 0.0017(4) 0.0031(4) 0.0117(4) Si2 0.0313(5) 0.0374(6) 0.0338(5) 0.0035(4) 0.0020(4) -0.0108(4) N2 0.0264(14) 0.0333(15) 0.0222(14) 0.0018(11) 0.0009(11) 0.0048(12) N4 0.0277(15) 0.0327(15) 0.0220(14) 0.0000(11) 0.0034(11) -0.0033(12) _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 Cu1 N1 1.896(3) . ? Cu1 N2 1.908(3) 2_765 ? Cu1 Cu1 2.473(2) 2_765 ? N1 C1 1.356(4) . ? N1 Si1 1.764(3) . ? C1 N2 1.331(4) . ? C1 C2 1.509(4) . ? C2 C7 1.387(5) . ? C2 C3 1.396(5) . ? C3 C4 1.381(5) . ? C3 H3A 0.9400 . ? C4 C5 1.376(7) . ? C4 H4A 0.9400 . ? C5 C6 1.382(7) . ? C5 H5A 0.9400 . ? C6 C7 1.393(5) . ? C6 H6A 0.9400 . ? C7 H7A 0.9400 . ? C8 N2 1.477(4) . ? C8 C9 1.513(5) . ? C8 C13 1.530(5) . ? C8 H8A 0.9900 . ? C9 C10 1.529(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.520(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.513(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.540(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 Si1 1.868(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 Si1 1.860(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 Si1 1.872(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? Cu2 N3 1.901(3) . ? Cu2 N4 1.905(3) 2_655 ? Cu2 Cu2 2.482(2) 2_655 ? N3 C17 1.350(4) . ? N3 Si2 1.766(3) . ? C17 N4 1.332(4) . ? C17 C18 1.519(4) . ? C18 C23 1.372(5) . ? C18 C19 1.391(5) . ? C19 C20 1.397(5) . ? C19 H19A 0.9400 . ? C20 C21 1.370(6) . ? C20 H20A 0.9400 . ? C21 C22 1.376(6) . ? C21 H21A 0.9400 . ? C22 C23 1.396(5) . ? C22 H22A 0.9400 . ? C23 H23A 0.9400 . ? C24 N4 1.482(4) . ? C24 C29 1.516(5) . ? C24 C25 1.519(5) . ? C24 H24A 0.9900 . ? C25 C26 1.528(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.513(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.520(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.538(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 Si2 1.870(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 Si2 1.859(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 Si2 1.862(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? N2 Cu1 1.908(3) 2_765 ? N4 Cu2 1.905(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 176.41(10) . 2_765 ? N1 Cu1 Cu1 89.11(10) . 2_765 ? N2 Cu1 Cu1 87.34(10) 2_765 2_765 ? C1 N1 Si1 124.7(2) . . ? C1 N1 Cu1 119.6(2) . . ? Si1 N1 Cu1 115.78(14) . . ? N2 C1 N1 122.4(3) . . ? N2 C1 C2 119.2(3) . . ? N1 C1 C2 118.4(3) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 120.7(3) . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C7 119.9(4) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C2 C7 C6 120.5(4) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? N2 C8 C9 110.4(3) . . ? N2 C8 C13 110.1(3) . . ? C9 C8 C13 111.8(3) . . ? N2 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? C13 C8 H8A 108.2 . . ? C8 C9 C10 112.2(3) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 110.5(4) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 111.3(4) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.6(3) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.5(3) . . ? C8 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C8 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 Cu2 N4 176.37(10) . 2_655 ? N3 Cu2 Cu2 89.22(11) . 2_655 ? N4 Cu2 Cu2 87.16(11) 2_655 2_655 ? C17 N3 Si2 125.3(2) . . ? C17 N3 Cu2 118.9(2) . . ? Si2 N3 Cu2 115.72(15) . . ? N4 C17 N3 123.3(3) . . ? N4 C17 C18 118.3(3) . . ? N3 C17 C18 118.4(3) . . ? C23 C18 C19 118.4(3) . . ? C23 C18 C17 120.2(3) . . ? C19 C18 C17 121.3(3) . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C18 C23 C22 121.0(4) . . ? C18 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? N4 C24 C29 110.6(3) . . ? N4 C24 C25 110.1(3) . . ? C29 C24 C25 111.8(3) . . ? N4 C24 H24A 108.1 . . ? C29 C24 H24A 108.1 . . ? C25 C24 H24A 108.1 . . ? C24 C25 C26 111.5(3) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 111.9(4) . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 111.4(4) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C29 111.9(4) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C24 C29 C28 111.0(3) . . ? C24 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? C24 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 Si1 C15 112.36(17) . . ? N1 Si1 C14 114.54(18) . . ? C15 Si1 C14 110.5(2) . . ? N1 Si1 C16 107.49(15) . . ? C15 Si1 C16 105.8(2) . . ? C14 Si1 C16 105.5(2) . . ? N3 Si2 C31 112.78(18) . . ? N3 Si2 C32 114.66(18) . . ? C31 Si2 C32 109.7(2) . . ? N3 Si2 C30 107.57(15) . . ? C31 Si2 C30 106.3(2) . . ? C32 Si2 C30 105.2(2) . . ? C1 N2 C8 120.2(3) . . ? C1 N2 Cu1 121.4(2) . 2_765 ? C8 N2 Cu1 118.1(2) . 2_765 ? C17 N4 C24 120.4(3) . . ? C17 N4 Cu2 121.3(2) . 2_655 ? C24 N4 Cu2 118.2(2) . 2_655 ? 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 N2 Cu1 N1 C1 -11.4(19) 2_765 . . . ? Cu1 Cu1 N1 C1 -2.6(2) 2_765 . . . ? N2 Cu1 N1 Si1 169.9(17) 2_765 . . . ? Cu1 Cu1 N1 Si1 178.70(13) 2_765 . . . ? Si1 N1 C1 N2 -176.9(2) . . . . ? Cu1 N1 C1 N2 4.4(4) . . . . ? Si1 N1 C1 C2 2.9(4) . . . . ? Cu1 N1 C1 C2 -175.7(2) . . . . ? N2 C1 C2 C7 -93.2(4) . . . . ? N1 C1 C2 C7 86.9(4) . . . . ? N2 C1 C2 C3 85.5(4) . . . . ? N1 C1 C2 C3 -94.4(4) . . . . ? C7 C2 C3 C4 -2.2(5) . . . . ? C1 C2 C3 C4 179.1(3) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C4 C5 C6 C7 -1.1(7) . . . . ? C3 C2 C7 C6 2.2(5) . . . . ? C1 C2 C7 C6 -179.1(3) . . . . ? C5 C6 C7 C2 -0.6(6) . . . . ? N2 C8 C9 C10 176.7(3) . . . . ? C13 C8 C9 C10 53.8(4) . . . . ? C8 C9 C10 C11 -55.9(5) . . . . ? C9 C10 C11 C12 56.9(5) . . . . ? C10 C11 C12 C13 -56.1(5) . . . . ? N2 C8 C13 C12 -175.1(3) . . . . ? C9 C8 C13 C12 -52.0(4) . . . . ? C11 C12 C13 C8 53.3(5) . . . . ? N4 Cu2 N3 C17 5.0(18) 2_655 . . . ? Cu2 Cu2 N3 C17 1.8(2) 2_655 . . . ? N4 Cu2 N3 Si2 -176.8(16) 2_655 . . . ? Cu2 Cu2 N3 Si2 180.00(13) 2_655 . . . ? Si2 N3 C17 N4 178.5(2) . . . . ? Cu2 N3 C17 N4 -3.4(4) . . . . ? Si2 N3 C17 C18 -1.8(4) . . . . ? Cu2 N3 C17 C18 176.3(2) . . . . ? N4 C17 C18 C23 91.1(4) . . . . ? N3 C17 C18 C23 -88.6(4) . . . . ? N4 C17 C18 C19 -87.9(4) . . . . ? N3 C17 C18 C19 92.4(4) . . . . ? C23 C18 C19 C20 0.3(6) . . . . ? C17 C18 C19 C20 179.4(3) . . . . ? C18 C19 C20 C21 0.4(6) . . . . ? C19 C20 C21 C22 -1.0(7) . . . . ? C20 C21 C22 C23 0.9(7) . . . . ? C19 C18 C23 C22 -0.5(5) . . . . ? C17 C18 C23 C22 -179.5(3) . . . . ? C21 C22 C23 C18 -0.1(6) . . . . ? N4 C24 C25 C26 -178.3(3) . . . . ? C29 C24 C25 C26 -54.9(4) . . . . ? C24 C25 C26 C27 54.5(5) . . . . ? C25 C26 C27 C28 -54.1(6) . . . . ? C26 C27 C28 C29 54.1(6) . . . . ? N4 C24 C29 C28 177.7(4) . . . . ? C25 C24 C29 C28 54.6(5) . . . . ? C27 C28 C29 C24 -54.3(5) . . . . ? C1 N1 Si1 C15 60.7(3) . . . . ? Cu1 N1 Si1 C15 -120.6(2) . . . . ? C1 N1 Si1 C14 -66.5(3) . . . . ? Cu1 N1 Si1 C14 112.2(2) . . . . ? C1 N1 Si1 C16 176.7(3) . . . . ? Cu1 N1 Si1 C16 -4.7(2) . . . . ? C17 N3 Si2 C31 -62.5(3) . . . . ? Cu2 N3 Si2 C31 119.4(2) . . . . ? C17 N3 Si2 C32 64.0(3) . . . . ? Cu2 N3 Si2 C32 -114.1(2) . . . . ? C17 N3 Si2 C30 -179.4(3) . . . . ? Cu2 N3 Si2 C30 2.5(2) . . . . ? N1 C1 N2 C8 -178.3(3) . . . . ? C2 C1 N2 C8 1.9(4) . . . . ? N1 C1 N2 Cu1 -3.9(4) . . . 