data_mo_dm15131_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Cl3 Li N6 O4 Sc' _chemical_formula_weight 744.05 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'trigonal' _symmetry_space_group_name_H-M 'R 3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 12.5688(12) _cell_length_b 12.5688(12) _cell_length_c 43.147(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5903.0(10) _cell_formula_units_Z 6 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4399 _cell_measurement_theta_min 2.659 _cell_measurement_theta_max 22.982 _exptl_crystal_description block _exptl_crystal_colour brown _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 1.256 _exptl_crystal_density_method ? _exptl_crystal_F_000 2364 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8998 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18932 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.74 _reflns_number_total 3524 _reflns_number_gt 2870 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1306P)^2^+0.4888P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(6) _refine_ls_number_reflns 3524 _refine_ls_number_parameters 162 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.133 _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 Sc1 Sc 0.3333 0.6667 0.08003(3) 0.0334(2) Uani 1 3 d S . . Cl1 Cl 0.51782(9) 0.81197(8) 0.10777(3) 0.0499(3) Uani 1 1 d . . . N1 N 0.1875(2) 0.5499(2) 0.04418(7) 0.0349(5) Uani 1 1 d . . . N2 N 0.2150(2) 0.5718(2) 0.01316(7) 0.0323(5) Uani 1 1 d . . . C6 C 0.0079(4) 0.4039(4) 0.07598(13) 0.0627(12) Uani 1 1 d . . . H6A H 0.0176 0.3336 0.0814 0.094 Uiso 1 1 calc R . . H6B H -0.0797 0.3769 0.0741 0.094 Uiso 1 1 calc R . . H6C H 0.0445 0.4666 0.0922 0.094 Uiso 1 1 calc R . . C4 C 0.0711(3) 0.4571(3) 0.04567(11) 0.0446(8) Uani 1 1 d . . . C3 C 0.0249(3) 0.4200(3) 0.01560(11) 0.0487(9) Uani 1 1 d . . . H3 H -0.0550 0.3561 0.0101 0.058 Uiso 1 1 calc R . . C2 C 0.1184(3) 0.4947(3) -0.00457(10) 0.0402(7) Uani 1 1 d . . . C5 C 0.1221(4) 0.4985(4) -0.03896(12) 0.0518(9) Uani 1 1 d . . . H5A H 0.1110 0.5661 -0.0463 0.078 Uiso 1 1 calc R . . H5B H 0.0561 0.4206 -0.0472 0.078 Uiso 1 1 calc R . . H5C H 0.2016 0.5111 -0.0461 0.078 Uiso 1 1 calc R . . C1 C 0.3333 0.6667 0.00222(13) 0.0288(9) Uani 1 3 d S . . O1 O 0.3507(4) 0.8176(4) 0.20874(10) 0.0679(9) Uani 1 1 d U . . C7 C 0.3982(6) 0.8627(5) 0.17868(17) 0.0729(12) Uani 1 1 d DU . . H7A H 0.3557 0.7973 0.1630 0.087 Uiso 1 1 calc R . . H7B H 0.4871 0.8910 0.1779 0.087 Uiso 1 1 calc R . . C8 C 0.3765(6) 0.9675(6) 0.1724(2) 0.0914(15) Uani 1 1 d DU . . H8A H 0.3549 0.9693 0.1504 0.110 Uiso 1 1 calc R . . H8B H 0.4491 1.0473 0.1779 0.110 Uiso 1 1 calc R . . C9 C 0.2687(8) 0.9364(8) 0.1937(2) 0.1065(18) Uani 1 1 d DU . . H9A H 0.1899 0.8773 0.1838 0.128 Uiso 1 1 calc RD . . H9B H 0.2661 1.0112 0.1996 0.128 Uiso 1 1 calc R . . C10 C 0.2949(8) 0.8796(8) 0.2217(2) 0.0984(17) Uani 1 1 d DU . . H10A H 0.3509 0.9437 0.2364 0.118 Uiso 1 1 calc R . . H10B H 0.2180 0.8220 0.2326 0.118 Uiso 1 1 calc R . . Li1 Li 0.3333 0.6667 0.2220(4) 0.065(3) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.2672(2) 0.127(3) Uani 1 3 d SDU . . C11 C 0.387(3) 0.7945(9) 0.2795(3) 0.131(4) Uani 0.33 1 d PDU . . H11B H 0.3242 0.8162 0.2818 0.157 Uiso 0.33 1 d PR . . H11A H 0.4508 0.8532 0.2663 0.157 Uiso 0.33 1 d PR . . C12 C 0.4378(15) 0.7748(12) 0.3092(3) 0.130(4) Uani 0.33 1 d PDU . . H12B H 0.4536 0.8420 0.3226 0.157 Uiso 0.33 1 d PR . . H12A H 0.5117 0.7709 0.3068 0.157 Uiso 0.33 1 d PR . . C13 C 0.3333 0.6667 0.3210(2) 0.139(4) Uani 1 3 d SDU . . H13B H 0.2834 0.6814 0.3353 0.167 Uiso 0.33 1 d PR . . H13A H 0.3644 0.6203 0.3314 0.167 Uiso 0.33 1 d PR . . C14 C 0.260(2) 0.599(2) 0.2938(3) 0.134(4) Uani 0.33 1 d PDU . . H14B H 0.2451 0.5161 0.2936 0.161 Uiso 0.33 1 d PR . . H14A H 0.1817 0.5957 0.2936 0.161 Uiso 0.33 1 d PR . . 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 Sc1 0.0338(3) 0.0338(3) 0.0326(4) 0.000 0.000 0.01688(14) Cl1 0.0450(4) 0.0477(4) 0.0481(5) -0.0041(4) -0.0119(4) 0.0165(3) N1 0.0318(11) 0.0316(11) 0.0380(14) -0.0001(10) 0.0035(10) 0.0135(9) N2 0.0283(11) 0.0275(10) 0.0392(14) -0.0028(9) -0.0009(10) 0.0125(9) C6 0.0403(18) 0.055(2) 0.063(3) 0.001(2) 0.0144(18) 0.0016(16) C4 0.0330(15) 0.0385(15) 0.053(2) -0.0038(14) 0.0048(14) 0.0111(12) C3 0.0311(14) 0.0365(15) 0.066(3) -0.0102(16) -0.0058(15) 0.0077(12) C2 0.0347(14) 0.0349(14) 0.050(2) -0.0113(13) -0.0078(14) 0.0169(12) C5 0.052(2) 0.0489(18) 0.051(2) -0.0154(16) -0.0168(17) 0.0232(16) C1 0.0256(12) 0.0256(12) 0.035(2) 0.000 0.000 0.0128(6) O1 0.0799(19) 0.0651(17) 0.061(2) -0.0038(15) 0.0162(16) 0.0376(15) C7 0.076(2) 0.065(2) 0.078(3) 0.009(2) 0.012(2) 0.036(2) C8 0.094(3) 0.076(2) 0.104(3) 0.014(2) 0.007(2) 0.043(2) C9 0.103(3) 0.092(3) 0.122(3) 0.008(3) 0.009(3) 0.047(2) C10 0.106(3) 0.087(3) 0.103(3) -0.008(2) 0.021(3) 0.048(2) Li1 0.076(5) 0.076(5) 0.043(7) 0.000 0.000 0.038(3) O2 0.160(5) 0.160(5) 0.063(5) 0.000 0.000 0.080(3) C11 0.164(6) 0.158(6) 0.074(6) -0.005(4) -0.003(4) 0.083(5) C12 0.163(7) 0.160(7) 0.079(7) -0.005(4) -0.001(4) 0.089(5) C13 0.168(6) 0.168(6) 0.081(6) 0.000 0.000 0.084(3) C14 0.163(6) 0.162(6) 0.074(6) 0.005(4) 0.000(4) 0.078(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 Sc1 N1 2.284(3) 3_565 ? Sc1 N1 2.284(3) . ? Sc1 N1 2.284(3) 2_665 ? Sc1 Cl1 2.4309(10) 2_665 ? Sc1 Cl1 2.4309(10) . ? Sc1 Cl1 2.4309(10) 3_565 ? N1 C4 1.341(4) . ? N1 N2 1.375(4) . ? N2 C2 1.350(4) . ? N2 C1 1.443(3) . ? C6 C4 1.502(6) . ? C4 C3 1.402(6) . ? C3 C2 1.385(6) . ? C2 C5 1.484(6) . ? C1 N2 1.443(3) 3_565 ? C1 N2 1.443(3) 2_665 ? O1 C10 1.399(8) . ? O1 C7 1.422(8) . ? O1 Li1 1.886(7) . ? C7 C8 1.497(7) . ? C8 C9 1.518(8) . ? C9 C10 1.519(9) . ? Li1 O1 1.886(7) 2_665 ? Li1 O1 1.886(7) 3_565 ? Li1 O2 1.951(19) . ? O2 C14 1.454(10) 3_565 ? O2 C14 1.454(10) . ? O2 C14 1.454(10) 2_665 ? O2 C11 1.495(11) . ? O2 C11 1.495(11) 2_665 ? O2 C11 1.495(10) 3_565 ? C11 C14 0.89(3) 3_565 ? C11 C12 1.507(10) . ? C11 C14 1.88(4) 2_665 ? C12 C14 1.28(4) 3_565 ? C12 C14 1.43(4) 2_665 ? C12 C13 1.431(10) . ? C13 C12 1.431(10) 2_665 ? C13 C12 1.431(10) 3_565 ? C13 C14 1.475(10) 3_565 ? C13 C14 1.475(10) . ? C13 C14 1.475(10) 2_665 ? C14 C11 0.89(3) 2_665 ? C14 C12 1.28(4) 2_665 ? C14 C12 1.43(4) 3_565 ? C14 C14 1.548(15) 3_565 ? C14 C14 1.548(15) 2_665 ? C14 C11 1.88(4) 3_565 ? 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 Sc1 N1 79.15(11) 3_565 . ? N1 Sc1 N1 79.15(11) 3_565 2_665 ? N1 Sc1 N1 79.15(11) . 2_665 ? N1 Sc1 Cl1 90.31(8) 3_565 2_665 ? N1 Sc1 Cl1 91.21(7) . 2_665 ? N1 Sc1 Cl1 166.84(9) 2_665 2_665 ? N1 Sc1 Cl1 91.21(7) 3_565 . ? N1 Sc1 Cl1 166.84(9) . . ? N1 Sc1 Cl1 90.31(8) 2_665 . ? Cl1 Sc1 Cl1 97.85(5) 2_665 . ? N1 Sc1 Cl1 166.84(9) 3_565 3_565 ? N1 Sc1 Cl1 90.31(8) . 3_565 ? N1 Sc1 Cl1 91.21(7) 2_665 3_565 ? Cl1 Sc1 Cl1 97.85(5) 2_665 3_565 ? Cl1 Sc1 Cl1 97.85(5) . 3_565 ? C4 N1 N2 106.0(3) . . ? C4 N1 Sc1 134.6(3) . . ? N2 N1 Sc1 119.34(18) . . ? C2 N2 N1 111.2(3) . . ? C2 N2 C1 126.4(3) . . ? N1 N2 C1 122.4(3) . . ? N1 C4 C3 109.6(4) . . ? N1 C4 C6 122.2(4) . . ? C3 C4 C6 128.2(3) . . ? C2 C3 C4 106.6(3) . . ? N2 C2 C3 106.5(3) . . ? N2 C2 C5 122.8(3) . . ? C3 C2 C5 130.7(3) . . ? N2 C1 N2 109.8(2) 3_565 . ? N2 C1 N2 109.8(2) 3_565 2_665 ? N2 C1 N2 109.8(2) . 2_665 ? C10 O1 C7 111.6(5) . . ? C10 O1 Li1 127.0(6) . . ? C7 O1 Li1 119.5(5) . . ? O1 C7 C8 107.0(5) . . ? C7 C8 C9 101.3(6) . . ? C8 C9 C10 103.1(6) . . ? O1 C10 C9 103.4(6) . . ? O1 Li1 O1 111.2(5) . 2_665 ? O1 Li1 O1 111.2(5) . 3_565 ? O1 Li1 O1 111.2(5) 2_665 3_565 ? O1 Li1 O2 107.7(5) . . ? O1 Li1 O2 107.7(5) 2_665 . ? O1 Li1 O2 107.7(5) 3_565 . ? C14 O2 C14 64.3(5) 3_565 . ? C14 O2 C14 64.3(5) 3_565 2_665 ? C14 O2 C14 64.3(5) . 2_665 ? C14 O2 C11 35.2(13) 3_565 . ? C14 O2 C11 99.5(13) . . ? C14 O2 C11 79.3(19) 2_665 . ? C14 O2 C11 79.3(19) 3_565 2_665 ? C14 O2 C11 35.2(13) . 2_665 ? C14 O2 C11 99.5(13) 2_665 2_665 ? C11 O2 C11 108.2(4) . 2_665 ? C14 O2 C11 99.5(13) 3_565 3_565 ? C14 O2 C11 79.3(19) . 3_565 ? C14 O2 C11 35.2(13) 2_665 3_565 ? C11 O2 C11 108.2(4) . 3_565 ? C11 O2 C11 108.2(4) 2_665 3_565 ? C14 O2 Li1 142.1(3) 3_565 . ? C14 O2 Li1 142.1(3) . . ? C14 O2 Li1 142.1(3) 2_665 . ? C11 O2 Li1 110.7(4) . . ? C11 O2 Li1 110.7(4) 2_665 . ? C11 O2 Li1 110.7(4) 3_565 . ? C14 C11 O2 69.9(10) 3_565 . ? C14 C11 C12 58(3) 3_565 . ? O2 C11 C12 97.2(8) . . ? C14 C11 C14 55(2) 3_565 2_665 ? O2 C11 C14 49.4(10) . 2_665 ? C12 C11 C14 48.4(9) . 2_665 ? C14 C12 C14 69.5(10) 3_565 2_665 ? C14 C12 C13 65.8(12) 3_565 . ? C14 C12 C13 62.1(11) 2_665 . ? C14 C12 C11 36.2(14) 3_565 . ? C14 C12 C11 79.6(10) 2_665 . ? C13 C12 C11 101.3(8) . . ? C12 C13 C12 108.0(4) 2_665 . ? C12 C13 C12 108.0(4) 2_665 3_565 ? C12 C13 C12 108.0(4) . 3_565 ? C12 C13 C14 58.9(19) 2_665 3_565 ? C12 C13 C14 52.1(18) . 3_565 ? C12 C13 C14 106.2(6) 3_565 3_565 ? C12 C13 C14 52.1(18) 2_665 . ? C12 C13 C14 106.2(6) . . ? C12 C13 C14 58.9(19) 3_565 . ? C14 C13 C14 63.3(6) 3_565 . ? C12 C13 C14 106.2(6) 2_665 2_665 ? C12 C13 C14 58.9(19) . 2_665 ? C12 C13 C14 52.1(18) 3_565 2_665 ? C14 C13 C14 63.3(6) 3_565 2_665 ? C14 C13 C14 63.3(6) . 2_665 ? C11 C14 C12 86(4) 2_665 2_665 ? C11 C14 C12 155(4) 2_665 3_565 ? C12 C14 C12 117.5(12) 2_665 3_565 ? C11 C14 O2 74.9(12) 2_665 . ? C12 C14 O2 111(2) 2_665 . ? C12 C14 O2 103(2) 3_565 . ? C11 C14 C13 146(5) 2_665 . ? C12 C14 C13 62.2(10) 2_665 . ? C12 C14 C13 59.0(10) 3_565 . ? O2 C14 C13 104.8(6) . . ? C11 C14 C14 97(4) 2_665 3_565 ? C12 C14 C14 60(3) 2_665 3_565 ? C12 C14 C14 103(2) 3_565 3_565 ? O2 C14 C14 57.8(3) . 3_565 ? C13 C14 C14 58.4(3) . 3_565 ? C11 C14 C14 132.7(11) 2_665 2_665 ? C12 C14 C14 110(2) 2_665 2_665 ? C12 C14 C14 51(2) 3_565 2_665 ? O2 C14 C14 57.8(3) . 2_665 ? C13 C14 C14 58.4(3) . 2_665 ? C14 C14 C14 60.000(6) 3_565 2_665 ? C11 C14 C11 117.0(18) 2_665 3_565 ? C12 C14 C11 137.8(11) 2_665 3_565 ? C12 C14 C11 52.0(13) 3_565 3_565 ? O2 C14 C11 51.3(11) . 3_565 ? C13 C14 C11 84.3(15) . 3_565 ? C14 C14 C11 81(2) 3_565 3_565 ? C14 C14 C11 28(2) 2_665 3_565 ? 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 N1 Sc1 N1 C4 -139.1(4) 3_565 . . . ? N1 Sc1 N1 C4 140.0(4) 2_665 . . . ? Cl1 Sc1 N1 C4 -49.0(3) 2_665 . . . ? Cl1 Sc1 N1 C4 177.3(3) . . . . ? Cl1 Sc1 N1 C4 48.8(3) 3_565 . . . ? N1 Sc1 N1 N2 40.51(17) 3_565 . . . ? N1 Sc1 N1 N2 -40.38(17) 2_665 . . . ? Cl1 Sc1 N1 N2 130.6(2) 2_665 . . . ? Cl1 Sc1 N1 N2 -3.0(5) . . . . ? Cl1 Sc1 N1 N2 -131.6(2) 3_565 . . . ? C4 N1 N2 C2 -0.1(4) . . . . ? Sc1 N1 N2 C2 -179.8(2) . . . . ? C4 N1 N2 C1 179.6(2) . . . . ? Sc1 N1 N2 C1 -0.1(3) . . . . ? N2 N1 C4 C3 0.2(4) . . . . ? Sc1 N1 C4 C3 179.9(2) . . . . ? N2 N1 C4 C6 178.4(4) . . . . ? Sc1 N1 C4 C6 -1.9(6) . . . . ? N1 C4 C3 C2 -0.2(4) . . . . ? C6 C4 C3 C2 -178.4(4) . . . . ? N1 N2 C2 C3 -0.1(4) . . . . ? C1 N2 C2 C3 -179.7(3) . . . . ? N1 N2 C2 C5 179.6(3) . . . . ? C1 N2 C2 C5 -0.1(5) . . . . ? C4 C3 C2 N2 0.2(4) . . . . ? C4 C3 C2 C5 -179.4(4) . . . . ? C2 N2 C1 N2 119.2(4) . . . 3_565 ? N1 N2 C1 N2 -60.4(4) . . . 3_565 ? C2 N2 C1 N2 -119.8(4) . . . 2_665 ? N1 N2 C1 N2 60.5(4) . . . 2_665 ? C10 O1 C7 C8 3.0(8) . . . . ? Li1 O1 C7 C8 168.4(5) . . . . ? O1 C7 C8 C9 -24.3(8) . . . . ? C7 C8 C9 C10 35.3(8) . . . . ? C7 O1 C10 C9 19.8(8) . . . . ? Li1 O1 C10 C9 -144.2(6) . . . . ? C8 C9 C10 O1 -34.3(8) . . . . ? C10 O1 Li1 O1 77.5(11) . . . 2_665 ? C7 O1 Li1 O1 -85.4(6) . . . 2_665 ? C10 O1 Li1 O1 -158.0(7) . . . 3_565 ? C7 O1 Li1 O1 39.2(9) . . . 3_565 ? C10 O1 Li1 O2 -40.2(6) . . . . ? C7 O1 Li1 O2 156.9(4) . . . . ? O1 Li1 O2 C14 2(3) . . . 3_565 ? O1 Li1 O2 C14 -118(3) 2_665 . . 3_565 ? O1 Li1 O2 C14 122(3) 3_565 . . 3_565 ? O1 Li1 O2 C14 122(3) . . . . ? O1 Li1 O2 C14 2(3) 2_665 . . . ? O1 Li1 O2 C14 -118(3) 3_565 . . . ? O1 Li1 O2 C14 -118(3) . . . 2_665 ? O1 Li1 O2 C14 122(3) 2_665 . . 2_665 ? O1 Li1 O2 C14 2(3) 3_565 . . 2_665 ? O1 Li1 O2 C11 -18.6(15) . . . . ? O1 Li1 O2 C11 -138.6(15) 2_665 . . . ? O1 Li1 O2 C11 101.4(15) 3_565 . . . ? O1 Li1 O2 C11 101.4(15) . . . 2_665 ? O1 Li1 O2 C11 -18.6(15) 2_665 . . 2_665 ? O1 Li1 O2 C11 -138.6(15) 3_565 . . 2_665 ? O1 Li1 O2 C11 -138.6(15) . . . 3_565 ? O1 Li1 O2 C11 101.4(15) 2_665 . . 3_565 ? O1 Li1 O2 C11 -18.6(15) 3_565 . . 3_565 ? C14 O2 C11 C14 1(5) . . . 3_565 ? C14 O2 C11 C14 -60(4) 2_665 . . 3_565 ? C11 O2 C11 C14 36(3) 2_665 . . 3_565 ? C11 O2 C11 C14 -81(3) 3_565 . . 3_565 ? Li1 O2 C11 C14 158(3) . . . 3_565 ? C14 O2 C11 C12 52(3) 3_565 . . . ? C14 O2 C11 C12 53(2) . . . . ? C14 O2 C11 C12 -8.5(14) 2_665 . . . ? C11 O2 C11 C12 88.1(8) 2_665 . . . ? C11 O2 C11 C12 -28.8(13) 3_565 . . . ? Li1 O2 C11 C12 -150.3(10) . . . . ? C14 O2 C11 C14 60(4) 3_565 . . 2_665 ? C14 O2 C11 C14 61.4(11) . . . 2_665 ? C11 O2 C11 C14 96.6(9) 2_665 . . 2_665 ? C11 O2 C11 C14 -20.4(8) 3_565 . . 2_665 ? Li1 O2 C11 C14 -141.9(7) . . . 2_665 ? O2 C11 C12 C14 -60.7(11) . . . 3_565 ? C14 C11 C12 C14 -69(2) 2_665 . . 3_565 ? C14 C11 C12 C14 69(2) 3_565 . . 2_665 ? O2 C11 C12 C14 8.6(16) . . . 2_665 ? C14 C11 C12 C13 10.8(16) 3_565 . . . ? O2 C11 C12 C13 -49.9(16) . . . . ? C14 C11 C12 C13 -58.5(10) 2_665 . . . ? C14 C12 C13 C12 -19.8(9) 3_565 . . 2_665 ? C14 C12 C13 C12 -98.5(6) 2_665 . . 2_665 ? C11 C12 C13 C12 -26.7(13) . . . 2_665 ? C14 C12 C13 C12 96.9(8) 3_565 . . 3_565 ? C14 C12 C13 C12 18.1(8) 2_665 . . 3_565 ? C11 C12 C13 C12 89.9(9) . . . 3_565 ? C14 C12 C13 C14 -78.7(10) 2_665 . . 3_565 ? C11 C12 C13 C14 -7.0(12) . . . 3_565 ? C14 C12 C13 C14 35(3) 3_565 . . . ? C14 C12 C13 C14 -44(2) 2_665 . . . ? C11 C12 C13 C14 28(2) . . . . ? C14 C12 C13 C14 78.7(10) 3_565 . . 2_665 ? C11 C12 C13 C14 71.7(12) . . . 2_665 ? C14 O2 C14 C11 109(5) 3_565 . . 2_665 ? C14 O2 C14 C11 -179(5) 2_665 . . 2_665 ? C11 O2 C14 C11 108(2) . . . 2_665 ? C11 O2 C14 C11 -145(2) 3_565 . . 2_665 ? Li1 O2 C14 C11 -35(5) . . . 2_665 ? C14 O2 C14 C12 29.2(14) 3_565 . . 2_665 ? C14 O2 C14 C12 101.6(13) 2_665 . . 2_665 ? C11 O2 C14 C12 28.4(19) . . . 2_665 ? C11 O2 C14 C12 -80(4) 2_665 . . 2_665 ? C11 O2 C14 C12 135.3(17) 3_565 . . 2_665 ? Li1 O2 C14 C12 -114.6(13) . . . 2_665 ? C14 O2 C14 C12 -97.0(14) 3_565 . . 3_565 ? C14 O2 C14 C12 -24.6(15) 2_665 . . 3_565 ? C11 O2 C14 C12 -97.8(19) . . . 3_565 ? C11 O2 C14 C12 154(4) 2_665 . . 3_565 ? C11 O2 C14 C12 9.1(17) 3_565 . . 3_565 ? Li1 O2 C14 C12 119.2(14) . . . 3_565 ? C14 O2 C14 C13 -36.20(13) 3_565 . . . ? C14 O2 C14 C13 36.20(12) 2_665 . . . ? C11 O2 C14 C13 -37(3) . . . . ? C11 O2 C14 C13 -145(5) 2_665 . . . ? C11 O2 C14 C13 70(3) 3_565 . . . ? Li1 O2 C14 C13 180.000(1) . . . . ? C14 O2 C14 C14 72.4(2) 2_665 . . 3_565 ? C11 O2 C14 C14 -1(3) . . . 3_565 ? C11 O2 C14 C14 -109(5) 2_665 . . 3_565 ? C11 O2 C14 C14 106(3) 3_565 . . 3_565 ? Li1 O2 C14 C14 -143.80(13) . . . 3_565 ? C14 O2 C14 C14 -72.4(3) 3_565 . . 2_665 ? C11 O2 C14 C14 -73(3) . . . 2_665 ? C11 O2 C14 C14 179(5) 2_665 . . 2_665 ? C11 O2 C14 C14 34(3) 3_565 . . 2_665 ? Li1 O2 C14 C14 143.80(13) . . . 2_665 ? C14 O2 C14 C11 -106(3) 3_565 . . 3_565 ? C14 O2 C14 C11 -34(3) 2_665 . . 3_565 ? C11 O2 C14 C11 -106.9(5) . . . 3_565 ? C11 O2 C14 C11 145(2) 2_665 . . 3_565 ? Li1 O2 C14 C11 110(3) . . . 3_565 ? C12 C13 C14 C11 21(3) 2_665 . . 2_665 ? C12 C13 C14 C11 -79(3) . . . 2_665 ? C12 C13 C14 C11 179(100) 3_565 . . 2_665 ? C14 C13 C14 C11 -49(3) 3_565 . . 2_665 ? C14 C13 C14 C11 -121(3) 2_665 . . 2_665 ? C12 C13 C14 C12 -100.5(4) . . . 2_665 ? C12 C13 C14 C12 158.0(8) 3_565 . . 2_665 ? C14 C13 C14 C12 -70(3) 3_565 . . 2_665 ? C14 C13 C14 C12 -142(3) 2_665 . . 2_665 ? C12 C13 C14 C12 -158.0(8) 2_665 . . 3_565 ? C12 C13 C14 C12 101.6(5) . . . 3_565 ? C14 C13 C14 C12 132(3) 3_565 . . 3_565 ? C14 C13 C14 C12 60(3) 2_665 . . 3_565 ? C12 C13 C14 O2 106(3) 2_665 . . . ? C12 C13 C14 O2 6(3) . . . . ? C12 C13 C14 O2 -96(3) 3_565 . . . ? C14 C13 C14 O2 35.97(14) 3_565 . . . ? C14 C13 C14 O2 -35.97(14) 2_665 . . . ? C12 C13 C14 C14 70(3) 2_665 . . 3_565 ? C12 C13 C14 C14 -30(3) . . . 3_565 ? C12 C13 C14 C14 -132(3) 3_565 . . 3_565 ? C14 C13 C14 C14 -71.9(3) 2_665 . . 3_565 ? C12 C13 C14 C14 142(3) 2_665 . . 2_665 ? C12 C13 C14 C14 42(3) . . . 2_665 ? C12 C13 C14 C14 -60(3) 3_565 . . 2_665 ? C14 C13 C14 C14 71.9(3) 3_565 . . 2_665 ? C12 C13 C14 C11 153.5(15) 2_665 . . 3_565 ? C12 C13 C14 C11 53.1(15) . . . 3_565 ? C12 C13 C14 C11 -48.5(11) 3_565 . . 3_565 ? C14 C13 C14 C11 83.4(17) 3_565 . . 3_565 ? C14 C13 C14 C11 11.5(18) 2_665 . . 3_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.593 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.078 #===END data_mo_dm15761_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Cl3 Li N6 O4 Y' _chemical_formula_weight 788.00 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c :H' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 12.554(3) _cell_length_b 12.554(3) _cell_length_c 43.637(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5956(3) _cell_formula_units_Z 6 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 1708 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 19.35 _exptl_crystal_description block _exptl_crystal_colour brick-red _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 1.318 _exptl_crystal_density_method ? _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.7482 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15020 _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.60 _reflns_number_total 3030 _reflns_number_gt 2093 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0856P)^2^+2.6323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(14) _refine_ls_number_reflns 3030 _refine_ls_number_parameters 162 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.036 _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 Y1 Y 0.3333 0.6667 0.08213(3) 0.0366(2) Uani 1 3 d S . . Cl1 Cl 0.53408(15) 0.81759(15) 0.10965(4) 0.0523(4) Uani 1 1 d . . . N1 N 0.1825(4) 0.5500(4) 0.04294(12) 0.0381(11) Uani 1 1 d . . . N2 N 0.2138(4) 0.5736(4) 0.01214(10) 0.0327(10) Uani 1 1 d . . . C6 C -0.0007(6) 0.4074(7) 0.07253(16) 0.0597(19) Uani 1 1 d . . . H6A H 0.0264 0.3532 0.0814 0.090 Uiso 1 1 calc R . . H6B H -0.0892 0.3600 0.0684 0.090 Uiso 1 1 calc R . . H6C H 0.0164 0.4740 0.0869 0.090 Uiso 1 1 calc R . . C4 C 0.0663(5) 0.4602(6) 0.04355(15) 0.0453(14) Uani 1 1 d . . . C3 C 0.0234(6) 0.4243(5) 0.01330(16) 0.0477(15) Uani 1 1 d . . . H3 H -0.0560 0.3606 0.0074 0.057 Uiso 1 1 calc R . . C2 C 0.1170(5) 0.4981(5) -0.00583(14) 0.0387(13) Uani 1 1 d . . . C5 C 0.1228(7) 0.5030(6) -0.03938(14) 0.0540(17) Uani 1 1 d . . . H5A H 0.0902 0.5546 -0.0469 0.081 Uiso 1 1 calc R . . H5B H 0.0736 0.4197 -0.0477 0.081 Uiso 1 1 calc R . . H5C H 0.2085 0.5378 -0.0460 0.081 Uiso 1 1 calc R . . C1 C 0.3333 0.6667 0.0016(2) 0.036(2) Uani 1 3 d S . . O1 O 0.3550(6) 0.8182(5) 0.20858(13) 0.0761(14) Uani 1 1 d U . . C7 C 0.4040(9) 0.8657(8) 0.1791(2) 0.0810(19) Uani 1 1 d DU . . H7A H 0.3642 0.8007 0.1633 0.097 Uiso 1 1 calc R . . H7B H 0.4937 0.8967 0.1787 0.097 Uiso 1 1 calc R . . C8 C 0.3786(9) 0.9684(9) 0.1730(2) 0.096(2) Uani 1 1 d DU . . H8A H 0.4488 1.0488 0.1792 0.115 Uiso 1 1 calc R . . H8B H 0.3601 0.9718 0.1511 0.115 Uiso 1 1 calc R . . C9 C 0.2687(9) 0.9329(10) 0.1926(2) 0.106(2) Uani 1 1 d DU . . H9A H 0.1921 0.8738 0.1819 0.127 Uiso 1 1 calc RD . . H9B H 0.2630 1.0060 0.1985 0.127 Uiso 1 1 calc R . . C10 C 0.2907(10) 0.8744(10) 0.2201(2) 0.101(2) Uani 1 1 d DU . . H10A H 0.3403 0.9372 0.2357 0.121 Uiso 1 1 calc R . . H10B H 0.2119 0.8128 0.2295 0.121 Uiso 1 1 calc R . . Li1 Li 0.3333 0.6667 0.2233(5) 0.080(7) Uani 1 3 d S . . O2 O 0.3333 0.6667 0.2671(2) 0.134(4) Uani 1 3 d SDU . . C11 C 0.336(4) 0.7782(19) 0.2794(3) 0.136(5) Uani 0.33 1 d PDU . . H11B H 0.2729 0.7999 0.2817 0.163 Uiso 0.33 1 d PR . . H11A H 0.3995 0.8369 0.2662 0.163 Uiso 0.33 1 d PR . . C12 C 0.419(2) 0.7896(11) 0.3054(3) 0.141(5) Uani 0.33 1 d PDU . . H12B H 0.4351 0.8569 0.3188 0.169 Uiso 0.33 1 d PR . . H12A H 0.4932 0.7857 0.3030 0.169 Uiso 0.33 1 d PR . . C13 C 0.3333 0.6667 0.3172(3) 0.142(5) Uani 1 3 d SDU . . H13B H 0.2834 0.6814 0.3314 0.170 Uiso 0.33 1 d PR . . H13A H 0.3644 0.6203 0.3276 0.170 Uiso 0.33 1 d PR . . C14 C 0.2427(9) 0.637(3) 0.2915(3) 0.139(5) Uani 0.33 1 d PDU . . H14B H 0.2284 0.5543 0.2913 0.167 Uiso 0.33 1 d PR . . H14A H 0.1649 0.6339 0.2913 0.167 Uiso 0.33 1 d PR . . 