2_765 ? C2 C1 N2 Cu1 176.3(2) . . . 2_765 ? C9 C8 N2 C1 110.5(3) . . . . ? C13 C8 N2 C1 -125.6(3) . . . . ? C9 C8 N2 Cu1 -64.1(3) . . . 2_765 ? C13 C8 N2 Cu1 59.8(3) . . . 2_765 ? N3 C17 N4 C24 179.1(3) . . . . ? C18 C17 N4 C24 -0.6(4) . . . . ? N3 C17 N4 Cu2 3.3(4) . . . 2_655 ? C18 C17 N4 Cu2 -176.4(2) . . . 2_655 ? C29 C24 N4 C17 121.4(3) . . . . ? C25 C24 N4 C17 -114.5(3) . . . . ? C29 C24 N4 Cu2 -62.6(3) . . . 2_655 ? C25 C24 N4 Cu2 61.5(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.339 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.068 data_s545b _database_code_depnum_ccdc_archive 'CCDC 865607' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 Mg N4 O Si2' _chemical_formula_weight 645.37 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.456(17) _cell_length_b 9.444(8) _cell_length_c 21.882(20) _cell_angle_alpha 90.00 _cell_angle_beta 93.237(17) _cell_angle_gamma 90.00 _cell_volume 4015(6) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 1198 _cell_measurement_theta_min 2.4055 _cell_measurement_theta_max 19.791 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9736 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area scan' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10747 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3562 _reflns_number_gt 2039 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following restraints were used to restrict the atomic displacement parameters of the related atoms or to restrict the distances among atoms in the diethyl ether. OMIT -3 50.1 DFIX 1.54 0.007 C18B C17B C18A C17A O1 C17A O1 C17B DELU 0.01 O1 C17B DELU 0.01 O1 c17A DELU 0.01 C17A C18A SIMU 0.01 SI1 C8 C9 C10 ISOR 0.01 SI1 C8 C9 C10 ISOR 0.01 C17A C17B C18A C18B ; _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^)+(0.0867P)^2^+5.1132P] 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 3562 _refine_ls_number_parameters 223 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.993 _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 0.0000 0.21991(18) 0.2500 0.0357(5) Uani 1 2 d S . . N1 N 0.04906(15) 0.2456(3) 0.34025(13) 0.0386(7) Uani 1 1 d . . . N2 N 0.09096(14) 0.3407(3) 0.25511(13) 0.0392(8) Uani 1 1 d . . . Si1 Si 0.04375(6) 0.18662(13) 0.41415(5) 0.0444(3) Uani 1 1 d U . . C1 C 0.09399(17) 0.3347(4) 0.31541(16) 0.0379(9) Uani 1 1 d . . . C2 C 0.14410(19) 0.4224(4) 0.35452(16) 0.0417(9) Uani 1 1 d . . . C3 C 0.2132(2) 0.3869(5) 0.3618(2) 0.0583(12) Uani 1 1 d . . . H3 H 0.2295 0.3081 0.3408 0.070 Uiso 1 1 calc R . . C4 C 0.2587(2) 0.4646(6) 0.3993(2) 0.0767(15) Uani 1 1 d . . . H4 H 0.3052 0.4376 0.4039 0.092 Uiso 1 1 calc R . . C5 C 0.2360(3) 0.5804(6) 0.4296(2) 0.0778(16) Uani 1 1 d . . . H5 H 0.2670 0.6340 0.4546 0.093 Uiso 1 1 calc R . . C6 C 0.1680(3) 0.6188(6) 0.4234(3) 0.0865(17) Uani 1 1 d . . . H6 H 0.1524 0.6980 0.4447 0.104 Uiso 1 1 calc R . . C7 C 0.1215(2) 0.5397(5) 0.3854(2) 0.0703(14) Uani 1 1 d . . . H7 H 0.0750 0.5668 0.3809 0.084 Uiso 1 1 calc R . . C8 C 0.1251(3) 0.1129(7) 0.4479(2) 0.103(2) Uani 1 1 d U . . H8A H 0.1416 0.0399 0.4212 0.155 Uiso 1 1 calc R . . H8B H 0.1173 0.0724 0.4876 0.155 Uiso 1 1 calc R . . H8C H 0.1592 0.1877 0.4526 0.155 Uiso 1 1 calc R . . C9 C 0.0137(4) 0.3180(7) 0.4695(2) 0.112(2) Uani 1 1 d U . . H9A H 0.0476 0.3930 0.4750 0.169 Uiso 1 1 calc R . . H9B H 0.0077 0.2720 0.5085 0.169 Uiso 1 1 calc R . . H9C H -0.0298 0.3579 0.4541 0.169 Uiso 1 1 calc R . . C10 C -0.0244(3) 0.0499(7) 0.4105(2) 0.123(2) Uani 1 1 d U . . H10A H -0.0633 0.0832 0.3848 0.184 Uiso 1 1 calc R . . H10B H -0.0390 0.0314 0.4514 0.184 Uiso 1 1 calc R . . H10C H -0.0066 -0.0365 0.3935 0.184 Uiso 1 1 calc R . . C11 C 0.13174(18) 0.4393(4) 0.22028(17) 0.0433(9) Uani 1 1 d . . . H11 H 0.1593 0.5000 0.2493 0.052 Uiso 1 1 calc R . . C12 C 0.1803(2) 0.3592(5) 0.1805(2) 0.0619(12) Uani 1 1 d . . . H12A H 0.1537 0.2915 0.1548 0.074 Uiso 1 1 calc R . . H12B H 0.2133 0.3055 0.2068 0.074 Uiso 1 1 calc R . . C13 C 0.2199(2) 0.4596(5) 0.1392(2) 0.0742(14) Uani 1 1 d . . . H13A H 0.2507 0.5201 0.1648 0.089 Uiso 1 1 calc R . . H13B H 0.2482 0.4036 0.1126 0.089 Uiso 1 1 calc R . . C14 C 0.1703(2) 0.5521(5) 0.1000(2) 0.0672(13) Uani 1 1 d . . . H14A H 0.1966 0.6194 0.0765 0.081 Uiso 1 1 calc R . . H14B H 0.1433 0.4924 0.0710 0.081 Uiso 1 1 calc R . . C15 C 0.1225(2) 0.6320(5) 0.1395(2) 0.0599(12) Uani 1 1 d . . . H15A H 0.0894 0.6857 0.1132 0.072 Uiso 1 1 calc R . . H15B H 0.1492 0.6997 0.1651 0.072 Uiso 1 1 calc R . . C16 C 0.0837(2) 0.5328(4) 0.18028(19) 0.0507(10) Uani 1 1 d . . . H16A H 0.0530 0.4725 0.1545 0.061 Uiso 1 1 calc R . . H16B H 0.0552 0.5892 0.2066 0.061 Uiso 1 1 calc R . . C17A C 0.0485(5) -0.1153(9) 0.2668(6) 0.148(4) Uani 0.71 1 d PDU . 1 H17A H 0.0416 -0.1984 0.2403 0.177 Uiso 0.71 1 calc PR . 1 H17B H 0.0464 -0.1434 0.3098 0.177 Uiso 0.71 1 calc PR . 1 C18A C 0.1138(5) -0.0364(11) 0.2549(5) 0.117(4) Uani 0.71 1 d PDU A 1 H18A H 0.1117 -0.0030 0.2129 0.176 Uiso 0.71 1 calc PR A 1 H18B H 0.1529 -0.0993 0.2616 0.176 Uiso 0.71 1 calc PR A 1 H18C H 0.1188 0.0437 0.2825 0.176 Uiso 0.71 1 calc PR A 1 C17B C 0.0748(5) -0.0562(17) 0.2471(7) 0.056(4) Uani 0.29 1 d PDU . 2 H17C H 0.0774 -0.1066 0.2082 0.068 Uiso 0.29 1 calc PR . 2 H17D H 0.1050 0.0265 0.2453 0.068 Uiso 0.29 1 calc PR . 2 C18B C 0.1060(8) -0.1538(16) 0.2974(7) 0.070(5) Uani 0.29 1 d PDU . 2 H18D H 0.1096 -0.1029 0.3360 0.105 Uiso 0.29 1 calc PR . 2 H18E H 0.1513 -0.1842 0.2867 0.105 Uiso 0.29 1 calc PR . 2 H18F H 0.0766 -0.2359 0.3014 0.105 Uiso 0.29 1 calc PR . 2 O1 O 0.0000 -0.0001(4) 0.2500 0.0731(13) Uani 1 2 d SDU . . 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 0.0339(9) 0.0390(10) 0.0338(9) 0.000 -0.0016(7) 0.000 N1 0.0347(16) 0.0457(18) 0.0349(17) 0.0002(15) -0.0030(13) -0.0025(15) N2 0.0353(16) 0.0458(19) 0.0362(17) 0.0021(14) -0.0009(13) -0.0102(15) Si1 0.0453(6) 0.0554(7) 0.0322(6) 0.0023(5) -0.0005(4) 0.0018(6) C1 0.034(2) 0.038(2) 0.041(2) -0.0012(17) -0.0025(16) 0.0051(17) C2 0.042(2) 0.044(2) 0.039(2) 0.0031(18) -0.0043(17) -0.0041(19) C3 0.044(2) 0.068(3) 0.061(3) -0.012(2) -0.014(2) 0.008(2) C4 0.054(3) 0.095(4) 0.078(3) -0.011(3) -0.022(3) -0.004(3) C5 0.071(4) 0.088(4) 0.071(3) -0.016(3) -0.017(3) -0.029(3) C6 0.084(4) 0.075(4) 0.100(4) -0.042(3) -0.002(3) -0.009(3) C7 0.057(3) 0.061(3) 0.091(4) -0.023(3) -0.011(3) 0.003(2) C8 0.074(3) 0.159(5) 0.076(3) 0.057(4) 0.011(3) 0.040(4) C9 0.164(6) 0.111(5) 0.063(3) 0.003(3) 0.016(3) 0.050(4) C10 0.150(5) 0.154(5) 0.062(3) 0.028(4) -0.001(3) -0.082(5) C11 0.040(2) 0.049(2) 0.040(2) 0.0008(19) -0.0006(17) -0.0116(19) C12 0.048(3) 0.062(3) 0.078(3) 0.011(2) 0.020(2) 0.002(2) C13 0.063(3) 0.073(3) 0.090(4) 0.004(3) 0.039(3) -0.002(3) C14 0.072(3) 0.080(3) 0.051(3) 0.008(3) 0.010(2) -0.031(3) C15 0.054(3) 0.066(3) 0.060(3) 0.017(2) 0.003(2) -0.006(2) C16 0.047(2) 0.051(2) 0.054(2) 0.006(2) 0.0051(19) 0.001(2) C17A 0.179(8) 0.099(7) 0.163(9) 0.009(7) -0.001(7) 0.026(6) C18A 0.106(6) 0.103(7) 0.140(7) -0.027(6) -0.023(6) 0.044(5) C17B 0.080(8) 0.023(7) 0.067(8) 0.001(6) 0.014(8) 0.012(7) C18B 0.065(8) 0.072(8) 0.069(8) 0.002(7) -0.026(7) 0.017(7) O1 0.108(4) 0.046(3) 0.063(3) 0.000 -0.009(3) 0.000 _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 2.078(5) . ? Mg1 N2 2.104(3) . ? Mg1 N2 2.104(3) 2 ? Mg1 N1 2.158(3) . ? Mg1 N1 2.158(3) 2 ? Mg1 C1 2.504(4) 2 ? N1 C1 1.350(5) . ? N1 Si1 1.719(3) . ? N2 C1 1.319(4) . ? N2 C11 1.465(4) . ? Si1 C8 1.845(5) . ? Si1 C10 1.849(6) . ? Si1 C9 1.852(6) . ? C1 C2 1.508(5) . ? C2 C7 1.382(6) . ? C2 C3 1.386(5) . ? C3 C4 1.383(6) . ? C3 H3 0.9400 . ? C4 C5 1.366(7) . ? C4 H4 0.9400 . ? C5 C6 1.370(7) . ? C5 H5 0.9400 . ? C6 C7 1.409(6) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.521(5) . ? C11 C16 1.525(5) . ? C11 H11 0.9900 . ? C12 C13 1.545(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.529(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.507(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.523(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17A O1 1.473(6) . ? C17A C18A 1.509(7) . ? C17A C17A 1.985(19) 2 ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18A H18C 0.9700 . ? C17B C18B 1.534(7) . ? C17B O1 1.553(7) . ? C17B H17C 0.9800 . ? C17B H17D 0.9800 . ? C18B H18D 0.9700 . ? C18B H18E 0.9700 . ? C18B H18F 0.9700 . ? O1 C17A 1.473(6) 2 ? O1 C17B 1.553(7) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N2 122.86(10) . . ? O1 Mg1 N2 122.86(10) . 2 ? N2 Mg1 N2 114.29(19) . 2 ? O1 Mg1 N1 96.45(9) . . ? N2 Mg1 N1 64.09(12) . . ? N2 Mg1 N1 108.37(12) 2 . ? O1 Mg1 N1 96.45(9) . 2 ? N2 Mg1 N1 108.37(12) . 2 ? N2 Mg1 N1 64.09(11) 2 2 ? N1 Mg1 N1 167.10(19) . 2 ? O1 Mg1 C1 115.65(9) . 2 ? N2 Mg1 C1 112.37(14) . 2 ? N2 Mg1 C1 31.76(11) 2 2 ? N1 Mg1 C1 138.19(13) . 2 ? N1 Mg1 C1 32.58(11) 2 2 ? C1 N1 Si1 131.0(3) . . ? C1 N1 Mg1 88.0(2) . . ? Si1 N1 Mg1 141.04(18) . . ? C1 N2 C11 123.6(3) . . ? C1 N2 Mg1 91.1(2) . . ? C11 N2 Mg1 142.7(2) . . ? N1 Si1 C8 113.8(2) . . ? N1 Si1 C10 105.5(2) . . ? C8 Si1 C10 110.5(3) . . ? N1 Si1 C9 115.9(2) . . ? C8 Si1 C9 106.6(3) . . ? C10 Si1 C9 104.1(3) . . ? N2 C1 N1 115.9(3) . . ? N2 C1 C2 122.3(3) . . ? N1 C1 C2 121.8(3) . . ? C7 C2 C3 118.1(4) . . ? C7 C2 C1 120.3(3) . . ? C3 C2 C1 121.6(4) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 120.2(4) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 110.7(3) . . ? N2 C11 C16 109.5(3) . . ? C12 C11 C16 109.8(3) . . ? N2 C11 H11 108.9 . . ? C12 C11 H11 108.9 . . ? C16 C11 H11 108.9 . . ? C11 C12 C13 112.1(4) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111.0(4) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 110.8(4) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.7(4) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C11 112.6(3) . . ? C15 C16 H16A 109.1 . . ? C11 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C11 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? O1 C17A C18A 97.2(6) . . ? O1 C17A C17A 47.6(4) . 2 ? C18A C17A C17A 136.7(10) . 2 ? O1 C17A H17A 112.3 . . ? C18A C17A H17A 112.3 . . ? C17A C17A H17A 71.7 2 . ? O1 C17A H17B 112.3 . . ? C18A C17A H17B 112.3 . . ? C17A C17A H17B 105.5 2 . ? H17A C17A H17B 109.9 . . ? C18B C17B O1 120.6(10) . . ? C18B C17B H17C 107.2 . . ? O1 C17B H17C 107.2 . . ? C18B C17B H17D 107.2 . . ? O1 C17B H17D 107.2 . . ? H17C C17B H17D 106.8 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17A O1 C17A 84.7(9) . 2 ? C17A O1 C17B 33.9(6) . . ? C17A O1 C17B 109.0(9) 2 . ? C17A O1 C17B 109.0(9) . 2 ? C17A O1 C17B 33.9(6) 2 2 ? C17B O1 C17B 140.1(13) . 2 ? C17A O1 Mg1 137.6(4) . . ? C17A O1 Mg1 137.6(4) 2 . ? C17B O1 Mg1 110.0(7) . . ? C17B O1 Mg1 109.9(7) 2 . ? 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 Mg1 N1 C1 129.19(19) . . . . ? N2 Mg1 N1 C1 5.68(19) . . . . ? N2 Mg1 N1 C1 -103.0(2) 2 . . . ? N1 Mg1 N1 C1 -50.81(19) 2 . . . ? C1 Mg1 N1 C1 -89.6(3) 2 . . . ? O1 Mg1 N1 Si1 -48.8(3) . . . . ? N2 Mg1 N1 Si1 -172.3(3) . . . . ? N2 Mg1 N1 Si1 79.0(3) 2 . . . ? N1 Mg1 N1 Si1 131.2(3) 2 . . . ? C1 Mg1 N1 Si1 92.4(3) 2 . . . ? O1 Mg1 N2 C1 -86.3(2) . . . . ? N2 Mg1 N2 C1 93.7(2) 2 . . . ? N1 Mg1 N2 C1 -5.8(2) . . . . ? N1 Mg1 N2 C1 162.9(2) 2 . . . ? C1 Mg1 N2 C1 128.3(2) 2 . . . ? O1 Mg1 N2 C11 113.6(4) . . . . ? N2 Mg1 N2 C11 -66.4(4) 2 . . . ? N1 Mg1 N2 C11 -165.9(4) . . . . ? N1 Mg1 N2 C11 2.8(4) 2 . . . ? C1 Mg1 N2 C11 -31.8(4) 2 . . . ? C1 N1 Si1 C8 -51.7(4) . . . . ? Mg1 N1 Si1 C8 125.7(4) . . . . ? C1 N1 Si1 C10 -173.0(4) . . . . ? Mg1 N1 Si1 C10 4.4(4) . . . . ? C1 N1 Si1 C9 72.4(4) . . . . ? Mg1 N1 Si1 C9 -110.2(4) . . . . ? C11 N2 C1 N1 175.0(3) . . . . ? Mg1 N2 C1 N1 9.3(3) . . . . ? C11 N2 C1 C2 -4.6(5) . . . . ? Mg1 N2 C1 C2 -170.3(3) . . . . ? Si1 N1 C1 N2 169.3(3) . . . . ? Mg1 N1 C1 N2 -9.1(3) . . . . ? Si1 N1 C1 C2 -11.1(5) . . . . ? Mg1 N1 C1 C2 170.5(3) . . . . ? N2 C1 C2 C7 104.8(5) . . . . ? N1 C1 C2 C7 -74.7(5) . . . . ? N2 C1 C2 C3 -76.6(5) . . . . ? N1 C1 C2 C3 103.8(4) . . . . ? C7 C2 C3 C4 0.8(7) . . . . ? C1 C2 C3 C4 -177.8(4) . . . . ? C2 C3 C4 C5 -0.9(8) . . . . ? C3 C4 C5 C6 0.8(8) . . . . ? C4 C5 C6 C7 -0.7(9) . . . . ? C3 C2 C7 C6 -0.7(7) . . . . ? C1 C2 C7 C6 177.9(4) . . . . ? C5 C6 C7 C2 0.6(8) . . . . ? C1 N2 C11 C12 117.6(4) . . . . ? Mg1 N2 C11 C12 -86.6(5) . . . . ? C1 N2 C11 C16 -121.1(4) . . . . ? Mg1 N2 C11 C16 34.7(5) . . . . ? N2 C11 C12 C13 175.4(3) . . . . ? C16 C11 C12 C13 54.3(5) . . . . ? C11 C12 C13 C14 -55.4(5) . . . . ? C12 C13 C14 C15 55.1(5) . . . . ? C13 C14 C15 C16 -55.3(5) . . . . ? C14 C15 C16 C11 55.8(5) . . . . ? N2 C11 C16 C15 -176.3(3) . . . . ? C12 C11 C16 C15 -54.5(5) . . . . ? C18A C17A O1 C17A 151.3(13) . . . 2 ? C18A C17A O1 C17B 15.0(15) . . . . ? C17A C17A O1 C17B -136(2) 2 . . . ? C18A C17A O1 C17B 175.4(9) . . . 2 ? C17A C17A O1 C17B 24.1(10) 2 . . 2 ? C18A C17A O1 Mg1 -28.7(13) . . . . ? C17A C17A O1 Mg1 180.0 2 . . . ? C18B C17B O1 C17A -28.5(12) . . . . ? C18B C17B O1 C17A -75.2(18) . . . 2 ? C18B C17B O1 C17B -58.2(14) . . . 2 ? C18B C17B O1 Mg1 121.8(14) . . . . ? N2 Mg1 O1 C17A 18.1(8) . . . . ? N2 Mg1 O1 C17A -161.9(8) 2 . . . ? N1 Mg1 O1 C17A -45.1(8) . . . . ? N1 Mg1 O1 C17A 134.9(8) 2 . . . ? C1 Mg1 O1 C17A 162.5(8) 2 . . . ? N2 Mg1 O1 C17A -161.9(8) . . . 2 ? N2 Mg1 O1 C17A 18.1(8) 2 . . 2 ? N1 Mg1 O1 C17A 134.9(8) . . . 2 ? N1 Mg1 O1 C17A -45.1(8) 2 . . 2 ? C1 Mg1 O1 C17A -17.5(8) 2 . . 2 ? N2 Mg1 O1 C17B -6.1(6) . . . . ? N2 Mg1 O1 C17B 173.9(6) 2 . . . ? N1 Mg1 O1 C17B -69.3(6) . . . . ? N1 Mg1 O1 C17B 110.7(6) 2 . . . ? C1 Mg1 O1 C17B 138.3(6) 2 . . . ? N2 Mg1 O1 C17B 173.9(6) . . . 2 ? N2 Mg1 O1 C17B -6.1(6) 2 . . 2 ? N1 Mg1 O1 C17B 110.7(6) . . . 2 ? N1 Mg1 O1 C17B -69.3(6) 2 . . 2 ? C1 Mg1 O1 C17B -41.7(6) 2 . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.268 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.049 data_s560b _database_code_depnum_ccdc_archive 'CCDC 865608' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H41 Li N4 Si' _chemical_formula_weight 396.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.240(3) _cell_length_b 12.316(4) _cell_length_c 20.617(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2600.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 234(2) _cell_measurement_reflns_used 5632 _cell_measurement_theta_min 2.2275 _cell_measurement_theta_max 21.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9698 _exptl_absorpt_correction_T_max 0.9797 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 234(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area scan' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18242 _diffrn_reflns_av_R_equivalents 0.1701 _diffrn_reflns_av_sigmaI/netI 0.1132 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4610 _reflns_number_gt 3344 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. These following restraints are used to restrict the atomic displacement parameters of carbon atoms and the bond distance between C17 and C18. OMIT -3 50.1 DFIX 1.54 0.02 C17 C18 SIMU 0.008 $C ; _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^)+(0.0819P)^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 SHELXL _refine_ls_extinction_coef 0.026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(2) _refine_ls_number_reflns 4610 _refine_ls_number_parameters 261 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.3065(4) 0.4996(5) 0.9004(2) 0.0459(10) Uani 1 1 d . . . N1 N 0.2923(2) 0.4922(3) 0.80493(10) 0.0487(6) Uani 1 1 d . . . N2 N 0.4851(2) 0.4960(2) 0.85958(10) 0.0447(6) Uani 1 1 d . . . N4 N 0.2509(3) 0.6380(2) 0.95352(14) 0.0604(8) Uani 1 1 d . . . N5 N 0.2045(4) 0.4096(3) 0.97049(16) 0.0769(10) Uani 1 1 d . . . Si1 Si 0.64833(7) 0.49413(8) 0.87529(4) 0.0479(3) Uani 1 1 d . . . C1 C 0.2138(3) 0.4981(3) 0.74573(13) 0.0499(7) Uani 1 1 d U . . H1 H 0.2728 0.5065 0.7080 0.060 Uiso 1 1 calc R . . C2 C 0.1378(5) 0.3925(3) 0.7386(2) 0.0791(11) Uani 1 1 d U . . H2A H 0.0816 0.3824 0.7766 0.095 Uiso 1 1 calc R . . H2B H 0.1990 0.3315 0.7368 0.095 Uiso 1 1 calc R . . C3 C 0.0538(5) 0.3932(5) 0.6772(2) 0.0999(15) Uani 1 1 d U . . H3A H 0.1105 0.3968 0.6390 0.120 Uiso 1 1 calc R . . H3B H 0.0035 0.3257 0.6748 0.120 Uiso 1 1 calc R . . C4 C -0.0371(4) 0.4872(5) 0.67674(19) 0.0913(13) Uani 1 1 d U . . H4A H -0.1014 0.4782 0.7115 0.110 Uiso 1 1 calc R . . H4B H -0.0844 0.4886 0.6354 0.110 Uiso 1 1 calc R . . C5 C 0.0333(5) 0.5941(5) 0.6858(2) 0.0946(14) Uani 1 1 d U . . H5A H -0.0309 0.6528 0.6896 0.114 Uiso 1 1 calc R . . H5B H 0.0876 0.6088 0.6477 0.114 Uiso 1 1 calc R . . C6 C 0.1202(4) 0.5921(3) 0.74725(18) 0.0745(11) Uani 1 1 d U . . H6A H 0.1695 0.6602 0.7501 0.089 Uiso 1 1 calc R . . H6B H 0.0648 0.5865 0.7858 0.089 Uiso 1 1 calc R . . C7 C 0.4191(2) 0.5050(3) 0.80354(12) 0.0383(6) Uani 1 1 d U . . C8 C 0.4904(3) 0.5341(2) 0.74209(13) 0.0380(7) Uani 1 1 d U . . C9 C 0.5110(4) 0.6431(3) 0.72657(16) 0.0575(9) Uani 1 1 d U . . H9 H 0.4784 0.6974 0.7542 0.069 Uiso 1 1 calc R . . C10 C 0.5785(4) 0.6726(3) 0.67122(18) 0.0678(10) Uani 1 1 d U . . H10 H 0.5911 0.7464 0.6616 0.081 Uiso 1 1 calc R . . C11 C 0.6273(3) 0.5944(3) 0.63024(16) 0.0613(9) Uani 1 1 d U . . H11 H 0.6744 0.6142 0.5930 0.074 Uiso 1 1 calc R . . C12 C 0.6060(3) 0.4867(3) 0.64456(15) 0.0595(9) Uani 1 1 d U . . H12 H 0.6377 0.4326 0.6165 0.071 Uiso 1 1 calc R . . C13 C 0.5389(3) 0.4574(3) 0.69965(15) 0.0499(8) Uani 1 1 d U . . H13 H 0.5257 0.3834 0.7086 0.060 Uiso 1 1 calc R . . C14 C 0.7426(4) 0.6183(4) 0.8512(2) 0.0867(14) Uani 1 1 d . . . H14A H 0.7515 0.6204 0.8044 0.130 Uiso 1 1 calc R . . H14B H 0.8285 0.6162 0.8710 0.130 Uiso 1 1 calc R . . H14C H 0.6964 0.6826 0.8658 0.130 Uiso 1 1 calc R . . C15 C 0.7357(4) 0.3755(4) 0.8387(2) 0.0738(12) Uani 1 1 d . . . H15A H 0.6920 0.3088 0.8512 0.111 Uiso 1 1 calc R . . H15B H 0.8252 0.3741 0.8540 0.111 Uiso 1 1 calc R . . H15C H 0.7350 0.3821 0.7918 0.111 Uiso 1 1 calc R . . C16 C 0.6658(4) 0.4815(3) 0.96557(16) 0.0728(11) Uani 1 1 d . . . H16A H 0.6268 0.5442 0.9864 0.109 Uiso 1 1 calc R . . H16B H 0.7577 0.4777 0.9768 0.109 Uiso 1 1 calc R . . H16C H 0.6221 0.4161 0.9802 0.109 Uiso 1 1 calc R . . C17 C 0.1743(9) 0.4904(5) 1.0199(4) 0.179(3) Uani 1 1 d DU . . H17A H 0.0882 0.4719 1.0374 0.215 Uiso 1 1 calc R . . H17B H 0.2372 0.4800 1.0552 0.215 Uiso 1 1 calc R . . C18 C 0.1722(8) 0.5976(4) 1.0066(3) 0.135(2) Uani 1 1 d DU . . H18A H 0.1991 0.6363 1.0459 0.161 Uiso 1 1 calc R . . H18B H 0.0814 0.6180 0.9979 0.161 Uiso 1 1 calc R . . C19 C 0.3648(5) 0.6952(4) 0.9787(3) 0.1034(17) Uani 1 1 d . . . H19A H 0.4171 0.7219 0.9428 0.155 Uiso 1 1 calc R . . H19B H 0.4167 0.6459 1.0048 0.155 Uiso 1 1 calc R . . H19C H 0.3365 0.7559 1.0052 0.155 Uiso 1 1 calc R . . C20 C 0.1747(5) 0.7132(4) 0.9138(2) 0.1023(17) Uani 1 1 d . . . H20A H 0.0952 0.6777 0.8995 0.153 Uiso 1 1 calc R . . H20B H 0.2257 0.7347 0.8763 0.153 Uiso 1 1 calc R . . H20C H 0.1528 0.7769 0.9392 0.153 Uiso 1 1 calc R . . C21 C 0.2936(8) 0.3343(5) 1.0039(3) 0.144(3) Uani 1 1 d . . . H21A H 0.3674 0.3743 1.0211 0.217 Uiso 1 1 calc R . . H21B H 0.3245 0.2800 0.9734 0.217 Uiso 1 1 calc R . . H21C H 0.2476 0.2988 1.0391 0.217 Uiso 1 1 calc R . . C22 C 0.1007(6) 0.3472(7) 0.9418(4) 0.155(3) Uani 1 1 d . . . H22A H 0.0620 0.3005 0.9744 0.232 Uiso 1 1 calc R . . H22B H 0.1355 0.3031 0.9069 0.232 Uiso 1 1 calc R . . H22C H 0.0347 0.3959 0.9247 0.232 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 Li1 0.045(2) 0.055(3) 0.038(2) 0.000(3) 0.0027(18) -0.003(3) N1 0.0400(12) 0.0726(17) 0.0336(11) -0.0004(14) -0.0005(9) -0.0082(16) N2 0.0411(12) 0.0557(14) 0.0374(12) 0.0035(13) -0.0010(9) -0.0018(13) N4 0.0693(19) 0.0547(17) 0.0573(17) -0.0069(14) -0.0050(15) 0.0042(15) N5 0.100(3) 0.0606(19) 0.070(2) 0.0007(18) 0.0343(19) -0.0096(19) Si1 0.0403(4) 0.0593(5) 0.0441(4) 0.0034(5) -0.0057(3) -0.0024(5) C1 0.0394(14) 0.0741(18) 0.0361(13) -0.0006(17) -0.0017(11) -0.0049(18) C2 0.091(3) 0.072(2) 0.074(2) -0.010(2) -0.034(2) -0.010(2) C3 0.102(3) 0.112(3) 0.085(3) -0.014(3) -0.047(2) -0.023(3) C4 0.0540(19) 0.154(4) 0.066(2) 0.000(3) -0.0204(16) -0.004(3) C5 0.097(3) 0.120(3) 0.067(2) -0.005(2) -0.029(2) 0.034(3) C6 0.086(3) 0.078(2) 0.059(2) -0.0048(19) -0.0209(19) 0.018(2) C7 0.0411(14) 0.0374(14) 0.0365(13) -0.0003(14) 0.0027(10) 0.0013(15) C8 0.0354(13) 0.0434(16) 0.0351(14) -0.0009(12) -0.0020(11) 0.0011(11) C9 0.079(2) 0.0435(18) 0.0500(18) -0.0012(15) 0.0120(17) -0.0029(16) C10 0.083(2) 0.059(2) 0.061(2) 0.0143(17) 0.0074(18) -0.0141(19) C11 0.060(2) 0.078(2) 0.0459(17) 0.0100(18) 0.0129(15) -0.0032(18) C12 0.0633(18) 0.069(2) 0.0456(15) -0.0062(17) 0.0107(13) 0.0154(18) C13 0.0546(18) 0.0468(16) 0.0482(17) 0.0021(14) 0.0051(15) 0.0072(14) C14 0.072(3) 0.088(3) 0.100(3) 0.017(3) -0.011(2) -0.029(2) C15 0.058(2) 0.088(3) 0.075(3) -0.005(2) -0.0119(18) 0.021(2) C16 0.064(2) 0.102(3) 0.0525(18) 