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 Y1 0.0350(3) 0.0350(3) 0.0399(4) 0.000 0.000 0.01749(14) Cl1 0.0428(8) 0.0464(9) 0.0596(10) -0.0050(8) -0.0120(8) 0.0163(7) N1 0.030(2) 0.034(2) 0.046(3) -0.001(2) 0.003(2) 0.013(2) N2 0.027(2) 0.034(2) 0.034(2) 0.0029(19) 0.0041(19) 0.0125(19) C6 0.031(3) 0.054(4) 0.074(5) 0.004(4) 0.014(3) 0.006(3) C4 0.032(3) 0.037(3) 0.062(4) -0.003(3) 0.004(3) 0.014(3) C3 0.035(3) 0.030(3) 0.068(4) -0.009(3) -0.004(3) 0.009(3) C2 0.033(3) 0.028(3) 0.054(4) -0.005(3) -0.009(3) 0.015(2) C5 0.064(4) 0.042(4) 0.049(4) -0.012(3) -0.017(3) 0.020(3) C1 0.034(3) 0.034(3) 0.038(5) 0.000 0.000 0.0172(14) O1 0.084(3) 0.072(3) 0.081(3) -0.004(2) 0.016(3) 0.046(2) C7 0.084(3) 0.073(3) 0.093(4) 0.010(3) 0.014(3) 0.045(3) C8 0.094(3) 0.086(3) 0.108(3) 0.006(3) 0.008(3) 0.046(3) C9 0.101(3) 0.094(3) 0.125(4) -0.002(3) 0.010(3) 0.051(3) C10 0.100(3) 0.092(3) 0.107(3) -0.010(3) 0.018(3) 0.044(3) Li1 0.095(12) 0.095(12) 0.050(13) 0.000 0.000 0.048(6) O2 0.170(7) 0.170(7) 0.062(6) 0.000 0.000 0.085(4) C11 0.172(8) 0.173(8) 0.067(7) -0.003(4) 0.001(4) 0.089(5) C12 0.174(8) 0.176(8) 0.071(7) -0.004(4) 0.002(4) 0.087(6) C13 0.177(8) 0.177(8) 0.072(7) 0.000 0.000 0.088(4) C14 0.172(8) 0.176(8) 0.068(6) -0.001(3) 0.003(3) 0.087(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 Y1 N1 2.425(5) 3_565 ? Y1 N1 2.425(5) . ? Y1 N1 2.425(5) 2_665 ? Y1 Cl1 2.5706(17) 2_665 ? Y1 Cl1 2.5706(17) . ? Y1 Cl1 2.5706(17) 3_565 ? N1 C4 1.325(7) . ? N1 N2 1.390(7) . ? N2 C2 1.356(7) . ? N2 C1 1.441(5) . ? C6 C4 1.479(9) . ? C4 C3 1.412(9) . ? C3 C2 1.359(9) . ? C2 C5 1.466(9) . ? C1 N2 1.441(5) 3_565 ? C1 N2 1.441(5) 2_665 ? O1 C10 1.405(11) . ? O1 C7 1.422(11) . ? O1 Li1 1.893(10) . ? C7 C8 1.498(8) . ? C8 C9 1.491(8) . ? C9 C10 1.504(8) . ? Li1 O1 1.893(10) 2_665 ? Li1 O1 1.893(10) 3_565 ? Li1 O2 1.91(3) . ? O2 C14 1.464(10) . ? O2 C14 1.464(10) 3_565 ? O2 C14 1.464(10) 2_665 ? O2 C11 1.487(10) . ? O2 C11 1.487(10) 2_665 ? O2 C11 1.487(10) 3_565 ? C11 C14 1.04(3) 3_565 ? C11 C12 1.503(10) . ? C11 C14 1.65(4) . ? C12 C14 0.712(16) 3_565 ? C12 C13 1.465(10) . ? C13 C12 1.465(10) 2_665 ? C13 C12 1.465(10) 3_565 ? C13 C14 1.505(10) 3_565 ? C13 C14 1.505(10) . ? C13 C14 1.505(10) 2_665 ? C14 C12 0.712(16) 2_665 ? C14 C11 1.04(3) 2_665 ? C14 C14 1.74(2) 3_565 ? C14 C14 1.74(2) 2_665 ? 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 Y1 N1 75.77(18) 3_565 . ? N1 Y1 N1 75.77(18) 3_565 2_665 ? N1 Y1 N1 75.77(18) . 2_665 ? N1 Y1 Cl1 90.22(13) 3_565 2_665 ? N1 Y1 Cl1 91.62(12) . 2_665 ? N1 Y1 Cl1 162.98(12) 2_665 2_665 ? N1 Y1 Cl1 91.62(12) 3_565 . ? N1 Y1 Cl1 162.98(12) . . ? N1 Y1 Cl1 90.22(13) 2_665 . ? Cl1 Y1 Cl1 99.94(6) 2_665 . ? N1 Y1 Cl1 162.98(12) 3_565 3_565 ? N1 Y1 Cl1 90.22(13) . 3_565 ? N1 Y1 Cl1 91.62(12) 2_665 3_565 ? Cl1 Y1 Cl1 99.94(6) 2_665 3_565 ? Cl1 Y1 Cl1 99.94(6) . 3_565 ? C4 N1 N2 105.9(5) . . ? C4 N1 Y1 134.0(4) . . ? N2 N1 Y1 120.1(3) . . ? C2 N2 N1 110.5(4) . . ? C2 N2 C1 126.0(5) . . ? N1 N2 C1 123.5(5) . . ? N1 C4 C3 109.5(6) . . ? N1 C4 C6 122.4(6) . . ? C3 C4 C6 128.0(6) . . ? C2 C3 C4 107.2(5) . . ? N2 C2 C3 106.8(5) . . ? N2 C2 C5 122.7(5) . . ? C3 C2 C5 130.6(6) . . ? N2 C1 N2 110.2(4) 3_565 . ? N2 C1 N2 110.2(4) 3_565 2_665 ? N2 C1 N2 110.2(4) . 2_665 ? C10 O1 C7 110.6(7) . . ? C10 O1 Li1 123.6(7) . . ? C7 O1 Li1 122.8(8) . . ? O1 C7 C8 106.8(7) . . ? C9 C8 C7 101.8(8) . . ? C8 C9 C10 103.7(8) . . ? O1 C10 C9 104.5(8) . . ? O1 Li1 O1 109.2(7) . 2_665 ? O1 Li1 O1 109.2(7) . 3_565 ? O1 Li1 O1 109.2(7) 2_665 3_565 ? O1 Li1 O2 109.8(7) . . ? O1 Li1 O2 109.8(7) 2_665 . ? O1 Li1 O2 109.8(7) 3_565 . ? C14 O2 C14 72.9(8) . 3_565 ? C14 O2 C14 72.9(8) . 2_665 ? C14 O2 C14 72.9(8) 3_565 2_665 ? C14 O2 C11 67.9(18) . . ? C14 O2 C11 41.2(14) 3_565 . ? C14 O2 C11 109.7(10) 2_665 . ? C14 O2 C11 41.2(14) . 2_665 ? C14 O2 C11 109.7(10) 3_565 2_665 ? C14 O2 C11 67.9(18) 2_665 2_665 ? C11 O2 C11 107.6(4) . 2_665 ? C14 O2 C11 109.7(10) . 3_565 ? C14 O2 C11 67.9(18) 3_565 3_565 ? C14 O2 C11 41.2(14) 2_665 3_565 ? C11 O2 C11 107.6(4) . 3_565 ? C11 O2 C11 107.6(4) 2_665 3_565 ? C14 O2 Li1 136.7(5) . . ? C14 O2 Li1 136.7(5) 3_565 . ? C14 O2 Li1 136.7(5) 2_665 . ? C11 O2 Li1 111.2(4) . . ? C11 O2 Li1 111.2(4) 2_665 . ? C11 O2 Li1 111.2(4) 3_565 . ? C14 C11 O2 68.2(10) 3_565 . ? C14 C11 C12 24.9(8) 3_565 . ? O2 C11 C12 92.7(8) . . ? C14 C11 C14 77(2) 3_565 . ? O2 C11 C14 55.4(10) . . ? C12 C11 C14 87.0(9) . . ? C14 C12 C13 79.3(12) 3_565 . ? C14 C12 C11 38(3) 3_565 . ? C13 C12 C11 93.0(9) . . ? C12 C13 C12 108.4(4) 2_665 . ? C12 C13 C12 108.4(4) 2_665 3_565 ? C12 C13 C12 108.4(4) . 3_565 ? C12 C13 C14 92.0(13) 2_665 3_565 ? C12 C13 C14 27.7(6) . 3_565 ? C12 C13 C14 93.9(9) 3_565 3_565 ? C12 C13 C14 27.7(6) 2_665 . ? C12 C13 C14 93.9(9) . . ? C12 C13 C14 92.0(13) 3_565 . ? C14 C13 C14 70.6(8) 3_565 . ? C12 C13 C14 93.9(9) 2_665 2_665 ? C12 C13 C14 92.0(14) . 2_665 ? C12 C13 C14 27.7(6) 3_565 2_665 ? C14 C13 C14 70.6(8) 3_565 2_665 ? C14 C13 C14 70.6(8) . 2_665 ? C12 C14 C11 117(3) 2_665 2_665 ? C12 C14 O2 167.3(15) 2_665 . ? C11 C14 O2 70.6(11) 2_665 . ? C12 C14 C13 73.0(12) 2_665 . ? C11 C14 C13 114(3) 2_665 . ? O2 C14 C13 94.8(9) . . ? C12 C14 C11 117(3) 2_665 . ? C11 C14 C11 125.1(14) 2_665 . ? O2 C14 C11 56.7(10) . . ? C13 C14 C11 86.0(8) . . ? C12 C14 C14 115(2) 2_665 3_565 ? C11 C14 C14 118(2) 2_665 3_565 ? O2 C14 C14 53.5(4) . 3_565 ? C13 C14 C14 54.7(4) . 3_565 ? C11 C14 C14 35.6(13) . 3_565 ? C12 C14 C14 118(2) 2_665 2_665 ? C11 C14 C14 67(3) 2_665 2_665 ? O2 C14 C14 53.5(4) . 2_665 ? C13 C14 C14 54.7(4) . 2_665 ? C11 C14 C14 90.8(15) . 2_665 ? C14 C14 C14 60.000(16) 3_565 2_665 ? 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 N1 Y1 N1 C4 -140.7(6) 3_565 . . . ? N1 Y1 N1 C4 140.7(6) 2_665 . . . ? Cl1 Y1 N1 C4 -50.9(6) 2_665 . . . ? Cl1 Y1 N1 C4 176.1(4) . . . . ? Cl1 Y1 N1 C4 49.0(5) 3_565 . . . ? N1 Y1 N1 N2 39.7(3) 3_565 . . . ? N1 Y1 N1 N2 -38.9(3) 2_665 . . . ? Cl1 Y1 N1 N2 129.5(4) 2_665 . . . ? Cl1 Y1 N1 N2 -3.5(7) . . . . ? Cl1 Y1 N1 N2 -130.5(4) 3_565 . . . ? C4 N1 N2 C2 -0.1(6) . . . . ? Y1 N1 N2 C2 179.6(3) . . . . ? C4 N1 N2 C1 179.5(4) . . . . ? Y1 N1 N2 C1 -0.8(6) . . . . ? N2 N1 C4 C3 1.0(6) . . . . ? Y1 N1 C4 C3 -178.6(4) . . . . ? N2 N1 C4 C6 179.1(6) . . . . ? Y1 N1 C4 C6 -0.5(9) . . . . ? N1 C4 C3 C2 -1.6(7) . . . . ? C6 C4 C3 C2 -179.6(6) . . . . ? N1 N2 C2 C3 -0.9(6) . . . . ? C1 N2 C2 C3 179.5(4) . . . . ? N1 N2 C2 C5 179.3(5) . . . . ? C1 N2 C2 C5 -0.2(8) . . . . ? C4 C3 C2 N2 1.5(7) . . . . ? C4 C3 C2 C5 -178.8(6) . . . . ? C2 N2 C1 N2 119.1(7) . . . 3_565 ? N1 N2 C1 N2 -60.5(6) . . . 3_565 ? C2 N2 C1 N2 -119.0(7) . . . 2_665 ? N1 N2 C1 N2 61.5(6) . . . 2_665 ? C10 O1 C7 C8 5.7(11) . . . . ? Li1 O1 C7 C8 166.6(7) . . . . ? O1 C7 C8 C9 -25.5(10) . . . . ? C7 C8 C9 C10 34.9(10) . . . . ? C7 O1 C10 C9 16.7(11) . . . . ? Li1 O1 C10 C9 -144.1(9) . . . . ? C8 C9 C10 O1 -32.5(11) . . . . ? C10 O1 Li1 O1 74.6(14) . . . 2_665 ? C7 O1 Li1 O1 -83.9(9) . . . 2_665 ? C10 O1 Li1 O1 -166.2(8) . . . 3_565 ? C7 O1 Li1 O1 35.4(12) . . . 3_565 ? C10 O1 Li1 O2 -45.8(8) . . . . ? C7 O1 Li1 O2 155.8(7) . . . . ? O1 Li1 O2 C14 86(2) . . . . ? O1 Li1 O2 C14 -34(2) 2_665 . . . ? O1 Li1 O2 C14 -154(2) 3_565 . . . ? O1 Li1 O2 C14 -34(2) . . . 3_565 ? O1 Li1 O2 C14 -154(2) 2_665 . . 3_565 ? O1 Li1 O2 C14 86(2) 3_565 . . 3_565 ? O1 Li1 O2 C14 -154(2) . . . 2_665 ? O1 Li1 O2 C14 86(2) 2_665 . . 2_665 ? O1 Li1 O2 C14 -34(2) 3_565 . . 2_665 ? O1 Li1 O2 C11 6.6(16) . . . . ? O1 Li1 O2 C11 -113.4(16) 2_665 . . . ? O1 Li1 O2 C11 126.6(16) 3_565 . . . ? O1 Li1 O2 C11 126.6(16) . . . 2_665 ? O1 Li1 O2 C11 6.6(16) 2_665 . . 2_665 ? O1 Li1 O2 C11 -113.4(16) 3_565 . . 2_665 ? O1 Li1 O2 C11 -113.4(16) . . . 3_565 ? O1 Li1 O2 C11 126.6(16) 2_665 . . 3_565 ? O1 Li1 O2 C11 6.6(16) 3_565 . . 3_565 ? C14 O2 C11 C14 89(3) . . . 3_565 ? C14 O2 C11 C14 28(3) 2_665 . . 3_565 ? C11 O2 C11 C14 100.1(17) 2_665 . . 3_565 ? C11 O2 C11 C14 -16(2) 3_565 . . 3_565 ? Li1 O2 C11 C14 -137.8(18) . . . 3_565 ? C14 O2 C11 C12 84.4(15) . . . . ? C14 O2 C11 C12 -4.6(13) 3_565 . . . ? C14 O2 C11 C12 23(2) 2_665 . . . ? C11 O2 C11 C12 95.5(7) 2_665 . . . ? C11 O2 C11 C12 -20.3(12) 3_565 . . . ? Li1 O2 C11 C12 -142.4(9) . . . . ? C14 O2 C11 C14 -89(3) 3_565 . . . ? C14 O2 C11 C14 -61.1(11) 2_665 . . . ? C11 O2 C11 C14 11.1(10) 2_665 . . . ? C11 O2 C11 C14 -104.7(8) 3_565 . . . ? Li1 O2 C11 C14 133.2(8) . . . . ? O2 C11 C12 C14 10(3) . . . 3_565 ? C14 C11 C12 C14 65(4) . . . 3_565 ? C14 C11 C12 C13 -68(3) 3_565 . . . ? O2 C11 C12 C13 -58.2(12) . . . . ? C14 C11 C12 C13 -3.1(10) . . . . ? C14 C12 C13 C12 -56(3) 3_565 . . 2_665 ? C11 C12 C13 C12 -20.7(12) . . . 2_665 ? C14 C12 C13 C12 61(3) 3_565 . . 3_565 ? C11 C12 C13 C12 96.8(8) . . . 3_565 ? C11 C12 C13 C14 36(3) . . . 3_565 ? C14 C12 C13 C14 -32(4) 3_565 . . . ? C11 C12 C13 C14 3.4(11) . . . . ? C14 C12 C13 C14 39(3) 3_565 . . 2_665 ? C11 C12 C13 C14 74.1(9) . . . 2_665 ? C14 O2 C14 C12 -23(17) 3_565 . . 2_665 ? C14 O2 C14 C12 54(17) 2_665 . . 2_665 ? C11 O2 C14 C12 -66(18) . . . 2_665 ? C11 O2 C14 C12 130(20) 2_665 . . 2_665 ? C11 O2 C14 C12 35(19) 3_565 . . 2_665 ? Li1 O2 C14 C12 -164(17) . . . 2_665 ? C14 O2 C14 C11 -153(3) 3_565 . . 2_665 ? C14 O2 C14 C11 -76(3) 2_665 . . 2_665 ? C11 O2 C14 C11 163.9(18) . . . 2_665 ? C11 O2 C14 C11 -94.5(9) 3_565 . . 2_665 ? Li1 O2 C14 C11 66(3) . . . 2_665 ? C14 O2 C14 C13 -38.4(2) 3_565 . . . ? C14 O2 C14 C13 38.4(2) 2_665 . . . ? C11 O2 C14 C13 -82.0(15) . . . . ? C11 O2 C14 C13 114(3) 2_665 . . . ? C11 O2 C14 C13 20(2) 3_565 . . . ? Li1 O2 C14 C13 180.000(10) . . . . ? C14 O2 C14 C11 43.6(14) 3_565 . . . ? C14 O2 C14 C11 120.4(17) 2_665 . . . ? C11 O2 C14 C11 -163.9(18) 2_665 . . . ? C11 O2 C14 C11 101.6(10) 3_565 . . . ? Li1 O2 C14 C11 -98.0(15) . . . . ? C14 O2 C14 C14 76.9(5) 2_665 . . 3_565 ? C11 O2 C14 C14 -43.6(14) . . . 3_565 ? C11 O2 C14 C14 153(3) 2_665 . . 3_565 ? C11 O2 C14 C14 58(2) 3_565 . . 3_565 ? Li1 O2 C14 C14 -141.6(2) . . . 3_565 ? C14 O2 C14 C14 -76.9(5) 3_565 . . 2_665 ? C11 O2 C14 C14 -120.4(17) . . . 2_665 ? C11 O2 C14 C14 76(3) 2_665 . . 2_665 ? C11 O2 C14 C14 -19(3) 3_565 . . 2_665 ? Li1 O2 C14 C14 141.6(2) . . . 2_665 ? C12 C13 C14 C12 -123(2) . . . 2_665 ? C12 C13 C14 C12 128(2) 3_565 . . 2_665 ? C14 C13 C14 C12 -139(4) 3_565 . . 2_665 ? C14 C13 C14 C12 146(4) 2_665 . . 2_665 ? C12 C13 C14 C11 -113(3) 2_665 . . 2_665 ? C12 C13 C14 C11 123.8(11) . . . 2_665 ? C12 C13 C14 C11 15.2(11) 3_565 . . 2_665 ? C14 C13 C14 C11 108.7(12) 3_565 . . 2_665 ? C14 C13 C14 C11 33.1(15) 2_665 . . 2_665 ? C12 C13 C14 O2 176(4) 2_665 . . . ? C12 C13 C14 O2 53.0(15) . . . . ? C12 C13 C14 O2 -55.7(14) 3_565 . . . ? C14 C13 C14 O2 37.8(2) 3_565 . . . ? C14 C13 C14 O2 -37.8(2) 2_665 . . . ? C12 C13 C14 C11 120(3) 2_665 . . . ? C12 C13 C14 C11 -3.1(10) . . . . ? C12 C13 C14 C11 -111.8(8) 3_565 . . . ? C14 C13 C14 C11 -18.3(11) 3_565 . . . ? C14 C13 C14 C11 -93.9(13) 2_665 . . . ? C12 C13 C14 C14 139(4) 2_665 . . 3_565 ? C12 C13 C14 C14 15.2(14) . . . 3_565 ? C12 C13 C14 C14 -93.4(13) 3_565 . . 3_565 ? C14 C13 C14 C14 -75.6(4) 2_665 . . 3_565 ? C12 C13 C14 C14 -146(4) 2_665 . . 2_665 ? C12 C13 C14 C14 90.7(17) . . . 2_665 ? C12 C13 C14 C14 -17.9(16) 3_565 . . 2_665 ? C14 C13 C14 C14 75.6(5) 3_565 . . 2_665 ? C14 C11 C14 C12 94.6(18) 3_565 . . 2_665 ? O2 C11 C14 C12 167(2) . . . 2_665 ? C12 C11 C14 C12 72(2) . . . 2_665 ? C14 C11 C14 C11 -91(4) 3_565 . . 2_665 ? O2 C11 C14 C11 -19(2) . . . 2_665 ? C12 C11 C14 C11 -114(3) . . . 2_665 ? C14 C11 C14 O2 -72(2) 3_565 . . . ? C12 C11 C14 O2 -95.4(14) . . . . ? C14 C11 C14 C13 26.2(10) 3_565 . . . ? O2 C11 C14 C13 98.4(16) . . . . ? C12 C11 C14 C13 3.1(10) . . . . ? O2 C11 C14 C14 72(2) . . . 3_565 ? C12 C11 C14 C14 -23.1(10) . . . 3_565 ? C14 C11 C14 C14 -28.4(10) 3_565 . . 2_665 ? O2 C11 C14 C14 43.9(12) . . . 2_665 ? C12 C11 C14 C14 -51.5(9) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.559 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.081 #===END data_mo_dm14564_0m _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Cl3 Li Lu N6 O4' _chemical_formula_weight 874.06 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 161 _space_group_name_H-M_alt 'R 3 c :H' _space_group_name_Hall 'R 3 -2"c' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 12.5731(12) _cell_length_b 12.5731(12) _cell_length_c 43.468(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5950.9(13) _cell_formula_units_Z 6 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5388 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.17 _exptl_crystal_description block _exptl_crystal_colour brick-red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_F_000 2664 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 2.731 _shelx_estimated_absorpt_T_min 0.548 _shelx_estimated_absorpt_T_max 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5754 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18902 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 2.092 _diffrn_reflns_theta_max 30.765 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4113 _reflns_number_gt 3059 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.988 _reflns_Friedel_fraction_max 0.991 _reflns_Friedel_fraction_full 0.998 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.8107P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.008(9) _chemical_absolute_configuration ad _refine_ls_number_reflns 4113 _refine_ls_number_parameters 166 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.6667 0.3333 -0.05215(3) 0.03276(10) Uani 1 3 d S T P . . Cl1 Cl 0.71300(16) 0.18394(15) -0.07984(4) 0.0502(3) Uani 1 1 d . . . . . N1 N 0.6348(4) 0.4505(4) -0.01402(11) 0.0342(9) Uani 1 1 d . . . . . N2 N 0.6417(4) 0.4268(4) 0.01679(10) 0.0323(9) Uani 1 1 d . . . . . C1 C 0.6667 0.3333 0.0277(2) 0.0295(15) Uani 1 3 d S T P . . C5 C 0.6229(6) 0.4982(6) 0.06885(13) 0.0494(15) Uani 1 1 d . . . . . H5A H 0.6057 0.5600 0.0775 0.074 Uiso 1 1 calc R U . . . H5B H 0.5604 0.4164 0.0759 0.074 Uiso 1 1 calc R U . . . H5C H 0.7041 0.5149 0.0757 0.074 Uiso 1 1 calc R U . . . C2 C 0.6207(5) 0.5030(5) 0.03488(13) 0.0383(12) Uani 1 1 d . . . . . C3 C 0.6008(6) 0.5770(5) 0.01544(16) 0.0472(14) Uani 1 1 d . . . . . H3A H 0.5848 0.6405 0.0212 0.057 Uiso 1 1 calc R U . . . C4 C 0.6083(6) 0.5411(5) -0.01468(14) 0.0431(12) Uani 1 1 d . . . . . C6 C 0.5969(8) 0.5945(6) -0.04442(16) 0.0603(18) Uani 1 1 d . . . . . H6A H 0.5773 0.6594 -0.0402 0.090 Uiso 1 1 calc R U . . . H6B H 0.6747 0.6292 -0.0557 0.090 Uiso 1 1 calc R U . . . H6C H 0.5313 0.5300 -0.0568 0.090 Uiso 1 1 calc R U . . . O1 O 0.6458(5) 0.1821(5) 0.32044(12) 0.0694(12) Uani 1 1 d . U . . . C7 C 0.5975(9) 0.1337(9) 0.3502(3) 0.0767(19) Uani 1 1 d . U . . . H7A H 0.5077 0.1013 0.3507 0.092 Uiso 1 1 calc R U . . . H7B H 0.6367 0.1985 0.3660 0.092 Uiso 1 1 calc R U . . . C8 C 0.6249(9) 0.0346(9) 0.3558(3) 0.095(2) Uani 1 1 d . U . . . H8A H 0.6475 0.0337 0.3776 0.114 Uiso 1 1 calc R U . . . H8B H 0.5536 -0.0465 0.3505 0.114 Uiso 1 1 calc R U . . . C9 C 0.7277(11) 0.0645(10) 0.3356(3) 0.108(3) Uani 1 1 d . U . . . H9A H 0.8064 0.1217 0.3457 0.130 Uiso 1 1 calc R U . . . H9B H 0.7291 -0.0104 0.3294 0.130 Uiso 1 1 calc R U . . . C10 C 0.7069(11) 0.1203(10) 0.3101(3) 0.104(3) Uani 1 1 d . U . . . H10A H 0.6560 0.0574 0.2947 0.124 Uiso 1 1 calc R U . . . H10B H 0.7860 0.1793 0.3004 0.124 Uiso 1 1 calc R U . . . Li1 Li 0.6667 0.3333 0.3063(9) 0.085(3) Uani 1 3 d S TU P . . O2 O 0.6667 0.3333 0.2631(3) 0.101(3) Uani 1 3 d DS TU P . . C11 C 0.593(3) 0.373(4) 0.2454(5) 0.101(5) Uani 0.3333 1 d D U P . . H11A H 0.5833 0.4337 0.2566 0.122 Uiso 0.3333 1 d R U P . . H11B H 0.5138 0.3053 0.2406 0.122 Uiso 0.3333 1 d R U P . . C12 C 0.664(4) 0.423(4) 0.2163(5) 0.104(5) Uani 0.3333 1 d D U P . . H12A H 0.7283 0.5060 0.2196 0.125 Uiso 0.3333 1 d R U P . . H12B H 0.6137 0.4200 0.1995 0.125 Uiso 0.3333 1 d R U P . . C13 C 0.714(4) 0.337(4) 0.2110(5) 0.105(5) Uani 0.3333 1 d D U P . . H13A H 0.7983 0.3847 0.2044 0.126 Uiso 0.3333 1 d R U P . . H13B H 0.6683 0.2789 0.1953 0.126 Uiso 0.3333 1 d R U P . . C14 C 0.709(4) 0.275(3) 0.2412(6) 0.111(4) Uani 0.3333 1 d D U P . . H14A H 0.6536 0.1878 0.2392 0.133 Uiso 0.3333 1 d R U P . . H14B H 0.7883 0.2883 0.2471 0.133 Uiso 0.3333 1 d R U P . . 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 Lu1 0.03310(11) 0.03310(11) 0.03209(15) 0.000 0.000 0.01655(6) Cl1 0.0580(10) 0.0471(9) 0.0501(7) -0.0044(7) 0.0070(7) 0.0298(8) N1 0.035(2) 0.031(2) 0.039(2) -0.0037(19) -0.005(2) 0.0174(18) N2 0.033(2) 0.031(2) 0.035(2) -0.0036(18) -0.0045(18) 0.0177(16) C1 0.028(2) 0.028(2) 0.033(4) 0.000 0.000 0.0138(11) C5 0.053(4) 0.047(3) 0.044(3) -0.011(3) 0.007(3) 0.022(3) C2 0.033(3) 0.034(3) 0.045(3) -0.011(2) 0.000(2) 0.014(2) C3 0.049(3) 0.035(3) 0.062(4) -0.008(3) -0.002(3) 0.024(3) C4 0.047(3) 0.038(3) 0.052(3) -0.005(3) -0.009(3) 0.027(3) C6 0.086(5) 0.055(4) 0.064(4) -0.002(3) -0.014(4) 0.053(4) O1 0.076(3) 0.074(3) 0.067(3) -0.005(2) 0.012(2) 0.044(2) C7 0.069(4) 0.068(4) 0.094(5) 0.011(4) 0.017(4) 0.035(3) C8 0.083(4) 0.072(4) 0.129(5) 0.023(4) 0.014(4) 0.038(4) C9 0.092(5) 0.082(4) 0.152(6) 0.012(5) 0.019(5) 0.046(4) C10 0.100(5) 0.090(5) 0.116(5) -0.012(4) 0.030(4) 0.044(4) Li1 0.091(4) 0.091(4) 0.071(6) 0.000 0.000 0.046(2) O2 0.111(4) 0.111(4) 0.082(5) 0.000 0.000 0.056(2) C11 0.113(7) 0.114(7) 0.086(7) 0.006(6) 0.000(6) 0.063(6) C12 0.117(8) 0.113(7) 0.093(8) 0.005(7) 0.001(7) 0.065(7) C13 0.117(7) 0.115(7) 0.098(7) 0.002(7) 0.004(7) 0.068(7) C14 0.119(5) 0.118(5) 0.103(5) 0.000(5) 0.004(5) 0.066(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 Lu1 N1 2.380(5) 3_665 ? Lu1 N1 2.380(5) 2_655 ? Lu1 N1 2.380(5) . ? Lu1 Cl1 2.5320(16) . ? Lu1 Cl1 2.5320(16) 2_655 ? Lu1 Cl1 2.5320(16) 3_665 ? N1 C4 1.338(7) . ? N1 N2 1.384(6) . ? N2 C2 1.364(7) . ? N2 C1 1.440(5) . ? C1 N2 1.440(5) 3_665 ? C1 N2 1.440(5) 2_655 ? C5 C2 1.478(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C2 C3 1.369(9) . ? C3 C4 1.403(9) . ? C3 H3A 0.9500 . ? C4 C6 1.497(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O1 C10 1.412(11) . ? O1 C7 1.428(12) . ? O1 Li1 1.887(14) . ? C7 C8 1.471(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.448(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.403(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? Li1 O2 1.88(4) . ? Li1 O1 1.887(14) 2_655 ? Li1 O1 1.887(14) 3_665 ? O2 C14 1.460(13) 3_665 ? O2 C14 1.460(13) 2_655 ? O2 C14 1.460(13) . ? O2 C11 1.470(14) . ? O2 C11 1.470(14) 2_655 ? O2 C11 1.470(14) 3_665 ? C11 C14 0.93(3) 3_665 ? C11 C12 1.494(14) . ? C11 C13 1.72(5) 2_655 ? C11 C14 1.45(3) 2_655 ? C11 C12 2.01(5) 2_655 ? C11 C13 2.00(4) 3_665 ? C11 C11 2.17(3) 3_665 ? C11 C11 2.17(3) 2_655 ? C11 H11A 0.9602 . ? C11 H11B 0.9600 . ? C12 C13 0.61(5) 2_655 ? C12 C14 1.29(4) 2_655 ? C12 C13 1.507(14) . ? C12 C13 1.55(7) 3_665 ? C12 C12 1.97(5) 2_655 ? C12 C12 1.97(5) 3_665 ? C12 C11 2.01(5) 3_665 ? C12 C14 1.84(4) 3_665 ? C12 H12A 0.9600 . ? C12 H12B 0.9598 . ? C13 C12 0.61(5) 3_665 ? C13 C13 1.00(6) 2_655 ? C13 C13 1.00(6) 3_665 ? C13 C14 1.513(14) . ? C13 C11 1.72(5) 3_665 ? C13 C12 1.55(7) 2_655 ? C13 C11 2.00(4) 2_655 ? C13 C14 1.75(5) 2_655 ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C14 C11 0.93(3) 2_655 ? C14 C12 1.29(4) 3_665 ? C14 C11 1.45(3) 3_665 ? C14 C13 1.75(5) 3_665 ? C14 C12 1.84(4) 2_655 ? C14 H14A 0.9601 . ? C14 H14B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Lu1 N1 76.88(17) 3_665 2_655 ? N1 Lu1 N1 76.88(17) 3_665 . ? N1 Lu1 N1 76.88(17) 2_655 . ? N1 Lu1 Cl1 90.12(13) 3_665 . ? N1 Lu1 Cl1 91.63(12) 2_655 . ? N1 Lu1 Cl1 164.23(12) . . ? N1 Lu1 Cl1 91.63(12) 3_665 2_655 ? N1 Lu1 Cl1 164.23(12) 2_655 2_655 ? N1 Lu1 Cl1 90.12(13) . 2_655 ? Cl1 Lu1 Cl1 99.26(6) . 2_655 ? N1 Lu1 Cl1 164.23(12) 3_665 3_665 ? N1 Lu1 Cl1 90.12(13) 2_655 3_665 ? N1 Lu1 Cl1 91.63(12) . 3_665 ? Cl1 Lu1 Cl1 99.26(6) . 3_665 ? Cl1 Lu1 Cl1 99.26(6) 2_655 3_665 ? C4 N1 N2 105.8(4) . . ? C4 N1 Lu1 134.7(4) . . ? N2 N1 Lu1 119.5(3) . . ? C2 N2 N1 110.6(4) . . ? C2 N2 C1 125.6(5) . . ? N1 N2 C1 123.8(5) . . ? N2 C1 N2 109.7(4) 3_665 2_655 ? N2 C1 N2 109.7(4) 3_665 . ? N2 C1 N2 109.7(4) 2_655 . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C2 C3 106.7(5) . . ? N2 C2 C5 122.2(5) . . ? C3 C2 C5 131.2(5) . . ? C2 C3 C4 107.0(5) . . ? C2 C3 H3A 126.5 . . ? C4 C3 H3A 126.5 . . ? N1 C4 C3 109.8(5) . . ? N1 C4 C6 121.4(5) . . ? C3 C4 C6 128.7(5) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 O1 C7 106.6(7) . . ? C10 O1 Li1 127.7(10) . . ? C7 O1 Li1 122.6(11) . . ? O1 C7 C8 106.4(8) . . ? O1 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O1 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C7 103.6(9) . . ? C9 C8 H8A 111.0 . . ? C7 C8 H8A 111.0 . . ? C9 C8 H8B 111.0 . . ? C7 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? C10 C9 C8 104.1(9) . . ? C10 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? C10 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 109.0 . . ? C9 C10 O1 108.3(9) . . ? C9 C10 H10A 110.0 . . ? O1 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? O1 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? O2 Li1 O1 109.0(11) . 2_655 ? O2 Li1 O1 109.0(11) . 3_665 ? O1 Li1 O1 109.9(11) 2_655 3_665 ? O2 Li1 O1 109.0(11) . . ? O1 Li1 O1 109.9(11) 2_655 . ? O1 Li1 O1 109.9(11) 3_665 . ? C14 O2 C14 81.8(14) 3_665 2_655 ? C14 O2 C14 81.8(14) 3_665 . ? C14 O2 C14 81.8(14) 2_655 . ? C14 O2 C11 37.0(14) 3_665 . ? C14 O2 C11 59.4(13) 2_655 . ? C14 O2 C11 106.2(9) . . ? C14 O2 C11 59.4(13) 3_665 2_655 ? C14 O2 C11 106.2(9) 2_655 2_655 ? C14 O2 C11 37.0(14) . 2_655 ? C11 O2 C11 95.0(12) . 2_655 ? C14 O2 C11 106.2(9) 3_665 3_665 ? C14 O2 C11 37.0(14) 2_655 3_665 ? C14 O2 C11 59.4(13) . 3_665 ? C11 O2 C11 95.0(12) . 3_665 ? C11 O2 C11 95.0(12) 2_655 3_665 ? C14 O2 Li1 130.9(9) 3_665 . ? C14 O2 Li1 130.9(9) 2_655 . ? C14 O2 Li1 130.9(9) . . ? C11 O2 Li1 121.6(9) . . ? C11 O2 Li1 121.6(9) 2_655 . ? C11 O2 Li1 121.6(9) 3_665 . ? C14 C11 O2 70.9(13) 3_665 . ? C14 C11 C12 96(3) 3_665 . ? O2 C11 C12 103.8(10) . . ? C14 C11 C13 76(3) 3_665 2_655 ? O2 C11 C13 94.0(18) . 2_655 ? C12 C11 C13 20.3(17) . 2_655 ? C14 C11 C14 105(3) 3_665 2_655 ? O2 C11 C14 60.0(9) . 2_655 ? C12 C11 C14 52.0(17) . 2_655 ? C13 C11 C14 56.3(15) 2_655 2_655 ? C14 C11 C12 30(3) 3_665 2_655 ? O2 C11 C12 82.5(15) . 2_655 ? C12 C11 C12 66(3) . 2_655 ? C13 C11 C12 46.8(13) 2_655 2_655 ? C14 C11 C12 88(2) 2_655 2_655 ? C14 C11 C13 46(2) 3_665 3_665 ? O2 C11 C13 83.2(15) . 3_665 ? C12 C11 C13 50(2) . 3_665 ? C13 C11 C13 30(2) 2_655 3_665 ? C14 C11 C13 74(2) 2_655 3_665 ? C12 C11 C13 17.4(14) 2_655 3_665 ? C14 C11 C11 88.9(17) 3_665 3_665 ? O2 C11 C11 42.5(6) . 3_665 ? C12 C11 C11 63.6(17) . 3_665 ? C13 C11 C11 60.7(15) 2_655 3_665 ? C14 C11 C11 19.2(10) 2_655 3_665 ? C12 C11 C11 79.2(13) 2_655 3_665 ? C13 C11 C11 67.9(9) 3_665 3_665 ? C14 C11 C11 30.9(14) 3_665 2_655 ? O2 C11 C11 42.5(6) . 2_655 ? C12 C11 C11 91.6(10) . 2_655 ? C13 C11 C11 72.7(12) 2_655 2_655 ? C14 C11 C11 77.9(11) 2_655 2_655 ? C12 C11 C11 41.7(8) 2_655 2_655 ? C13 C11 C11 48.5(14) 3_665 2_655 ? C11 C11 C11 59.999(3) 3_665 2_655 ? C14 C11 H11A 148.7 3_665 . ? O2 C11 H11A 111.0 . . ? C12 C11 H11A 112.9 . . ? C13 C11 H11A 133.1 2_655 . ? C14 C11 H11A 102.5 2_655 . ? C12 C11 H11A 165.6 2_655 . ? C13 C11 H11A 161.4 3_665 . ? C11 C11 H11A 113.9 3_665 . ? C11 C11 H11A 149.6 2_655 . ? C14 C11 H11B 47.2 3_665 . ? O2 C11 H11B 111.2 . . ? C12 C11 H11B 108.9 . . ? C13 C11 H11B 96.9 2_655 . ? C14 C11 H11B 148.2 2_655 . ? C12 C11 H11B 59.8 2_655 . ? C13 C11 H11B 75.0 3_665 . ? C11 C11 H11B 135.7 3_665 . ? C11 C11 H11B 77.5 2_655 . ? H11A C11 H11B 109.0 . . ? C13 C12 C14 99(4) 2_655 2_655 ? C13 C12 C11 101(5) 2_655 . ? C14 C12 C11 62.3(14) 2_655 . ? C13 C12 C13 26(7) 2_655 . ? C14 C12 C13 77(2) 2_655 . ? C11 C12 C13 102.1(11) . . ? C13 C12 C13 20(5) 2_655 3_665 ? C14 C12 C13 96(2) 2_655 3_665 ? C11 C12 C13 82(2) . 3_665 ? C13 C12 C13 38(2) . 3_665 ? C13 C12 C12 34(4) 2_655 2_655 ? C14 C12 C12 95.0(15) 2_655 2_655 ? C11 C12 C12 69(3) . 2_655 ? C13 C12 C12 51(2) . 2_655 ? C13 C12 C12 14.4(15) 3_665 2_655 ? C13 C12 C12 39(5) 2_655 3_665 ? C14 C12 C12 65(2) 2_655 3_665 ? C11 C12 C12 99.8(12) . 3_665 ? C13 C12 C12 13.1(18) . 3_665 ? C13 C12 C12 48.9(16) 3_665 3_665 ? C12 C12 C12 60.000(4) 2_655 3_665 ? C13 C12 C11 80(4) 2_655 3_665 ? C14 C12 C11 21.0(18) 2_655 3_665 ? C11 C12 C11 74.8(12) . 3_665 ? C13 C12 C11 56.3(15) . 3_665 ? C13 C12 C11 80.7(17) 3_665 3_665 ? C12 C12 C11 84.1(10) 2_655 3_665 ? C12 C12 C11 44.0(9) 3_665 3_665 ? C13 C12 C14 71(5) 2_655 3_665 ? C14 C12 C14 72.9(11) 2_655 3_665 ? C11 C12 C14 30.2(14) . 3_665 ? C13 C12 C14 77.5(14) . 3_665 ? C13 C12 C14 52.1(14) 3_665 3_665 ? C12 C12 C14 39.4(19) 2_655 3_665 ? C12 C12 C14 79.8(17) 3_665 3_665 ? C11 C12 C14 74.7(7) 3_665 3_665 ? C13 C12 H12A 134.7 2_655 . ? C14 C12 H12A 68.1 2_655 . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 112.3 . . ? C13 C12 H12A 150.4 3_665 . ? C12 C12 H12A 159.8 2_655 . ? C12 C12 H12A 101.5 3_665 . ? C11 C12 H12A 76.3 3_665 . ? C14 C12 H12A 135.5 3_665 . ? C13 C12 H12B 88.3 2_655 . ? C14 C12 H12B 171.4 2_655 . ? C11 C12 H12B 112.5 . . ? C13 C12 H12B 111.4 . . ? C13 C12 H12B 90.1 3_665 . ? C12 C12 H12B 89.1 2_655 . ? C12 C12 H12B 123.5 3_665 . ? C11 C12 H12B 167.5 3_665 . ? C14 C12 H12B 106.2 3_665 . ? H12A C12 H12B 109.3 . . ? C12 C13 C13 148(8) 3_665 2_655 ? C12 C13 C13 138(10) 3_665 3_665 ? C13 C13 C13 60.002(16) 2_655 3_665 ? C12 C13 C12 133(6) 3_665 . ? C13 C13 C12 16(3) 2_655 . ? C13 C13 C12 73(4) 3_665 . ? C12 C13 C14 57(3) 3_665 . ? C13 C13 C14 112.9(18) 2_655 . ? C13 C13 C14 86(4) 3_665 . ? C12 C13 C14 108.3(7) . . ? C12 C13 C11 58(4) 3_665 3_665 ? C13 C13 C11 91(3) 2_655 3_665 ? C13 C13 C11 115.8(9) 3_665 3_665 ? C12 C13 C11 76.9(19) . 3_665 ? C14 C13 C11 52.9(15) . 3_665 ? C12 C13 C12 126(6) 3_665 2_655 ? C13 C13 C12 69(4) 2_655 2_655 ? C13 C13 C12 12(3) 3_665 2_655 ? C12 C13 C12 80.3(17) . 2_655 ? C14 C13 C12 74(2) . 2_655 ? C11 C13 C12 109.3(12) 3_665 2_655 ? C12 C13 C11 82(4) 3_665 2_655 ? C13 C13 C11 96(3) 2_655 2_655 ? C13 C13 C11 59(3) 3_665 2_655 ? C12 C13 C11 98.0(11) . 2_655 ? C14 C13 C11 26.3(13) . 2_655 ? C11 C13 C11 70.9(9) 3_665 2_655 ? C12 C13 C11 47.7(13) 2_655 2_655 ? C12 C13 C14 89(5) 3_665 2_655 ? C13 C13 C14 60(2) 2_655 2_655 ? C13 C13 C14 97(2) 3_665 2_655 ? C12 C13 C14 46.0(15) . 2_655 ? C14 C13 C14 71.5(12) . 2_655 ? C11 C13 C14 31.1(13) 3_665 2_655 ? C12 C13 C14 95.8(19) 2_655 2_655 ? C11 C13 C14 77.1(6) 2_655 2_655 ? C12 C13 H13A 53.1 3_665 . ? C13 C13 H13A 118.7 2_655 . ? C13 C13 H13A 162.6 3_665 . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 109.4 . . ? C11 C13 H13A 81.2 3_665 . ? C12 C13 H13A 167.7 2_655 . ? C11 C13 H13A 135.3 2_655 . ? C14 C13 H13A 96.5 2_655 . ? C12 C13 H13B 116.8 3_665 . ? C13 C13 H13B 95.1 2_655 . ? C13 C13 H13B 56.2 3_665 . ? C12 C13 H13B 110.3 . . ? C14 C13 H13B 111.4 . . ? C11 C13 H13B 164.3 3_665 . ? C12 C13 H13B 60.0 2_655 . ? C11 C13 H13B 94.0 2_655 . ? C14 C13 H13B 151.4 2_655 . ? H13A C13 H13B 108.4 . . ? C11 C14 C12 129(4) 2_655 3_665 ? C11 C14 O2 72.0(14) 2_655 . ? C12 C14 O2 116(2) 3_665 . ? C11 C14 C13 108(3) 2_655 . ? C12 C14 C13 23(2) 3_665 . ? O2 C14 C13 103.6(9) . . ? C11 C14 C11 129.8(19) 2_655 3_665 ? C12 C14 C11 65.7(17) 3_665 3_665 ? O2 C14 C11 60.6(10) . 3_665 ? C13 C14 C11 71(2) . 3_665 ? C11 C14 C13 73(3) 2_655 3_665 ? C12 C14 C13 57.1(16) 3_665 3_665 ? O2 C14 C13 93.1(18) . 3_665 ? C13 C14 C13 35(3) . 3_665 ? C11 C14 C13 93(2) 3_665 3_665 ? C11 C14 C12 54(2) 2_655 2_655 ? C12 C14 C12 76(3) 3_665 2_655 ? O2 C14 C12 89.1(18) . 2_655 ? C13 C14 C12 54(3) . 2_655 ? C11 C14 C12 108(3) 3_665 2_655 ? C13 C14 C12 19.3(18) 3_665 2_655 ? C11 C14 H14A 43.3 2_655 . ? C12 C14 H14A 117.5 3_665 . ? O2 C14 H14A 113.0 . . ? C13 C14 H14A 109.6 . . ? C11 C14 H14A 173.1 3_665 . ? C13 C14 H14A 84.2 3_665 . ? C12 C14 H14A 68.6 2_655 . ? C11 C14 H14B 138.8 2_655 . ? C12 C14 H14B 88.4 3_665 . ? O2 C14 H14B 109.9 . . ? C13 C14 H14B 111.6 . . ? C11 C14 H14B 76.7 3_665 . ? C13 C14 H14B 144.8 3_665 . ? C12 C14 H14B 159.3 2_655 . ? H14A C14 H14B 109.0 . . ? 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 C4 N1 N2 C2 -0.5(6) . . . . ? Lu1 N1 N2 C2 -179.9(3) . . . . ? C4 N1 N2 C1 178.9(4) . . . . ? Lu1 N1 N2 C1 -0.5(6) . . . . ? C2 N2 C1 N2 -120.1(7) . . . 3_665 ? N1 N2 C1 N2 60.6(6) . . . 3_665 ? C2 N2 C1 N2 119.3(7) . . . 2_655 ? N1 N2 C1 N2 -60.0(6) . . . 2_655 ? N1 N2 C2 C3 -0.4(6) . . . . ? C1 N2 C2 C3 -179.8(4) . . . . ? N1 N2 C2 C5 -179.8(5) . . . . ? C1 N2 C2 C5 0.8(8) . . . . ? N2 C2 C3 C4 1.1(6) . . . . ? C5 C2 C3 C4 -179.6(6) . . . . ? N2 N1 C4 C3 1.2(6) . . . . ? Lu1 N1 C4 C3 -179.6(4) . . . . ? N2 N1 C4 C6 178.2(6) . . . . ? Lu1 N1 C4 C6 -2.5(9) . . . . ? C2 C3 C4 N1 -1.4(7) . . . . ? C2 C3 C4 C6 -178.2(7) . . . . ? C10 O1 C7 C8 -4.2(11) . . . . ? Li1 O1 C7 C8 -165.6(8) . . . . ? O1 C7 C8 C9 22.7(12) . . . . ? C7 C8 C9 C10 -32.6(11) . . . . ? C8 C9 C10 O1 31.3(11) . . . . ? C7 O1 C10 C9 -17.0(12) . . . . ? Li1 O1 C10 C9 143.2(12) . . . . ? C10 O1 Li1 O2 46.4(10) . . . . ? C7 O1 Li1 O2 -156.3(7) . . . . ? C10 O1 Li1 O1 -73(2) . . . 2_655 ? C7 O1 Li1 O1 84.3(12) . . . 2_655 ? C10 O1 Li1 O1 165.8(11) . . . 3_665 ? C7 O1 Li1 O1 -36.9(18) . . . 3_665 ? O1 Li1 O2 C14 -152(2) 2_655 . . 3_665 ? O1 Li1 O2 C14 -32(2) 3_665 . . 3_665 ? O1 Li1 O2 C14 88(2) . . . 3_665 ? O1 Li1 O2 C14 -32(2) 2_655 . . 2_655 ? O1 Li1 O2 C14 88(2) 3_665 . . 2_655 ? O1 Li1 O2 C14 -152(2) . . . 2_655 ? O1 Li1 O2 C14 88(2) 2_655 . . . ? O1 Li1 O2 C14 -152(2) 3_665 . . . ? O1 Li1 O2 C14 -32(2) . . . . ? O1 Li1 O2 C11 -107(2) 2_655 . . . ? O1 Li1 O2 C11 13(2) 3_665 . . . ? O1 Li1 O2 C11 133(2) . . . . ? O1 Li1 O2 C11 133(2) 2_655 . . 2_655 ? O1 Li1 O2 C11 -107(2) 3_665 . . 2_655 ? O1 Li1 O2 C11 13(2) . . . 2_655 ? O1 Li1 O2 C11 13(2) 2_655 . . 3_665 ? O1 Li1 O2 C11 133(2) 3_665 . . 3_665 ? O1 Li1 O2 C11 -107(2) . . . 3_665 ? C14 O2 C11 C14 121(4) 2_655 . . 3_665 ? C14 O2 C11 C14 51(2) . . . 3_665 ? C11 O2 C11 C14 15(3) 2_655 . . 3_665 ? C11 O2 C11 C14 110.4(17) 3_665 . . 3_665 ? Li1 O2 C11 C14 -117(2) . . . 3_665 ? C14 O2 C11 C12 -92(3) 3_665 . . . ? C14 O2 C11 C12 29(2) 2_655 . . . ? C14 O2 C11 C12 -41(3) . . . . ? C11 O2 C11 C12 -76.9(18) 2_655 . . . ? C11 O2 C11 C12 19(2) 3_665 . . . ? Li1 O2 C11 C12 151(2) . . . . ? C14 O2 C11 C13 -74(3) 3_665 . . 2_655 ? C14 O2 C11 C13 46.9(10) 2_655 . . 2_655 ? C14 O2 C11 C13 -23(2) . . . 2_655 ? C11 O2 C11 C13 -58.9(8) 2_655 . . 2_655 ? C11 O2 C11 C13 36.6(18) 3_665 . . 2_655 ? Li1 O2 C11 C13 168.8(12) . . . 2_655 ? C14 O2 C11 C14 -121(4) 3_665 . . 2_655 ? C14 O2 C11 C14 -69.9(17) . . . 2_655 ? C11 O2 C11 C14 -105.9(10) 2_655 . . 2_655 ? C11 O2 C11 C14 -10(2) 3_665 . . 2_655 ? Li1 O2 C11 C14 121.9(14) . . . 2_655 ? C14 O2 C11 C12 -28(3) 3_665 . . 2_655 ? C14 O2 C11 C12 92.5(17) 2_655 . . 2_655 ? C14 O2 C11 C12 22.6(17) . . . 2_655 ? C11 O2 C11 C12 -13.4(14) 2_655 . . 2_655 ? C11 O2 C11 C12 82.1(12) 3_665 . . 2_655 ? Li1 O2 C11 C12 -145.7(11) . . . 2_655 ? C14 O2 C11 C13 -45.8(18) 3_665 . . 3_665 ? C14 O2 C11 C13 75(2) 2_655 . . 3_665 ? C14 O2 C11 C13 5.0(18) . . . 3_665 ? C11 O2 C11 C13 -31.0(18) 2_655 . . 3_665 ? C11 O2 C11 C13 64.6(8) 3_665 . . 3_665 ? Li1 O2 C11 C13 -163.2(12) . . . 3_665 ? C14 O2 C11 C11 -110.4(17) 3_665 . . 3_665 ? C14 O2 C11 C11 10(2) 2_655 . . 3_665 ? C14 O2 C11 C11 -59.5(15) . . . 3_665 ? C11 O2 C11 C11 -95.5(14) 2_655 . . 3_665 ? Li1 O2 C11 C11 132.2(7) . . . 3_665 ? C14 O2 C11 C11 -15(3) 3_665 . . 2_655 ? C14 O2 C11 C11 105.9(10) 2_655 . . 2_655 ? C14 O2 C11 C11 36.0(16) . . . 2_655 ? C11 O2 C11 C11 95.5(14) 3_665 . . 2_655 ? Li1 O2 C11 C11 -132.2(7) . . . 2_655 ? C14 C11 C12 C13 -9(7) 3_665 . . 2_655 ? O2 C11 C12 C13 63(7) . . . 2_655 ? C14 C11 C12 C13 95(6) 2_655 . . 2_655 ? C12 C11 C12 C13 -13(5) 2_655 . . 2_655 ? C13 C11 C12 C13 -6(6) 3_665 . . 2_655 ? C11 C11 C12 C13 76(6) 3_665 . . 2_655 ? C11 C11 C12 C13 21(7) 2_655 . . 2_655 ? C14 C11 C12 C14 -104(2) 3_665 . . 2_655 ? O2 C11 C12 C14 -32(2) . . . 2_655 ? C13 C11 C12 C14 -95(6) 2_655 . . 2_655 ? C12 C11 C12 C14 -108(3) 2_655 . . 2_655 ? C13 C11 C12 C14 -101(3) 3_665 . . 2_655 ? C11 C11 C12 C14 -18.2(17) 3_665 . . 2_655 ? C11 C11 C12 C14 -73.3(19) 2_655 . . 2_655 ? C14 C11 C12 C13 -36(3) 3_665 . . . ? O2 C11 C12 C13 36(3) . . . . ? C13 C11 C12 C13 -27(7) 2_655 . . . ? C14 C11 C12 C13 68(3) 2_655 . . . ? C12 C11 C12 C13 -39.6(19) 2_655 . . . ? C13 C11 C12 C13 -32.7(17) 3_665 . . . ? C11 C11 C12 C13 50(2) 3_665 . . . ? C11 C11 C12 C13 -5(3) 2_655 . . . ? C14 C11 C12 C13 -3(2) 3_665 . . 3_665 ? O2 C11 C12 C13 69(3) . . . 3_665 ? C13 C11 C12 C13 6(6) 2_655 . . 3_665 ? C14 C11 C12 C13 101(3) 2_655 . . 3_665 ? C12 C11 C12 C13 -6.8(14) 2_655 . . 3_665 ? C11 C11 C12 C13 82.5(19) 3_665 . . 3_665 ? C11 C11 C12 C13 27(2) 2_655 . . 3_665 ? C14 C11 C12 C12 4(2) 3_665 . . 2_655 ? O2 C11 C12 C12 75(3) . . . 2_655 ? C13 C11 C12 C12 13(5) 2_655 . . 2_655 ? C14 C11 C12 C12 108(2) 2_655 . . 2_655 ? C13 C11 C12 C12 6.8(14) 3_665 . . 2_655 ? C11 C11 C12 C12 89.3(13) 3_665 . . 2_655 ? C11 C11 C12 C12 34(2) 2_655 . . 2_655 ? C14 C11 C12 C12 -49(3) 3_665 . . 3_665 ? O2 C11 C12 C12 23(3) . . . 3_665 ? C13 C11 C12 C12 -40(5) 2_655 . . 3_665 ? C14 C11 C12 C12 55(3) 2_655 . . 3_665 ? C12 C11 C12 C12 -52.7(8) 2_655 . . 3_665 ? C13 C11 C12 C12 -45.9(18) 3_665 . . 3_665 ? C11 C11 C12 C12 37(2) 3_665 . . 3_665 ? C11 C11 C12 C12 -18(3) 2_655 . . 3_665 ? C14 C11 C12 C11 -85.8(16) 3_665 . . 3_665 ? O2 C11 C12 C11 -13.9(15) . . . 3_665 ? C13 C11 C12 C11 -76(6) 2_655 . . 3_665 ? C14 C11 C12 C11 18.2(16) 2_655 . . 3_665 ? C12 C11 C12 C11 -89.3(13) 2_655 . . 3_665 ? C13 C11 C12 C11 -82.5(19) 3_665 . . 3_665 ? C11 C11 C12 C11 -55.1(9) 2_655 . . 3_665 ? O2 C11 C12 C14 71.8(16) . . . 3_665 ? C13 C11 C12 C14 9(7) 2_655 . . 3_665 ? C14 C11 C12 C14 104(2) 2_655 . . 3_665 ? C12 C11 C12 C14 -4(2) 2_655 . . 3_665 ? C13 C11 C12 C14 3(2) 3_665 . . 3_665 ? C11 C11 C12 C14 85.8(16) 3_665 . . 3_665 ? C11 C11 C12 C14 30.7(14) 2_655 . . 3_665 ? C13 C12 C13 C12 -172(14) 2_655 . . 3_665 ? C14 C12 C13 C12 -24(5) 2_655 . . 3_665 ? C11 C12 C13 C12 -81(5) . . . 3_665 ? C13 C12 C13 C12 -141(7) 3_665 . . 3_665 ? C12 C12 C13 C12 -131(6) 2_655 . . 3_665 ? C11 C12 C13 C12 -19(5) 3_665 . . 3_665 ? C14 C12 C13 C12 -99(5) 3_665 . . 3_665 ? C14 C12 C13 C13 148(9) 2_655 . . 2_655 ? C11 C12 C13 C13 91(9) . . . 2_655 ? C13 C12 C13 C13 31(7) 3_665 . . 2_655 ? C12 C12 C13 C13 41(8) 2_655 . . 2_655 ? C12 C12 C13 C13 172(14) 3_665 . . 2_655 ? C11 C12 C13 C13 153(9) 3_665 . . 2_655 ? C14 C12 C13 C13 73(9) 3_665 . . 2_655 ? C13 C12 C13 C13 -31(7) 2_655 . . 3_665 ? C14 C12 C13 C13 118(2) 2_655 . . 3_665 ? C11 C12 C13 C13 60(3) . . . 3_665 ? C12 C12 C13 C13 9.9(14) 2_655 . . 3_665 ? C12 C12 C13 C13 141(7) 3_665 . . 3_665 ? C11 C12 C13 C13 122(2) 3_665 . . 3_665 ? C14 C12 C13 C13 42.6(18) 3_665 . . 3_665 ? C13 C12 C13 C14 -110(10) 2_655 . . . ? C14 C12 C13 C14 38(3) 2_655 . . . ? C11 C12 C13 C14 -19(4) . . . . ? C13 C12 C13 C14 -79(4) 3_665 . . . ? C12 C12 C13 C14 -69(3) 2_655 . . . ? C12 C12 C13 C14 62(5) 3_665 . . . ? C11 C12 C13 C14 43(2) 3_665 . . . ? C14 C12 C13 C14 -37(3) 3_665 . . . ? C13 C12 C13 C11 -153(9) 2_655 . . 3_665 ? C14 C12 C13 C11 -4.8(15) 2_655 . . 3_665 ? C11 C12 C13 C11 -62(3) . . . 3_665 ? C13 C12 C13 C11 -122(2) 3_665 . . 3_665 ? C12 C12 C13 C11 -112.6(12) 2_655 . . 3_665 ? C12 C12 C13 C11 19(6) 3_665 . . 3_665 ? C14 C12 C13 C11 -79.9(10) 3_665 . . 3_665 ? C13 C12 C13 C12 -41(8) 2_655 . . 2_655 ? C14 C12 C13 C12 107.8(17) 2_655 . . 2_655 ? C11 C12 C13 C12 50(3) . . . 2_655 ? C13 C12 C13 C12 -9.9(14) 3_665 . . 2_655 ? C12 C12 C13 C12 131(6) 3_665 . . 2_655 ? C11 C12 C13 C12 112.6(12) 3_665 . . 2_655 ? C14 C12 C13 C12 32.8(14) 3_665 . . 2_655 ? C13 C12 C13 C11 -85(9) 2_655 . . 2_655 ? C14 C12 C13 C11 63.3(18) 2_655 . . 2_655 ? C11 C12 C13 C11 6(3) . . . 2_655 ? C13 C12 C13 C11 -54(2) 3_665 . . 2_655 ? C12 C12 C13 C11 -44.5(13) 2_655 . . 2_655 ? C12 C12 C13 C11 87(5) 3_665 . . 2_655 ? C11 C12 C13 C11 68.1(10) 3_665 . . 2_655 ? C14 C12 C13 C11 -11.7(15) 3_665 . . 2_655 ? C13 C12 C13 C14 -148(9) 2_655 . . 2_655 ? C11 C12 C13 C14 -57.4(16) . . . 2_655 ? C13 C12 C13 C14 -118(2) 3_665 . . 2_655 ? C12 C12 C13 C14 -107.8(17) 2_655 . . 2_655 ? C12 C12 C13 C14 24(5) 3_665 . . 2_655 ? C11 C12 C13 C14 4.8(15) 3_665 . . 2_655 ? C14 C12 C13 C14 -75.1(12) 3_665 . . 2_655 ? C14 O2 C14 C11 -48(3) 3_665 . . 2_655 ? C14 O2 C14 C11 -131(2) 2_655 . . 2_655 ? C11 O2 C14 C11 -76(2) . . . 2_655 ? C11 O2 C14 C11 -163(3) 3_665 . . 2_655 ? Li1 O2 C14 C11 90(2) . . . 2_655 ? C14 O2 C14 C12 77.2(19) 3_665 . . 3_665 ? C14 O2 C14 C12 -6(3) 2_655 . . 3_665 ? C11 O2 C14 C12 49(3) . . . 3_665 ? C11 O2 C14 C12 126(5) 2_655 . . 3_665 ? C11 O2 C14 C12 -37(2) 3_665 . . 3_665 ? Li1 O2 C14 C12 -144(2) . . . 3_665 ? C14 O2 C14 C13 56(2) 3_665 . . . ? C14 O2 C14 C13 -27(2) 2_655 . . . ? C11 O2 C14 C13 28(3) . . . . ? C11 O2 C14 C13 104(3) 2_655 . . . ? C11 O2 C14 C13 -58(3) 3_665 . . . ? Li1 O2 C14 C13 -165(2) . . . . ? C14 O2 C14 C11 114.4(13) 3_665 . . 3_665 ? C14 O2 C14 C11 31.5(19) 2_655 . . 3_665 ? C11 O2 C14 C11 86.2(15) . . . 3_665 ? C11 O2 C14 C11 163(3) 2_655 . . 3_665 ? Li1 O2 C14 C11 -107.0(15) . . . 3_665 ? C14 O2 C14 C13 22.4(13) 3_665 . . 3_665 ? C14 O2 C14 C13 -60.4(14) 2_655 . . 3_665 ? C11 O2 C14 C13 -6(2) . . . 3_665 ? C11 O2 C14 C13 71(3) 2_655 . . 3_665 ? C11 O2 C14 C13 -92.0(17) 3_665 . . 3_665 ? Li1 O2 C14 C13 161.0(13) . . . 3_665 ? C14 O2 C14 C12 3.6(17) 3_665 . . 2_655 ? C14 O2 C14 C12 -79.3(9) 2_655 . . 2_655 ? C11 O2 C14 C12 -24.6(17) . . . 2_655 ? C11 O2 C14 C12 51.9(16) 2_655 . . 2_655 ? C11 O2 C14 C12 -111(2) 3_665 . . 2_655 ? Li1 O2 C14 C12 142.2(13) . . . 2_655 ? C12 C13 C14 C11 -160(6) 3_665 . . 2_655 ? C13 C13 C14 C11 54(6) 2_655 . . 2_655 ? C13 C13 C14 C11 0(5) 3_665 . . 2_655 ? C12 C13 C14 C11 70(4) . . . 2_655 ? C11 C13 C14 C11 127(2) 3_665 . . 2_655 ? C12 C13 C14 C11 -3(3) 2_655 . . 2_655 ? C14 C13 C14 C11 98(2) 2_655 . . 2_655 ? C13 C13 C14 C12 -146(11) 2_655 . . 3_665 ? C13 C13 C14 C12 160(9) 3_665 . . 3_665 ? C12 C13 C14 C12 -130(7) . . . 3_665 ? C11 C13 C14 C12 -73(6) 3_665 . . 3_665 ? C12 C13 C14 C12 157(6) 2_655 . . 3_665 ? C11 C13 C14 C12 160(6) 2_655 . . 3_665 ? C14 C13 C14 C12 -101(7) 2_655 . . 3_665 ? C12 C13 C14 O2 125(6) 3_665 . . . ? C13 C13 C14 O2 -21(6) 2_655 . . . ? C13 C13 C14 O2 -75(5) 3_665 . . . ? C12 C13 C14 O2 -5(4) . . . . ? C11 C13 C14 O2 51.8(15) 3_665 . . . ? C12 C13 C14 O2 -79(2) 2_655 . . . ? C11 C13 C14 O2 -75.2(16) 2_655 . . . ? C14 C13 C14 O2 23.3(15) 2_655 . . . ? C12 C13 C14 C11 73(6) 3_665 . . 3_665 ? C13 C13 C14 C11 -73(6) 2_655 . . 3_665 ? C13 C13 C14 C11 -127(4) 3_665 . . 3_665 ? C12 C13 C14 C11 -57(3) . . . 3_665 ? C12 C13 C14 C11 -130(2) 2_655 . . 3_665 ? C11 C13 C14 C11 -127(2) 2_655 . . 3_665 ? C14 C13 C14 C11 -28.6(14) 2_655 . . 3_665 ? C12 C13 C14 C13 -160(9) 3_665 . . 3_665 ? C13 C13 C14 C13 54.7(17) 2_655 . . 3_665 ? C12 C13 C14 C13 71(3) . . . 3_665 ? C11 C13 C14 C13 127(4) 3_665 . . 3_665 ? C12 C13 C14 C13 -3(4) 2_655 . . 3_665 ? C11 C13 C14 C13 0(5) 2_655 . . 3_665 ? C14 C13 C14 C13 99(3) 2_655 . . 3_665 ? C12 C13 C14 C12 -157(6) 3_665 . . 2_655 ? C13 C13 C14 C12 58(5) 2_655 . . 2_655 ? C13 C13 C14 C12 3(4) 3_665 . . 2_655 ? C12 C13 C14 C12 74(2) . . . 2_655 ? C11 C13 C14 C12 130(2) 3_665 . . 2_655 ? C11 C13 C14 C12 3(3) 2_655 . . 2_655 ? C14 C13 C14 C12 102(2) 2_655 . . 2_655 ? _refine_diff_density_max 0.761 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.073 _shelxl_version_number 2014-3 _shelx_res_file ; TITL mo_dm14564_0m in R3c CELL 0.71073 12.5731 12.5731 43.4681 90 90 120 ZERR 6 0.0012 0.0012 0.0043 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -Y,-X,0.5+Z SYMM +Y-X,+Y,0.5+Z SYMM +X,+X-Y,0.5+Z SFAC C H N Cl Lu O Li UNIT 192 318 36 18 6 24 6 L.S. 64 PLAN 20 SIZE 0.12 0.2 0.25 TEMP -140 BOND $h simu 0.005 o1 > last wpdb -1 MORE -1 CONF fmap 2 acta REM D:/data/guest/dm14564/mo_dm14564_0m.hkl dfix 1.48 0.01 o2 c11 o2 c14 dfix 1.52 0.01 c11 c12 c12 c13 c13 c14 sadi 0.01 o2 c12 o2 c13 c11 c13 c11 c14 WGHT 0.046700 1.810700 FVAR 0.04736 LU1 5 0.666667 0.333333 -0.052146 10.33333 0.03310 0.03310 = 0.03209 0.00000 0.00000 0.01655 CL1 4 0.712996 0.183937 -0.079840 11.00000 0.05803 0.04709 = 0.05005 -0.00435 0.00697 0.02978 N1 3 0.634812 0.450480 -0.014023 11.00000 0.03483 0.03059 = 0.03871 -0.00372 -0.00467 0.01742 N2 3 0.641729 0.426836 0.016794 11.00000 0.03316 0.03096 = 0.03517 -0.00360 -0.00453 0.01772 C1 1 0.666667 0.333333 0.027705 10.33333 0.02769 0.02769 = 0.03300 0.00000 0.00000 0.01384 C5 1 0.622922 0.498158 0.068847 11.00000 0.05337 0.04688 = 0.04437 -0.01067 0.00712 0.02227 AFIX 33 H5A 2 0.605681 0.559968 0.077485 11.00000 -1.50000 H5B 2 0.560436 0.416371 0.075886 11.00000 -1.50000 H5C 2 0.704141 0.514905 0.075682 11.00000 -1.50000 AFIX 0 C2 1 0.620669 0.503029 0.034885 11.00000 0.03287 0.03424 = 0.04458 -0.01076 -0.00006 0.01447 C3 1 0.600758 0.576963 0.015440 11.00000 0.04901 0.03501 = 0.06156 -0.00843 -0.00205 0.02391 AFIX 43 H3A 2 0.584841 0.640537 0.021239 11.00000 -1.20000 AFIX 0 C4 1 0.608305 0.541093 -0.014678 11.00000 0.04673 0.03773 = 0.05230 -0.00499 -0.00930 0.02664 C6 1 0.596902 0.594530 -0.044421 11.00000 0.08644 0.05499 = 0.06354 -0.00223 -0.01437 0.05340 AFIX 33 H6A 2 0.577260 0.659378 -0.040226 11.00000 -1.50000 H6B 2 0.674701 0.629225 -0.055691 11.00000 -1.50000 H6C 2 0.531280 0.529978 -0.056822 11.00000 -1.50000 AFIX 0 O1 6 0.645752 0.182119 0.320442 11.00000 0.07607 0.07352 = 0.06728 -0.00496 0.01192 0.04395 C7 1 0.597456 0.133746 0.350162 11.00000 0.06930 0.06835 = 0.09364 0.01109 0.01732 0.03536 AFIX 23 H7A 2 0.507702 0.101326 0.350657 11.00000 -1.20000 H7B 2 0.636654 0.198472 0.366034 11.00000 -1.20000 AFIX 0 C8 1 0.624891 0.034579 0.355791 11.00000 0.08313 0.07248 = 0.12889 0.02308 0.01374 0.03774 AFIX 23 H8A 2 0.647500 0.033695 0.377568 11.00000 -1.20000 H8B 2 0.553623 -0.046461 0.350546 11.00000 -1.20000 AFIX 0 C9 1 0.727667 0.064542 0.335590 11.00000 0.09219 0.08242 = 0.15201 0.01229 0.01888 0.04572 AFIX 23 H9A 2 0.806433 0.121686 0.345740 11.00000 -1.20000 H9B 2 0.729139 -0.010448 0.329361 11.00000 -1.20000 AFIX 0 C10 1 0.706909 0.120337 0.310137 11.00000 0.09960 0.09009 = 0.11598 -0.01216 0.02961 0.04368 AFIX 23 H10A 2 0.655999 0.057395 0.294693 11.00000 -1.20000 H10B 2 0.786020 0.179335 0.300423 11.00000 -1.20000 AFIX 0 LI1 7 0.666667 0.333333 0.306306 10.33333 0.09145 0.09145 = 0.07071 0.00000 0.00000 0.04572 O2 6 0.666667 0.333333 0.263148 10.33333 0.11102 0.11102 = 0.08206 0.00000 0.00000 0.05551 C11 1 0.593380 0.373402 0.245428 10.33333 0.11311 0.11352 = 0.08596 0.00585 -0.00048 0.06280 AFIX 3 H11A 2 0.583260 0.433662 0.256588 10.33333 -1.20000 H11B 2 0.513840 0.305272 0.240578 10.33333 -1.20000 AFIX 0 C12 1 0.664426 0.422674 0.216298 10.33333 0.11662 0.11260 = 0.09262 0.00488 0.00071 0.06521 AFIX 3 H12A 2 0.728316 0.506003 0.219578 10.33333 -1.20000 H12B 2 0.613746 0.420034 0.199468 10.33333 -1.20000 AFIX 0 C13 1 0.714416 0.337410 0.211039 10.33333 0.11685 0.11465 = 0.09800 0.00179 0.00419 0.06783 AFIX 3 H13A 2 0.798296 0.384720 0.204419 10.33333 -1.20000 H13B 2 0.668346 0.278851 0.195259 10.33333 -1.20000 AFIX 0 C14 1 0.708902 0.274581 0.241170 10.33333 0.11912 0.11830 = 0.10312 0.00006 0.00354 0.06587 AFIX 3 H14A 2 0.653562 0.187831 0.239250 10.33333 -1.20000 H14B 2 0.788322 