0.003(2) -0.0166(15) 0.009(2) C17 0.265(7) 0.114(4) 0.159(5) -0.008(4) 0.158(5) -0.008(5) C18 0.213(6) 0.089(3) 0.102(3) -0.015(3) 0.088(4) 0.002(4) C19 0.107(4) 0.087(3) 0.117(4) -0.034(3) -0.031(3) -0.001(3) C20 0.120(4) 0.084(3) 0.103(3) -0.014(3) -0.036(3) 0.034(3) C21 0.226(8) 0.123(4) 0.084(4) 0.030(3) -0.034(5) -0.031(5) C22 0.101(4) 0.189(7) 0.174(7) 0.066(5) -0.026(4) -0.068(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N1 1.976(5) . ? Li1 N2 2.013(5) . ? Li1 N5 2.100(6) . ? Li1 N4 2.105(6) . ? N1 C7 1.309(3) . ? N1 C1 1.463(3) . ? N2 C7 1.343(3) . ? N2 Si1 1.703(2) . ? N4 C18 1.447(6) . ? N4 C19 1.458(5) . ? N4 C20 1.462(5) . ? N5 C22 1.439(7) . ? N5 C17 1.457(7) . ? N5 C21 1.473(7) . ? Si1 C15 1.873(4) . ? Si1 C14 1.876(4) . ? Si1 C16 1.877(3) . ? C1 C6 1.503(5) . ? C1 C2 1.523(5) . ? C1 H1 0.9900 . ? C2 C3 1.532(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.485(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.513(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.548(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.506(4) . ? C8 C13 1.381(4) . ? C8 C9 1.396(4) . ? C9 C10 1.383(5) . ? C9 H9 0.9400 . ? C10 C11 1.375(5) . ? C10 H10 0.9400 . ? C11 C12 1.376(5) . ? C11 H11 0.9400 . ? C12 C13 1.376(5) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.349(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Li1 N2 69.50(17) . . ? N1 Li1 N5 128.6(3) . . ? N2 Li1 N5 136.7(3) . . ? N1 Li1 N4 122.4(3) . . ? N2 Li1 N4 118.7(3) . . ? N5 Li1 N4 86.3(2) . . ? C7 N1 C1 121.4(2) . . ? C7 N1 Li1 86.7(2) . . ? C1 N1 Li1 150.4(2) . . ? C7 N2 Si1 131.20(19) . . ? C7 N2 Li1 84.30(19) . . ? Si1 N2 Li1 144.34(18) . . ? C18 N4 C19 110.0(4) . . ? C18 N4 C20 110.1(4) . . ? C19 N4 C20 108.7(3) . . ? C18 N4 Li1 105.4(3) . . ? C19 N4 Li1 111.1(3) . . ? C20 N4 Li1 111.4(3) . . ? C22 N5 C17 119.7(6) . . ? C22 N5 C21 108.2(5) . . ? C17 N5 C21 103.6(5) . . ? C22 N5 Li1 111.5(4) . . ? C17 N5 Li1 103.1(3) . . ? C21 N5 Li1 110.3(4) . . ? N2 Si1 C15 113.76(16) . . ? N2 Si1 C14 116.32(18) . . ? C15 Si1 C14 106.51(19) . . ? N2 Si1 C16 106.47(14) . . ? C15 Si1 C16 106.84(18) . . ? C14 Si1 C16 106.3(2) . . ? N1 C1 C6 111.8(3) . . ? N1 C1 C2 108.5(3) . . ? C6 C1 C2 109.5(3) . . ? N1 C1 H1 109.0 . . ? C6 C1 H1 109.0 . . ? C2 C1 H1 109.0 . . ? C1 C2 C3 111.2(3) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 111.2(4) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 112.3(3) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 111.2(4) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C1 C6 C5 111.2(3) . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N1 C7 N2 118.1(2) . . ? N1 C7 C8 121.9(2) . . ? N2 C7 C8 120.0(2) . . ? C13 C8 C9 117.3(3) . . ? C13 C8 C7 123.0(3) . . ? C9 C8 C7 119.7(3) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 121.6(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N5 122.0(5) . . ? C18 C17 H17A 106.8 . . ? N5 C17 H17A 106.8 . . ? C18 C17 H17B 106.8 . . ? N5 C17 H17B 106.8 . . ? H17A C17 H17B 106.7 . . ? C17 C18 N4 118.8(5) . . ? C17 C18 H18A 107.6 . . ? N4 C18 H18A 107.6 . . ? C17 C18 H18B 107.6 . . ? N4 C18 H18B 107.6 . . ? H18A C18 H18B 107.0 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 N2 Li1 N1 C7 -7.2(2) . . . . ? N5 Li1 N1 C7 -141.3(4) . . . . ? N4 Li1 N1 C7 104.6(3) . . . . ? N2 Li1 N1 C1 -169.8(6) . . . . ? N5 Li1 N1 C1 56.1(8) . . . . ? N4 Li1 N1 C1 -58.0(7) . . . . ? N1 Li1 N2 C7 7.0(2) . . . . ? N5 Li1 N2 C7 132.1(4) . . . . ? N4 Li1 N2 C7 -109.6(3) . . . . ? N1 Li1 N2 Si1 -178.0(4) . . . . ? N5 Li1 N2 Si1 -52.9(7) . . . . ? N4 Li1 N2 Si1 65.4(5) . . . . ? N1 Li1 N4 C18 132.9(4) . . . . ? N2 Li1 N4 C18 -144.3(4) . . . . ? N5 Li1 N4 C18 -1.5(4) . . . . ? N1 Li1 N4 C19 -108.0(4) . . . . ? N2 Li1 N4 C19 -25.2(4) . . . . ? N5 Li1 N4 C19 117.6(3) . . . . ? N1 Li1 N4 C20 13.4(4) . . . . ? N2 Li1 N4 C20 96.2(4) . . . . ? N5 Li1 N4 C20 -121.0(3) . . . . ? N1 Li1 N5 C22 -9.0(6) . . . . ? N2 Li1 N5 C22 -110.2(5) . . . . ? N4 Li1 N5 C22 120.5(4) . . . . ? N1 Li1 N5 C17 -138.7(6) . . . . ? N2 Li1 N5 C17 120.1(6) . . . . ? N4 Li1 N5 C17 -9.2(5) . . . . ? N1 Li1 N5 C21 111.3(5) . . . . ? N2 Li1 N5 C21 10.1(6) . . . . ? N4 Li1 N5 C21 -119.2(3) . . . . ? C7 N2 Si1 C15 -63.5(4) . . . . ? Li1 N2 Si1 C15 123.2(4) . . . . ? C7 N2 Si1 C14 60.9(4) . . . . ? Li1 N2 Si1 C14 -112.5(4) . . . . ? C7 N2 Si1 C16 179.1(3) . . . . ? Li1 N2 Si1 C16 5.8(5) . . . . ? C7 N1 C1 C6 -115.9(4) . . . . ? Li1 N1 C1 C6 43.6(7) . . . . ? C7 N1 C1 C2 123.2(4) . . . . ? Li1 N1 C1 C2 -77.3(7) . . . . ? N1 C1 C2 C3 -179.7(4) . . . . ? C6 C1 C2 C3 58.0(5) . . . . ? C1 C2 C3 C4 -56.9(6) . . . . ? C2 C3 C4 C5 54.4(5) . . . . ? C3 C4 C5 C6 -53.4(5) . . . . ? N1 C1 C6 C5 -177.2(3) . . . . ? C2 C1 C6 C5 -56.9(5) . . . . ? C4 C5 C6 C1 54.9(5) . . . . ? C1 N1 C7 N2 -178.5(3) . . . . ? Li1 N1 C7 N2 11.5(4) . . . . ? C1 N1 C7 C8 4.2(5) . . . . ? Li1 N1 C7 C8 -165.8(3) . . . . ? Si1 N2 C7 N1 172.6(3) . . . . ? Li1 N2 C7 N1 -11.3(4) . . . . ? Si1 N2 C7 C8 -10.1(5) . . . . ? Li1 N2 C7 C8 166.0(3) . . . . ? N1 C7 C8 C13 -90.0(4) . . . . ? N2 C7 C8 C13 92.8(4) . . . . ? N1 C7 C8 C9 90.8(4) . . . . ? N2 C7 C8 C9 -86.4(4) . . . . ? C13 C8 C9 C10 -0.7(5) . . . . ? C7 C8 C9 C10 178.6(3) . . . . ? C8 C9 C10 C11 -0.2(6) . . . . ? C9 C10 C11 C12 1.1(6) . . . . ? C10 C11 C12 C13 -1.1(5) . . . . ? C11 C12 C13 C8 0.2(5) . . . . ? C9 C8 C13 C12 0.7(5) . . . . ? C7 C8 C13 C12 -178.6(3) . . . . ? C22 N5 C17 C18 -103.0(9) . . . . ? C21 N5 C17 C18 136.4(9) . . . . ? Li1 N5 C17 C18 21.5(10) . . . . ? N5 C17 C18 N4 -26.2(14) . . . . ? C19 N4 C18 C17 -105.7(8) . . . . ? C20 N4 C18 C17 134.5(8) . . . . ? Li1 N4 C18 C17 14.2(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.572 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.053 data_s588b_33 _database_code_depnum_ccdc_archive 'CCDC 865609' #TrackingRef 'cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H74 Li2 N4 O3 Si2' _chemical_formula_weight 777.