0.288321 0.247130 10.33333 -1.20000 AFIX 0 HKLF 4 REM mo_dm14564_0m in R3c REM R1 = 0.0280 for 3059 Fo > 4sig(Fo) and 0.0464 for all 4113 data REM 166 parameters refined using 90 restraints END WGHT 0.0354 3.4085 REM Highest difference peak 0.761, deepest hole -0.506, 1-sigma level 0.073 Q1 1 0.6667 0.3333 -0.0721 10.33333 0.05 0.76 Q2 1 0.6667 0.3333 -0.0323 10.33333 0.05 0.67 Q3 1 0.6667 0.3333 0.0906 10.33333 0.05 0.51 Q4 1 0.7071 0.3061 0.2625 11.00000 0.05 0.47 Q5 1 0.7330 0.0698 0.3526 11.00000 0.05 0.42 Q6 1 0.3999 0.6996 -0.0337 11.00000 0.05 0.39 Q7 1 0.7803 0.1808 0.3201 11.00000 0.05 0.39 Q8 1 0.5215 0.4515 0.0750 11.00000 0.05 0.38 Q9 1 0.8128 0.2848 -0.0794 11.00000 0.05 0.37 Q10 1 0.6667 0.3333 0.2108 10.33333 0.05 0.36 Q11 1 0.6437 0.0013 0.3285 11.00000 0.05 0.35 Q12 1 0.6387 0.4266 0.2419 11.00000 0.05 0.34 Q13 1 0.6667 0.3333 0.1854 10.33333 0.05 0.33 Q14 1 0.5466 0.0799 0.3356 11.00000 0.05 0.33 Q15 1 0.8007 0.5881 0.0596 11.00000 0.05 0.29 Q16 1 0.5975 0.5919 0.0398 11.00000 0.05 0.29 Q17 1 0.6482 -0.0561 0.3758 11.00000 0.05 0.29 Q18 1 0.6655 0.4659 0.0736 11.00000 0.05 0.28 Q19 1 0.6191 0.5657 0.0005 11.00000 0.05 0.27 Q20 1 0.7474 0.3864 -0.0621 11.00000 0.05 0.27 ; _shelx_res_checksum 58650 _shelx_hkl_file ; 1 -2 0 641.59 31.22 1 -2 0 653.03 35.58 2 -1 0 665.27 31.19 2 -1 0 648.41 35.63 -1 -1 0 643.52 31.59 -1 -1 0 652.32 35.60 -1 -1 0 652.58 31.19 0 -3 0 397.88 20.14 0 -3 0 409.39 20.39 3 0 0 405.70 22.99 0 -3 0 386.48 22.89 3 -3 0 429.16 22.98 3 -3 0 448.01 20.14 -3 0 0 447.21 20.40 2 -4 0 66.87 3.41 2 -4 0 69.06 3.80 4 -2 0 64.18 3.92 -2 -2 0 67.69 3.83 -2 -2 0 65.59 3.43 4 -2 0 67.21 3.32 -2 -2 0 65.62 3.34 4 -5 0 294.87 15.53 -5 1 0 292.22 13.82 4 -5 0 292.01 13.65 -1 -4 0 274.75 15.44 5 -1 0 271.63 15.60 -1 -4 0 275.68 13.81 5 -1 0 264.85 13.50 -1 -4 0 273.87 13.61 1 -5 0 247.49 15.31 1 -5 0 271.65 13.73 4 1 0 281.86 15.47 1 -5 0 273.61 13.57 5 -4 0 278.09 15.49 -4 -1 0 292.03 13.44 -4 -1 0 293.27 13.74 5 -4 0 288.32 13.51 3 3 0 172.32 9.31 3 -6 0 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9.37 1.73 7 -5 -54 8.97 1.61 -5 -2 -54 8.49 1.73 -7 5 54 7.01 1.55 2 -7 54 7.61 1.69 5 2 54 7.84 1.95 -5 1 -54 9.63 1.65 4 -5 -54 8.76 1.52 5 -1 54 7.04 1.89 -4 5 54 9.16 1.74 -1 -4 54 6.01 1.57 1 -5 -54 10.41 1.75 -4 -1 54 14.72 1.77 5 -4 54 12.46 2.11 -1 5 54 9.87 1.90 7 -2 -54 9.29 1.60 -2 -5 -54 5.87 1.52 5 -7 54 4.49 1.62 2 5 54 6.87 1.78 -7 2 54 6.55 1.48 6 -6 -54 7.95 1.51 -6 0 -54 3.32 1.29 -6 6 54 4.22 1.38 0 -6 54 6.46 1.64 6 0 54 6.45 1.85 3 -6 -54 9.62 1.61 -6 3 -54 6.82 1.54 6 -3 54 8.17 1.92 0 -6 -54 7.85 1.60 -6 0 54 8.45 1.55 6 -6 54 5.63 1.72 -7 -1 -54 7.41 1.77 8 -7 -54 10.96 1.76 -8 7 54 7.70 1.72 7 1 54 5.86 1.99 1 -8 54 10.97 1.85 -7 2 -54 6.46 1.54 5 -7 -54 8.09 1.53 7 -2 54 7.36 1.95 2 -7 -54 5.09 1.40 7 -5 54 11.52 2.05 -5 -2 54 5.63 1.37 -1 -7 -54 10.29 1.88 -8 1 54 9.88 1.84 7 -8 54 6.85 1.83 -8 1 -54 9.28 1.85 7 -8 -54 8.79 1.62 8 -1 54 7.56 2.05 -7 8 54 11.91 1.92 4 -8 -54 11.47 1.77 -8 4 -54 10.12 1.82 -4 -4 54 10.94 1.70 8 -4 54 7.06 1.96 1 -8 -54 9.29 1.73 -7 -1 54 8.22 1.59 8 -7 54 7.02 1.88 1 -1 -55 -0.56 0.80 -1 0 -55 0.15 0.83 0 1 -55 -0.41 0.73 0 -1 55 0.60 1.24 -1 1 55 0.13 1.37 1 0 55 -0.30 1.26 -2 -1 -55 0.93 0.97 3 -2 -55 0.81 0.92 2 1 55 -0.81 1.30 1 -3 55 0.77 1.37 -3 2 55 0.67 1.25 2 0 -55 -1.15 0.77 0 -2 -55 -0.46 0.84 -2 2 -55 -0.49 0.79 -2 0 55 0.29 1.20 2 -2 55 1.26 1.34 0 2 55 0.21 1.35 -3 -2 -55 0.17 0.94 5 -3 -55 0.30 0.93 2 -5 55 1.84 1.28 -5 3 55 0.27 1.02 3 2 55 -1.25 1.36 2 -3 -55 2.00 1.06 -3 1 -55 1.95 1.03 -1 -2 55 0.98 1.23 -2 3 55 -1.65 1.23 3 -1 55 1.54 1.44 4 -1 -55 3.75 1.13 -1 -3 -55 1.99 1.11 3 -4 55 0.63 1.31 1 3 55 -0.10 1.37 -4 -3 -55 -0.11 1.01 7 -4 -55 0.44 1.00 3 -7 55 -0.23 1.25 -7 4 55 0.16 1.05 4 3 55 -1.41 1.35 -4 0 -55 0.54 0.93 4 -4 -55 0.01 0.85 4 0 55 1.05 1.48 -4 4 55 0.60 1.27 0 -4 55 0.45 1.24 -4 3 -55 0.64 0.95 1 -4 -55 1.29 1.02 4 -3 55 -0.48 1.41 -3 -1 55 2.99 1.32 -1 4 55 0.47 1.35 -2 -4 -55 0.01 0.93 6 -2 -55 -0.09 0.94 -6 2 55 -1.72 0.93 4 -6 55 -0.36 1.20 2 4 55 0.08 1.36 -5 -1 -55 0.03 1.01 6 -5 -55 0.70 0.97 1 -6 55 0.82 1.32 5 1 55 -1.77 1.41 -6 5 55 -0.50 1.05 3 -5 -55 0.44 0.96 -5 2 -55 0.75 1.00 5 -2 55 -0.64 1.36 -2 -3 55 1.86 1.25 -3 5 55 0.54 1.27 0 -5 -55 -0.29 0.91 5 -5 55 1.16 1.42 -5 0 55 0.25 0.99 0 5 55 -0.80 1.25 8 -3 -55 2.17 1.15 -3 -5 -55 0.17 1.05 3 5 55 0.74 1.46 5 -8 55 -0.84 1.27 -8 3 55 -1.27 1.02 -6 -2 -55 -0.20 1.07 8 -6 -55 0.71 1.08 -8 6 55 -1.46 1.09 6 2 55 -0.24 1.52 2 -8 55 -0.05 1.19 5 -6 -55 -0.57 0.91 -6 1 -55 -1.08 0.95 6 -1 55 0.41 1.55 -1 -5 55 -0.55 1.13 -5 6 55 1.37 1.25 2 -6 -55 0.46 0.97 -4 -2 55 0.83 0.98 6 -4 55 1.23 1.42 -1 -6 -55 1.40 1.08 7 -1 -55 0.57 0.99 6 -7 55 -1.85 1.23 -7 1 55 -1.38 0.96 7 -7 -55 0.35 1.01 -7 0 -55 0.32 1.15 7 0 55 -0.63 1.64 -7 7 55 -1.93 1.03 0 -7 55 -1.86 1.13 4 -7 -55 0.12 0.93 -7 3 -55 -0.64 0.98 7 -3 55 0.20 1.55 1 -7 -55 0.04 0.94 -6 -1 55 -0.77 0.92 7 -6 55 0.63 1.39 -8 2 -55 0.85 1.16 6 -8 -55 1.12 1.04 8 -2 55 -1.33 1.53 3 -8 -55 0.66 1.05 -5 -3 55 0.74 0.99 8 -5 55 1.54 1.67 -1 1 -56 9.19 1.56 0 -1 -56 11.19 1.68 1 0 -56 12.41 1.69 -1 0 56 10.20 1.85 0 1 56 10.45 1.95 1 -1 56 11.82 2.02 2 -2 -56 10.85 1.68 -2 0 -56 9.87 1.61 2 0 56 10.95 2.06 0 -2 56 9.09 1.87 -2 2 56 8.52 1.83 -1 -2 -56 9.13 1.68 3 -1 -56 15.70 1.85 -3 1 56 13.90 2.03 2 -3 56 16.62 2.23 1 2 56 11.04 2.10 4 -3 -56 11.83 1.68 -3 -1 -56 8.02 1.56 -4 3 56 6.71 1.65 3 1 56 7.98 1.92 1 -4 56 6.87 1.72 -3 2 -56 10.75 1.74 1 -3 -56 14.49 1.94 3 -2 56 12.94 2.17 -2 -1 56 15.31 2.07 -1 3 56 17.28 2.24 -2 -3 -56 9.09 1.69 5 -2 -56 11.97 1.69 2 3 56 9.79 1.98 3 -5 56 6.18 1.70 -4 -2 -56 5.02 1.49 6 -4 -56 8.64 1.57 2 -6 56 7.31 1.72 4 2 56 7.60 1.95 -6 4 56 5.84 1.46 3 -4 -56 10.69 1.66 -4 1 -56 7.84 1.53 4 -1 56 4.33 1.81 -1 -3 56 6.92 1.64 -3 4 56 7.74 1.71 0 -4 -56 10.10 1.77 4 0 -56 14.81 1.80 0 4 56 12.50 2.08 4 -4 56 15.29 2.25 -3 -4 -56 3.88 1.37 7 -3 -56 7.47 1.52 4 -7 56 5.47 1.68 3 4 56 4.97 1.73 -7 3 56 4.27 1.40 -5 0 -56 6.81 1.54 5 -5 -56 9.12 1.61 -5 5 56 6.30 1.63 5 0 56 6.06 1.85 0 -5 56 4.57 1.52 2 -5 -56 8.46 1.60 -5 3 -56 6.01 1.40 -2 5 56 6.85 1.67 5 -3 56 7.14 1.88 -1 -5 -56 3.11 1.27 6 -1 -56 8.42 1.48 5 -6 56 4.94 1.64 1 5 56 5.69 1.72 -6 1 56 4.56 1.34 7 -6 -56 9.56 1.65 -6 -1 -56 4.30 1.46 6 1 56 5.19 1.87 -7 6 56 5.59 1.52 1 -7 56 6.52 1.70 -6 2 -56 4.43 1.41 4 -6 -56 7.93 1.51 -4 6 56 6.56 1.67 6 -2 56 5.74 1.81 1 -6 -56 4.35 1.28 -5 -1 56 5.41 1.35 6 -5 56 6.98 1.83 6 -7 -56 7.54 1.49 -7 1 -56 7.40 1.65 7 -1 56 7.25 2.01 3 -7 -56 3.63 1.28 7 -4 56 4.20 1.77 0 0 -57 -0.81 0.75 0 0 57 0.07 1.42 2 -1 -57 0.49 0.93 -1 -1 -57 1.68 0.99 1 1 57 -1.44 1.33 -2 1 57 1.31 1.34 1 -2 57 0.73 1.36 1 1 -57 -0.07 0.80 1 -2 -57 0.24 0.84 -2 1 -57 -0.49 0.81 -1 -1 57 0.84 1.34 -1 2 57 -1.29 1.28 2 -1 57 -0.34 1.36 -2 -2 -57 1.34 1.06 4 -2 -57 1.79 1.02 2 -4 57 0.78 1.31 2 2 57 1.47 1.58 -3 0 -57 0.88 0.96 3 -3 -57 2.27 1.07 0 -3 57 0.09 1.20 -3 3 57 -0.09 1.24 3 0 57 -0.57 1.43 0 -3 -57 0.31 0.93 3 0 -57 1.13 0.93 0 3 57 1.43 1.38 -3 0 57 -0.68 1.25 3 -3 57 -0.36 1.35 6 -3 -57 -0.56 0.90 -3 -3 -57 0.86 1.06 3 -6 57 -1.06 1.24 -6 3 57 -0.27 0.99 3 3 57 -1.20 1.39 5 -4 -57 0.66 1.03 -4 -1 -57 -0.69 0.89 1 -5 57 -0.40 1.27 4 1 57 -2.99 1.32 -4 2 -57 0.97 1.03 2 -4 -57 2.13 1.13 -2 4 57 1.28 1.39 -2 -2 57 1.79 1.34 4 -2 57 0.58 1.46 -1 -4 -57 -0.60 0.91 5 -1 -57 -0.38 0.89 1 4 57 0.15 1.40 4 -5 57 -0.99 1.29 7 -5 -57 1.00 1.09 -5 -2 -57 -0.17 1.10 -7 5 57 0.88 1.24 2 -7 57 -0.80 1.20 5 2 57 -0.20 1.53 -5 1 -57 -0.68 0.90 4 -5 -57 0.60 0.99 -4 5 57 -0.91 1.27 5 -1 57 2.86 1.61 -1 -4 57 -1.33 1.08 1 -5 -57 0.02 0.89 5 -4 57 -0.21 1.36 -1 5 57 -1.50 1.28 -2 -5 -57 0.73 1.07 7 -2 -57 1.40 1.12 2 5 57 -1.50 1.25 5 -7 57 -0.84 1.30 -7 2 57 -1.56 0.98 6 -6 -57 1.35 1.08 -6 0 -57 -1.22 0.95 0 -6 57 -0.02 1.26 6 0 57 -0.51 1.54 -6 3 -57 -0.65 0.94 3 -6 -57 -1.17 0.87 -3 6 57 -0.67 1.30 6 -3 57 -0.82 1.46 0 -6 -57 0.43 1.05 6 -6 57 -1.82 1.22 -6 0 57 -0.19 0.99 0 6 57 0.68 1.43 -7 2 -57 -0.21 1.06 5 -7 -57 1.73 1.10 7 -2 57 -1.05 1.49 -5 7 57 0.37 1.26 2 -7 -57 0.21 0.93 -5 -2 57 0.99 1.02 7 -5 57 -0.43 1.44 0 1 -58 9.24 1.58 1 -1 -58 8.81 1.53 -1 0 -58 9.47 1.58 -1 1 58 11.23 1.99 1 0 58 12.06 2.05 0 -1 58 12.45 2.01 3 -2 -58 11.10 1.63 -2 -1 -58 9.49 1.65 1 -3 58 9.24 1.89 2 1 58 9.53 2.03 -3 2 58 7.59 1.82 2 0 -58 10.59 1.62 0 -2 -58 8.17 1.56 0 2 58 10.72 2.05 2 -2 58 11.49 2.07 -2 0 58 6.92 1.73 5 -3 -58 8.06 1.51 -3 -2 -58 4.88 1.41 3 2 58 5.62 1.87 2 -5 58 6.07 1.68 2 -3 -58 11.92 1.73 -3 1 -58 8.43 1.54 3 -1 58 6.71 1.91 -2 3 58 8.77 1.85 -1 -2 58 6.54 1.75 -1 -3 -58 6.47 1.52 4 -1 -58 12.38 1.72 3 -4 58 9.00 1.93 1 3 58 7.15 1.88 4 -4 -58 12.50 1.78 -4 0 -58 7.54 1.60 0 -4 58 6.04 1.63 4 0 58 9.36 2.04 -4 4 58 8.44 1.87 1 -4 -58 8.67 1.61 4 -3 58 10.69 2.06 -1 4 58 9.27 1.94 -2 -4 -58 3.80 1.35 6 -2 -58 7.82 1.49 4 -6 58 4.06 1.62 2 4 58 1.24 1.52 -5 -1 -58 5.10 1.49 6 -5 -58 9.47 1.64 1 -6 58 3.96 1.64 5 1 58 6.97 1.93 -5 2 -58 5.38 1.42 3 -5 -58 9.61 1.65 -3 5 58 5.25 1.70 5 -2 58 6.04 1.89 0 -5 -58 5.44 1.44 0 5 58 5.00 1.71 5 -5 58 7.13 1.85 -6 1 -58 5.23 1.51 5 -6 -58 9.06 1.62 -5 6 58 4.06 1.58 6 -1 58 5.48 1.90 -1 -5 58 4.58 1.59 2 -6 -58 4.83 1.39 6 -4 58 4.75 1.80 -2 6 58 4.47 1.62 0 -1 -59 -0.11 0.90 -1 1 -59 -0.17 0.86 1 0 -59 -0.52 0.82 0 1 59 0.23 1.40 1 -1 59 1.02 1.45 -1 0 59 -0.48 1.31 -2 0 -59 -0.54 0.87 2 -2 -59 0.14 0.96 -2 2 59 -2.31 1.34 2 0 59 -0.66 1.45 0 -2 59 -0.44 1.30 3 -1 -59 1.32 1.00 -1 -2 -59 0.97 1.02 1 2 59 0.18 1.45 -3 1 59 -2.13 1.25 2 -3 59 0.23 1.41 -3 -1 -59 -0.05 0.93 4 -3 -59 1.12 1.06 1 -4 59 -0.12 1.39 3 1 59 -0.75 1.45 1 -3 -59 -0.30 0.84 -3 2 -59 0.30 0.97 3 -2 59 -0.31 1.45 -2 -1 59 1.00 1.32 -1 3 59 0.80 1.46 5 -2 -59 0.05 0.98 -2 -3 -59 0.02 0.95 2 3 59 -0.40 1.44 3 -5 59 -1.60 1.29 -4 1 -59 2.21 1.09 3 -4 -59 2.51 1.16 4 -1 59 2.54 1.66 -1 -3 59 0.68 1.37 -3 4 59 1.40 1.43 0 -4 -59 -0.41 0.95 4 -4 59 -1.43 1.35 0 4 59 -0.25 1.42 5 -5 -59 0.90 1.06 -5 0 -59 0.24 1.07 0 -5 59 -0.90 1.27 5 0 59 -1.08 1.49 2 -5 -59 -0.93 0.96 5 -3 59 -1.40 1.39 -2 5 59 -0.10 1.39 0 0 -60 7.87 1.51 0 0 60 10.94 2.06 2 -1 -60 9.18 1.61 -1 -1 -60 6.91 1.49 1 -2 60 5.53 1.79 -2 1 60 7.99 1.88 1 1 60 8.90 2.06 -2 1 -60 5.96 1.38 1 -2 -60 5.46 1.37 2 -1 60 10.93 2.07 -1 -1 60 6.15 1.78 -1 2 60 5.92 1.80 -2 -2 -60 6.75 1.59 4 -2 -60 15.92 1.92 2 2 60 7.41 2.03 2 -4 60 9.73 1.99 3 -3 -60 13.41 1.90 -3 0 -60 9.53 1.70 0 -3 60 7.84 1.81 -3 3 60 6.95 1.89 3 0 60 10.82 2.20 0 -3 -60 5.57 1.49 0 3 60 5.65 1.84 3 -3 60 11.90 2.11 -4 2 -60 9.45 1.64 2 -4 -60 9.04 1.68 4 -2 60 5.35 1.85 -2 -2 60 7.76 1.82 -2 4 60 7.15 1.86 1 -1 -61 0.68 0.97 -1 0 -61 0.33 0.96 0 -1 61 -1.68 1.40 1 0 61 0.81 1.46 -1 1 61 2.62 1.53 -2 -1 -61 0.39 0.96 3 -2 -61 -0.09 0.98 2 1 61 -0.15 1.56 -3 2 61 -1.74 1.40 1 -3 61 0.89 1.46 0 -2 -61 -0.41 0.97 2 -2 61 -0.85 1.44 -2 0 61 -1.70 1.37 0 2 61 1.84 1.60 2 -3 -61 -0.77 0.95 -3 1 -61 -0.08 0.96 -1 -2 61 -0.58 1.38 -2 3 61 1.02 1.52 3 -1 61 0.95 1.64 1 0 -62 4.61 1.28 0 -1 -62 7.65 1.49 -1 0 62 5.21 1.85 0 1 62 4.92 1.84 1 -1 62 9.09 2.03 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 11013 #===END data_mo_dm15754_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H51 N6 O Si2 Y' _chemical_formula_weight 632.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 '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 11.8719(19) _cell_length_b 14.452(2) _cell_length_c 21.102(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.097(3) _cell_angle_gamma 90.00 _cell_volume 3478.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2463 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 22.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method ? _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6182 _exptl_absorpt_correction_T_max 0.6655 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'Bruker APEX-II CCD' _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 28060 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.59 _reflns_number_total 7984 _reflns_number_gt 4857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^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 7984 _refine_ls_number_parameters 355 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.029 _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 Y1 Y 0.37470(3) 0.89565(2) 0.813217(18) 0.02418(12) Uani 1 1 d . . . Si1 Si 0.61597(11) 0.74582(8) 0.92704(6) 0.0327(3) Uani 1 1 d . . . Si2 Si 0.12899(10) 0.92736(8) 0.89701(6) 0.0302(3) Uani 1 1 d . . . O1 O 0.5112(2) 1.01681(17) 0.83812(12) 0.0295(7) Uani 1 1 d . . . N1 N 0.2214(3) 0.8041(2) 0.74222(15) 0.0251(7) Uani 1 1 d . . . N3 N 0.2522(3) 1.0156(2) 0.74414(15) 0.0248(7) Uani 1 1 d . . . N5 N 0.4214(3) 0.8947(2) 0.70645(15) 0.0293(8) Uani 1 1 d . . . N2 N 0.1687(3) 0.8336(2) 0.67909(15) 0.0245(7) Uani 1 1 d . . . N4 N 0.1956(3) 0.9959(2) 0.67962(15) 0.0235(7) Uani 1 1 d . . . N6 N 0.3295(3) 0.8959(2) 0.64887(15) 0.0270(7) Uani 1 1 d . . . C1 C 0.2087(3) 0.9102(2) 0.64694(18) 0.0266(9) Uani 1 1 d . . . C5 C 0.0018(4) 0.7937(3) 0.5824(2) 0.0433(12) Uani 1 1 d . . . H5A H 0.0509 0.8080 0.5533 0.065 Uiso 1 1 calc R . . H5B H -0.0512 0.8456 0.5825 0.065 Uiso 1 1 calc R . . H5C H -0.0442 0.7378 0.5666 0.065 Uiso 1 1 calc R . . C2 C 0.0775(4) 0.7779(3) 0.6504(2) 0.0313(10) Uani 1 1 d . . . C3 C 0.0720(4) 0.7107(3) 0.6954(2) 0.0359(11) Uani 1 1 d . . . H3 H 0.0170 0.6615 0.6892 0.043 Uiso 1 1 calc R . . C4 C 0.1618(3) 0.7287(3) 0.7513(2) 0.0300(9) Uani 1 1 d . . . C6 C 0.1953(4) 0.6732(3) 0.8131(2) 0.0387(11) Uani 1 1 d . . . H6A H 0.2581 0.6300 0.8114 0.058 Uiso 1 1 calc R . . H6B H 0.1271 0.6384 0.8176 0.058 Uiso 1 1 calc R . . H6C H 0.2229 0.7146 0.8510 0.058 Uiso 1 1 calc R . . C10 C 0.0519(4) 1.0641(3) 0.5819(2) 0.0411(12) Uani 1 1 d . . . H10A H 0.0971 1.0359 0.5545 0.062 Uiso 1 1 calc R . . H10B H 0.0298 1.1273 0.5667 0.062 Uiso 1 1 calc R . . H10C H -0.0190 1.0275 0.5785 0.062 Uiso 1 1 calc R . . C7 C 0.1243(4) 1.0664(3) 0.6518(2) 0.0290(9) Uani 1 1 d . . . C8 C 0.1368(3) 1.1341(3) 0.69885(19) 0.0293(9) Uani 1 1 d . . . H8 H 0.0987 1.1926 0.6937 0.035 Uiso 1 1 calc R . . C9 C 0.2154(3) 1.1005(2) 0.75494(19) 0.0262(9) Uani 1 1 d . . . C11 C 0.2586(4) 1.1455(3) 0.82105(19) 0.0327(10) Uani 1 1 d . . . H11A H 0.2670 1.0987 0.8557 0.049 Uiso 1 1 calc R . . H11B H 0.2024 1.1927 0.8260 0.049 Uiso 1 1 calc R . . H11C H 0.3348 1.1745 0.8249 0.049 Uiso 1 1 calc R . . C15 C 0.2938(4) 0.8806(3) 0.5276(2) 0.0403(11) Uani 1 1 d . . . H15A H 0.2529 0.8210 0.5197 0.060 Uiso 1 1 calc R . . H15B H 0.3412 0.8880 0.4966 0.060 Uiso 1 1 calc R . . H15C H 0.2362 0.9308 0.5212 0.060 Uiso 1 1 calc R . . C12 C 0.3711(4) 0.8835(3) 0.59613(19) 0.0311(10) Uani 1 1 d . . . C13 C 0.4901(4) 0.8745(3) 0.6193(2) 0.0395(11) Uani 1 1 d . . . H13 H 0.5435 0.8649 0.5937 0.047 Uiso 1 1 calc R . . C14 C 0.5175(4) 0.8822(3) 0.6869(2) 0.0352(10) Uani 1 1 d . . . C16 C 0.6351(4) 0.8767(3) 0.7359(2) 0.0512(13) Uani 1 1 d . . . H16A H 0.6290 0.8971 0.7791 0.077 Uiso 1 1 calc R . . H16B H 0.6903 0.9166 0.7218 0.077 Uiso 1 1 calc R . . H16C H 0.6632 0.8126 0.7391 0.077 Uiso 1 1 calc R . . C17 C 0.4977(4) 0.7640(3) 0.8524(2) 0.0366(11) Uani 1 1 d . . . H17A H 0.4421 0.7129 0.8523 0.044 Uiso 1 1 calc R . . H17B H 0.5331 0.7496 0.8162 0.044 Uiso 1 1 calc R . . C18 C 0.7551(4) 0.7964(3) 0.9183(2) 0.0440(12) Uani 1 1 d . . . H18A H 0.7806 0.7620 0.8847 0.066 Uiso 1 1 calc R . . H18B H 0.8156 0.7923 0.9606 0.066 Uiso 1 1 calc R . . H18C H 0.7423 0.8614 0.9051 0.066 Uiso 1 1 calc R . . C19 C 0.6484(5) 0.6212(3) 0.9501(3) 0.0580(15) Uani 1 1 d . . . H19A H 0.5777 0.5913 0.9558 0.087 Uiso 1 1 calc R . . H19B H 0.7112 0.6176 0.9915 0.087 Uiso 1 1 calc R . . H19C H 0.6732 0.5897 0.9151 0.087 Uiso 1 1 calc R . . C20 C 0.5844(4) 0.8011(3) 1.0000(2) 0.0424(12) Uani 1 1 d . . . H20A H 0.5787 0.8683 0.9936 0.064 Uiso 1 1 calc R . . H20B H 0.6478 0.7868 1.0397 0.064 Uiso 1 1 calc R . . H20C H 0.5101 0.7772 1.0051 0.064 Uiso 1 1 calc R . . C21 C 0.2853(3) 0.9182(3) 0.90156(19) 0.0279(9) Uani 1 1 d . . . H21A H 0.3154 0.8670 0.9329 0.033 Uiso 1 1 calc R . . H21B H 0.3214 0.9754 0.9242 0.033 Uiso 1 1 calc R . . C22 C 0.0977(4) 1.0311(3) 0.9422(2) 0.0459(12) Uani 1 1 d . . . H22A H 0.1388 1.0252 0.9892 0.069 Uiso 1 1 calc R . . H22B H 0.0131 1.0355 0.9366 0.069 Uiso 1 1 calc R . . H22C H 0.1247 1.0869 0.9244 0.069 Uiso 1 1 calc R . . C23 C 0.0288(4) 0.9360(3) 0.8113(2) 0.0403(11) Uani 1 1 d . . . H23A H 0.0516 0.9891 0.7888 0.060 Uiso 1 1 calc R . . H23B H -0.0521 0.9441 0.8133 0.060 Uiso 1 1 calc R . . H23C H 0.0344 0.8792 0.7870 0.060 Uiso 1 1 calc R . . C24 C 0.0775(4) 0.8247(3) 0.9348(2) 0.0464(12) Uani 1 1 d . . . H24A H 0.0945 0.7682 0.9134 0.070 Uiso 1 1 calc R . . H24B H -0.0071 0.8295 0.9287 0.070 Uiso 1 1 calc R . . H24C H 0.1182 0.8224 0.9820 0.070 Uiso 1 1 calc R . . C25 C 0.5831(4) 1.0351(3) 0.9053(2) 0.0387(10) Uani 1 1 d U . . H25A H 0.6278 0.9792 0.9246 0.046 Uiso 1 1 calc R . . H25B H 0.5336 1.0546 0.9337 0.046 Uiso 1 1 calc R . . C26 C 0.6638(5) 1.1108(4) 0.8987(3) 0.0676(13) Uani 1 1 d DU . . H26B H 0.6570 1.1635 0.9274 0.081 Uiso 1 1 calc R . . H26A H 0.7459 1.0886 0.9120 0.081 Uiso 1 1 calc R . . C27 C 0.6327(5) 1.1386(4) 0.8328(3) 0.0734(14) Uani 1 1 d DU . . H27A H 0.7008 1.1308 0.8148 0.088 Uiso 1 1 calc R . . H27B H 0.6118 1.2051 0.8301 0.088 Uiso 1 1 calc R . . C28 C 0.5355(4) 1.0863(3) 0.7935(2) 0.0410(11) Uani 1 1 d U . . H28A H 0.5561 1.0565 0.7560 0.049 Uiso 1 1 calc R . . H28B H 0.4665 1.1267 0.7761 0.049 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 Y1 0.0237(2) 0.02214(19) 0.0245(2) -0.00184(17) 0.00297(15) -0.00032(18) Si1 0.0322(7) 0.0283(6) 0.0338(7) 0.0000(5) 0.0025(6) 0.0073(5) Si2 0.0264(6) 0.0301(6) 0.0342(7) 0.0019(5) 0.0085(5) 0.0004(5) O1 0.0322(16) 0.0281(14) 0.0265(15) 0.0020(12) 0.0053(13) -0.0078(12) N1 0.0263(18) 0.0197(16) 0.0272(18) -0.0003(14) 0.0039(15) -0.0013(14) N3 0.0283(19) 0.0210(16) 0.0225(17) -0.0021(14) 0.0029(15) -0.0002(14) N5 0.0288(18) 0.0337(18) 0.0248(17) -0.0070(15) 0.0063(15) 0.0010(16) N2 0.0245(18) 0.0215(17) 0.0247(17) -0.0020(14) 0.0023(14) 0.0020(14) N4 0.0247(18) 0.0205(16) 0.0227(17) -0.0002(13) 0.0022(14) -0.0006(14) N6 0.0300(19) 0.0227(16) 0.0259(17) -0.0032(15) 0.0034(15) 0.0002(15) C1 0.030(2) 0.023(2) 0.025(2) -0.0023(16) 0.0039(18) -0.0014(17) C5 0.045(3) 0.040(3) 0.036(3) -0.002(2) -0.003(2) -0.011(2) C2 0.030(2) 0.028(2) 0.032(2) -0.0061(19) 0.0021(19) -0.0028(19) C3 0.032(3) 0.028(2) 0.043(3) -0.007(2) 0.003(2) -0.0098(19) C4 0.027(2) 0.028(2) 0.033(2) -0.0019(18) 0.0045(19) -0.0001(18) C6 0.043(3) 0.036(2) 0.034(2) 0.003(2) 0.005(2) -0.009(2) C10 0.045(3) 0.037(2) 0.032(2) 0.002(2) -0.005(2) 0.008(2) C7 0.029(2) 0.028(2) 0.031(2) 0.0065(18) 0.0092(19) 0.0061(18) C8 0.034(2) 0.0228(19) 0.031(2) 0.0001(17) 0.008(2) 0.0025(18) C9 0.030(2) 0.0225(19) 0.027(2) -0.0014(18) 0.0087(17) -0.0025(18) C11 0.042(3) 0.021(2) 0.033(2) -0.0028(18) 0.008(2) 0.0006(19) C15 0.057(3) 0.037(3) 0.028(2) -0.005(2) 0.013(2) -0.003(2) C12 0.043(3) 0.026(2) 0.027(2) -0.0040(18) 0.014(2) 0.0019(19) C13 0.041(3) 0.041(3) 0.041(3) -0.008(2) 0.019(2) 0.000(2) C14 0.035(2) 0.038(3) 0.035(2) -0.012(2) 0.015(2) 0.002(2) C16 0.025(2) 0.076(4) 0.050(3) -0.015(3) 0.005(2) 0.007(2) C17 0.030(2) 0.030(2) 0.044(3) -0.002(2) 0.001(2) 0.0037(19) C18 0.034(3) 0.051(3) 0.042(3) -0.013(2) 0.002(2) 0.006(2) C19 0.065(4) 0.036(3) 0.064(3) 0.008(2) 0.002(3) 0.016(2) C20 0.051(3) 0.040(3) 0.035(3) 0.006(2) 0.011(2) 0.006(2) C21 0.028(2) 0.027(2) 0.028(2) 0.0010(17) 0.0061(18) -0.0011(17) C22 0.045(3) 0.050(3) 0.047(3) -0.001(2) 0.020(2) 0.006(2) C23 0.027(2) 0.048(3) 0.044(3) 0.002(2) 0.007(2) 0.005(2) C24 0.041(3) 0.042(3) 0.055(3) 0.012(2) 0.012(2) -0.003(2) C25 0.045(3) 0.038(2) 0.030(2) -0.0019(19) 0.006(2) -0.010(2) C26 0.070(3) 0.066(2) 0.057(2) 0.011(2) 0.001(2) -0.031(2) C27 0.078(3) 0.073(2) 0.061(2) 0.011(2) 0.005(2) -0.034(2) C28 0.048(3) 0.041(2) 0.039(2) 0.0079(19) 0.019(2) -0.012(2) _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 Y1 O1 2.344(3) . ? Y1 C17 2.402(4) . ? Y1 N1 2.407(3) . ? Y1 C21 2.409(4) . ? Y1 N3 2.464(3) . ? Y1 N5 2.465(3) . ? Si1 C17 1.816(4) . ? Si1 C18 1.861(5) . ? Si1 C20 1.863(4) . ? Si1 C19 1.877(4) . ? Si2 C21 1.836(4) . ? Si2 C24 1.865(4) . ? Si2 C22 1.868(4) . ? Si2 C23 1.873(4) . ? O1 C28 1.459(5) . ? O1 C25 1.461(5) . ? N1 C4 1.341(5) . ? N1 N2 1.373(4) . ? N3 C9 1.343(4) . ? N3 N4 1.371(4) . ? N5 C14 1.329(5) . ? N5 N6 1.390(4) . ? N2 C2 1.350(5) . ? N2 C1 1.446(5) . ? N4 C7 1.350(5) . ? N4 C1 1.448(4) . ? N6 C12 1.349(5) . ? N6 C1 1.438(5) . ? C5 C2 1.484(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C2 C3 1.372(6) . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C6 1.489(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C10 C7 1.487(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C7 C8 1.373(6) . ? C8 C9 1.377(5) . ? C8 H8 0.9500 . ? C9 C11 1.495(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C15 C12 1.483(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C12 C13 1.366(6) . ? C13 C14 1.376(6) . ? C13 H13 0.9500 . ? C14 C16 1.492(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.486(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.395(7) . ? C26 H26B 0.9900 . ? C26 H26A 0.9900 . ? C27 C28 1.435(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 Y1 C17 101.43(12) . . ? O1 Y1 N1 155.00(10) . . ? C17 Y1 N1 93.52(12) . . ? O1 Y1 C21 98.68(11) . . ? C17 Y1 C21 101.38(14) . . ? N1 Y1 C21 97.84(12) . . ? O1 Y1 N3 82.24(10) . . ? C17 Y1 N3 164.58(13) . . ? N1 Y1 N3 78.34(10) . . ? C21 Y1 N3 92.76(12) . . ? O1 Y1 N5 83.82(10) . . ? C17 Y1 N5 92.31(13) . . ? N1 Y1 N5 75.58(11) . . ? C21 Y1 N5 165.22(12) . . ? N3 Y1 N5 73.07(11) . . ? C17 Si1 C18 110.6(2) . . ? C17 Si1 C20 111.8(2) . . ? C18 Si1 C20 107.5(2) . . ? C17 Si1 C19 114.7(2) . . ? C18 Si1 C19 106.2(2) . . ? C20 Si1 C19 105.7(2) . . ? C21 Si2 C24 111.48(19) . . ? C21 Si2 C22 111.9(2) . . ? C24 Si2 C22 106.6(2) . . ? C21 Si2 C23 114.66(19) . . ? C24 Si2 C23 105.6(2) . . ? C22 Si2 C23 106.1(2) . . ? C28 O1 C25 109.5(3) . . ? C28 O1 Y1 128.2(2) . . ? C25 O1 Y1 122.3(2) . . ? C4 N1 N2 105.9(3) . . ? C4 N1 Y1 134.0(3) . . ? N2 N1 Y1 119.7(2) . . ? C9 N3 N4 105.4(3) . . ? C9 N3 Y1 135.2(2) . . ? N4 N3 Y1 119.2(2) . . ? C14 N5 N6 105.3(3) . . ? C14 N5 Y1 135.6(3) . . ? N6 N5 Y1 118.6(2) . . ? C2 N2 N1 110.1(3) . . ? C2 N2 C1 125.0(3) . . ? N1 N2 C1 124.9(3) . . ? C7 N4 N3 110.5(3) . . ? C7 N4 C1 125.2(3) . . ? N3 N4 C1 124.3(3) . . ? C12 N6 N5 110.0(3) . . ? C12 N6 C1 125.9(3) . . ? N5 N6 C1 124.1(3) . . ? N6 C1 N2 109.4(3) . . ? N6 C1 N4 110.4(3) . . ? N2 C1 N4 109.8(3) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C2 C3 107.3(3) . . ? N2 C2 C5 122.5(4) . . ? C3 C2 C5 130.2(4) . . ? C2 C3 C4 106.5(4) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? N1 C4 C3 110.2(4) . . ? N1 C4 C6 122.6(4) . . ? C3 C4 C6 127.1(4) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C7 C8 107.1(3) . . ? N4 C7 C10 122.3(4) . . ? C8 C7 C10 130.5(4) . . ? C7 C8 C9 106.4(3) . . ? C7 C8 H8 126.8 . . ? C9 C8 H8 126.8 . . ? N3 C9 C8 110.6(3) . . ? N3 C9 C11 120.8(3) . . ? C8 C9 C11 128.6(4) . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N6 C12 C13 107.2(4) . . ? N6 C12 C15 122.6(4) . . ? C13 C12 C15 130.2(4) . . ? C12 C13 C14 106.7(4) . . ? C12 C13 H13 126.7 . . ? C14 C13 H13 126.7 . . ? N5 C14 C13 110.9(4) . . ? N5 C14 C16 120.7(4) . . ? C13 C14 C16 128.4(4) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 Y1 131.5(2) . . ? Si1 C17 H17A 104.4 . . ? Y1 C17 H17A 104.4 . . ? Si1 C17 H17B 104.4 . . ? Y1 C17 H17B 104.4 . . ? H17A C17 H17B 105.6 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 Y1 128.67(19) . . ? Si2 C21 H21A 105.1 . . ? Y1 C21 H21A 105.1 . . ? Si2 C21 H21B 105.1 . . ? Y1 C21 H21B 105.1 . . ? H21A C21 H21B 105.9 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 C26 105.2(4) . . ? O1 C25 H25A 110.7 . . ? C26 C25 H25A 110.7 . . ? O1 C25 H25B 110.7 . . ? C26 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? C27 C26 C25 107.8(4) . . ? C27 C26 H26B 110.1 . . ? C25 C26 H26B 110.1 . . ? C27 C26 H26A 110.1 . . ? C25 C26 H26A 110.1 . . ? H26B C26 H26A 108.5 . . ? C26 C27 C28 111.8(5) . . ? 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 O1 105.2(4) . . ? C27 C28 H28A 110.7 . . ? O1 C28 H28A 110.7 . . ? C27 C28 H28B 110.7 . . ? O1 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? 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 C17 Y1 O1 C28 124.3(3) . . . . ? N1 Y1 O1 C28 -1.3(5) . . . . ? C21 Y1 O1 C28 -132.1(3) . . . . ? N3 Y1 O1 C28 -40.5(3) . . . . ? N5 Y1 O1 C28 33.2(3) . . . . ? C17 Y1 O1 C25 -58.6(3) . . . . ? N1 Y1 O1 C25 175.9(3) . . . . ? C21 Y1 O1 C25 45.0(3) . . . . ? N3 Y1 O1 C25 136.6(3) . . . . ? N5 Y1 O1 C25 -149.7(3) . . . . ? O1 Y1 N1 C4 179.1(3) . . . . ? C17 Y1 N1 C4 52.1(4) . . . . ? C21 Y1 N1 C4 -49.9(4) . . . . ? N3 Y1 N1 C4 -141.1(4) . . . . ? N5 Y1 N1 C4 143.6(4) . . . . ? O1 Y1 N1 N2 -8.6(4) . . . . ? C17 Y1 N1 N2 -135.6(3) . . . . ? C21 Y1 N1 N2 122.4(3) . . . . ? N3 Y1 N1 N2 31.2(3) . . . . ? N5 Y1 N1 N2 -44.1(3) . . . . ? O1 Y1 N3 C9 -56.3(4) . . . . ? C17 Y1 N3 C9 -161.3(5) . . . . ? N1 Y1 N3 C9 139.5(4) . . . . ? C21 Y1 N3 C9 42.1(4) . . . . ? N5 Y1 N3 C9 -142.2(4) . . . . ? O1 Y1 N3 N4 130.5(3) . . . . ? C17 Y1 N3 N4 25.5(6) . . . . ? N1 Y1 N3 N4 -33.7(3) . . . . ? C21 Y1 N3 N4 -131.1(3) . . . . ? N5 Y1 N3 N4 44.6(3) . . . . ? O1 Y1 N5 C14 59.6(4) . . . . ? C17 Y1 N5 C14 -41.6(4) . . . . ? N1 Y1 N5 C14 -134.7(4) . . . . ? C21 Y1 N5 C14 160.3(4) . . . . ? N3 Y1 N5 C14 143.3(4) . . . . ? O1 Y1 N5 N6 -130.2(3) . . . . ? C17 Y1 N5 N6 128.5(3) . . . . ? N1 Y1 N5 N6 35.5(2) . . . . ? C21 Y1 N5 N6 -29.6(6) . . . . ? N3 Y1 N5 N6 -46.5(2) . . . . ? C4 N1 N2 C2 0.8(4) . . . . ? Y1 N1 N2 C2 -173.5(2) . . . . ? C4 N1 N2 C1 -176.3(3) . . . . ? Y1 N1 N2 C1 9.4(5) . . . . ? C9 N3 N4 C7 -1.0(4) . . . . ? Y1 N3 N4 C7 174.1(2) . . . . ? C9 N3 N4 C1 -179.4(3) . . . . ? Y1 N3 N4 C1 -4.4(5) . . . . ? C14 N5 N6 C12 0.5(4) . . . . ? Y1 N5 N6 C12 -172.4(2) . . . . ? C14 N5 N6 C1 -178.4(3) . . . . ? Y1 N5 N6 C1 8.7(4) . . . . ? C12 N6 C1 N2 115.9(4) . . . . ? N5 N6 C1 N2 -65.4(4) . . . . ? C12 N6 C1 N4 -123.2(4) . . . . ? N5 N6 C1 N4 55.6(4) . . . . ? C2 N2 C1 N6 -121.7(4) . . . . ? N1 N2 C1 N6 55.0(4) . . . . ? C2 N2 C1 N4 117.1(4) . . . . ? N1 N2 C1 N4 -66.3(4) . . . . ? C7 N4 C1 N6 123.2(4) . . . . ? N3 N4 C1 N6 -58.5(5) . . . . ? C7 N4 C1 N2 -116.1(4) . . . . ? N3 N4 C1 N2 62.1(5) . . . . ? N1 N2 C2 C3 -0.7(4) . . . . ? C1 N2 C2 C3 176.4(4) . . . . ? N1 N2 C2 C5 178.6(4) . . . . ? C1 N2 C2 C5 -4.3(6) . . . . ? N2 C2 C3 C4 0.3(5) . . . . ? C5 C2 C3 C4 -178.9(4) . . . . ? N2 N1 C4 C3 -0.6(4) . . . . ? Y1 N1 C4 C3 172.5(3) . . . . ? N2 N1 C4 C6 177.1(4) . . . . ? Y1 N1 C4 C6 -9.8(6) . . . . ? C2 C3 C4 N1 0.2(5) . . . . ? C2 C3 C4 C6 -177.4(4) . . . . ? N3 N4 C7 C8 1.3(5) . . . . ? C1 N4 C7 C8 179.7(4) . . . . ? N3 N4 C7 C10 179.9(4) . . . . ? C1 N4 C7 C10 -1.6(6) . . . . ? N4 C7 C8 C9 -1.0(5) . . . . ? C10 C7 C8 C9 -179.6(4) . . . . ? N4 N3 C9 C8 0.3(4) . . . . ? Y1 N3 C9 C8 -173.6(3) . . . . ? N4 N3 C9 C11 179.7(3) . . . . ? Y1 N3 C9 C11 5.9(6) . . . . ? C7 C8 C9 N3 0.5(5) . . . . ? C7 C8 C9 C11 -178.9(4) . . . . ? N5 N6 C12 C13 -0.2(4) . . . . ? C1 N6 C12 C13 178.6(3) . . . . ? N5 N6 C12 C15 179.4(3) . . . . ? C1 N6 C12 C15 -1.7(6) . . . . ? N6 C12 C13 C14 -0.1(5) . . . . ? C15 C12 C13 C14 -179.8(4) . . . . ? N6 N5 C14 C13 -0.6(5) . . . . ? Y1 N5 C14 C13 170.4(3) . . . . ? N6 N5 C14 C16 -179.6(4) . . . . ? Y1 N5 C14 C16 -8.6(6) . . . . ? C12 C13 C14 N5 0.5(5) . . . . ? C12 C13 C14 C16 179.4(4) . . . . ? C18 Si1 C17 Y1 -81.3(3) . . . . ? C20 Si1 C17 Y1 38.5(4) . . . . ? C19 Si1 C17 Y1 158.8(3) . . . . ? O1 Y1 C17 Si1 42.8(3) . . . . ? N1 Y1 C17 Si1 -157.3(3) . . . . ? C21 Y1 C17 Si1 -58.6(3) . . . . ? N3 Y1 C17 Si1 145.2(3) . . . . ? N5 Y1 C17 Si1 127.0(3) . . . . ? C24 Si2 C21 Y1 111.0(3) . . . . ? C22 Si2 C21 Y1 -129.7(2) . . . . ? C23 Si2 C21 Y1 -8.9(3) . . . . ? O1 Y1 C21 Si2 129.3(2) . . . . ? C17 Y1 C21 Si2 -127.1(2) . . . . ? N1 Y1 C21 Si2 -31.8(2) . . . . ? N3 Y1 C21 Si2 46.8(2) . . . . ? N5 Y1 C21 Si2 30.6(6) . . . . ? C28 O1 C25 C26 -7.3(5) . . . . ? Y1 O1 C25 C26 175.1(3) . . . . ? O1 C25 C26 C27 4.6(6) . . . . ? C25 C26 C27 C28 -0.2(8) . . . . ? C26 C27 C28 O1 -4.3(7) . . . . ? C25 O1 C28 C27 7.2(5) . . . . ? Y1 O1 C28 C27 -175.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.538 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.088 #===END data_mo_dm15102_0m _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H51 Lu N6 O Si2' _chemical_formula_weight 718.89 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' 'Lu' 'Lu' -0.4720 5.8584 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8087(8) _cell_length_b 14.4867(10) _cell_length_c 21.0202(14) _cell_angle_alpha 90 _cell_angle_beta 105.7480(10) _cell_angle_gamma 90 _cell_volume 3460.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 7189 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_F_000 1472 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 2.950 _shelx_estimated_absorpt_T_min 0.590 _shelx_estimated_absorpt_T_max 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5688 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34456 _diffrn_reflns_av_unetI/netI 0.0516 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.729 _diffrn_reflns_theta_max 30.579 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 10616 _reflns_number_gt 7976 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.8999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10616 _refine_ls_number_parameters 355 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.022 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.12545(2) 0.10333(2) 0.18912(2) 0.01947(4) Uani 1 1 d . . . . . Si2 Si 0.36904(7) 0.07370(6) 0.10426(4) 0.02636(18) Uani 1 1 d . . . . . Si1 Si -0.11552(8) 0.25111(6) 0.07481(4) 0.0283(2) Uani 1 1 d . . . . . O1 O -0.00841(17) -0.01590(15) 0.16404(10) 0.0257(5) Uani 1 1 d . . . . . N3 N 0.2751(2) 0.19545(17) 0.25689(11) 0.0226(5) Uani 1 1 d . . . . . N5 N 0.2465(2) -0.01556(17) 0.25578(11) 0.0208(5) Uani 1 1 d . . . . . N1 N 0.0767(2) 0.10341(18) 0.29436(12) 0.0247(5) Uani 1 1 d . . . . . N4 N 0.3291(2) 0.16666(17) 0.32105(11) 0.0224(5) Uani 1 1 d . . . . . N6 N 0.3046(2) 0.00421(16) 0.32096(11) 0.0208(5) Uani 1 1 d . . . . . N2 N 0.1680(2) 0.10231(17) 0.35172(11) 0.0221(5) Uani 1 1 d . . . . . C21 C 0.2122(3) 0.0833(2) 0.10072(15) 0.0254(6) Uani 1 1 d . . . . . H21A H 0.1753 0.0269 0.0775 0.030 Uiso 1 1 calc R U . . . H21B H 0.1823 0.1351 0.0701 0.030 Uiso 1 1 calc R U . . . C17 C 0.0020(3) 0.2315(2) 0.15050(16) 0.0314(7) Uani 1 1 d . . . . . H17A H -0.0354 0.2441 0.1864 0.038 Uiso 1 1 calc R U . . . H17B H 0.0573 0.2832 0.1517 0.038 Uiso 1 1 calc R U . . . C11 C 0.3002(3) 0.3255(2) 0.18507(16) 0.0367(8) Uani 1 1 d . . . . . H11A H 0.2701 0.2838 0.1475 0.055 Uiso 1 1 calc R U . . . H11B H 0.3692 0.3584 0.1793 0.055 Uiso 1 1 calc R U . . . H11C H 0.2390 0.3701 0.1873 0.055 Uiso 1 1 calc R U . . . C9 C 0.3340(3) 0.2710(2) 0.24724(15) 0.0267(7) Uani 1 1 d . . . . . C8 C 0.4249(3) 0.2898(2) 0.30388(16) 0.0307(7) Uani 1 1 d . . . . . H8 H 0.4795 0.3393 0.3098 0.037 Uiso 1 1 calc R U . . . C7 C 0.4201(3) 0.2228(2) 0.34946(15) 0.0278(7) Uani 1 1 d . . . . . C10 C 0.4974(3) 0.2075(3) 0.41720(15) 0.0381(8) Uani 1 1 d . . . . . H10A H 0.4518 0.1791 0.4446 0.057 Uiso 1 1 calc R U . . . H10B H 0.5292 0.2668 0.4365 0.057 Uiso 1 1 calc R U . . . H10C H 0.5624 0.1665 0.4152 0.057 Uiso 1 1 calc R U . . . C16 C 0.2414(3) -0.1450(2) 0.17821(15) 0.0301(7) Uani 1 1 d . . . . . H16A H 0.1662 -0.1759 0.1750 0.045 Uiso 1 1 calc R U . . . H16B H 0.2996 -0.1905 0.1730 0.045 Uiso 1 1 calc R U . . . H16C H 0.2307 -0.0983 0.1433 0.045 Uiso 1 1 calc R U . . . C14 C 0.2836(3) -0.0995(2) 0.24426(14) 0.0229(6) Uani 1 1 d . . . . . C13 C 0.3639(3) -0.1331(2) 0.30064(14) 0.0265(7) Uani 1 1 d . . . . . H13 H 0.4031 -0.1910 0.3054 0.032 Uiso 1 1 calc R U . . . C12 C 0.3755(3) -0.0657(2) 0.34822(15) 0.0252(6) Uani 1 1 d . . . . . C15 C 0.4497(3) -0.0637(3) 0.41794(16) 0.0366(8) Uani 1 1 d . . . . . H15A H 0.5199 -0.0260 0.4208 0.055 Uiso 1 1 calc R U . . . H15B H 0.4736 -0.1267 0.4326 0.055 Uiso 1 1 calc R U . . . H15C H 0.4046 -0.0370 0.4463 0.055 Uiso 1 1 calc R U . . . C6 C -0.1390(3) 0.1208(3) 0.26448(18) 0.0449(10) Uani 1 1 d . . . . . H6A H -0.1690 0.1841 0.2631 0.067 Uiso 1 1 calc R U . . . H6B H -0.1934 0.0785 0.2776 0.067 Uiso 1 1 calc R U . . . H6C H -0.1321 0.1035 0.2206 0.067 Uiso 1 1 calc R U . . . C4 C -0.0211(3) 0.1152(2) 0.31332(16) 0.0313(7) Uani 1 1 d . . . . . C3 C 0.0059(3) 0.1226(2) 0.38198(16) 0.0347(8) Uani 1 1 d . . . . . H3 H -0.0480 0.1319 0.4077 0.042 Uiso 1 1 calc R U . . . C2 C 0.1253(3) 0.1140(2) 0.40476(15) 0.0285(7) Uani 1 1 d . . . . . C5 C 0.2038(3) 0.1176(2) 0.47373(16) 0.0364(8) Uani 1 1 d . . . . . H5A H 0.2601 0.0664 0.4806 0.055 Uiso 1 1 calc R U . . . H5B H 0.1562 0.1125 0.5052 0.055 Uiso 1 1 calc R U . . . H5C H 0.2466 0.1764 0.4806 0.055 Uiso 1 1 calc R U . . . C1 C 0.2895(3) 0.08963(19) 0.35315(14) 0.0220(6) Uani 1 1 d . . . . . C22 C 0.4722(3) 0.0657(3) 0.18998(17) 0.0366(8) Uani 1 1 d . . . . . H22A H 0.4661 0.1221 0.2146 0.055 Uiso 1 1 calc R U . . . H22B H 0.5532 0.0587 0.1870 0.055 Uiso 1 1 calc R U . . . H22C H 0.4511 0.0122 0.2129 0.055 Uiso 1 1 calc R U . . . C23 C 0.4194(3) 0.1762(3) 0.06522(18) 0.0406(9) Uani 1 1 d . . . . . H23A H 0.3756 0.1794 0.0184 0.061 Uiso 1 1 calc R U . . . H23B H 0.5037 0.1704 0.0690 0.061 Uiso 1 1 calc R U . . . H23C H 0.4054 0.2325 0.0878 0.061 Uiso 1 1 calc R U . . . C24 C 0.4000(3) -0.0297(3) 0.05861(18) 0.0428(9) Uani 1 1 d . . . . . H24A H 0.3703 -0.0851 0.0754 0.064 Uiso 1 1 calc R U . . . H24B H 0.4851 -0.0355 0.0651 0.064 Uiso 1 1 calc R U . . . H24C H 0.3609 -0.0227 0.0114 0.064 Uiso 1 1 calc R U . . . C19 C -0.0820(3) 0.1985(3) 0.00057(16) 0.0373(8) Uani 1 1 d . . . . . H19A H -0.0081 0.2240 -0.0045 0.056 Uiso 1 1 calc R U . . . H19B H -0.1459 0.2126 -0.0389 0.056 Uiso 1 1 calc R U . . . H19C H -0.0746 0.1315 0.0063 0.056 Uiso 1 1 calc R U . . . C20 C -0.1443(4) 0.3757(3) 0.0535(2) 0.0506(11) Uani 1 1 d . . . . . H20A H -0.1695 0.4067 0.0888 0.076 Uiso 1 1 calc R U . . . H20B H -0.2064 0.3811 0.0119 0.076 Uiso 1 1 calc R U . . . H20C H -0.0722 0.4048 0.0487 0.076 Uiso 1 1 calc R U . . . C18 C -0.2575(3) 0.2021(3) 0.08223(17) 0.0394(9) Uani 1 1 d . . . . . H18A H -0.2487 0.1355 0.0903 0.059 Uiso 1 1 calc R U . . . H18B H -0.3192 0.2132 0.0412 0.059 Uiso 1 1 calc R U . . . H18C H -0.2793 0.2318 0.1191 0.059 Uiso 1 1 calc R U . . . C25 C -0.0798(3) -0.0332(2) 0.09619(15) 0.0333(7) Uani 1 1 d . U . . . H25A H -0.0298 -0.0539 0.0680 0.040 Uiso 1 1 calc R U . . . H25B H -0.1226 0.0233 0.0767 0.040 Uiso 1 1 calc R U . . . C26 C -0.1636(4) -0.1072(3) 0.1027(2) 0.0638(12) Uani 1 1 d . U . . . H26A H -0.2433 -0.0811 0.0968 0.077 Uiso 1 1 calc R U . . . H26B H -0.1679 -0.1554 0.0687 0.077 Uiso 1 1 calc R U . . . C27 C -0.1222(4) -0.1451(3) 0.1659(2) 0.0706(12) Uani 1 1 d . U . . . H27A H -0.0879 -0.2067 0.1627 0.085 Uiso 1 1 calc R U . . . H27B H -0.1885 -0.1530 0.1858 0.085 Uiso 1 1 calc R U . . . C28 C -0.0339(3) -0.0860(2) 0.20772(17) 0.0346(8) Uani 1 1 d . U . . . H28A H 0.0379 -0.1217 0.2290 0.042 Uiso 1 1 calc R U . . . H28B H -0.0642 -0.0573 0.2426 0.042 Uiso 1 1 calc R U . . . 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 Lu1 0.01915(6) 0.01910(6) 0.01848(6) -0.00125(5) 0.00223(4) -0.00032(5) Si2 0.0229(4) 0.0280(4) 0.0284(5) 0.0024(4) 0.0074(3) 0.0004(3) Si1 0.0280(5) 0.0253(5) 0.0279(5) -0.0005(4) 0.0014(4) 0.0059(4) O1 0.0264(11) 0.0266(11) 0.0231(11) 0.0013(9) 0.0050(9) -0.0072(9) N3 0.0231(13) 0.0213(12) 0.0207(12) -0.0008(10) 0.0013(10) 0.0015(10) N5 0.0231(12) 0.0225(12) 0.0156(11) -0.0012(9) 0.0034(9) 0.0006(10) N1 0.0215(12) 0.0300(14) 0.0207(12) -0.0059(11) 0.0027(10) 0.0012(11) N4 0.0250(13) 0.0198(12) 0.0202(12) -0.0017(10) 0.0024(10) -0.0008(10) N6 0.0238(13) 0.0193(12) 0.0168(11) -0.0018(9) 0.0014(9) 0.0000(10) N2 0.0252(13) 0.0224(12) 0.0178(11) -0.0035(10) 0.0045(9) 0.0002(10) C21 0.0259(16) 0.0252(16) 0.0248(15) 0.0018(12) 0.0063(12) -0.0014(12) C17 0.0271(17) 0.0279(17) 0.0334(17) -0.0013(14) -0.0020(13) 0.0050(13) C11 0.039(2) 0.0292(18) 0.0379(19) 0.0062(15) 0.0038(15) -0.0077(15) C9 0.0288(17) 0.0215(15) 0.0289(16) -0.0020(12) 0.0062(13) -0.0027(12) C8 0.0270(16) 0.0274(17) 0.0347(18) -0.0051(14) 0.0032(13) -0.0093(13) C7 0.0258(16) 0.0238(16) 0.0300(17) -0.0038(13) 0.0009(13) -0.0031(12) C10 0.039(2) 0.043(2) 0.0253(17) -0.0028(15) -0.0040(14) -0.0103(16) C16 0.0412(19) 0.0235(16) 0.0261(16) -0.0041(13) 0.0099(14) 0.0004(14) C14 0.0261(15) 0.0193(14) 0.0235(14) -0.0003(12) 0.0072(11) -0.0015(12) C13 0.0310(17) 0.0218(14) 0.0266(16) 0.0034(12) 0.0076(13) 0.0040(12) C12 0.0253(16) 0.0258(15) 0.0238(15) 0.0022(12) 0.0056(12) 0.0039(12) C15 0.039(2) 0.039(2) 0.0258(17) 0.0014(15) -0.0013(14) 0.0109(16) C6 0.0262(18) 0.071(3) 0.036(2) -0.0130(19) 0.0067(15) 0.0048(17) C4 0.0270(17) 0.036(2) 0.0320(17) -0.0070(14) 0.0104(13) 0.0041(13) C3 0.0352(19) 0.042(2) 0.0300(17) -0.0111(14) 0.0137(14) 0.0013(14) C2 0.0387(19) 0.0234(16) 0.0255(15) -0.0027(12) 0.0121(13) -0.0016(13) C5 0.044(2) 0.043(2) 0.0241(16) -0.0083(14) 0.0109(15) -0.0054(16) C1 0.0242(15) 0.0200(15) 0.0202(14) -0.0033(11) 0.0034(11) 0.0004(11) C22 0.0220(16) 0.047(2) 0.039(2) 0.0017(17) 0.0043(14) 0.0032(15) C23 0.0292(18) 0.041(2) 0.050(2) 0.0076(18) 0.0092(16) -0.0054(15) C24 0.045(2) 0.042(2) 0.044(2) 0.0026(17) 0.0169(17) 0.0109(17) C19 0.044(2) 0.038(2) 0.0293(17) 0.0043(15) 0.0085(15) 0.0029(16) C20 0.055(3) 0.036(2) 0.054(3) 0.0044(18) 0.003(2) 0.0118(18) C18 0.0280(18) 0.050(2) 0.0362(19) -0.0066(17) 0.0026(14) 0.0032(16) C25 0.0378(18) 0.0350(18) 0.0240(15) 0.0001(13) 0.0029(13) -0.0111(14) C26 0.068(2) 0.064(2) 0.046(2) 0.0110(19) -0.0071(19) -0.037(2) C27 0.079(3) 0.064(2) 0.055(2) 0.014(2) -0.005(2) -0.044(2) C28 0.0387(18) 0.0361(19) 0.0313(17) 0.0056(14) 0.0135(14) -0.0126(14) _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 Lu1 O1 2.304(2) . ? Lu1 N3 2.360(2) . ? Lu1 C17 2.364(3) . ? Lu1 C21 2.371(3) . ? Lu1 N5 2.426(2) . ? Lu1 N1 2.433(2) . ? Si2 C21 1.838(3) . ? Si2 C24 1.868(4) . ? Si2 C23 1.870(4) . ? Si2 C22 1.885(3) . ? Si1 C17 1.827(3) . ? Si1 C18 1.866(4) . ? Si1 C20 1.869(4) . ? Si1 C19 1.873(3) . ? O1 C28 1.454(4) . ? O1 C25 1.468(3) . ? N3 C9 1.341(4) . ? N3 N4 1.390(3) . ? N5 C14 1.337(4) . ? N5 N6 1.386(3) . ? N1 C4 1.330(4) . ? N1 N2 1.383(3) . ? N4 C7 1.351(4) . ? N4 C1 1.446(4) . ? N6 C12 1.340(4) . ? N6 C1 1.444(3) . ? N2 C2 1.353(4) . ? N2 C1 1.438(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C11 C9 1.485(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9 C8 1.396(4) . ? C8 C7 1.376(4) . ? C8 H8 0.9500 . ? C7 C10 1.485(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C16 C14 1.495(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C14 C13 1.389(4) . ? C13 C12 1.377(4) . ? C13 H13 0.9500 . ? C12 C15 1.490(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C6 C4 1.491(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C4 C3 1.395(4) . ? C3 C2 1.366(5) . ? C3 H3 0.9500 . ? C2 C5 1.495(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C25 C26 1.491(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.397(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.448(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 Lu1 N3 156.52(8) . . ? O1 Lu1 C17 100.91(10) . . ? N3 Lu1 C17 93.11(10) . . ? O1 Lu1 C21 98.30(9) . . ? N3 Lu1 C21 97.49(9) . . ? C17 Lu1 C21 100.64(11) . . ? O1 Lu1 N5 81.95(8) . . ? N3 Lu1 N5 79.95(8) . . ? C17 Lu1 N5 165.38(10) . . ? C21 Lu1 N5 93.06(9) . . ? O1 Lu1 N1 83.76(8) . . ? N3 Lu1 N1 76.95(8) . . ? C17 Lu1 N1 92.04(10) . . ? C21 Lu1 N1 166.47(9) . . ? N5 Lu1 N1 73.92(8) . . ? C21 Si2 C24 112.04(16) . . ? C21 Si2 C23 111.07(15) . . ? C24 Si2 C23 106.32(18) . . ? C21 Si2 C22 115.21(15) . . ? C24 Si2 C22 106.03(17) . . ? C23 Si2 C22 105.55(16) . . ? C17 Si1 C18 110.81(16) . . ? C17 Si1 C20 113.87(17) . . ? C18 Si1 C20 106.18(18) . . ? C17 Si1 C19 112.34(15) . . ? C18 Si1 C19 108.22(16) . . ? C20 Si1 C19 105.01(18) . . ? C28 O1 C25 109.4(2) . . ? C28 O1 Lu1 128.73(17) . . ? C25 O1 Lu1 121.83(17) . . ? C9 N3 N4 105.8(2) . . ? C9 N3 Lu1 134.8(2) . . ? N4 N3 Lu1 119.14(17) . . ? C14 N5 N6 105.6(2) . . ? C14 N5 Lu1 135.40(19) . . ? N6 N5 Lu1 118.70(17) . . ? C4 N1 N2 106.0(2) . . ? C4 N1 Lu1 135.3(2) . . ? N2 N1 Lu1 118.14(17) . . ? C7 N4 N3 110.4(2) . . ? C7 N4 C1 125.3(2) . . ? N3 N4 C1 124.3(2) . . ? C12 N6 N5 110.5(2) . . ? C12 N6 C1 126.1(2) . . ? N5 N6 C1 123.3(2) . . ? C2 N2 N1 109.9(2) . . ? C2 N2 C1 126.3(2) . . ? N1 N2 C1 123.9(2) . . ? Si2 C21 Lu1 128.49(15) . . ? Si2 C21 H21A 105.2 . . ? Lu1 C21 H21A 105.2 . . ? Si2 C21 H21B 105.2 . . ? Lu1 C21 H21B 105.2 . . ? H21A C21 H21B 105.9 . . ? Si1 C17 Lu1 132.29(17) . . ? Si1 C17 H17A 104.2 . . ? Lu1 C17 H17A 104.2 . . ? Si1 C17 H17B 104.2 . . ? Lu1 C17 H17B 104.2 . . ? H17A C17 H17B 105.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C9 C8 109.9(3) . . ? N3 C9 C11 122.7(3) . . ? C8 C9 C11 127.4(3) . . ? C7 C8 C9 106.8(3) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N4 C7 C8 107.1(3) . . ? N4 C7 C10 122.9(3) . . ? C8 C7 C10 130.0(3) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C14 C13 110.2(3) . . ? N5 C14 C16 121.7(3) . . ? C13 C14 C16 128.0(3) . . ? C12 C13 C14 106.3(3) . . ? C12 C13 H13 126.8 . . ? C14 C13 H13 126.8 . . ? N6 C12 C13 107.3(3) . . ? N6 C12 C15 122.6(3) . . ? C13 C12 C15 130.1(3) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C4 C3 110.3(3) . . ? N1 C4 C6 121.7(3) . . ? C3 C4 C6 128.0(3) . . ? C2 C3 C4 106.2(3) . . ? C2 C3 H3 126.9 . . ? C4 C3 H3 126.9 . . ? N2 C2 C3 107.6(3) . . ? N2 C2 C5 122.1(3) . . ? C3 C2 C5 130.2(3) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C1 N6 110.4(2) . . ? N2 C1 N4 109.8(2) . . ? N6 C1 N4 110.2(2) . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C25 C26 104.7(3) . . ? O1 C25 H25A 110.8 . . ? C26 C25 H25A 110.8 . . ? O1 C25 H25B 110.8 . . ? C26 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C25 107.5(3) . . ? C27 C26 H26A 110.2 . . ? C25 C26 H26A 110.2 . . ? C27 C26 H26B 110.2 . . ? C25 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C26 C27 C28 110.7(4) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 O1 105.6(3) . . ? C27 C28 H28A 110.6 . . ? O1 C28 H28A 110.6 . . ? C27 C28 H28B 110.6 . . ? O1 C28 H28B 110.6 . . ? H28A C28 H28B 108.8 . . ? 