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 32.031(19) _cell_length_b 9.999(6) _cell_length_c 15.155(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4854(5) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 3349 _cell_measurement_theta_min 2.444 _cell_measurement_theta_max 28.413 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9673 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area scan' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24229 _diffrn_reflns_av_R_equivalents 0.1433 _diffrn_reflns_av_sigmaI/netI 0.1695 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7313 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+0.6000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(3) _refine_ls_number_reflns 7313 _refine_ls_number_parameters 498 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1664 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2462 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 0.0939(3) -0.0442(11) 0.1035(7) 0.048(3) Uani 1 1 d . A 4 Li2 Li 0.1338(3) 0.1065(13) 0.0048(8) 0.058(3) Uani 1 1 d . A 4 N1 N 0.14776(16) -0.1032(5) 0.0323(3) 0.0454(14) Uani 1 1 d . A 4 N2 N 0.13710(16) -0.0068(6) -0.1034(4) 0.0464(14) Uani 1 1 d . A 4 N3 N 0.09658(16) 0.0716(6) 0.2126(4) 0.0447(13) Uani 1 1 d . A 4 N4 N 0.07925(15) 0.1669(5) 0.0788(3) 0.0415(13) Uani 1 1 d . A 4 O1 O 0.04542(13) -0.1529(5) 0.0925(4) 0.0642(14) Uani 1 1 d . A 4 O2 O 0.18057(15) 0.2244(5) 0.0165(4) 0.0772(16) Uani 1 1 d U A 4 Si1 Si 0.13454(6) 0.0113(2) -0.21540(16) 0.0498(5) Uani 1 1 d . A 4 Si2 Si 0.04971(6) 0.2584(2) 0.00609(16) 0.0484(5) Uani 1 1 d . A 4 C1 C 0.15348(19) -0.1049(7) -0.0530(4) 0.0427(16) Uani 1 1 d . A 4 C2 C 0.1803(2) -0.2079(8) -0.0982(4) 0.0535(19) Uani 1 1 d . A 4 C3 C 0.1621(3) -0.3224(8) -0.1303(6) 0.070(2) Uani 1 1 d . A 4 H3 H 0.1334 -0.3381 -0.1233 0.084 Uiso 1 1 calc R A 4 C4 C 0.1878(5) -0.4153(10) -0.1740(7) 0.111(4) Uani 1 1 d . A 4 H4 H 0.1762 -0.4951 -0.1958 0.133 Uiso 1 1 calc R A 4 C5 C 0.2294(5) -0.3912(15) -0.1852(8) 0.117(4) Uani 1 1 d . A 4 H5 H 0.2459 -0.4534 -0.2158 0.141 Uiso 1 1 calc R A 4 C6 C 0.2466(4) -0.2815(14) -0.1534(8) 0.109(4) Uani 1 1 d . A 4 H6 H 0.2753 -0.2655 -0.1613 0.130 Uiso 1 1 calc R A 4 C7 C 0.2225(2) -0.1914(10) -0.1089(6) 0.075(3) Uani 1 1 d . A 4 H7 H 0.2353 -0.1152 -0.0847 0.090 Uiso 1 1 calc R A 4 C8 C 0.17227(18) -0.1977(7) 0.0870(4) 0.0441(16) Uani 1 1 d . A 4 H8 H 0.1826 -0.2700 0.0481 0.053 Uiso 1 1 calc R A 4 C9 C 0.1461(2) -0.2606(8) 0.1582(5) 0.064(2) Uani 1 1 d . A 4 H9A H 0.1235 -0.3117 0.1306 0.076 Uiso 1 1 calc R A 4 H9B H 0.1333 -0.1895 0.1936 0.076 Uiso 1 1 calc R A 4 C10 C 0.1707(3) -0.3538(8) 0.2198(5) 0.068(2) Uani 1 1 d . A 4 H10A H 0.1527 -0.3828 0.2684 0.082 Uiso 1 1 calc R A 4 H10B H 0.1795 -0.4335 0.1870 0.082 Uiso 1 1 calc R A 4 C11 C 0.2090(3) -0.2841(9) 0.2572(6) 0.074(2) Uani 1 1 d . A 4 H11A H 0.2257 -0.3486 0.2907 0.089 Uiso 1 1 calc R A 4 H11B H 0.2002 -0.2131 0.2977 0.089 Uiso 1 1 calc R A 4 C12 C 0.2355(3) -0.2242(9) 0.1837(6) 0.079(3) Uani 1 1 d . A 4 H12A H 0.2464 -0.2962 0.1463 0.094 Uiso 1 1 calc R A 4 H12B H 0.2593 -0.1766 0.2095 0.094 Uiso 1 1 calc R A 4 C13 C 0.2099(2) -0.1274(8) 0.1272(5) 0.060(2) Uani 1 1 d . A 4 H13A H 0.2004 -0.0525 0.1637 0.072 Uiso 1 1 calc R A 4 H13B H 0.2275 -0.0913 0.0800 0.072 Uiso 1 1 calc R A 4 C14 C 0.1823(2) -0.0351(10) -0.2805(5) 0.079(3) Uani 1 1 d . A 4 H14A H 0.2070 -0.0032 -0.2501 0.118 Uiso 1 1 calc R A 4 H14B H 0.1809 0.0056 -0.3386 0.118 Uiso 1 1 calc R A 4 H14C H 0.1837 -0.1315 -0.2866 0.118 Uiso 1 1 calc R A 4 C15 C 0.1259(3) 0.1918(9) -0.2395(6) 0.079(2) Uani 1 1 d . A 4 H15A H 0.1037 0.2258 -0.2022 0.119 Uiso 1 1 calc R A 4 H15B H 0.1181 0.2025 -0.3010 0.119 Uiso 1 1 calc R A 4 H15C H 0.1514 0.2412 -0.2280 0.119 Uiso 1 1 calc R A 4 C16 C 0.0902(2) -0.0868(10) -0.2629(5) 0.077(3) Uani 1 1 d . A 4 H16A H 0.0960 -0.1816 -0.2571 0.116 Uiso 1 1 calc R A 4 H16B H 0.0870 -0.0644 -0.3248 0.116 Uiso 1 1 calc R A 4 H16C H 0.0647 -0.0652 -0.2314 0.116 Uiso 1 1 calc R A 4 C17 C 0.07944(18) 0.1711(7) 0.1676(4) 0.0396(15) Uani 1 1 d . A 4 C18 C 0.05806(19) 0.2870(7) 0.2138(4) 0.0404(16) Uani 1 1 d . A 4 C19 C 0.0191(2) 0.2718(8) 0.2541(5) 0.0543(19) Uani 1 1 d . A 4 H19 H 0.0067 0.1866 0.2560 0.065 Uiso 1 1 calc R A 4 C20 C -0.0013(2) 0.3778(9) 0.2909(5) 0.066(2) Uani 1 1 d . A 4 H20 H -0.0275 0.3648 0.3176 0.079 Uiso 1 1 calc R A 4 C21 C 0.0162(3) 0.5035(10) 0.2893(6) 0.071(2) Uani 1 1 d . A 4 H21 H 0.0016 0.5772 0.3126 0.085 Uiso 1 1 calc R A 4 C22 C 0.0547(3) 0.5195(8) 0.2533(6) 0.076(3) Uani 1 1 d . A 4 H22 H 0.0676 0.6039 0.2549 0.091 Uiso 1 1 calc R A 4 C23 C 0.0756(2) 0.4114(8) 0.2137(5) 0.0557(19) Uani 1 1 d . A 4 H23 H 0.1017 0.4249 0.1871 0.067 Uiso 1 1 calc R A 4 C24 C 0.0995(2) 0.0737(7) 0.3091(4) 0.0489(18) Uani 1 1 d . A 4 H24 H 0.0827 0.1490 0.3322 0.059 Uiso 1 1 calc R A 4 C25 C 0.0822(3) -0.0564(10) 0.3446(5) 0.077(3) Uani 1 1 d . A 4 H25A H 0.0961 -0.1312 0.3149 0.092 Uiso 1 1 calc R A 4 H25B H 0.0523 -0.0614 0.3306 0.092 Uiso 1 1 calc R A 4 C26 C 0.0879(3) -0.0712(12) 0.4455(5) 0.088(3) Uani 1 1 d . A 4 H26A H 0.0717 -0.0024 0.4762 0.105 Uiso 1 1 calc R A 4 H26B H 0.0778 -0.1590 0.4646 0.105 Uiso 1 1 calc R A 4 C27 C 0.1329(3) -0.0570(11) 0.4682(6) 0.088(3) Uani 1 1 d . A 4 H27A H 0.1487 -0.1301 0.4409 0.105 Uiso 1 1 calc R A 4 H27B H 0.1363 -0.0641 0.5323 0.105 Uiso 1 1 calc R A 4 C28 C 0.1503(3) 0.0738(13) 0.4376(6) 0.103(4) Uani 1 1 d . A 4 H28A H 0.1802 0.0778 0.4513 0.124 Uiso 1 1 calc R A 4 H28B H 0.1364 0.1470 0.4690 0.124 Uiso 1 1 calc R A 4 C29 C 0.1439(2) 0.0914(10) 0.3371(5) 0.076(3) Uani 1 1 d . A 4 H29A H 0.1533 0.1809 0.3198 0.091 Uiso 1 1 calc R A 4 H29B H 0.1613 0.0261 0.3058 0.091 Uiso 1 1 calc R A 4 C30 C 0.0339(2) 0.1401(8) -0.0832(5) 0.061(2) Uani 1 1 d . A 4 H30A H 0.0585 0.0952 -0.1062 0.092 Uiso 1 1 calc R A 4 H30B H 0.0204 0.1893 -0.1303 0.092 Uiso 1 1 calc R A 4 H30C H 0.0147 0.0742 -0.0595 0.092 Uiso 1 1 calc R A 4 C31 C 0.0823(3) 0.3969(8) -0.0425(6) 0.072(2) Uani 1 1 d . A 4 H31A H 0.0909 0.4576 0.0040 0.108 Uiso 1 1 calc R A 4 H31B H 0.0659 0.4454 -0.0859 0.108 Uiso 1 1 calc R A 4 H31C H 0.1068 0.3591 -0.0707 0.108 Uiso 1 1 calc R A 4 C32 C -0.0001(3) 0.3356(10) 0.0461(6) 0.079(3) Uani 1 1 d . A 4 H32A H -0.0168 0.2681 0.0754 0.119 Uiso 1 1 calc R A 4 H32B H -0.0155 0.3715 -0.0037 0.119 Uiso 1 1 calc R A 4 H32C H 0.0063 0.4070 0.0873 0.119 Uiso 1 1 calc R A 4 C33 C 0.0372(3) -0.2405(9) 0.0200(7) 0.082(3) Uani 1 1 d . A 4 H33A H 0.0509 -0.3269 0.0302 0.099 Uiso 1 1 calc R A 4 H33B H 0.0486 -0.2021 -0.0344 0.099 Uiso 1 1 calc R A 4 C34 C -0.0076(3) -0.2596(11) 0.0111(7) 0.095(3) Uani 1 1 d . A 4 H34A H -0.0143 -0.3526 -0.0035 0.114 Uiso 1 1 calc R A 4 H34B H -0.0192 -0.2009 -0.0346 0.114 Uiso 1 1 calc R A 4 C35 C -0.0243(3) -0.2221(11) 0.1026(6) 0.091(3) Uani 1 1 d . A 4 H35A H -0.0522 -0.1821 0.0988 0.110 Uiso 1 1 calc R A 4 H35B H -0.0254 -0.3001 0.1417 0.110 Uiso 1 1 calc R A 4 C36 C 0.0069(2) -0.1236(10) 0.1334(6) 0.078(3) Uani 1 1 d . A 4 H36A H -0.0020 -0.0329 0.1180 0.094 Uiso 1 1 calc R A 4 H36B H 0.0098 -0.1289 0.1977 0.094 Uiso 1 1 calc R A 4 C37 C 0.2162(3) 0.2262(12) -0.0368(7) 0.105(3) Uani 1 1 d U A 4 H37A H 0.2089 0.2581 -0.0960 0.126 Uiso 1 1 calc R A 4 H37B H 0.2275 0.1355 -0.0423 0.126 Uiso 1 1 calc R A 4 C38 C 0.2465(3) 0.3112(14) 0.0007(10) 0.141(3) Uani 1 1 d U A 4 H38A H 0.2721 0.2610 0.0140 0.169 Uiso 1 1 calc R A 4 H38B H 0.2534 0.3840 -0.0400 0.169 Uiso 1 1 calc R A 4 C39 C 0.2293(4) 0.3616(16) 0.0773(10) 0.157(4) Uani 1 1 d U A 4 H39A H 0.2284 0.4594 0.0741 0.188 Uiso 1 1 calc R A 4 H39B H 0.2467 0.3365 0.1278 0.188 Uiso 1 1 calc R A 4 C40 C 0.1870(3) 0.3098(14) 0.0903(9) 0.126(3) Uani 1 1 d U A 4 H40A H 0.1849 0.2597 0.1458 0.152 Uiso 1 1 calc R A 4 H40B H 0.1665 0.3826 0.0910 0.152 Uiso 1 1 calc R A 4 O3 O 0.3162(7) 0.056(4) 0.018(3) 0.210(13) Uiso 0.49(3) 1 d PD B 1 C41 C 0.3416(10) 0.088(4) 0.088(3) 0.207(19) Uiso 0.49(3) 1 d PD B 1 H41A H 0.3322 0.0452 0.1423 0.249 Uiso 0.49(3) 1 calc PR B 1 H41B H 0.3430 0.1853 0.0969 0.249 Uiso 0.49(3) 1 calc PR B 1 C42 C 0.3827(9) 0.033(5) 0.057(2) 0.183(16) Uiso 0.49(3) 1 d PD B 1 H42A H 0.4054 0.0926 0.0754 0.220 Uiso 0.49(3) 1 calc PR B 1 H42B H 0.3874 -0.0550 0.0838 0.220 Uiso 0.49(3) 1 calc PR B 1 C43 C 0.3821(9) 0.021(4) -0.041(2) 0.161(14) Uiso 0.49(3) 1 d PD B 1 H43A H 0.3939 0.0994 -0.0711 0.193 Uiso 0.49(3) 1 calc PR B 1 H43B H 0.3957 -0.0608 -0.0625 0.193 Uiso 0.49(3) 1 calc PR B 1 C44 C 0.3357(10) 0.015(5) -0.047(2) 0.194(18) Uiso 0.49(3) 1 d PD B 1 H44A H 0.3269 0.0661 -0.0991 0.233 Uiso 0.49(3) 1 calc PR B 1 H44B H 0.3276 -0.0787 -0.0576 0.233 Uiso 0.49(3) 1 calc PR B 1 O3' O 0.3183(8) -0.050(4) 0.001(3) 0.230(14) Uiso 0.51(3) 1 d PD B 2 C41' C 0.3522(11) -0.041(4) -0.055(2) 0.181(16) Uiso 0.51(3) 1 d PD B 2 H41C H 0.3519 0.0428 -0.0886 0.217 Uiso 0.51(3) 1 calc PR B 2 H41D H 0.3537 -0.1168 -0.0954 0.217 Uiso 0.51(3) 1 calc PR B 2 C42' C 0.3873(8) -0.043(3) 0.011(2) 0.157(12) Uiso 0.51(3) 1 d PD B 2 H42C H 0.3966 -0.1352 0.0214 0.188 Uiso 0.51(3) 1 calc PR B 2 H42D H 0.4111 0.0089 -0.0107 0.188 Uiso 0.51(3) 1 calc PR B 2 C43' C 0.3715(10) 0.016(4) 0.096(2) 0.198(18) Uiso 0.51(3) 1 d PD B 2 H43C H 0.3842 -0.0239 0.1487 0.237 Uiso 0.51(3) 1 calc PR B 2 H43D H 0.3741 0.1141 0.0981 0.237 Uiso 0.51(3) 1 calc PR B 2 C44' C 0.3281(9) -0.030(4) 0.080(2) 0.178(16) Uiso 0.51(3) 1 d PD B 2 H44C H 0.3237 -0.1134 0.1124 0.214 Uiso 0.51(3) 1 calc PR B 2 H44D H 0.3088 0.0366 0.1040 0.214 Uiso 0.51(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.051(6) 0.044(7) 0.048(7) -0.001(5) -0.003(5) 0.010(5) Li2 0.048(6) 0.079(9) 0.047(7) 0.006(7) 0.006(6) 0.002(6) N1 0.051(3) 0.051(4) 0.034(3) -0.002(3) 0.004(2) 0.007(3) N2 0.047(3) 0.057(4) 0.035(3) -0.002(3) -0.002(2) 0.008(3) N3 0.054(3) 0.050(4) 0.030(3) -0.011(3) -0.001(2) 0.008(3) N4 0.042(3) 0.053(4) 0.030(3) 0.000(3) 0.000(2) 0.008(3) O1 0.049(3) 0.073(4) 0.070(3) -0.026(3) 0.007(2) -0.008(2) O2 0.057(3) 0.091(4) 0.084(4) -0.043(3) 0.015(3) -0.023(3) Si1 0.0511(11) 0.0626(14) 0.0356(9) -0.0040(9) 0.0001(9) 0.0001(10) Si2 0.0484(10) 0.0550(13) 0.0418(9) -0.0007(10) -0.0044(9) 0.0102(9) C1 0.038(4) 0.051(5) 0.039(4) -0.009(3) 0.003(3) 0.000(3) C2 0.066(5) 0.055(5) 0.039(4) -0.008(4) 0.003(3) 0.009(4) C3 0.092(6) 0.056(6) 0.062(5) -0.015(4) 0.003(4) 0.003(5) C4 0.204(14) 0.057(6) 0.071(7) -0.020(5) 0.006(8) 0.020(8) C5 0.139(11) 0.126(12) 0.087(8) -0.013(8) 0.032(8) 0.054(10) C6 0.094(8) 0.132(11) 0.100(9) -0.008(8) 0.029(7) 0.060(8) C7 0.055(5) 0.105(8) 0.065(5) -0.010(5) 0.014(4) 0.021(5) C8 0.044(4) 0.048(4) 0.040(4) -0.010(3) 0.004(3) 0.006(3) C9 0.060(5) 0.076(6) 0.055(4) 0.015(4) -0.008(4) 0.003(4) C10 0.080(6) 0.074(6) 0.051(5) 0.011(4) -0.005(4) 0.004(4) C11 0.090(6) 0.076(6) 0.058(5) -0.007(5) -0.019(4) 0.027(5) C12 0.072(6) 0.087(7) 0.076(6) 0.001(5) -0.026(5) 0.001(5) C13 0.052(4) 0.062(5) 0.067(5) 0.005(4) -0.012(4) -0.004(4) C14 0.065(5) 0.124(8) 0.047(5) 0.009(5) 0.004(4) -0.007(5) C15 0.111(7) 0.073(6) 0.054(5) 0.011(4) -0.001(5) -0.001(5) C16 0.070(5) 0.107(8) 0.055(5) -0.015(5) -0.002(4) -0.006(5) C17 0.034(3) 0.050(4) 0.035(4) -0.009(3) 0.004(3) -0.005(3) C18 0.044(4) 0.041(5) 0.037(3) -0.007(3) 0.002(3) 0.003(3) C19 0.056(4) 0.050(5) 0.057(4) -0.007(4) 0.016(3) 0.006(4) C20 0.071(5) 0.074(6) 0.053(5) -0.008(4) 0.024(4) 0.013(5) C21 0.087(6) 0.069(6) 0.057(5) -0.016(4) 0.013(5) 0.022(5) C22 0.098(7) 0.039(5) 0.090(7) -0.013(4) 0.010(5) -0.001(5) C23 0.060(4) 0.052(5) 0.055(4) -0.014(4) 0.007(4) -0.003(4) C24 0.052(4) 0.059(5) 0.035(4) -0.007(3) 0.002(3) 0.013(4) C25 0.072(5) 0.115(8) 0.042(4) 0.015(5) 0.004(4) -0.017(5) C26 0.087(7) 0.135(9) 0.042(5) 0.027(5) 0.013(4) 0.009(6) C27 0.088(7) 0.127(9) 0.048(5) 0.029(5) -0.011(4) -0.008(6) C28 0.095(7) 0.152(11) 0.062(6) -0.002(7) -0.023(5) -0.024(7) C29 0.066(5) 0.112(7) 0.049(5) 0.003(5) -0.014(4) -0.029(5) C30 0.064(5) 0.070(6) 0.049(4) -0.005(4) -0.010(3) 0.011(4) C31 0.094(6) 0.053(5) 0.070(6) 0.021(4) -0.016(4) -0.003(5) C32 0.068(5) 0.115(7) 0.055(5) -0.003(5) -0.010(4) 0.032(5) C33 0.077(6) 0.078(6) 0.093(7) -0.049(6) 0.009(5) -0.013(5) C34 0.086(6) 0.112(7) 0.088(7) -0.034(6) -0.009(6) -0.018(6) C35 0.071(6) 0.129(9) 0.073(6) -0.001(6) 0.000(5) -0.029(6) C36 0.052(5) 0.103(8) 0.080(6) -0.022(5) 0.012(4) -0.007(5) C37 0.074(5) 0.132(7) 0.109(6) -0.044(5) 0.029(5) -0.036(5) C38 0.083(6) 0.189(8) 0.151(8) -0.060(7) 0.019(6) -0.031(6) C39 0.094(6) 0.211(8) 0.165(8) -0.097(7) 0.008(6) -0.037(6) C40 0.095(6) 0.165(7) 0.120(7) -0.079(6) 0.015(5) -0.035(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1 1.904(12) . ? Li1 N3 2.021(12) . ? Li1 N1 2.118(12) . ? Li1 N4 2.194(12) . ? Li1 C17 2.407(13) . ? Li1 Li2 2.477(16) . ? Li2 O2 1.915(13) . ? Li2 N2 1.996(14) . ? Li2 N4 2.162(12) . ? Li2 N1 2.184(14) . ? Li2 C1 2.374(14) . ? Li2 Si2 3.092(11) . ? N1 C1 1.306(8) . ? N1 C8 1.482(8) . ? N2 C1 1.349(9) . ? N2 Si1 1.709(6) . ? N3 C17 1.325(8) . ? N3 C24 1.465(8) . ? N4 C17 1.346(8) . ? N4 Si2 1.717(5) . ? O1 C36 1.411(8) . ? O1 C33 1.429(9) . ? O2 C37 1.399(10) . ? O2 C40 1.422(11) . ? Si1 C15 1.862(9) . ? Si1 C16 1.869(8) . ? Si1 C14 1.879(8) . ? Si2 C30 1.868(8) . ? Si2 C32 1.873(8) . ? Si2 C31 1.884(8) . ? C1 C2 1.507(9) . ? C2 C7 1.369(10) . ? C2 C3 1.374(11) . ? C3 C4 1.408(13) . ? C3 H3 0.9400 . ? C4 C5 1.363(17) . ? C4 H4 0.9400 . ? C5 C6 1.319(16) . ? C5 H5 0.9400 . ? C6 C7 1.365(12) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.505(10) . ? C8 C13 1.522(9) . ? C8 H8 0.9900 . ? C9 C10 1.538(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.520(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.523(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.530(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.517(9) . ? C18 C23 1.364(9) . ? C18 C19 1.399(9) . ? C19 C20 1.364(10) . ? C19 H19 0.9400 . ? C20 C21 1.377(11) . ? C20 H20 0.9400 . ? C21 C22 1.360(11) . ? C21 H21 0.9400 . ? C22 C23 1.405(10) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C29 1.494(10) . ? C24 C25 1.514(11) . ? C24 H24 0.9900 . ? C25 C26 1.547(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.489(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.496(14) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.548(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.455(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.534(13) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C36 1.479(11) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.410(13) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.381(16) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.464(14) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? O3 C44 1.24(3) . ? O3 C41 1.37(3) . ? C41 C42 1.502(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.498(10) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.490(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? O3' C44' 1.25(3) . ? O3' C41' 1.38(3) . ? C41' C42' 