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 C9 N3 N4 C7 -1.0(3) . . . . ? Lu1 N3 N4 C7 173.5(2) . . . . ? C9 N3 N4 C1 176.7(3) . . . . ? Lu1 N3 N4 C1 -8.8(3) . . . . ? C14 N5 N6 C12 0.2(3) . . . . ? Lu1 N5 N6 C12 -174.19(19) . . . . ? C14 N5 N6 C1 179.6(3) . . . . ? Lu1 N5 N6 C1 5.2(3) . . . . ? C4 N1 N2 C2 -0.4(3) . . . . ? Lu1 N1 N2 C2 172.50(19) . . . . ? C4 N1 N2 C1 179.1(3) . . . . ? Lu1 N1 N2 C1 -8.0(3) . . . . ? C24 Si2 C21 Lu1 128.8(2) . . . . ? C23 Si2 C21 Lu1 -112.5(2) . . . . ? C22 Si2 C21 Lu1 7.4(3) . . . . ? C18 Si1 C17 Lu1 83.2(3) . . . . ? C20 Si1 C17 Lu1 -157.2(2) . . . . ? C19 Si1 C17 Lu1 -38.0(3) . . . . ? N4 N3 C9 C8 0.7(3) . . . . ? Lu1 N3 C9 C8 -172.5(2) . . . . ? N4 N3 C9 C11 -177.4(3) . . . . ? Lu1 N3 C9 C11 9.4(5) . . . . ? N3 C9 C8 C7 -0.2(4) . . . . ? C11 C9 C8 C7 177.8(3) . . . . ? N3 N4 C7 C8 0.9(4) . . . . ? C1 N4 C7 C8 -176.8(3) . . . . ? N3 N4 C7 C10 -177.8(3) . . . . ? C1 N4 C7 C10 4.6(5) . . . . ? C9 C8 C7 N4 -0.5(4) . . . . ? C9 C8 C7 C10 178.1(3) . . . . ? N6 N5 C14 C13 -0.1(3) . . . . ? Lu1 N5 C14 C13 172.9(2) . . . . ? N6 N5 C14 C16 -179.3(3) . . . . ? Lu1 N5 C14 C16 -6.2(5) . . . . ? N5 C14 C13 C12 -0.1(4) . . . . ? C16 C14 C13 C12 179.0(3) . . . . ? N5 N6 C12 C13 -0.3(3) . . . . ? C1 N6 C12 C13 -179.7(3) . . . . ? N5 N6 C12 C15 179.7(3) . . . . ? C1 N6 C12 C15 0.3(5) . . . . ? C14 C13 C12 N6 0.2(4) . . . . ? C14 C13 C12 C15 -179.7(3) . . . . ? N2 N1 C4 C3 0.6(4) . . . . ? Lu1 N1 C4 C3 -170.5(2) . . . . ? N2 N1 C4 C6 179.4(3) . . . . ? Lu1 N1 C4 C6 8.4(5) . . . . ? N1 C4 C3 C2 -0.6(4) . . . . ? C6 C4 C3 C2 -179.3(3) . . . . ? N1 N2 C2 C3 0.1(3) . . . . ? C1 N2 C2 C3 -179.4(3) . . . . ? N1 N2 C2 C5 -178.8(3) . . . . ? C1 N2 C2 C5 1.7(5) . . . . ? C4 C3 C2 N2 0.3(4) . . . . ? C4 C3 C2 C5 179.0(3) . . . . ? C2 N2 C1 N6 122.7(3) . . . . ? N1 N2 C1 N6 -56.7(3) . . . . ? C2 N2 C1 N4 -115.6(3) . . . . ? N1 N2 C1 N4 65.0(3) . . . . ? C12 N6 C1 N2 -122.2(3) . . . . ? N5 N6 C1 N2 58.5(3) . . . . ? C12 N6 C1 N4 116.3(3) . . . . ? N5 N6 C1 N4 -63.0(3) . . . . ? C7 N4 C1 N2 121.9(3) . . . . ? N3 N4 C1 N2 -55.4(3) . . . . ? C7 N4 C1 N6 -116.2(3) . . . . ? N3 N4 C1 N6 66.5(3) . . . . ? C28 O1 C25 C26 9.1(4) . . . . ? Lu1 O1 C25 C26 -173.2(3) . . . . ? O1 C25 C26 C27 -14.5(5) . . . . ? C25 C26 C27 C28 14.8(7) . . . . ? C26 C27 C28 O1 -8.9(6) . . . . ? C25 O1 C28 C27 -0.7(4) . . . . ? Lu1 O1 C28 C27 -178.2(3) . . . . ? _refine_diff_density_max 1.348 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.118 _shelxl_version_number 2014-3 _shelx_res_file ; TITL mo_dm15102_0m in P21/c #14 CELL 0.71073 11.8087 14.4867 21.0202 90 105.748 90 ZERR 4 0.0008 0.001 0.0014 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Lu N O Si UNIT 112 204 4 24 4 8 L.S. 32 ACTA 52 BOND $H FMAP 2 PLAN 20 CONF MORE -1 SIZE 0.08 0.12 0.2 SIMU 0.005 0.01 2 C28 C27 C26 C25 TEMP -143.15 WGHT 0.027500 0.899900 FVAR 0.06253 LU1 3 0.125453 0.103326 0.189124 11.00000 0.01915 0.01910 = 0.01848 -0.00125 0.00223 -0.00032 SI2 6 0.369040 0.073696 0.104258 11.00000 0.02287 0.02802 = 0.02845 0.00237 0.00740 0.00043 SI1 6 -0.115520 0.251106 0.074815 11.00000 0.02799 0.02525 = 0.02793 -0.00049 0.00141 0.00586 O1 5 -0.008408 -0.015902 0.164045 11.00000 0.02642 0.02660 = 0.02312 0.00134 0.00497 -0.00721 N3 4 0.275138 0.195449 0.256892 11.00000 0.02310 0.02134 = 0.02074 -0.00082 0.00130 0.00151 N5 4 0.246503 -0.015564 0.255778 11.00000 0.02313 0.02252 = 0.01564 -0.00117 0.00343 0.00056 N1 4 0.076653 0.103411 0.294360 11.00000 0.02150 0.02997 = 0.02070 -0.00589 0.00267 0.00118 N4 4 0.329076 0.166656 0.321053 11.00000 0.02496 0.01983 = 0.02019 -0.00169 0.00237 -0.00077 N6 4 0.304581 0.004214 0.320959 11.00000 0.02376 0.01934 = 0.01682 -0.00176 0.00143 0.00002 N2 4 0.168006 0.102307 0.351721 11.00000 0.02524 0.02240 = 0.01779 -0.00351 0.00446 0.00021 C21 1 0.212206 0.083251 0.100716 11.00000 0.02588 0.02519 = 0.02476 0.00184 0.00631 -0.00139 AFIX 23 H21A 2 0.175289 0.026869 0.077484 11.00000 -1.20000 H21B 2 0.182267 0.135146 0.070131 11.00000 -1.20000 AFIX 0 C17 1 0.001994 0.231487 0.150504 11.00000 0.02712 0.02786 = 0.03336 -0.00130 -0.00201 0.00498 AFIX 23 H17A 2 -0.035412 0.244142 0.186430 11.00000 -1.20000 H17B 2 0.057304 0.283237 0.151737 11.00000 -1.20000 AFIX 0 C11 1 0.300207 0.325484 0.185072 11.00000 0.03922 0.02922 = 0.03788 0.00615 0.00379 -0.00773 AFIX 137 H11A 2 0.270087 0.283834 0.147548 11.00000 -1.50000 H11B 2 0.369241 0.358446 0.179339 11.00000 -1.50000 H11C 2 0.239017 0.370094 0.187308 11.00000 -1.50000 AFIX 0 C9 1 0.333971 0.271037 0.247244 11.00000 0.02883 0.02153 = 0.02888 -0.00198 0.00619 -0.00265 C8 1 0.424863 0.289815 0.303880 11.00000 0.02697 0.02740 = 0.03475 -0.00509 0.00325 -0.00927 AFIX 43 H8 2 0.479468 0.339342 0.309802 11.00000 -1.20000 AFIX 0 C7 1 0.420123 0.222780 0.349465 11.00000 0.02580 0.02378 = 0.02998 -0.00379 0.00093 -0.00308 C10 1 0.497442 0.207509 0.417196 11.00000 0.03895 0.04257 = 0.02533 -0.00275 -0.00396 -0.01032 AFIX 137 H10A 2 0.451798 0.179140 0.444621 11.00000 -1.50000 H10B 2 0.529187 0.266792 0.436516 11.00000 -1.50000 H10C 2 0.562381 0.166512 0.415162 11.00000 -1.50000 AFIX 0 C16 1 0.241397 -0.144979 0.178215 11.00000 0.04120 0.02345 = 0.02609 -0.00409 0.00989 0.00044 AFIX 137 H16A 2 0.166244 -0.175912 0.174997 11.00000 -1.50000 H16B 2 0.299568 -0.190548 0.173011 11.00000 -1.50000 H16C 2 0.230690 -0.098301 0.143337 11.00000 -1.50000 AFIX 0 C14 1 0.283636 -0.099485 0.244262 11.00000 0.02615 0.01925 = 0.02346 -0.00029 0.00719 -0.00151 C13 1 0.363933 -0.133077 0.300641 11.00000 0.03105 0.02180 = 0.02660 0.00335 0.00758 0.00404 AFIX 43 H13 2 0.403092 -0.190987 0.305424 11.00000 -1.20000 AFIX 0 C12 1 0.375468 -0.065710 0.348220 11.00000 0.02532 0.02579 = 0.02378 0.00216 0.00556 0.00394 C15 1 0.449719 -0.063661 0.417943 11.00000 0.03922 0.03882 = 0.02582 0.00138 -0.00135 0.01092 AFIX 137 H15A 2 0.519858 -0.025991 0.420802 11.00000 -1.50000 H15B 2 0.473578 -0.126662 0.432625 11.00000 -1.50000 H15C 2 0.404558 -0.036983 0.446261 11.00000 -1.50000 AFIX 0 C6 1 -0.139013 0.120806 0.264480 11.00000 0.02616 0.07098 = 0.03637 -0.01296 0.00667 0.00480 AFIX 137 H6A 2 -0.168982 0.184064 0.263131 11.00000 -1.50000 H6B 2 -0.193426 0.078528 0.277609 11.00000 -1.50000 H6C 2 -0.132135 0.103511 0.220610 11.00000 -1.50000 AFIX 0 C4 1 -0.021068 0.115196 0.313315 11.00000 0.02701 0.03633 = 0.03198 -0.00696 0.01037 0.00415 C3 1 0.005887 0.122641 0.381978 11.00000 0.03518 0.04164 = 0.03005 -0.01106 0.01372 0.00134 AFIX 43 H3 2 -0.047989 0.131875 0.407726 11.00000 -1.20000 AFIX 0 C2 1 0.125301 0.113989 0.404763 11.00000 0.03871 0.02338 = 0.02550 -0.00269 0.01205 -0.00164 C5 1 0.203796 0.117624 0.473730 11.00000 0.04356 0.04252 = 0.02405 -0.00827 0.01092 -0.00537 AFIX 137 H5A 2 0.260073 0.066431 0.480591 11.00000 -1.50000 H5B 2 0.156191 0.112472 0.505181 11.00000 -1.50000 H5C 2 0.246590 0.176350 0.480635 11.00000 -1.50000 AFIX 0 C1 1 0.289454 0.089633 0.353147 11.00000 0.02424 0.01999 = 0.02019 -0.00330 0.00340 0.00041 C22 1 0.472217 0.065724 0.189981 11.00000 0.02195 0.04689 = 0.03873 0.00166 0.00427 0.00324 AFIX 137 H22A 2 0.466085 0.122056 0.214646 11.00000 -1.50000 H22B 2 0.553151 0.058750 0.186975 11.00000 -1.50000 H22C 2 0.451056 0.012220 0.212890 11.00000 -1.50000 AFIX 0 C23 1 0.419437 0.176182 0.065216 11.00000 0.02923 0.04123 = 0.05047 0.00759 0.00920 -0.00535 AFIX 137 H23A 2 0.375616 0.179363 0.018442 11.00000 -1.50000 H23B 2 0.503692 0.170377 0.068992 11.00000 -1.50000 H23C 2 0.405414 0.232515 0.087753 11.00000 -1.50000 AFIX 0 C24 1 0.400018 -0.029673 0.058606 11.00000 0.04522 0.04224 = 0.04368 0.00262 0.01694 0.01085 AFIX 137 H24A 2 0.370280 -0.085138 0.075375 11.00000 -1.50000 H24B 2 0.485091 -0.035472 0.065115 11.00000 -1.50000 H24C 2 0.360939 -0.022652 0.011371 11.00000 -1.50000 AFIX 0 C19 1 -0.082023 0.198547 0.000568 11.00000 0.04411 0.03763 = 0.02932 0.00431 0.00855 0.00289 AFIX 137 H19A 2 -0.008068 0.224009 -0.004487 11.00000 -1.50000 H19B 2 -0.145906 0.212649 -0.038939 11.00000 -1.50000 H19C 2 -0.074567 0.131480 0.006276 11.00000 -1.50000 AFIX 0 C20 1 -0.144323 0.375746 0.053514 11.00000 0.05484 0.03603 = 0.05396 0.00444 0.00288 0.01184 AFIX 137 H20A 2 -0.169508 0.406691 0.088832 11.00000 -1.50000 H20B 2 -0.206363 0.381076 0.011885 11.00000 -1.50000 H20C 2 -0.072198 0.404819 0.048656 11.00000 -1.50000 AFIX 0 C18 1 -0.257532 0.202056 0.082234 11.00000 0.02802 0.05030 = 0.03620 -0.00663 0.00260 0.00317 AFIX 137 H18A 2 -0.248691 0.135478 0.090318 11.00000 -1.50000 H18B 2 -0.319192 0.213181 0.041158 11.00000 -1.50000 H18C 2 -0.279279 0.231754 0.119123 11.00000 -1.50000 AFIX 0 C25 1 -0.079766 -0.033184 0.096187 11.00000 0.03784 0.03496 = 0.02396 0.00013 0.00286 -0.01106 AFIX 23 H25A 2 -0.029782 -0.053946 0.067988 11.00000 -1.20000 H25B 2 -0.122565 0.023281 0.076687 11.00000 -1.20000 AFIX 0 C26 1 -0.163615 -0.107220 0.102717 11.00000 0.06795 0.06434 = 0.04594 0.01105 -0.00711 -0.03691 AFIX 23 H26A 2 -0.243292 -0.081109 0.096769 11.00000 -1.20000 H26B 2 -0.167909 -0.155374 0.068725 11.00000 -1.20000 AFIX 0 C27 1 -0.122187 -0.145095 0.165917 11.00000 0.07948 0.06375 = 0.05516 0.01441 -0.00462 -0.04410 AFIX 23 H27A 2 -0.087880 -0.206712 0.162733 11.00000 -1.20000 H27B 2 -0.188549 -0.152953 0.185821 11.00000 -1.20000 AFIX 0 C28 1 -0.033880 -0.085973 0.207721 11.00000 0.03870 0.03607 = 0.03133 0.00562 0.01346 -0.01257 AFIX 23 H28A 2 0.037861 -0.121694 0.229026 11.00000 -1.20000 H28B 2 -0.064176 -0.057265 0.242578 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_dm15102_0m in P21/c #14 REM R1 = 0.0323 for 7976 Fo > 4sig(Fo) and 0.0535 for all 10616 data REM 355 parameters refined using 18 restraints END WGHT 0.0275 0.9011 REM Highest difference peak 1.348, deepest hole -1.053, 1-sigma level 0.118 Q1 1 0.6216 0.1031 0.4307 11.00000 0.05 1.35 Q2 1 0.1320 0.1032 0.1528 11.00000 0.05 0.98 Q3 1 0.1194 0.1020 0.2266 11.00000 0.05 0.93 Q4 1 0.0485 0.1146 0.1898 11.00000 0.05 0.85 Q5 1 0.1686 0.0626 0.1935 11.00000 0.05 0.81 Q6 1 0.0755 0.1429 0.1801 11.00000 0.05 0.76 Q7 1 0.0834 0.0613 0.1853 11.00000 0.05 0.72 Q8 1 -0.0836 -0.1593 0.1665 11.00000 0.05 0.70 Q9 1 0.2164 0.1070 0.1926 11.00000 0.05 0.67 Q10 1 -0.1843 0.2154 0.0820 11.00000 0.05 0.63 Q11 1 -0.1714 -0.1118 0.1606 11.00000 0.05 0.63 Q12 1 0.1820 0.1415 0.1994 11.00000 0.05 0.61 Q13 1 0.3751 0.1368 0.1033 11.00000 0.05 0.54 Q14 1 -0.0559 0.2607 0.1204 11.00000 0.05 0.53 Q15 1 -0.1127 -0.1416 0.1031 11.00000 0.05 0.52 Q16 1 -0.1476 -0.1960 0.1882 11.00000 0.05 0.52 Q17 1 -0.2338 -0.1177 0.0585 11.00000 0.05 0.50 Q18 1 -0.0152 0.1216 0.3477 11.00000 0.05 0.48 Q19 1 0.3965 0.0183 0.0758 11.00000 0.05 0.48 Q20 1 0.3791 0.2470 0.3030 11.00000 0.05 0.47 ; _shelx_res_checksum 60665 _shelx_hkl_file ; 1 0 0 237.11 5.58 -1 0 0 242.51 5.58 2 0 0 -0.07 0.07 -2 0 0 0.19 0.17 -2 0 0 -0.15 0.11 -3 0 0 63.86 1.73 3 0 0 60.99 1.56 -4 0 0 249.06 6.05 4 0 0 232.11 5.73 -4 0 0 244.09 6.25 5 0 0 86.71 2.28 -5 0 0 94.38 2.82 -5 0 0 94.56 2.60 -6 0 0 1.04 0.22 -6 0 0 1.17 0.40 -6 0 0 1.39 0.33 -7 0 0 123.14 3.12 -7 0 0 125.92 3.56 -7 0 0 121.96 3.83 -8 0 0 188.90 5.59 -8 0 0 197.54 5.27 -8 0 0 188.09 4.69 -9 0 0 48.74 2.20 -9 0 0 46.59 1.89 -10 0 0 0.27 0.45 -10 0 0 0.50 0.54 -11 0 0 15.11 1.46 -11 0 0 17.93 1.29 -12 0 0 42.86 2.34 -12 0 0 46.69 2.17 -13 0 0 14.81 1.39 -13 0 0 12.95 1.52 -14 0 0 1.50 0.80 -15 0 0 8.39 1.38 -16 0 0 21.69 2.14 0 -1 0 -0.01 0.04 0 -1 0 -0.03 0.03 -1 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-27 3.11 1.00 -1 6 -27 6.70 1.32 8 -7 -27 0.27 0.77 -8 -7 27 0.08 0.93 -8 7 27 -0.10 0.91 7 -7 -27 0.07 0.77 -7 -7 27 0.44 1.04 -7 7 27 -0.10 0.92 -6 -7 27 -0.04 0.97 6 -7 -27 0.16 0.77 5 -7 -27 0.42 0.83 -5 -7 27 0.64 1.00 -4 -7 27 -0.83 0.95 4 -7 -27 -0.86 0.72 3 -7 -27 -0.54 0.76 -3 -7 27 0.15 1.04 2 -7 -27 0.87 0.80 -2 -7 27 0.96 1.06 -2 7 27 1.48 1.04 -1 -7 27 2.49 1.13 1 7 -27 1.24 0.93 0 -7 27 0.16 1.02 0 7 -27 1.04 0.85 7 -8 -27 16.47 1.87 -7 -8 27 19.74 2.17 -6 -8 27 9.76 1.66 6 -8 -27 13.35 1.68 -5 -8 27 0.31 1.00 5 -8 -27 -0.32 0.78 -4 -8 27 6.17 1.43 4 -8 -27 6.30 1.31 3 -8 -27 14.46 1.68 -3 -8 27 9.95 1.65 2 -8 -27 9.29 1.41 -2 -8 27 6.57 1.49 -1 -8 27 0.65 1.12 1 8 -27 0.20 0.77 -5 -9 27 18.18 2.15 4 -9 -27 12.38 1.65 -4 -9 27 10.70 1.78 -3 -9 27 -0.28 1.05 -10 0 28 15.91 2.03 -9 0 28 2.48 1.17 -8 0 28 0.39 0.95 -7 0 28 12.85 1.80 -6 0 28 14.55 1.89 -5 0 28 5.73 1.40 -4 0 28 0.69 1.00 -3 0 28 17.87 1.99 -2 0 28 15.10 1.84 -1 0 28 2.68 1.13 -1 0 -28 11.42 1.53 -10 -1 28 1.31 1.14 -10 1 28 0.29 1.02 -9 -1 28 2.93 1.22 -9 1 28 4.05 1.29 -8 -1 28 1.86 1.12 -8 1 28 2.22 1.15 -7 -1 28 1.13 1.08 -7 1 28 0.71 1.07 -6 -1 28 2.28 1.19 -6 1 28 1.38 1.08 -5 -1 28 5.73 1.40 -5 1 28 5.12 1.33 -4 -1 28 6.93 1.50 -4 1 28 9.32 1.58 -3 -1 28 1.98 1.13 -3 1 28 0.50 1.01 -2 -1 28 2.05 1.08 -2 1 28 1.78 1.09 -1 -1 28 11.22 1.65 -1 1 28 6.29 1.33 -1 1 -28 5.18 1.24 -10 -2 28 1.61 1.14 -10 2 28 1.04 1.09 -9 -2 28 -0.13 0.97 -9 2 28 -0.72 0.98 -8 -2 28 -0.12 1.01 -8 2 28 0.07 0.98 -7 -2 28 2.14 1.17 -7 2 28 1.28 1.07 -6 -2 28 1.30 1.08 -6 2 28 1.52 1.09 -5 -2 28 -0.58 0.92 -5 2 28 1.04 0.98 -4 -2 28 -0.07 0.99 -4 2 28 1.26 1.01 -3 -2 28 2.24 1.13 -3 2 28 3.49 1.19 -2 -2 28 1.16 1.12 -2 2 28 2.05 1.06 -1 -2 28 -0.36 0.95 -1 2 28 0.64 1.00 -1 2 -28 3.13 1.06 -9 -3 28 5.39 1.44 -9 3 28 6.32 1.50 -8 -3 28 6.94 1.47 -8 3 28 7.70 1.56 -7 -3 28 3.90 1.30 -7 3 28 2.68 1.22 -6 -3 28 2.05 1.14 -6 3 28 2.65 1.15 -5 -3 28 8.57 1.53 -5 3 28 10.29 1.63 -4 -3 28 18.58 2.06 -4 3 28 12.65 1.76 -3 -3 28 9.92 1.62 -3 3 28 6.77 1.43 -2 -3 28 2.21 1.13 -2 3 28 3.36 1.14 -1 -3 28 9.40 1.59 -1 3 28 6.12 1.40 -1 3 -28 3.13 1.01 -9 -4 28 -0.65 0.99 -9 4 28 1.73 1.12 -8 -4 28 0.90 1.03 -8 4 28 2.92 1.21 -7 -4 28 10.38 1.69 -7 4 28 6.85 1.48 -6 -4 28 8.84 1.65 -6 4 28 14.33 1.85 -5 -4 28 0.62 0.99 -5 4 28 1.35 1.11 -4 -4 28 1.70 1.17 -4 4 28 0.92 1.06 -3 -4 28 19.53 2.11 -3 4 28 17.83 2.06 -2 -4 28 13.94 1.85 -2 4 28 16.76 1.91 -1 -4 28 1.67 1.14 0 4 -28 0.73 0.84 -8 -5 28 0.14 0.98 -8 5 28 -0.41 0.93 -7 -5 28 -0.14 1.02 -7 5 28 0.68 1.04 -6 -5 28 0.41 0.99 -6 5 28 -1.09 0.82 -5 -5 28 1.78 1.07 -5 5 28 -1.18 0.91 -4 -5 28 2.12 1.12 -4 5 28 -0.07 0.98 -3 -5 28 1.31 1.14 -3 5 28 1.46 1.15 -2 -5 28 1.12 1.10 -2 5 28 2.66 1.17 -1 -5 28 0.20 1.02 0 5 -28 0.77 0.83 7 -6 -28 4.62 1.18 -7 -6 28 3.06 1.22 -7 6 28 4.07 1.26 6 -6 -28 4.87 1.15 -6 -6 28 3.76 1.26 -6 6 28 6.19 1.42 5 -6 -28 -0.17 0.77 -5 -6 28 0.51 1.04 -5 6 28 1.94 1.16 4 -6 -28 -0.06 0.76 -4 -6 28 0.91 1.05 -4 6 28 0.44 1.04 -3 -6 28 11.65 1.78 -3 6 28 6.54 1.47 -2 -6 28 12.22 1.79 -2 6 28 13.73 1.80 -1 -6 28 -0.03 0.96 6 -7 -28 3.58 1.12 -6 -7 28 3.85 1.31 5 -7 -28 14.97 1.70 -5 -7 28 10.50 1.72 4 -7 -28 13.21 1.62 -4 -7 28 15.53 1.98 -4 7 28 14.80 1.95 3 -7 -28 5.92 1.24 -3 7 28 6.92 1.47 -8 0 29 -0.67 0.91 -7 0 29 -0.43 0.97 -6 0 29 1.48 1.10 -5 0 29 0.31 1.02 -4 0 29 0.76 1.10 -3 0 29 0.16 0.98 -2 0 29 0.24 1.04 -8 -1 29 4.84 1.40 -8 1 29 4.83 1.36 -7 -1 29 3.55 1.30 -7 1 29 5.63 1.46 -6 -1 29 -0.93 0.97 -6 1 29 -1.12 0.99 -5 -1 29 8.23 1.58 -5 1 29 9.54 1.65 -4 -1 29 11.96 1.79 -4 1 29 9.18 1.64 -3 -1 29 6.92 1.45 -3 1 29 9.15 1.62 -2 -1 29 -1.00 0.93 -2 1 29 -1.34 0.93 -8 -2 29 -0.72 0.93 -8 2 29 -1.47 0.84 -7 -2 29 4.52 1.37 -7 2 29 5.23 1.34 -6 -2 29 12.85 1.85 -6 2 29 18.31 2.09 -5 -2 29 5.06 1.39 -5 2 29 3.23 1.29 -4 -2 29 0.24 1.01 -4 2 29 1.00 1.16 -3 -2 29 10.02 1.64 -3 2 29 7.48 1.54 -2 -2 29 20.87 2.16 -2 2 29 16.23 1.95 -1 -2 29 8.07 1.55 -8 -3 29 -0.06 1.02 -8 3 29 1.54 1.10 -7 -3 29 -0.97 1.01 -7 3 29 1.45 1.11 -6 -3 29 0.49 1.01 -6 3 29 0.08 0.98 -5 -3 29 0.61 1.07 -5 3 29 0.32 0.99 -4 -3 29 3.84 1.29 -4 3 29 1.93 1.15 -3 -3 29 1.50 1.16 -3 3 29 1.38 1.07 -2 -3 29 -0.94 0.97 -2 3 29 -0.64 0.92 -1 -3 29 0.54 1.05 -7 -4 29 -0.06 1.07 -7 4 29 0.09 1.04 -6 -4 29 4.97 1.38 -6 4 29 6.34 1.48 -5 -4 29 2.15 1.20 -5 4 29 2.46 1.20 -4 -4 29 0.65 1.14 -4 4 29 0.46 1.03 -3 -4 29 3.01 1.32 -3 4 29 2.89 1.25 -2 -4 29 4.13 1.33 -2 4 29 5.01 1.31 -6 -5 29 -0.58 1.00 -6 5 29 -0.14 1.01 -5 -5 29 6.38 1.51 -5 5 29 6.11 1.45 -4 -5 29 17.70 2.13 -4 5 29 13.01 1.87 -3 -5 29 9.50 1.66 -3 5 29 10.84 1.71 -5 0 30 12.24 1.88 -4 0 30 -1.33 0.91 -5 -1 30 1.08 1.09 -5 1 30 0.87 1.09 -4 -1 30 4.34 1.39 -4 1 30 2.90 1.24 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 16871 #===END data_dm15658 _audit_creation_date 2015-11-05 _audit_creation_method ; Olex2 1.2 (compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) ; _shelxl_version_number 2014-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C47 H42 Lu2 N16 Si' _chemical_formula_sum 'C46 H66 Lu2 N16 Si' _chemical_formula_weight 1220.17 _chemical_melting_point ? 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' 'Lu' 'Lu' -0.4720 5.8584 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 59 _space_group_name_H-M_alt 'P m m n' _space_group_name_Hall '-P 2ab 2a' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y, -z' '-x, y+1/2, -z' '-x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y, z' 'x, -y-1/2, z' 'x-1/2, y-1/2, -z' _cell_length_a 13.8939(13) _cell_length_b 17.3468(17) _cell_length_c 11.7131(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2823.0(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9328 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 30.29 _cell_measurement_theta_min 2.27 _shelx_estimated_absorpt_T_max 0.568 _shelx_estimated_absorpt_T_min 0.510 _exptl_absorpt_coefficient_mu 3.542 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1217 before and 0.0488 after correction. The Ratio of minimum to maximum transmission is 0.6765. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'orange' _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description 'block' _exptl_crystal_F_000 1218 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 28626 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.581 _diffrn_reflns_theta_min 1.878 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3832 _reflns_number_total 4619 _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 2.058 _refine_diff_density_min -3.135 _refine_diff_density_rms 0.175 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 222 _refine_ls_number_reflns 4619 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0434 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+13.6609P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.1185 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints C1 \\sim N4 \\sim N2: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C1) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(N5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 3. Others Fixed Sof: C8(0.5) C7(0.5) C9(0.5) C16(0.5) C15(0.25) H15(0.25) C12(0.25) H12(0.25) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C13(0.5) Si1(0.25) C10(0.5) C11(0.5) C20(0.5) C19(0.5) 4.a Aromatic/amide H refined with riding coordinates: C4(H4), C15(H15), C12(H12) 4.