1.508(14) . ? C41' H41C 0.9800 . ? C41' H41D 0.9800 . ? C42' C43' 1.501(14) . ? C42' H42C 0.9800 . ? C42' H42D 0.9800 . ? C43' C44' 1.489(14) . ? C43' H43C 0.9800 . ? C43' H43D 0.9800 . ? C44' H44C 0.9800 . ? C44' H44D 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 Li1 N3 115.7(6) . . ? O1 Li1 N1 117.5(6) . . ? N3 Li1 N1 122.8(6) . . ? O1 Li1 N4 111.1(5) . . ? N3 Li1 N4 66.2(4) . . ? N1 Li1 N4 110.8(5) . . ? O1 Li1 C17 112.9(5) . . ? N3 Li1 C17 33.4(3) . . ? N1 Li1 C17 127.7(6) . . ? N4 Li1 C17 33.6(3) . . ? O1 Li1 Li2 135.7(6) . . ? N3 Li1 Li2 97.1(6) . . ? N1 Li1 Li2 56.1(4) . . ? N4 Li1 Li2 54.7(4) . . ? C17 Li1 Li2 78.4(5) . . ? O2 Li2 N2 112.6(6) . . ? O2 Li2 N4 114.4(6) . . ? N2 Li2 N4 128.9(6) . . ? O2 Li2 N1 114.4(6) . . ? N2 Li2 N1 66.5(4) . . ? N4 Li2 N1 109.6(5) . . ? O2 Li2 C1 112.0(5) . . ? N2 Li2 C1 34.6(3) . . ? N4 Li2 C1 130.9(6) . . ? N1 Li2 C1 33.0(3) . . ? O2 Li2 Li1 136.2(7) . . ? N2 Li2 Li1 100.2(6) . . ? N4 Li2 Li1 56.0(4) . . ? N1 Li2 Li1 53.6(4) . . ? C1 Li2 Li1 79.5(5) . . ? O2 Li2 Si2 112.2(5) . . ? N2 Li2 Si2 109.3(5) . . ? N4 Li2 Si2 32.4(2) . . ? N1 Li2 Si2 130.5(5) . . ? C1 Li2 Si2 132.2(5) . . ? Li1 Li2 Si2 81.2(4) . . ? C1 N1 C8 118.1(6) . . ? C1 N1 Li1 128.4(5) . . ? C8 N1 Li1 108.9(5) . . ? C1 N1 Li2 81.5(5) . . ? C8 N1 Li2 145.9(5) . . ? Li1 N1 Li2 70.3(4) . . ? C1 N2 Si1 131.1(5) . . ? C1 N2 Li2 88.2(5) . . ? Si1 N2 Li2 138.9(5) . . ? C17 N3 C24 122.0(5) . . ? C17 N3 Li1 89.5(5) . . ? C24 N3 Li1 145.8(6) . . ? C17 N4 Si2 128.8(5) . . ? C17 N4 Li2 121.6(5) . . ? Si2 N4 Li2 105.1(4) . . ? C17 N4 Li1 81.9(5) . . ? Si2 N4 Li1 137.7(4) . . ? Li2 N4 Li1 69.3(5) . . ? C36 O1 C33 107.8(5) . . ? C36 O1 Li1 123.8(6) . . ? C33 O1 Li1 124.5(6) . . ? C37 O2 C40 109.2(7) . . ? C37 O2 Li2 126.4(6) . . ? C40 O2 Li2 123.7(7) . . ? N2 Si1 C15 107.8(3) . . ? N2 Si1 C16 111.3(3) . . ? C15 Si1 C16 108.7(4) . . ? N2 Si1 C14 117.2(3) . . ? C15 Si1 C14 104.9(4) . . ? C16 Si1 C14 106.7(4) . . ? N4 Si2 C30 106.0(3) . . ? N4 Si2 C32 118.8(3) . . ? C30 Si2 C32 105.4(4) . . ? N4 Si2 C31 109.7(3) . . ? C30 Si2 C31 109.4(4) . . ? C32 Si2 C31 107.2(4) . . ? N4 Si2 Li2 42.4(3) . . ? C30 Si2 Li2 85.4(3) . . ? C32 Si2 Li2 161.1(3) . . ? C31 Si2 Li2 82.9(3) . . ? N1 C1 N2 119.7(6) . . ? N1 C1 C2 122.6(6) . . ? N2 C1 C2 117.5(6) . . ? N1 C1 Li2 65.5(5) . . ? N2 C1 Li2 57.2(4) . . ? C2 C1 Li2 158.2(6) . . ? C7 C2 C3 118.5(7) . . ? C7 C2 C1 122.3(7) . . ? C3 C2 C1 119.2(7) . . ? C2 C3 C4 117.9(9) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 120.9(11) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.7(11) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 119.5(12) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 122.5(10) . . ? C6 C7 H7 118.8 . . ? C2 C7 H7 118.8 . . ? N1 C8 C9 111.8(5) . . ? N1 C8 C13 110.4(6) . . ? C9 C8 C13 110.3(6) . . ? N1 C8 H8 108.1 . . ? C9 C8 H8 108.1 . . ? C13 C8 H8 108.1 . . ? C8 C9 C10 113.7(6) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 111.3(7) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.9(7) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 111.1(7) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 110.8(6) . . ? C8 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N3 C17 N4 119.5(6) . . ? N3 C17 C18 121.5(5) . . ? N4 C17 C18 118.9(6) . . ? N3 C17 Li1 57.1(4) . . ? N4 C17 Li1 64.5(4) . . ? C18 C17 Li1 163.0(5) . . ? C23 C18 C19 117.8(6) . . ? C23 C18 C17 120.7(6) . . ? C19 C18 C17 121.4(6) . . ? C20 C19 C18 121.4(7) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 120.5(7) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 118.9(8) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 120.8(8) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C18 C23 C22 120.4(7) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? N3 C24 C29 110.2(6) . . ? N3 C24 C25 108.6(6) . . ? C29 C24 C25 110.5(6) . . ? N3 C24 H24 109.2 . . ? C29 C24 H24 109.2 . . ? C25 C24 H24 109.2 . . ? C24 C25 C26 112.9(7) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 109.6(7) . . ? C27 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? C27 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C26 C27 C28 111.8(8) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 110.8(8) . . ? C27 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C24 C29 C28 113.1(7) . . ? C24 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C24 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O1 C33 C34 109.4(7) . . ? O1 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O1 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C35 103.2(7) . . ? C33 C34 H34A 111.1 . . ? C35 C34 H34A 111.1 . . ? C33 C34 H34B 111.1 . . ? C35 C34 H34B 111.1 . . ? H34A C34 H34B 109.1 . . ? C36 C35 C34 102.3(7) . . ? C36 C35 H35A 111.3 . . ? C34 C35 H35A 111.3 . . ? C36 C35 H35B 111.3 . . ? C34 C35 H35B 111.3 . . ? H35A C35 H35B 109.2 . . ? O1 C36 C35 108.3(7) . . ? O1 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O1 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O2 C37 C38 109.6(9) . . ? O2 C37 H37A 109.7 . . ? C38 C37 H37A 109.7 . . ? O2 C37 H37B 109.7 . . ? C38 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C39 C38 C37 106.5(10) . . ? C39 C38 H38A 110.4 . . ? C37 C38 H38A 110.4 . . ? C39 C38 H38B 110.4 . . ? C37 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? C38 C39 C40 110.8(10) . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? O2 C40 C39 103.9(9) . . ? O2 C40 H40A 111.0 . . ? C39 C40 H40A 111.0 . . ? O2 C40 H40B 111.0 . . ? C39 C40 H40B 111.0 . . ? H40A C40 H40B 109.0 . . ? C44 O3 C41 113(2) . . ? O3 C41 C42 101(2) . . ? O3 C41 H41A 111.5 . . ? C42 C41 H41A 111.5 . . ? O3 C41 H41B 111.5 . . ? C42 C41 H41B 111.5 . . ? H41A C41 H41B 109.3 . . ? C43 C42 C41 109(2) . . ? C43 C42 H42A 109.9 . . ? C41 C42 H42A 109.8 . . ? C43 C42 H42B 109.9 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C44 C43 C42 94(2) . . ? C44 C43 H43A 112.9 . . ? C42 C43 H43A 112.9 . . ? C44 C43 H43B 112.9 . . ? C42 C43 H43B 112.8 . . ? H43A C43 H43B 110.3 . . ? O3 C44 C43 116(3) . . ? O3 C44 H44A 108.3 . . ? C43 C44 H44A 108.3 . . ? O3 C44 H44B 108.3 . . ? C43 C44 H44B 108.3 . . ? H44A C44 H44B 107.4 . . ? C44' O3' C41' 112(2) . . ? O3' C41' C42' 100(2) . . ? O3' C41' H41C 111.7 . . ? C42' C41' H41C 111.7 . . ? O3' C41' H41D 111.7 . . ? C42' C41' H41D 111.7 . . ? H41C C41' H41D 109.4 . . ? C43' C42' C41' 108(2) . . ? C43' C42' H42C 110.1 . . ? C41' C42' H42C 110.1 . . ? C43' C42' H42D 110.1 . . ? C41' C42' H42D 110.1 . . ? H42C C42' H42D 108.4 . . ? C44' C43' C42' 93(2) . . ? C44' C43' H43C 113.1 . . ? C42' C43' H43C 113.2 . . ? C44' C43' H43D 113.1 . . ? C42' C43' H43D 113.1 . . ? H43C C43' H43D 110.5 . . ? O3' C44' C43' 116(3) . . ? O3' C44' H44C 108.2 . . ? C43' C44' H44C 108.2 . . ? O3' C44' H44D 108.2 . . ? C43' C44' H44D 108.2 . . ? H44C C44' H44D 107.3 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.268 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.060