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.2500 0.84966(2) 0.80573(2) 0.02166(9) Uani 1 2 d S T P A . C1 C 0.2500 1.0486(3) 0.8108(4) 0.0166(8) Uani 1 2 d S TU P . . N1 N 0.3567(3) 0.9451(3) 0.7418(5) 0.0460(11) Uani 1 1 d . U . . . N2 N 0.3348(3) 1.0221(2) 0.7565(4) 0.0359(9) Uani 1 1 d . U . . . C18 C 0.2500 0.7500 0.6762(8) 0.041(3) Uani 1 4 d S T P A . N4 N 0.2500 1.0213(4) 0.9279(6) 0.0444(13) Uani 1 2 d S TU P . . N3 N 0.2500 0.9431(4) 0.9566(7) 0.062(2) Uani 1 2 d S TU P . . C8 C 0.2894(6) 0.9405(5) 1.0703(8) 0.0273(16) Uani 0.5 1 d . . . . . C7 C 0.2968(8) 0.8659(5) 1.1335(8) 0.0326(19) Uani 0.5 1 d . . . . . C9 C 0.2048(6) 1.0175(5) 1.1146(7) 0.0282(17) Uani 0.5 1 d . . . . . C3 C 0.4437(6) 0.9437(5) 0.6923(8) 0.078(2) Uani 1 1 d . U . . . C4 C 0.4771(7) 1.0190(5) 0.6737(9) 0.091(3) Uani 1 1 d . U . . . H4 H 0.5348 1.0335 0.6397 0.109 Uiso 1 1 calc R . . . . C5 C 0.4072(5) 1.0666(4) 0.7159(7) 0.0610(17) Uani 1 1 d . U . . . C6 C 0.4040(6) 1.1521(4) 0.7199(10) 0.077(3) Uani 1 1 d . U . . . H6A H 0.3530 1.1704 0.6717 0.115 Uiso 1 1 calc GR . . . . H6B H 0.4643 1.1726 0.6935 0.115 Uiso 1 1 calc GR . . . . H6C H 0.3928 1.1687 0.7969 0.115 Uiso 1 1 calc GR . . . . C2 C 0.4936(8) 0.8690(6) 0.6686(12) 0.114(4) Uani 1 1 d . U . . . H2A H 0.5477 0.8635 0.7190 0.171 Uiso 1 1 calc GR . . . . H2B H 0.5156 0.8683 0.5909 0.171 Uiso 1 1 calc GR . . . . H2C H 0.4497 0.8271 0.6806 0.171 Uiso 1 1 calc GR . . . . N5 N 0.1254(5) 0.7907(3) 0.9056(6) 0.0674(16) Uani 1 1 d . U . . . C16 C 0.0749(6) 0.8135(5) 1.0004(8) 0.0273(17) Uani 0.5 1 d . . . A 2 C15 C 0.0288(9) 0.7500 1.0479(12) 0.030(3) Uani 0.5 2 d S T P A 2 H15 H -0.0218 0.7500 1.0998 0.036 Uiso 0.5 2 calc RS T P A 2 C12 C -0.0318(8) 0.7500 0.9580(11) 0.027(2) Uani 0.5 2 d S T P A 1 H12 H -0.0932 0.7500 0.9896 0.032 Uiso 0.5 2 calc RS T P A 1 C14 C -0.0039(7) 0.8973(6) 0.9425(10) 0.037(2) Uani 0.5 1 d . . . A 1 H14A H 0.0057 0.9130 1.0202 0.055 Uiso 0.5 1 calc GR . . A 1 H14B H -0.0704 0.9038 0.9224 0.055 Uiso 0.5 1 calc GR . . A 1 H14C H 0.0353 0.9283 0.8931 0.055 Uiso 0.5 1 calc GR . . A 1 C17 C 0.0511(7) 0.8970(5) 1.0227(10) 0.036(2) Uani 0.5 1 d . . . A 2 H17A H 0.0951 0.9175 1.0781 0.055 Uiso 0.5 1 calc GR . . A 2 H17B H -0.0135 0.9009 1.0512 0.055 Uiso 0.5 1 calc GR . . A 2 H17C H 0.0566 0.9257 0.9529 0.055 Uiso 0.5 1 calc GR . . A 2 C13 C 0.0236(6) 0.8141(5) 0.9295(7) 0.0240(15) Uani 0.5 1 d . . . A 1 Si1 Si 0.2217(3) 0.7500 0.5249(3) 0.0410(10) Uani 0.5 2 d S T P . . C10 C 0.2163(6) 1.0649(5) 1.0232(7) 0.0263(16) Uani 0.5 1 d . . . . . C11 C 0.2165(8) 1.1517(5) 1.0195(11) 0.038(2) Uani 0.5 1 d . . . . . C20 C 0.2040(19) 0.6389(14) 0.469(2) 0.116(8) Uani 0.5 1 d . U . B 2 C19 C 0.133(2) 0.7172(16) 0.449(3) 0.151(11) Uani 0.5 1 d . U . B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.02526(13) 0.02118(13) 0.01855(12) 0.00300(9) 0.000 0.000 C1 0.0230(19) 0.0174(18) 0.0094(16) 0.0071(15) 0.000 0.000 N1 0.038(2) 0.0303(19) 0.070(3) 0.005(2) 0.014(2) -0.0011(17) N2 0.0360(18) 0.0250(16) 0.047(2) 0.0051(15) -0.0002(17) -0.0037(14) C18 0.071(8) 0.033(5) 0.020(4) 0.000 0.000 0.000 N4 0.071(3) 0.030(2) 0.032(2) 0.005(2) 0.000 0.000 N3 0.107(5) 0.038(3) 0.041(3) 0.003(3) 0.000 0.000 C8 0.029(4) 0.022(3) 0.031(4) 0.003(3) -0.003(3) -0.001(3) C7 0.047(5) 0.032(4) 0.019(4) 0.008(3) -0.006(4) -0.003(4) C9 0.029(4) 0.033(4) 0.023(4) -0.005(3) 0.002(3) 0.003(3) C3 0.058(3) 0.054(3) 0.120(5) 0.003(3) 0.031(3) -0.004(3) C4 0.069(4) 0.071(4) 0.132(5) 0.007(4) 0.031(4) -0.013(3) C5 0.048(3) 0.040(3) 0.095(4) 0.005(3) 0.012(3) -0.009(2) C6 0.057(4) 0.037(3) 0.136(7) 0.010(4) 0.007(4) -0.013(3) C2 0.075(5) 0.064(5) 0.204(9) 0.000(6) 0.057(6) 0.000(4) N5 0.085(3) 0.032(2) 0.086(3) 0.001(2) 0.059(3) 0.002(2) C16 0.024(4) 0.023(4) 0.035(4) -0.004(3) 0.002(3) 0.002(3) C15 0.019(5) 0.036(6) 0.034(6) 0.000 0.008(5) 0.000 C12 0.015(5) 0.040(6) 0.026(5) 0.000 0.005(4) 0.000 C14 0.026(4) 0.035(5) 0.049(6) 0.000(4) 0.006(4) 0.009(4) C17 0.036(5) 0.028(4) 0.046(6) 0.001(4) 0.019(4) 0.002(4) C13 0.020(3) 0.035(4) 0.017(3) 0.000(3) -0.002(3) 0.005(3) Si1 0.0301(19) 0.074(3) 0.0190(15) 0.000 -0.0051(12) 0.000 C10 0.030(4) 0.019(3) 0.030(4) 0.001(3) 0.004(3) 0.009(3) C11 0.035(4) 0.023(4) 0.055(6) 0.001(4) 0.002(4) 0.005(3) C20 0.116(9) 0.118(9) 0.113(9) -0.006(5) 0.000(5) -0.004(5) C19 0.157(12) 0.148(12) 0.147(12) -0.004(5) -0.010(5) 0.002(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 Lu1 Lu1 3.4575(6) 7_575 ? Lu1 N1 2.345(4) 6_655 ? Lu1 N1 2.345(5) . ? Lu1 C18 2.300(6) . ? Lu1 N3 2.398(8) . ? Lu1 N5 2.326(5) . ? Lu1 N5 2.326(5) 6_655 ? C1 N2 1.416(5) 6_655 ? C1 N2 1.416(5) . ? C1 N4 1.451(8) . ? N1 N2 1.381(6) . ? N1 C3 1.340(9) . ? N2 C5 1.354(7) . ? C18 Lu1 2.300(6) 7_575 ? C18 Si1 1.815(10) 6_655 ? C18 Si1 1.815(10) . ? N4 N3 1.398(9) . ? N4 C10 1.427(10) . ? N4 C10 1.427(10) 6_655 ? N3 C8 1.441(11) 6_655 ? N3 C8 1.441(11) . ? C8 C8 1.094(18) 6_655 ? C8 C7 1.913(13) 6_655 ? C8 C7 1.495(12) . ? C8 C9 1.434(12) 6_655 ? C8 C9 1.853(12) . ? C7 C8 1.913(13) 6_655 ? C7 C7 1.30(2) 6_655 ? C9 C8 1.434(12) 6_655 ? C9 C9 1.257(18) 6_655 ? C9 C10 1.739(12) 6_655 ? C9 C10 1.360(12) . ? C3 C4 1.404(12) . ? C3 C2 1.497(12) . ? C4 H4 0.9300 . ? C4 C5 1.367(11) . ? C5 C6 1.486(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N5 N5 1.411(10) 7_575 ? N5 C16 1.372(10) . ? N5 C13 1.498(10) . ? C16 C15 1.390(11) . ? C16 C17 1.508(12) . ? C15 C16 1.390(11) 7_575 ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C12 C13 1.393(11) 7_575 ? C12 C13 1.393(11) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 C13 1.501(13) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? Si1 Si1 0.785(8) 6_655 ? Si1 C20 2.28(2) 6_655 ? Si1 C20 2.05(2) 7_575 ? Si1 C20 2.28(2) 4_565 ? Si1 C20 2.05(2) . ? Si1 C19 2.27(3) 4_565 ? Si1 C19 2.27(3) 6_655 ? Si1 C19 1.62(3) . ? Si1 C19 1.62(3) 7_575 ? C10 C9 1.739(12) 6_655 ? C10 C10 0.936(17) 6_655 ? C10 C11 1.506(12) . ? C10 C11 1.771(12) 6_655 ? C11 C10 1.771(12) 6_655 ? C11 C11 0.93(2) 6_655 ? C20 Si1 2.28(2) 6_655 ? C20 C20 1.28(5) 6_655 ? C19 Si1 2.27(3) 6_655 ? C19 C19 1.14(6) 7_575 ? 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 Lu1 Lu1 134.90(12) . 7_575 ? N1 Lu1 Lu1 134.90(12) 6_655 7_575 ? N1 Lu1 N1 78.4(2) . 6_655 ? N1 Lu1 N3 75.99(19) 6_655 . ? N1 Lu1 N3 75.99(19) . . ? C18 Lu1 Lu1 41.26(18) . 7_575 ? C18 Lu1 N1 108.67(19) . . ? C18 Lu1 N1 108.67(19) . 6_655 ? C18 Lu1 N3 173.8(3) . . ? C18 Lu1 N5 90.06(18) . 6_655 ? C18 Lu1 N5 90.06(19) . . ? N3 Lu1 Lu1 132.53(18) . 7_575 ? N5 Lu1 Lu1 63.90(12) . 7_575 ? N5 Lu1 Lu1 63.91(12) 6_655 7_575 ? N5 Lu1 N1 160.30(17) . . ? N5 Lu1 N1 160.30(18) 6_655 6_655 ? N5 Lu1 N1 90.0(2) 6_655 . ? N5 Lu1 N1 90.0(2) . 6_655 ? N5 Lu1 N3 85.80(19) . . ? N5 Lu1 N3 85.80(19) 6_655 . ? N5 Lu1 N5 96.2(4) 6_655 . ? N2 C1 N2 112.7(5) 6_655 . ? N2 C1 N4 108.6(3) 6_655 . ? N2 C1 N4 108.6(3) . . ? N2 N1 Lu1 120.2(3) . . ? C3 N1 Lu1 134.0(5) . . ? C3 N1 N2 105.7(5) . . ? N1 N2 C1 123.6(4) . . ? C5 N2 C1 126.2(5) . . ? C5 N2 N1 110.1(5) . . ? Lu1 C18 Lu1 97.5(4) . 7_575 ? Si1 C18 Lu1 130.08(16) . . ? Si1 C18 Lu1 130.08(16) 6_655 7_575 ? Si1 C18 Lu1 130.08(16) 6_655 . ? Si1 C18 Lu1 130.08(16) . 7_575 ? Si1 C18 Si1 25.0(3) . 6_655 ? N3 N4 C1 122.9(6) . . ? N3 N4 C10 109.1(6) . . ? N3 N4 C10 109.1(6) . 6_655 ? C10 N4 C1 124.5(6) 6_655 . ? C10 N4 C1 124.5(6) . . ? C10 N4 C10 38.3(7) . 6_655 ? N4 N3 Lu1 118.7(5) . . ? N4 N3 C8 104.6(6) . . ? N4 N3 C8 104.6(6) . 6_655 ? C8 N3 Lu1 131.3(5) 6_655 . ? C8 N3 Lu1 131.3(5) . . ? C8 N3 C8 44.6(8) 6_655 . ? N3 C8 C7 120.7(8) . . ? N3 C8 C7 98.1(6) . 6_655 ? N3 C8 C9 89.7(6) . . ? C8 C8 N3 67.7(4) 6_655 . ? C8 C8 C7 94.0(5) 6_655 . ? C8 C8 C7 51.2(4) 6_655 6_655 ? C8 C8 C9 93.3(5) 6_655 6_655 ? C8 C8 C9 50.6(4) 6_655 . ? C7 C8 C7 42.7(7) . 6_655 ? C7 C8 C9 122.0(7) . . ? C9 C8 N3 109.1(7) 6_655 . ? C9 C8 C7 89.0(6) . 6_655 ? C9 C8 C7 121.7(7) 6_655 6_655 ? C9 C8 C7 128.6(8) 6_655 . ? C9 C8 C9 42.6(7) 6_655 . ? C8 C7 C8 34.8(6) . 6_655 ? C7 C7 C8 51.2(4) 6_655 6_655 ? C7 C7 C8 86.0(5) 6_655 . ? C8 C9 C8 36.1(6) 6_655 . ? C8 C9 C10 100.5(7) 6_655 6_655 ? C9 C9 C8 50.6(4) 6_655 . ? C9 C9 C8 86.7(5) 6_655 6_655 ? C9 C9 C10 83.2(5) 6_655 . ? C9 C9 C10 50.9(4) 6_655 6_655 ? C10 C9 C8 76.6(5) 6_655 . ? C10 C9 C8 98.1(6) . . ? C10 C9 C8 105.8(7) . 6_655 ? C10 C9 C10 32.3(6) . 6_655 ? N1 C3 C4 110.4(7) . . ? N1 C3 C2 120.9(7) . . ? C4 C3 C2 128.6(8) . . ? C3 C4 H4 127.2 . . ? C5 C4 C3 105.7(7) . . ? C5 C4 H4 127.2 . . ? N2 C5 C4 108.1(6) . . ? N2 C5 C6 122.5(7) . . ? C4 C5 C6 129.4(7) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N5 N5 Lu1 116.10(12) 7_575 . ? N5 N5 C13 105.7(4) 7_575 . ? C16 N5 Lu1 131.4(5) . . ? C16 N5 N5 106.8(4) . 7_575 ? C13 N5 Lu1 132.6(5) . . ? N5 C16 C15 109.3(7) . . ? N5 C16 C17 121.9(8) . . ? C15 C16 C17 126.2(8) . . ? C16 C15 C16 104.8(11) 7_575 . ? C16 C15 H15 127.6 7_575 . ? C16 C15 H15 127.6 . . ? C13 C12 H12 127.1 . . ? C13 C12 H12 127.1 7_575 . ? C13 C12 C13 105.9(10) . 7_575 ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C13 C14 121.4(7) . . ? C12 C13 N5 110.5(7) . . ? C12 C13 C14 127.0(8) . . ? C18 Si1 C20 109.9(8) . 7_575 ? C18 Si1 C20 109.9(8) . . ? C18 Si1 C20 100.6(7) . 4_565 ? C18 Si1 C20 100.6(7) . 6_655 ? C18 Si1 C19 101.0(8) . 6_655 ? C18 Si1 C19 101.0(8) . 4_565 ? Si1 Si1 C18 77.51(14) 6_655 . ? Si1 Si1 C20 63.1(6) 6_655 4_565 ? Si1 Si1 C20 96.9(7) 6_655 . ? Si1 Si1 C20 63.1(6) 6_655 6_655 ? Si1 Si1 C20 96.9(7) 6_655 7_575 ? Si1 Si1 C19 27.7(8) 6_655 4_565 ? Si1 Si1 C19 139.3(11) 6_655 . ? Si1 Si1 C19 139.3(11) 6_655 7_575 ? Si1 Si1 C19 27.7(8) 6_655 6_655 ? C20 Si1 C20 138.9(13) 7_575 6_655 ? C20 Si1 C20 33.8(13) 7_575 4_565 ? C20 Si1 C20 139.8(15) 7_575 . ? C20 Si1 C20 138.9(13) . 4_565 ? C20 Si1 C20 115.1(13) 4_565 6_655 ? C20 Si1 C20 33.8(13) . 6_655 ? C19 Si1 C18 134.4(11) . . ? C19 Si1 C18 134.4(11) 7_575 . ? C19 Si1 C19 111.6(18) 7_575 4_565 ? C19 Si1 C19 41(2) 7_575 . ? C19 Si1 C19 29.0(14) 4_565 6_655 ? C19 Si1 C19 123.0(18) . 4_565 ? C19 Si1 C19 123.0(18) 7_575 6_655 ? C19 Si1 C19 111.6(18) . 6_655 ? N4 C10 C9 91.3(5) . 6_655 ? N4 C10 C11 104.9(7) . 6_655 ? N4 C10 C11 120.4(8) . . ? C9 C10 N4 109.5(7) . . ? C9 C10 C9 45.9(7) . 6_655 ? C9 C10 C11 126.6(8) . 6_655 ? C9 C10 C11 128.9(9) . . ? C9 C10 C11 94.9(6) 6_655 6_655 ? C10 C10 N4 70.9(4) 6_655 . ? C10 C10 C9 50.9(4) 6_655 6_655 ? C10 C10 C9 96.8(5) 6_655 . ? C10 C10 C11 58.2(4) 6_655 6_655 ? C10 C10 C11 89.9(5) 6_655 . ? C11 C10 C9 119.3(8) . 6_655 ? C11 C10 C11 31.7(7) . 6_655 ? C10 C11 C10 31.9(6) . 6_655 ? C11 C11 C10 58.2(4) 6_655 6_655 ? C11 C11 C10 90.1(5) 6_655 . ? Si1 C20 Si1 20.0(3) . 6_655 ? C20 C20 Si1 83.1(7) 6_655 . ? C20 C20 Si1 63.1(6) 6_655 6_655 ? Si1 C19 Si1 13.0(4) . 6_655 ? C19 C19 Si1 69.4(10) 7_575 . ? C19 C19 Si1 75.5(7) 7_575 6_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 Lu1 N1 N2 C1 0.9(7) . . . . ? Lu1 N1 N2 C5 178.6(5) . . . . ? Lu1 N1 C3 C4 -178.7(6) . . . . ? Lu1 N1 C3 C2 -1.1(15) . . . . ? Lu1 C18 Si1 Si1 100.75(16) . . . 6_655 ? Lu1 C18 Si1 Si1 -100.75(16) 7_575 . . 6_655 ? Lu1 C18 Si1 C20 -7.8(8) 7_575 . . . ? Lu1 C18 Si1 C20 -166.3(8) . . . . ? Lu1 C18 Si1 C20 166.3(8) 7_575 . . 7_575 ? Lu1 C18 Si1 C20 -41.6(7) 7_575 . . 6_655 ? Lu1 C18 Si1 C20 159.9(7) . . . 6_655 ? Lu1 C18 Si1 C20 -159.9(7) 7_575 . . 4_565 ? Lu1 C18 Si1 C20 7.8(8) . . . 7_575 ? Lu1 C18 Si1 C20 41.6(7) . . . 4_565 ? Lu1 C18 Si1 C19 -115.5(7) 7_575 . . 4_565 ? Lu1 C18 Si1 C19 108.8(14) 7_575 . . 7_575 ? Lu1 C18 Si1 C19 86.0(7) . . . 4_565 ? Lu1 C18 Si1 C19 -49.7(15) . . . 7_575 ? Lu1 C18 Si1 C19 -86.0(7) 7_575 . . 6_655 ? Lu1 C18 Si1 C19 49.7(15) 7_575 . . . ? Lu1 C18 Si1 C19 115.5(7) . . . 6_655 ? Lu1 C18 Si1 C19 -108.8(14) . . . . ? Lu1 N3 C8 C8 -111.2(5) . . . 6_655 ? Lu1 N3 C8 C7 -30.2(11) . . . . ? Lu1 N3 C8 C7 -69.1(6) . . . 6_655 ? Lu1 N3 C8 C9 163.3(5) . . . 6_655 ? Lu1 N3 C8 C9 -158.0(4) . . . . ? Lu1 N5 C16 C15 -162.1(7) . . . . ? Lu1 N5 C16 C17 35.0(12) . . . . ? Lu1 N5 C13 C12 159.5(7) . . . . ? Lu1 N5 C13 C14 -31.6(11) . . . . ? C1 N2 C5 C4 177.8(7) . . . . ? C1 N2 C5 C6 -2.5(12) . . . . ? C1 N4 N3 Lu1 0.000(5) . . . . ? C1 N4 N3 C8 -156.9(4) . . . 6_655 ? C1 N4 N3 C8 156.9(4) . . . . ? C1 N4 C10 C9 165.6(5) . . . . ? C1 N4 C10 C9 -151.3(4) . . . 6_655 ? C1 N4 C10 C10 -103.8(4) . . . 6_655 ? C1 N4 C10 C11 -25.7(10) . . . . ? C1 N4 C10 C11 -55.9(7) . . . 6_655 ? N1 N2 C5 C4 0.3(9) . . . . ? N1 N2 C5 C6 179.9(8) . . . . ? N1 C3 C4 C5 1.0(12) . . . . ? N2 C1 N2 N1 -58.6(7) 6_655 . . . ? N2 C1 N2 C5 124.2(6) 6_655 . . . ? N2 C1 N4 N3 61.4(3) 6_655 . . . ? N2 C1 N4 N3 -61.4(3) . . . . ? N2 C1 N4 C10 95.1(6) . . . 6_655 ? N2 C1 N4 C10 -142.1(5) 6_655 . . 6_655 ? N2 C1 N4 C10 -95.1(6) 6_655 . . . ? N2 C1 N4 C10 142.1(5) . . . . ? N2 N1 C3 C4 -0.8(10) . . . . ? N2 N1 C3 C2 176.8(10) . . . . ? C18 Si1 C19 Si1 -132(2) . . . 6_655 ? C18 Si1 C19 C19 111.6(12) . . . 7_575 ? N4 C1 N2 N1 61.7(6) . . . . ? N4 C1 N2 C5 -115.6(7) . . . . ? N4 N3 C8 C8 96.1(3) . . . 6_655 ? N4 N3 C8 C7 138.2(4) . . . 6_655 ? N4 N3 C8 C7 177.1(7) . . . . ? N4 N3 C8 C9 10.5(8) . . . 6_655 ? N4 N3 C8 C9 49.3(5) . . . . ? N4 C10 C11 C10 -67.6(7) . . . 6_655 ? N4 C10 C11 C11 -67.6(7) . . . 6_655 ? N3 N4 C10 C9 6.3(8) . . . . ? N3 N4 C10 C9 49.4(5) . . . 6_655 ? N3 N4 C10 C10 96.9(3) . . . 6_655 ? N3 N4 C10 C11 175.0(7) . . . . ? N3 N4 C10 C11 144.8(5) . . . 6_655 ? N3 C8 C7 C8 -66.3(7) . . . 6_655 ? N3 C8 C7 C7 -66.3(7) . . . 6_655 ? N3 C8 C9 C8 60.8(6) . . . 6_655 ? N3 C8 C9 C9 -119.2(6) . . . 6_655 ? N3 C8 C9 C10 -69.2(5) . . . 6_655 ? N3 C8 C9 C10 -44.9(7) . . . . ? C8 N3 C8 C7 42.1(5) 6_655 . . 6_655 ? C8 N3 C8 C7 81.0(8) 6_655 . . . ? C8 N3 C8 C9 -46.8(5) 6_655 . . . ? C8 N3 C8 C9 -85.6(7) 6_655 . . 6_655 ? C8 C8 C7 C7 -0.003(2) 6_655 . . 6_655 ? C8 C8 C9 C9 180.003(1) 6_655 . . 6_655 ? C8 C8 C9 C10 -105.7(7) 6_655 . . . ? C8 C8 C9 C10 -130.1(5) 6_655 . . 6_655 ? C8 C9 C10 N4 23.5(8) . . . . ? C8 C9 C10 N4 -12.6(10) 6_655 . . . ? C8 C9 C10 C9 -84.7(6) 6_655 . . 6_655 ? C8 C9 C10 C9 -48.5(5) . . . 6_655 ? C8 C9 C10 C10 -84.7(6) 6_655 . . 6_655 ? C8 C9 C10 C10 -48.5(5) . . . 6_655 ? C8 C9 C10 C11 -143.9(9) . . . . ? C8 C9 C10 C11 -139.7(8) 6_655 . . 6_655 ? C8 C9 C10 C11 -103.6(8) . . . 6_655 ? C8 C9 C10 C11 180.0(9) 6_655 . . . ? C7 C8 C7 C8 0.003(3) 6_655 . . 6_655 ? C7 C8 C9 C8 -37.3(6) 6_655 . . 6_655 ? C7 C8 C9 C8 -66.0(9) . . . 6_655 ? C7 C8 C9 C9 142.7(6) 6_655 . . 6_655 ? C7 C8 C9 C9 114.0(9) . . . 6_655 ? C7 C8 C9 C10 164.0(8) . . . 6_655 ? C7 C8 C9 C10 -171.7(8) . . . . ? C7 C8 C9 C10 -167.3(6) 6_655 . . 6_655 ? C7 C8 C9 C10 -143.0(7) 6_655 . . . ? C9 C8 C7 C8 45.0(6) . . . 6_655 ? C9 C8 C7 C8 97.4(9) 6_655 . . 6_655 ? C9 C8 C7 C7 45.0(6) . . . 6_655 ? C9 C8 C7 C7 97.4(9) 6_655 . . 6_655 ? C9 C8 C9 C8 179.997(2) 6_655 . . 6_655 ? C9 C8 C9 C10 49.9(5) 6_655 . . 6_655 ? C9 C8 C9 C10 74.2(7) 6_655 . . . ? C9 C9 C10 N4 72.0(5) 6_655 . . . ? C9 C9 C10 C10 0.002(2) 6_655 . . 6_655 ? C9 C9 C10 C11 -55.1(7) 6_655 . . 6_655 ? C9 C9 C10 C11 -95.4(10) 6_655 . . . ? C9 C10 C11 C10 98.6(10) . . . 6_655 ? C9 C10 C11 C10 43.6(7) 6_655 . . 6_655 ? C9 C10 C11 C11 43.6(7) 6_655 . . 6_655 ? C9 C10 C11 C11 98.6(10) . . . 6_655 ? C3 N1 N2 C1 -177.3(6) . . . . ? C3 N1 N2 C5 0.3(8) . . . . ? C3 C4 C5 N2 -0.7(11) . . . . ? C3 C4 C5 C6 179.6(10) . . . . ? C2 C3 C4 C5 -176.4(11) . . . . ? N5 N5 C16 C15 -10.8(9) 7_575 . . . ? N5 N5 C16 C17 -173.7(7) 7_575 . . . ? N5 N5 C13 C12 7.8(8) 7_575 . . . ? N5 N5 C13 C14 176.7(7) 7_575 . . . ? N5 C16 C15 C16 17.1(14) . . . 7_575 ? C16 N5 C13 C12 -90.3(10) . . . . ? C16 N5 C13 C14 78.5(10) . . . . ? C17 C16 C15 C16 179.1(7) . . . 7_575 ? C13 N5 C16 C15 84.8(10) . . . . ? C13 N5 C16 C17 -78.1(10) . . . . ? C13 C12 C13 N5 -12.6(13) 7_575 . . . ? C13 C12 C13 C14 179.4(7) 7_575 . . . ? Si1 C18 Si1 C20 -92.9(8) 6_655 . . 7_575 ? Si1 C18 Si1 C20 -59.2(7) 6_655 . . 4_565 ? Si1 C18 Si1 C20 59.2(7) 6_655 . . 6_655 ? Si1 C18 Si1 C20 92.9(8) 6_655 . . . ? Si1 C18 Si1 C19 14.8(7) 6_655 . . 6_655 ? Si1 C18 Si1 C19 -150.5(14) 6_655 . . 7_575 ? Si1 C18 Si1 C19 150.5(14) 6_655 . . . ? Si1 C18 Si1 C19 -14.8(7) 6_655 . . 4_565 ? Si1 Si1 C19 C19 -115.9(14) 6_655 . . 7_575 ? C10 N4 N3 Lu1 -159.7(4) 6_655 . . . ? C10 N4 N3 Lu1 159.7(4) . . . . ? C10 N4 N3 C8 -2.8(6) 6_655 . . . ? C10 N4 N3 C8 2.8(6) . . . 6_655 ? C10 N4 N3 C8 -43.4(5) . . . . ? C10 N4 N3 C8 43.4(5) 6_655 . . 6_655 ? C10 N4 C10 C9 -90.6(7) 6_655 . . . ? C10 N4 C10 C9 -47.5(5) 6_655 . . 6_655 ? C10 N4 C10 C11 78.1(8) 6_655 . . . ? C10 N4 C10 C11 47.9(6) 6_655 . . 6_655 ? C10 C9 C10 N4 72.0(5) 6_655 . . . ? C10 C9 C10 C9 -0.002(4) 6_655 . . 6_655 ? C10 C9 C10 C11 -55.1(7) 6_655 . . 6_655 ? C10 C9 C10 C11 -95.4(10) 6_655 . . . ? C10 C10 C11 C11 0.000(1) 6_655 . . 6_655 ? C11 C10 C11 C10 0.000(1) 6_655 . . 6_655 ? C20 Si1 C19 Si1 -33.9(14) 6_655 . . 6_655 ? C20 Si1 C19 Si1 -50(2) . . . 6_655 ? C20 Si1 C19 Si1 104.9(14) 7_575 . . 6_655 ? C20 Si1 C19 Si1 81.2(15) 4_565 . . 6_655 ? C20 Si1 C19 C19 -166.3(10) . . . 7_575 ? C20 Si1 C19 C19 -149.8(7) 6_655 . . 7_575 ? C20 Si1 C19 C19 -11.0(8) 7_575 . . 7_575 ? C20 Si1 C19 C19 -34.7(8) 4_565 . . 7_575 ? C19 Si1 C19 Si1 30.2(12) 4_565 . . 6_655 ? C19 Si1 C19 Si1 115.9(14) 7_575 . . 6_655 ? C19 Si1 C19 Si1 -0.002(8) 6_655 . . 6_655 ? C19 Si1 C19 C19 -85.7(7) 4_565 . . 7_575 ? C19 Si1 C19 C19 -115.9(14) 6_655 . . 7_575 ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.250 0.250 0.415 210.6 39.4 ? 2 -0.250 0.750 0.585 210.6 40.8 ? 3 0.250 0.250 0.813 7.8 0.0 ? 4 0.750 0.750 0.187 7.8 0.0 ? _shelx_res_file ; TITL dm15658 in Pmmn CELL 0.71073 13.8939 17.3468 11.7131 90 90 90 ZERR 2 0.0013 0.0017 0.0011 0 0 0 LATT 1 SYMM 0.5+X,-Y,-Z SYMM -X,0.5+Y,-Z SYMM 0.5-X,0.5-Y,+Z SFAC C H Lu N Si UNIT 92 130 4 32 2 SIMU 0.005 0.01 2 C1 N4 N2 ISOR 0.005 0.01 C1 C19 C20 ISOR 0.005 0.01 N5 N3 N2 N1 C2 C3 C4 C5 C6 ISOR 0.005 0.01 N4 N3 L.S. 12 PLAN -5 0 0 SIZE 0.18 0.2 0.22 TEMP 23 BOND $H MORE -1 CONF fmap 2 acta REM D:/data/guest/dm15658/work/dm15658-mask.hkl WGHT 0.055700 13.660901 FVAR 0.07869 LU1 3 0.250000 0.849658 0.805726 10.50000 0.02526 0.02118 = 0.01855 0.00300 0.00000 0.00000 C1 1 0.250000 1.048621 0.810786 10.50000 0.02297 0.01739 = 0.00937 0.00711 0.00000 0.00000 N1 4 0.356737 0.945102 0.741822 11.00000 0.03751 0.03029 = 0.07012 0.00470 0.01351 -0.00110 N2 4 0.334813 1.022087 0.756502 11.00000 0.03604 0.02495 = 0.04665 0.00505 -0.00023 -0.00371 C18 1 0.250000 0.750000 0.676245 10.25000 0.07088 0.03312 = 0.02013 0.00000 0.00000 0.00000 N4 4 0.250000 1.021329 0.927918 10.50000 0.07150 0.03009 = 0.03158 0.00526 0.00000 0.00000 N3 4 0.250000 0.943092 0.956555 10.50000 0.10717 0.03802 = 0.04092 0.00318 0.00000 0.00000 C8 1 0.289381 0.940527 1.070330 10.50000 0.02893 0.02173 = 0.03121 0.00252 -0.00276 -0.00125 C7 1 0.296819 0.865886 1.133549 10.50000 0.04713 0.03157 = 0.01910 0.00766 -0.00558 -0.00343 C9 1 0.204760 1.017470 1.114551 10.50000 0.02905 0.03312 = 0.02250 -0.00481 0.00200 0.00277 C3 1 0.443686 0.943694 0.692299 11.00000 0.05826 0.05419 = 0.12024 0.00349 0.03062 -0.00430 C4 1 0.477118 1.019007 0.673679 11.00000 0.06872 0.07055 = 0.13230 0.00713 0.03072 -0.01286 AFIX 43 H4 2 0.534830 1.033535 0.639696 11.00000 -1.20000 AFIX 0 C5 1 0.407181 1.066566 0.715897 11.00000 0.04799 0.03987 = 0.09516 0.00522 0.01200 -0.00941 C6 1 0.404030 1.152150 0.719852 11.00000 0.05677 0.03718 = 0.13631 0.01039 0.00710 -0.01347 AFIX 137 H6A 2 0.353005 1.170424 0.671669 11.00000 -1.50000 H6B 2 0.464287 1.172592 0.693542 11.00000 -1.50000 H6C 2 0.392764 1.168725 0.796899 11.00000 -1.50000 AFIX 0 C2 1 0.493649 0.868964 0.668563 11.00000 0.07484 0.06372 = 0.20363 0.00006 0.05694 0.00036 AFIX 137 H2A 2 0.547696 0.863546 0.718990 11.00000 -1.50000 H2B 2 0.515630 0.868347 0.590866 11.00000 -1.50000 H2C 2 0.449672 0.827061 0.680606 11.00000 -1.50000 AFIX 0 N5 4 0.125424 0.790671 0.905605 11.00000 0.08458 0.03175 = 0.08574 0.00110 0.05931 0.00161 PART 2 C16 1 0.074920 0.813486 1.000408 10.50000 0.02367 0.02282 = 0.03534 -0.00368 0.00234 0.00239 C15 1 0.028753 0.750000 1.047852 10.25000 0.01949 0.03612 = 0.03440 0.00000 0.00848 0.00000 AFIX 43 H15 2 -0.021838 0.749999 1.099840 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C12 1 -0.031799 0.750000 0.958013 10.25000 0.01485 0.04000 = 0.02556 0.00000 0.00537 0.00000 AFIX 43 H12 2 -0.093217 0.750000 0.989582 10.25000 -1.20000 AFIX 0 C14 1 -0.003946 0.897273 0.942488 10.50000 0.02642 0.03475 = 0.04932 0.00020 0.00649 0.00858 AFIX 137 H14A 2 0.005674 0.912980 1.020244 10.50000 -1.50000 H14B 2 -0.070443 0.903752 0.922397 10.50000 -1.50000 H14C 2 0.035302 0.928304 0.893111 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C17 1 0.051135 0.896989 1.022662 10.50000 0.03570 0.02788 = 0.04563 0.00070 0.01874 0.00231 AFIX 137 H17A 2 0.095104 0.917496 1.078113 10.50000 -1.50000 H17B 2 -0.013464 0.900933 1.051153 10.50000 -1.50000 H17C 2 0.056627 0.925681 0.952882 10.50000 -1.50000 AFIX 0 PART 0 PART 1 C13 1 0.023617 0.814067 0.929529 10.50000 0.02030 0.03519 = 0.01656 -0.00023 -0.00170 0.00541 PART 0 SI1 5 0.221739 0.750000 0.524949 10.25000 0.03008 0.07402 = 0.01900 0.00000 -0.00513 0.00000 C10 1 0.216307 1.064923 1.023199 10.50000 0.03000 0.01940 = 0.02960 0.00138 0.00385 0.00943 C11 1 0.216509 1.151674 1.019454 10.50000 0.03528 0.02322 = 0.05495 0.00105 0.00156 0.00529 PART 2 C20 1 0.203977 0.638876 0.468582 10.50000 0.11629 0.11832 = 0.11290 -0.00625 0.00046 -0.00386 PART 0 PART 1 C19 1 0.133404 0.717181 0.449094 10.50000 0.15745 0.14846 = 0.14726 -0.00427 -0.00959 0.00222 HKLF 4 REM dm15658 in Pmmn REM R1 = 0.0434 for 3832 Fo > 4sig(Fo) and 0.0553 for all 4619 data REM 222 parameters refined using 90 restraints END WGHT 0.0557 13.6611 REM Highest difference peak 2.058, deepest hole -3.135, 1-sigma level 0.175 Q1 1 0.2115 0.9438 0.9611 11.00000 0.05 2.06 Q2 1 0.4843 1.0195 0.7272 11.00000 0.05 1.72 Q3 1 0.1528 0.7883 0.9431 11.00000 0.05 1.68 Q4 1 0.4434 0.9437 0.7411 11.00000 0.05 1.64 Q5 1 0.4252 0.9422 0.6468 11.00000 0.05 1.62 ; _shelx_res_checksum 69394 _shelx_hkl_file ; 0 0 2 252.31 4.12 0 0 3 17.92 1.09 0 0 4 167.85 4.04 0 0 5 94.75 2.12 0 0 6 22.84 0.98 0 0 7 100.54 2.67 0 0 8 147.78 3.99 0 0 9 1.70 0.40 0 0 10 88.50 2.65 0 0 11 46.08 1.35 0 0 12 26.46 1.25 0 0 13 56.59 2.07 0 0 14 2.84 0.72 0 0 15 38.03 2.62 0 0 16 28.90 2.44 0 1 1 311.15 7.73 0 1 2 173.78 1.61 0 1 3 6.87 0.14 0 1 4 88.98 1.38 0 1 5 1.48 0.16 0 1 6 146.32 2.38 0 1 7 89.39 1.90 0 1 8 21.80 0.64 0 1 9 87.76 1.57 0 1 10 16.10 1.20 0 1 11 44.73 1.25 0 1 12 36.59 1.01 0 1 13 0.08 0.36 0 1 14 37.54 1.23 0 1 15 6.36 1.33 0 1 16 7.46 1.20 0 2 0 13.98 0.32 0 2 1 0.16 0.12 0 2 2 72.97 1.33 0 2 3 102.12 1.56 0 2 4 5.26 0.29 0 2 5 23.18 0.40 0 2 6 28.54 0.81 0 2 7 7.24 0.42 0 2 8 18.97 0.69 0 2 9 1.23 0.26 0 2 10 16.38 0.69 0 2 11 2.18 0.46 0 2 12 2.48 0.55 0 2 13 1.66 0.39 0 2 14 0.75 0.42 0 2 15 5.28 0.73 0 2 16 0.02 0.66 0 3 1 14.13 0.25 0 3 2 0.03 0.14 0 3 3 14.94 0.44 0 3 4 23.71 0.56 0 3 5 0.18 0.09 0 3 6 33.12 0.66 0 3 7 8.39 0.39 0 3 8 1.69 0.27 0 3 9 7.43 0.49 0 3 10 0.03 0.27 0 3 11 2.71 0.35 0 3 12 14.96 0.73 0 3 13 0.42 0.35 0 3 14 1.85 0.54 0 3 15 1.14 0.43 0 3 16 0.05 0.68 0 4 0 164.35 3.49 0 4 1 41.55 0.86 0 4 2 126.50 2.59 0 4 3 108.51 2.14 0 4 4 5.14 0.31 0 4 5 242.68 4.01 0 4 6 78.52 1.38 0 4 7 17.51 0.45 0 4 8 85.31 1.74 0 4 9 0.03 0.24 0 4 10 75.08 1.67 0 4 11 21.86 0.82 0 4 12 12.08 0.65 0 4 13 29.49 1.11 0 4 14 0.12 0.44 0 4 15 15.23 0.95 0 4 16 12.54 1.22 0 5 1 268.29 4.27 0 5 2 125.90 2.70 0 5 3 64.82 1.57 0 5 4 308.74 5.67 0 5 5 12.54 0.43 0 5 6 246.11 3.69 0 5 7 88.64 1.58 0 5 8 16.84 0.62 0 5 9 200.00 3.58 0 5 10 19.42 0.98 0 5 11 30.54 0.94 0 5 12 56.80 1.43 0 5 13 3.66 0.59 0 5 14 33.59 1.35 0 5 15 10.89 0.86 0 5 16 14.17 0.99 0 6 0 246.66 5.58 0 6 1 23.98 0.54 0 6 2 230.09 4.34 0 6 3 171.55 3.60 0 6 4 0.01 0.18 0 6 5 157.39 3.07 0 6 6 19.11 0.58 0 6 7 45.40 0.89 0 6 8 56.96 1.29 0 6 9 2.08 0.47 0 6 10 71.47 1.59 0 6 11 29.80 1.12 0 6 12 9.97 1.50 0 6 13 25.94 1.13 0 6 14 0.01 0.44 0 6 15 16.27 1.00 0 6 16 13.66 1.02 0 7 1 2.85 0.13 0 7 2 41.17 1.00 0 7 3 0.81 0.21 0 7 4 16.80 0.58 0 7 5 1.58 0.24 0 7 6 15.69 0.45 0 7 7 3.82 0.31 0 7 8 0.01 0.21 0 7 9 9.19 1.01 0 7 10 0.32 0.32 0 7 11 5.17 0.47 0 7 12 9.54 0.83 0 7 13 0.70 0.46 0 7 14 3.17 0.57 0 7 15 0.58 0.49 0 7 16 2.38 0.60 0 8 0 3.16 0.46 0 8 1 9.19 0.45 0 8 2 4.81 0.19 0 8 3 49.95 1.46 0 8 4 4.18 0.35 0 8 5 13.70 0.59 0 8 6 12.29 0.59 0 8 7 5.73 0.42 0 8 8 4.38 0.36 0 8 9 0.00 0.24 0 8 10 4.51 0.41 0 8 11 0.58 0.31 0 8 12 3.20 0.48 0 8 13 2.92 0.54 0 8 14 0.93 0.49 0 8 15 0.34 0.52 0 9 1 65.52 1.28 0 9 2 20.70 0.50 0 9 3 37.60 0.94 0 9 4 170.74 3.57 0 9 5 12.01 0.56 0 9 6 55.04 1.43 0 9 7 79.03 1.62 0 9 8 4.94 0.51 0 9 9 49.81 1.17 0 9 10 4.59 0.45 0 9 11 36.20 1.08 0 9 12 30.57 1.15 0 9 13 0.18 0.42 0 9 14 20.90 1.12 0 9 15 6.92 0.77 0 10 0 439.07 9.94 0 10 1 8.82 0.70 0 10 2 216.12 3.63 0 10 3 106.12 2.36 0 10 4 34.21 1.01 0 10 5 145.50 3.03 0 10 6 51.05 1.76 0 10 7 36.98 1.55 0 10 8 101.48 2.27 0 10 9 1.27 0.33 0 10 10 53.09 1.32 0 10 11 20.23 0.84 0 10 12 15.79 1.59 0 10 13 42.90 1.47 0 10 14 3.38 0.62 0 10 15 17.95 1.10 0 11 1 140.08 2.40 0 11 2 25.14 0.77 0 11 3 48.40 1.24 0 11 4 110.94 2.47 0 11 5 0.13 0.28 0 11 6 88.04 2.18 0 11 7 63.13 1.95 0 11 8 7.04 0.55 0 11 9 23.29 0.78 0 11 10 2.34 0.40 0 11 11 25.50 1.06 0 11 12 23.72 1.09 0 11 13 0.31 0.46 0 11 14 20.57 1.07 0 11 15 1.23 0.55 0 12 0 6.47 0.48 0 12 1 1.04 0.44 0 12 2 3.96 0.25 0 12 3 5.10 0.42 0 12 4 4.18 0.38 0 12 5 16.58 0.75 0 12 6 4.38 0.40 0 12 7 4.25 0.44 0 12 8 6.46 0.49 0 12 9 0.03 0.36 0 12 10 5.66 0.50 0 12 11 0.02 0.38 0 12 12 2.34 0.50 0 12 13 1.10 0.49 0 12 14 0.01 0.47 0 13 1 44.98 1.02 0 13 2 2.32 0.26 0 13 3 6.75 0.50 0 13 4 0.65 0.28 0 13 5 0.35 0.25 0 13 6 13.86 0.82 0 13 7 0.68 0.36 0 13 8 0.04 0.33 0 13 9 1.03 0.41 0 13 10 0.40 0.32 0 13 11 0.62 0.40 0 13 12 6.55 0.65 0 13 13 0.00 0.45 0 13 14 0.01 0.47 0 14 0 96.82 2.74 0 14 1 9.88 0.52 0 14 2 58.31 1.24 0 14 3 51.52 1.42 0 14 4 0.00 0.26 0 14 5 35.97 1.12 0 14 6 12.37 0.72 0 14 7 7.96 0.67 0 14 8 32.08 1.17 0 14 9 0.01 0.37 0 14 10 25.81 1.42 0 14 11 11.85 0.77 0 14 12 3.47 1.04 0 14 13 18.55 1.50 0 15 1 45.60 1.08 0 15 2 79.19 1.61 0 15 3 9.25 0.79 0 15 4 119.95 2.78 0 15 5 11.45 0.75 0 15 6 60.33 2.23 0 15 7 37.91 1.29 0 15 8 6.24 0.61 0 15 9 69.00 2.83 0 15 10 2.24 0.46 0 15 11 27.59 1.17 0 15 12 29.75 1.26 0 15 13 0.94 0.54 0 16 0 37.43 1.37 0 16 1 8.60 0.47 0 16 2 43.49 1.06 0 16 3 61.51 1.68 0 16 4 0.26 0.33 0 16 5 53.92 1.57 0 16 6 3.35 0.45 0 16 7 21.08 0.91 0 16 8 26.96 1.09 0 16 9 0.00 0.48 0 16 10 25.82 1.09 0 16 11 7.19 0.71 0 16 12 5.22 0.73 0 17 1 14.30 0.57 0 17 2 5.53 0.41 0 17 3 5.94 0.51 0 17 4 4.10 0.47 0 17 5 0.00 0.31 0 17 6 4.70 0.53 0 17 7 0.05 0.32 0 17 8 1.42 0.42 0 17 9 1.73 0.63 0 17 10 0.00 0.61 0 17 11 0.08 0.48 0 17 12 0.01 0.45 0 18 0 5.35 0.56 0 18 1 0.30 0.24 0 18 2 1.60 0.31 0 18 3 6.70 0.58 0 18 4 0.01 0.32 0 18 5 3.40 0.45 0 18 6 1.32 0.40 0 18 7 0.79 0.41 0 18 8 1.48 0.45 0 18 9 0.01 0.44 0 18 10 0.60 0.55 0 18 11 1.28 0.63 0 19 1 34.87 1.02 0 19 2 11.18 0.59 0 19 3 6.48 0.59 0 19 4 25.98 1.04 0 19 5 0.11 0.37 0 19 6 16.89 0.92 0 19 7 13.95 0.97 0 19 8 2.71 0.59 0 19 9 20.36 1.26 0 19 10 3.82 1.24 0 20 0 60.83 2.11 0 20 1 10.94 0.60 0 20 2 22.00 1.00 0 20 3 25.25 1.09 0 20 4 3.11 0.52 0 20 5 39.00 1.37 0 20 6 11.36 0.78 0 20 7 11.24 0.79 0 20 8 31.86 1.51 0 20 9 1.01 1.07 0 21 1 26.24 1.06 0 21 2 16.35 0.92 0 21 3 5.61 0.59 0 21 4 24.74 1.61 0 21 5 0.56 0.39 0 21 6 15.90 0.91 0 21 7 10.35 0.93 0 21 8 0.73 1.03 0 22 0 13.81 0.99 0 22 1 1.80 0.39 0 22 2 3.40 0.55 0 22 3 0.81 0.40 0 22 4 1.62 0.46 0 22 5 0.74 0.42 0 22 6 0.00 0.37 0 22 7 3.25 1.23 0 23 1 2.29 0.38 0 23 2 0.54 0.39 0 23 3 1.16 0.43 0 23 4 1.10 0.46 0 23 5 0.00 0.60 0 23 6 0.19 0.95 0 24 0 31.38 1.56 0 24 1 4.19 0.62 0 24 2 7.35 0.70 0 24 3 2.12 0.83 0 24 4 2.30 0.81 1 0 1 1130.90 26.40 1 0 2 124.27 2.94 1 0 3 365.04 6.41 1 0 4 207.10 2.85 1 0 5 3.09 0.14 1 0 6 188.50 3.17 1 0 7 112.10 1.86 1 0 8 29.83 0.78 1 0 9 149.43 2.74 1 0 10 37.07 1.39 1 0 11 43.74 0.92 1 0 12 38.92 1.58 1 0 13 0.58 0.41 1 0 14 61.23 1.78 1 0 15 16.64 1.68 1 0 16 6.90 1.00 1 1 0 604.10 9.84 1 1 1 20.41 0.73 1 1 2 59.83 0.70 1 1 3 310.18 3.22 1 1 4 0.93 0.07 1 1 5 103.36 1.36 1 1 6 38.93 0.47 1 1 7 71.13 0.87 1 1 8 95.72 1.23 1 1 9 0.00 0.16 1 1 10 59.11 1.19 1 1 11 25.74 0.63 1 1 12 15.25 0.56 1 1 13 36.57 0.77 1 1 14 1.71 0.33 1 1 15 28.30 0.90 1 1 16 11.29 0.82 1 2 1 0.00 0.10 1 2 2 36.33 0.61 1 2 3 11.19 0.23 1 2 4 24.87 0.48 1 2 5 18.41 0.29 1 2 6 3.33 0.18 1 2 7 15.79 0.31 1 2 8 10.05 0.26 1 2 9 14.21 0.45 1 2 10 0.97 0.21 1 2 11 14.93 0.44 1 2 12 3.11 0.31 1 2 13 0.46 0.47 1 2 14 5.09 0.37 1 2 15 0.29 0.38 1 2 16 1.14 0.52 1 3 0 1.05 0.12 1 3 1 13.93 0.27 1 3 2 30.32 0.54 1 3 3 14.72 0.38 1 3 4 0.04 0.07 1 3 5 28.87 0.45 1 3 6 1.50 0.13 1 3 7 5.15 0.22 1 3 8 11.22 0.28 1 3 9 1.14 0.20 1 3 10 3.00 0.25 1 3 11 1.84 0.26 1 3 12 1.73 0.29 1 3 13 7.82 0.41 1 3 14 0.02 0.27 1 3 15 0.54 0.37 1 3 16 1.31 0.45 1 4 1 105.10 1.33 1 4 2 57.70 0.70 1 4 3 69.80 0.94 1 4 4 212.82 2.91 1 4 5 27.33 0.41 1 4 6 104.63 1.26 1 4 7 59.11 0.79 1 4 8 4.98 0.21 1 4 9 119.64 1.60 1 4 10 4.99 0.31 1 4 11 29.17 0.67 1 4 12 50.60 0.94 1 4 13 2.20 0.34 1 4 14 21.41 0.67 1 4 15 8.58 0.59 1 4 16 4.92 0.52 1 5 0 264.17 4.48 1 5 1 64.77 0.77 1 5 2 265.76 3.49 1 5 3 390.61 5.29 1 5 4 0.35 0.09 1 5 5 316.22 4.18 1 5 6 60.37 0.74 1 5 7 64.69 0.85 1 5 8 119.66 1.48 1 5 9 0.37 0.20 1 5 10 102.56 1.44 1 5 11 38.20 0.80 1 5 12 17.62 0.61 1 5 13 59.06 1.10 1 5 14 1.42 0.37 1 5 15 23.93 0.86 1 5 16 22.15 0.84 1 6 1 187.24 2.43 1 6 2 96.84 1.20 1 6 3 59.38 0.89 1 6 4 150.56 2.18 1 6 5 0.66 0.12 1 6 6 156.85 2.06 1 6 7 45.41 0.61 1 6 8 8.13 0.26 1 6 9 95.99 1.38 1 6 10 5.98 0.36 1 6 11 18.25 0.52 1 6 12 33.76 0.80 1 6 13 3.05 0.41 1 6 14 19.44 0.73 1 6 15 3.73 0.56 1 6 16 10.98 0.73 1 7 0 0.15 0.14 1 7 1 5.89 0.13 1 7 2 11.23 0.26 1 7 3 5.11 0.19 1 7 4 0.19 0.11 1 7 5 25.30 0.59 1 7 6 1.50 0.15 1 7 7 4.25 0.19 1 7 8 12.42 0.33 1 7 9 0.01 0.18 1 7 10 6.91 0.33 1 7 11 2.82 0.26 1 7 12 1.69 0.31 1 7 13 4.32 0.38 1 7 14 0.10 0.31 1 7 15 1.43 0.38 1 7 16 0.50 0.42 1 8 1 1.37 0.08 1 8 2 2.38 0.22 1 8 3 1.04 0.17 1 8 4 23.08 0.48 1 8 5 0.00 0.13 1 8 6 12.47 0.36 1 8 7 12.58 0.35 1 8 8 4.34 0.23 1 8 9 8.88 0.36 1 8 10 4.12 0.29 1 8 11 1.51 0.27 1 8 12 1.28 0.29 1 8 13 0.33 0.29 1 8 14 0.85 0.35 1 8 15 0.01 0.33 1 9 0 81.40 1.36 1 9 1 0.10 0.10 1 9 2 72.10 1.04 1 9 3 133.35 1.75 1 9 4 1.42 0.17 1 9 5 100.61 1.62 1 9 6 59.21 0.92 1 9 7 24.35 0.51 1 9 8 61.66 1.06 1 9 9 0.00 0.19 1 9 10 40.59 0.79 1 9 11 14.18 0.52 1 9 12 8.76 0.46 1 9 13 25.21 0.79 1 9 14 1.88 0.37 1 9 15 11.83 0.63 1 10 1 267.52 3.25 1 10 2 48.16 0.69 1 10 3 95.35 1.35 1 10 4 187.22 2.76 1 10 5 2.67 0.22 1 10 6 84.68 1.37 1 10 7 92.67 1.42 1 10 8 9.40 0.39 1 10 9 78.59 1.25 1 10 10 9.84 0.38 1 10 11 41.90 0.87 1 10 12 36.78 0.87 1 10 13 0.26 0.32 1 10 14 37.24 0.98 1 10 15 8.67 0.59 1 11 0 171.92 3.11 1 11 1 9.15 0.71 1 11 2 92.11 1.26 1 11 3 100.22 1.42 1 11 4 5.45 0.30 1 11 5 70.93 1.20 1 11 6 7.70 0.37 1 11 7 53.60 0.92 1 11 8 56.12 1.17 1 11 9 0.09 0.21 1 11 10 29.92 0.71 1 11 11 11.90 0.48 1 11 12 8.19 0.48 1 11 13 22.21 0.76 1 11 14 0.57 0.34 1 11 15 14.84 0.86 1 12 1 11.80 0.31 1 12 2 0.80 0.15 1 12 3 6.19 0.30 1 12 4 20.16 0.50 1 12 5 0.19 0.19 1 12 6 3.47 0.27 1 12 7 6.96 0.37 1 12 8 3.12 0.40 1 12 9 4.16 0.33 1 12 10 0.07 0.24 1 12 11 4.05 0.36 1 12 12 0.09 0.29 1 12 13 0.04 0.31 1 12 14 2.87 0.42 1 13 0 60.38 1.27 1 13 1 13.02 0.38 1 13 2 9.97 0.35 1 13 3 8.82 0.42 1 13 4 0.01 0.17 1 13 5 1.67 0.25 1 13 6 1.18 0.26 1 13 7 4.52 0.36 1 13 8 3.97 0.32 1 13 9 0.17 0.23 1 13 10 0.00 0.23 1 13 11 1.04 0.29 1 13 12 0.02 0.28 1 13 13 1.82 0.38 1 13 14 0.00 0.34 1 14 1 65.66 0.98 1 14 2 32.01 0.59 1 14 3 18.36 0.48 1 14 4 48.41 0.98 1 14 5 3.55 0.30 1 14 6 36.13 0.88 1 14 7 21.86 0.60 1 14 8 2.54 0.35 1 14 9 44.91 1.00 1 14 10 5.08 0.42 1 14 11 9.23 0.51 1 14 12 18.00 0.69 1 14 13 0.21 0.33 1 15 0 49.32 1.10 1 15 1 9.27 0.74 1 15 2 55.19 0.90 1 15 3 98.13 1.48 1 15 4 0.00 0.21 1 15 5 98.66 1.67 1 15 6 24.30 0.70 1 15 7 25.00 0.72 1 15 8 62.97 1.24 1 15 9 0.01 0.30 1 15 10 46.67 1.03 1 15 11 16.64 0.70 1 15 12 8.32 0.52 1 15 13 28.06 0.99 1 16 1 55.96 0.91 1 16 2 38.59 0.70 1 16 3 11.85 0.54 1 16 4 50.05 1.01 1 16 5 0.47 0.25 1 16 6 39.98 1.02 1 16 7 13.41 0.70 1 16 8 5.18 0.46 1 16 9 32.89 1.02 1 16 10 1.65 0.36 1 16 11 10.80 0.55 1 16 12 10.29 0.66 1 17 0 13.65 0.59 1 17 1 3.36 0.35 1 17 2 7.90 0.45 1 17 3 2.85 0.28 1 17 4 0.74 0.23 1 17 5 5.26 0.36 1 17 6 0.04 0.24 1 17 7 3.96 0.37 1 17 8 2.07 0.35 1 17 9 0.00 0.30 1 17 10 2.08 0.39 1 17 11 0.01 0.35 1 17 12 1.21 0.40 1 18 1 3.06 0.22 1 18 2 1.68 0.23 1 18 3 0.12 0.20 1 18 4 3.64 0.33 1 18 5 0.00 0.21 1 18 6 2.21 0.31 1 18 7 2.81 0.33 1 18 8 0.14 0.29 1 18 9 2.66 0.41 1 18 10 1.34 0.42 1 18 11 0.01 0.33 1 19 0 42.68 1.15 1 19 1 4.15 0.28 1 19 2 19.46 0.57 1 19 3 26.54 0.74 1 19 4 0.11 0.24 1 19 5 21.71 0.79 1 19 6 6.71 0.45 1 19 7 6.40 0.49 1 19 8 14.71 0.92 1 19 9 0.01 0.43 1 19 10 11.92 0.77 1 20 1 48.40 0.89 1 20 2 18.29 0.60 1 20 3 11.41 0.71 1 20 4 43.43 1.14 1 20 5 1.87 0.34 1 20 6 21.30 0.72 1 20 7 23.04 1.02 1 20 8 1.70 0.62 1 20 9 25.90 1.32 1 21 0 29.16 0.93 1 21 1 4.35 0.39 1 21 2 16.90 0.58 1 21 3 18.52 0.76 1 21 4 1.37 0.31 1 21 5 20.90 0.72 1 21 6 2.60 0.48 1 21 7 13.78 0.91 1 21 8 16.73 1.04 1 22 1 7.62 0.41 1 22 2 1.09 0.30 1 22 3 2.24 0.33 1 22 4 1.74 0.38 1 22 5 0.00 0.33 1 22 6 1.05 0.41 1 22 7 0.01 0.45 1 23 0 3.85 0.41 1 23 1 0.60 0.27 1 23 2 0.97 0.32 1 23 3 0.30 0.33 1 23 4 0.25 0.41 1 23 5 1.67 0.45 1 23 6 0.10 0.39 1 24 1 14.41 0.68 1 24 2 3.22 0.49 1 24 3 5.97 0.58 1 24 4 13.23 0.87 2 0 0 465.15 23.30 2 0 1 157.37 1.50 2 0 2 100.46 1.61 2 0 3 764.16 9.91 2 0 4 21.71 0.39 2 0 5 315.33 4.48 2 0 6 51.42 1.01 2 0 7 111.47 1.80 2 0 8 144.01 2.76 2 0 9 0.54 0.32 2 0 10 95.39 1.79 2 0 11 35.09 1.00 2 0 12 18.77 0.77 2 0 13 61.48 1.83 2 0 14 5.08 0.68 2 0 15 34.87 1.44 2 0 16 18.82 1.15 2 1 1 187.78 2.67 2 1 2 92.35 0.84 2 1 3 106.74 0.89 2 1 4 210.88 2.25 2 1 5 1.14 0.10 2 1 6 110.23 1.14 2 1 7 111.37 1.31 2 1 8 13.20 0.38 2 1 9 64.12 0.94 2 1 10 6.38 0.36 2 1 11 52.50 1.00 2 1 12 37.24 0.71 2 1 13 0.40 0.37 2 1 14 28.57 0.89 2 1 15 5.70 0.50 2 1 16 6.19 0.60 2 2 0 6.40 0.30 2 2 1 93.60 1.08 2 2 2 64.54 0.87 2 2 3 12.36 0.18 2 2 4 0.11 0.07 2 2 5 10.76 0.20 2 2 6 30.20 0.53 2 2 7 1.81 0.16 2 2 8 7.59 0.25 2 2 9 0.05 0.17 2 2 10 10.70 0.41 2 2 11 5.51 0.47 2 2 12 2.35 0.35 2 2 13 3.64 0.33 2 2 14 0.00 0.32 2 2 15 2.75 0.42 2 2 16 0.11 0.41 2 3 1 4.23 0.09 2 3 2 18.31 0.29 2 3 3 13.65 0.22 2 3 4 18.11 0.36 2 3 5 0.06 0.09 2 3 6 26.97 0.43 2 3 7 6.86 0.26 2 3 8 1.68 0.16 2 3 9 7.41 0.34 2 3 10 0.81 0.26 2 3 11 5.75 0.31 2 3 12 14.71 0.55 2 3 13 0.05 0.27 2 3 14 0.48 0.32 2 3 15 1.14 0.37 2 3 16 0.66 0.43 2 4 0 85.95 1.26 2 4 1 31.39 0.57 2 4 2 131.89 1.66 2 4 3 178.14 3.85 2 4 4 1.01 0.10 2 4 5 198.48 2.34 2 4 6 60.82 0.90 2 4 7 29.15 0.50 2 4 8 74.82 1.01 2 4 9 0.01 0.17 2 4 10 52.43 0.93 2 4 11 22.66 0.54 2 4 12 13.27 0.48 2 4 13 41.63 0.99 2 4 14 0.57 0.31 2 4 15 12.90 0.61 2 4 16 9.95 0.69 2 5 1 247.71 3.20 2 5 2 216.61 2.90 2 5 3 125.23 2.67 2 5 4 306.75 3.71 2 5 5 7.75 0.26 2 5 6 195.73 2.38 2 5 7 81.88 1.19 2 5 8 16.41 0.39 2 5 9 171.01 2.20 2 5 10 12.12 0.72 2 5 11 29.18 0.70 2 5 12 63.64 1.17 2 5 13 2.30 0.35 2 5 14 36.31 0.92 2 5 15 9.68 0.66 2 5 16 13.11 0.69 2 6 0 225.23 3.58 2 6 1 101.76 1.38 2 6 2 97.26 1.27 2 6 3 154.20 2.30 2 6 4 5.00 0.32 2 6 5 150.93 1.76 2 6 6 13.98 0.37 2 6 7 41.17 0.63 2 6 8 72.61 0.99 2 6 9 0.01 0.19 2 6 10 48.77 0.87 2 6 11 16.91 0.56 2 6 12 11.11 0.54 2 6 13 39.96 1.07 2 6 14 0.57 0.41 2 6 15 14.81 0.85 2 6 16 10.66 0.70 2 7 1 26.81 0.36 2 7 2 3.29 0.20 2 7 3 8.60 0.29 2 7 4 16.04 0.35 2 7 5 4.08 0.21 2 7 6 15.56 0.33 2 7 7 3.66 0.23 2 7 8 0.00 0.15 2 7 9 7.55 0.33 2 7 10 0.09 0.19 2 7 11 6.93 0.40 2 7 12 6.10 0.40 2 7 13 2.09 0.35 2 7 14 2.76 0.37 2 7 15 0.71 0.36 2 7 16 0.31 0.47 2 8 0 16.76 0.61 2 8 1 0.22 0.12 2 8 2 20.91 0.35 2 8 3 49.54 0.77 2 8 4 0.03 0.12 2 8 5 1.56 0.17 2 8 6 5.97 0.26 2 8 7 1.72 0.18 2 8 8 2.69 0.21 2 8 9 1.00 0.33 2 8 10 7.02 0.37 2 8 11 4.01 0.32 2 8 12 0.01 0.24 2 8 13 1.36 0.30 2 8 14 0.02 0.32 2 8 15 4.67 0.49 2 9 1 118.74 1.51 2 9 2 51.55 0.76 2 9 3 21.64 0.42 2 9 4 102.65 1.61 2 9 5 5.14 0.25 2 9 6 54.90 0.92 2 9 7 64.33 0.99 2 9 8 10.79 0.39 2 9 9 57.76 0.99 2 9 10 8.36 0.42 2 9 11 23.28 0.70 2 9 12 26.72 0.71 2 9 13 0.11 0.27 2 9 14 22.14 0.79 2 9 15 4.74 0.50 2 10 0 333.72 5.39 2 10 1 63.46 0.91 2 10 2 49.45 0.79 2 10 3 134.30 1.84 2 10 4 14.39 0.66 2 10 5 178.84 2.60 2 10 6 54.00 0.97 2 10 7 56.42 1.03 2 10 8 93.83 1.29 2 10 9 0.00 0.26 2 10 10 62.69 1.10 2 10 11 24.21 0.70 2 10 12 11.72 0.53 2 10 13 35.47 0.87 2 10 14 1.44 0.37 2 10 15 21.99 0.88 2 11 1 137.71 1.69 2 11 2 58.24 0.94 2 11 3 25.98 0.54 2 11 4 85.79 1.40 2 11 5 1.53 0.23 2 11 6 68.91 1.17 2 11 7 49.07 0.86 2 11 8 6.67 0.41 2 11 9 41.86 0.89 2 11 10 3.03 0.35 2 11 11 24.05 0.69 2 11 12 11.44 0.53 2 11 13 0.05 0.31 2 11 14 18.82 0.86 2 12 0 15.50 0.51 2 12 1 0.62 0.17 2 12 2 10.49 0.30 2 12 3 7.89 0.31 2 12 4 0.69 0.17 2 12 5 7.12 0.38 2 12 6 3.39 0.23 2 12 7 4.21 0.28 2 12 8 3.75 0.26 2 12 9 0.51 0.25 2 12 10 7.65 0.46 2 12 11 1.40 0.30 2 12 12 1.35 0.31 2 12 13 1.20 0.36 2 12 14 0.00 0.36 2 13 1 3.08 0.18 2 13 2 14.36 0.41 2 13 3 2.76 0.23 2 13 4 3.94 0.24 2 13 5 1.74 0.23 2 13 6 14.08 0.48 2 13 7 3.25 0.29 2 13 8 0.05 0.22 2 13 9 4.89 0.38 2 13 10 0.89 0.28 2 13 11 0.00 0.25 2 13 12 1.54 0.34 2 13 13 0.00 0.34 2 13 14 0.07 0.38 2 14 0 92.08 1.85 2 14 1 33.37 0.59 2 14 2 16.05 0.47 2 14 3 38.79 1.15 2 14 4 2.09 0.25 2 14 5 66.95 1.19 2 14 6 13.96 0.55 2 14 7 14.20 0.48 2 14 8 40.18 1.20 2 14 9 0.00 0.25 2 14 10 19.34 0.69 2 14 11 11.07 0.50 2 14 12 3.56 0.45 2 14 13 17.37 0.80 2 15 1 108.60 1.49 2 15 2 43.00 0.81 2 15 3 23.34 0.56 2 15 4 78.53 1.41 2 15 5 4.98 0.33 2 15 6 56.79 1.07 2 15 7 37.47 0.83 2 15 8 4.55 0.43 2 15 9 56.90 1.17 2 15 10 5.75 0.44 2 15 11 20.53 0.75 2 15 12 27.59 0.99 2 15 13 1.14 0.42 2 16 0 62.53 1.40 2 16 1 6.07 0.61 2 16 2 43.77 0.82 2 16 3 34.10 0.74 2 16 4 1.15 0.26 2 16 5 50.16 1.03 2 16 6 6.44 0.39 2 16 7 17.80 0.58 2 16 8 27.18 1.01 2 16 9 0.05 0.28 2 16 10 26.81 0.92 2 16 11 8.39 0.74 2 16 12 3.38 0.47 2 17 1 7.71 0.35 2 17 2 4.36 0.34 2 17 3 2.37 0.27 2 17 4 5.61 0.41 2 17 5 0.48 0.23 2 17 6 6.76 0.41 2 17 7 0.54 0.24 2 17 8 0.41 0.29 2 17 9 2.53 0.42 2 17 10 0.00 0.33 2 17 11 0.97 0.39 2 17 12 0.04 0.36 2 18 0 4.41 0.36 2 18 1 0.01 0.16 2 18 2 4.30 0.30 2 18 3 6.16 0.33 2 18 4 0.00 0.20 2 18 5 1.20 0.27 2 18 6 1.24 0.27 2 18 7 0.00 0.27 2 18 8 0.88 0.39 2 18 9 0.00 0.31 2 18 10 0.57 0.41 2 18 11 0.81 0.42 2 19 1 29.31 0.64 2 19 2 12.72 0.48 2 19 3 6.56 0.37 2 19 4 28.19 1.04 2 19 5 0.50 0.28 2 19 6 15.37 0.84 2 19 7 14.19 0.78 2 19 8 1.36 0.44 2 19 9 19.55 0.80 2 19 10 3.15 0.52 2 20 0 45.12 1.24 2 20 1 3.39 0.37 2 20 2 29.39 0.72 2 20 3 31.72 0.86 2 20 4 0.51 0.29 2 20 5 42.32 1.74 2 20 6 13.54 0.79 2 20 7 11.72 0.76 2 20 8 26.60 1.07 2 20 9 0.01 0.37 2 21 1 31.75 0.80 2 21 2 10.47 0.48 2 21 3 5.63 0.50 2 21 4 19.27 0.82 2 21 5 0.02 0.38 2 21 6 17.36 0.89 2 21 7 12.35 0.81 2 21 8 0.93 0.45 2 22 0 6.23 0.77 2 22 1 1.95 0.39 2 22 2 0.79 0.41 2 22 3 1.17 0.36 2 22 4 0.56 0.36 2 22 5 2.98 0.49 2 22 6 0.01 0.39 2 22 7 2.26 0.50 2 23 1 1.15 0.31 2 23 2 0.86 0.35 2 23 3 0.02 0.32 2 23 4 2.02 0.48 2 23 5 0.01 0.38 2 23 6 0.39 0.35 2 24 0 13.71 0.94 2 24 1 3.42 0.42 2 24 2 5.38 0.53 2 24 3 11.25 0.79 3 0 1 62.35 0.47 3 0 2 225.39 6.54 3 0 3 36.21 1.05 3 0 4 500.78 6.19 3 0 5 3.56 0.23 3 0 6 278.36 4.34 3 0 7 219.81 3.28 3 0 8 21.99 0.97 3 0 9 135.00 2.07 3 0 10 23.56 1.07 3 0 11 54.03 1.34 3 0 12 43.86 1.48 3 0 13 0.99 0.51 3 0 14 56.87 1.78 3 0 15 10.78 0.89 3 0 16 9.98 0.88 3 1 0 259.55 3.16 3 1 1 0.98 0.06 3 1 2 322.53 4.28 3 1 3 227.18 3.56 3 1 4 12.87 0.23 3 1 5 110.72 1.20 3 1 6 40.44 0.49 3 1 7 56.45 0.70 3 1 8 108.80 1.28 3 1 9 0.40 0.16 3 1 10 52.52 0.88 3 1 11 16.39 0.64 3 1 12 12.28 0.58 3 1 13 32.94 0.90 3 1 14 2.93 0.54 3 1 15 16.42 0.75 3 1 16 9.55 0.62 3 2 1 77.63 0.87 3 2 2 5.89 0.11 3 2 3 40.06 0.57 3 2 4 22.94 0.38 3 2 5 0.27 0.07 3 2 6 3.86 0.13 3 2 7 15.12 0.29 3 2 8 3.60 0.18 3 2 9 2.42 0.20 3 2 10 2.05 0.33 3 2 11 8.06 0.37 3 2 12 3.14 0.33 3 2 13 0.01 0.27 3 2 14 4.37 0.46 3 2 15 0.03 0.35 3 2 16 0.82 0.40 3 3 0 26.22 0.52 3 3 1 14.60 0.21 3 3 2 21.68 0.30 3 3 3 26.97 0.45 3 3 4 0.54 0.09 3 3 5 6.42 0.19 3 3 6 0.04 0.09 3 3 7 4.90 0.23 3 3 8 14.91 0.34 3 3 9 0.03 0.14 3 3 10 6.15 0.31 3 3 11 1.57 0.28 3 3 12 1.46 0.31 3 3 13 2.05 0.31 3 3 14 0.00 0.28 3 3 15 1.70 0.40 3 3 16 3.94 0.49 3 4 1 144.52 1.91 3 4 2 114.76 1.27 3 4 3 54.25 0.99 3 4 4 174.41 2.06 3 4 5 18.39 0.35 3 4 6 104.91 1.39 3 4 7 37.60 0.58 3 4 8 7.93 0.35 3 4 9 87.93 1.16 3 4 10 4.29 0.29 3 4 11 25.40 0.68 3 4 12 51.91 1.04 3 4 13 1.40 0.32 3 4 14 22.68 0.77 3 4 15 7.38 0.52 3 4 16 5.36 0.59 3 5 0 445.18 8.84 3 5 1 42.95 0.52 3 5 2 379.66 4.30 3 5 3 294.26 3.21 3 5 4 2.38 0.12 3 5 5 207.52 2.63 3 5 6 39.24 0.59 3 5 7 60.05 0.86 3 5 8 118.16 1.50 3 5 9 0.00 0.19 3 5 10 88.28 1.54 3 5 11 38.34 0.86 3 5 12 16.60 0.61 3 5 13 60.40 1.19 3 5 14 0.91 0.35 3 5 15 24.16 0.85 3 5 16 16.55 0.78 3 6 1 145.03 1.94 3 6 2 76.85 0.91 3 6 3 74.82 0.93 3 6 4 143.24 1.78 3 6 5 4.38 0.20 3 6 6 93.68 1.32 3 6 7 39.59 0.62 3 6 8 8.24 0.32 3 6 9 91.88 1.33 3 6 10 6.98 0.40 3 6 11 19.17 0.59 3 6 12 33.86 0.80 3 6 13 2.22 0.45 3 6 14 21.56 0.76 3 6 15 4.61 0.47 3 6 16 9.62 0.70 3 7 0 0.89 0.16 3 7 1 0.81 0.08 3 7 2 27.00 0.46 3 7 3 9.76 0.22 3 7 4 0.53 0.10 3 7 5 29.45 0.56 3 7 6 1.13 0.14 3 7 7 5.52 0.27 3 7 8 10.16 0.34 3 7 9 0.01 0.20 3 7 10 5.36 0.34 3 7 11 0.59 0.23 3 7 12 3.93 0.35 3 7 13 4.96 0.40 3 7 14 0.00 0.29 3 7 15 0.14 0.41 3 8 1 61.04 0.81 3 8 2 4.89 0.23 3 8 3 5.58 0.25 3 8 4 0.79 0.12 3 8 5 1.69 0.16 3 8 6 3.99 0.20 3 8 7 10.76 0.35 3 8 8 1.72 0.19 3 8 9 7.28 0.40 3 8 10 2.98 0.29 3 8 11 0.46 0.25 3 8 12 1.88 0.31 3 8 13 0.00 0.27 3 8 14 2.11 0.36 3 8 15 0.02 0.37 3 9 0 216.62 3.49 3 9 1 13.65 0.35 3 9 2 61.02 0.95 3 9 3 91.95 1.29 3 9 4 6.17 0.25 3 9 5 86.23 1.50 3 9 6 42.82 0.69 3 9 7 23.02 0.59 3 9 8 45.53 0.80 3 9 9 0.01 0.22 3 9 10 39.36 0.85 3 9 11 18.48 0.58 3 9 12 6.90 0.42 3 9 13 22.19 0.71 3 9 14 1.32 0.34 3 9 15 11.52 0.81 3 10 1 126.31 1.75 3 10 2 114.97 1.55 3 10 3 17.84 0.57 3 10 4 201.01 2.97 3 10 5 10.03 0.42 3 10 6 107.71 1.58 3 10 7 78.93 1.15 3 10 8 19.06 0.74 3 10 9 84.09 1.54 3 10 10 9.84 0.42 3 10 11 37.06 0.83 3 10 12 34.41 0.84 3 10 13 0.63 0.30 3 10 14 38.35 1.13 3 10 15 9.61 1.19 3 11 0 211.56 3.70 3 11 1 23.88 0.48 3 11 2 56.03 1.05 3 11 3 83.83 1.29 3 11 4 3.85 0.30 3 11 5 47.30 0.87 3 11 6 9.55 0.49 3 11 7 35.46 0.64 3 11 8 60.22 1.09 3 11 9 0.04 0.31 3 11 10 41.61 0.95 3 11 11 9.59 0.46 3 11 12 8.07 0.46 3 11 13 16.12 0.69 3 11 14 0.53 0.39 3 12 1 17.51 0.38 3 12 2 7.31 0.29 3 12 3 0.85 0.24 3 12 4 9.75 0.35 3 12 5 0.00 0.15 3 12 6 3.83 0.25 3 12 7 2.68 0.24 3 12 8 3.88 0.30 3 12 9 4.71 0.37 3 12 10 0.03 0.25 3 12 11 3.60 0.34 3 12 12 0.74 0.31 3 12 13 0.02 0.31 3 12 14 3.70 0.50 3 13 0 7.55 0.39 3 13 1 9.67 0.28 3 13 2 1.24 0.16 3 13 3 4.86 0.26 3 13 4 0.04 0.14 3 13 5 5.66 0.36 3 13 6 1.10 0.19 3 13 7 0.79 0.21 3 13 8 8.67 0.46 3 13 9 0.40 0.26 3 13 10 1.32 0.30 3 13 11 0.66 0.32 3 13 12 0.01 0.29 3 13 13 0.47 0.38 3 13 14 0.00 0.35 3 14 1 33.06 0.60 3 14 2 26.32 0.56 3 14 3 19.07 0.47 3 14 4 81.47 1.42 3 14 5 5.03 0.34 3 14 6 40.31 0.91 3 14 7 21.83 0.59 3 14 8 4.51 0.29 3 14 9 37.87 0.91 3 14 10 6.34 0.51 3 14 11 6.14 0.46 3 14 12 16.85 0.72 3 14 13 0.31 0.37 3 15 0 102.01 1.94 3 15 1 4.92 0.30 3 15 2 95.89 1.49 3 15 3 56.57 0.96 3 15 4 5.45 0.45 3 15 5 94.19 1.63 3 15 6 20.46 0.57 3 15 7 17.81 0.60 3 15 8 45.13 1.16 3 15 9 0.00 0.31 3 15 10 38.19 1.16 3 15 11 19.02 0.82 3 15 12 5.37 0.52 3 15 13 22.65 0.89 3 16 1 58.78 1.03 3 16 2 23.71 0.92 3 16 3 15.42 0.47 3 16 4 42.48 0.91 3 16 5 0.42 0.24 3 16 6 32.69 0.82 3 16 7 16.54 0.68 3 16 8 3.41 0.43 3 16 9 29.14 0.92 3 16 10 2.00 0.41 3 16 11 9.68 0.63 3 16 12 10.91 0.68 3 17 0 5.44 0.40 3 17 1 2.78 0.38 3 17 2 1.95 0.29 3 17 3 4.13 0.31 3 17 4 0.01 0.21 3 17 5 7.59 0.43 3 17 6 0.00 0.27 3 17 7 3.81 0.41 3 17 8 3.08 0.49 3 17 9 0.00 0.32 3 17 10 3.33 0.46 3 17 11 0.02 0.35 3 18 1 7.12 0.34 3 18 2 0.99 0.21 3 18 3 1.10 0.21 3 18 4 1.26 0.26 3 18 5 0.00 0.27 3 18 6 0.58 0.29 3 18 7 2.16 0.36 3 18 8 0.01 0.36 3 18 9 1.77 0.41 3 18 10 0.93 0.38 3 18 11 0.00 0.39 3 19 0 33.34 0.96 3 19 1 2.75 0.28 3 19 2 17.94 0.68 3 19 3 26.12 0.74 3 19 4 0.01 0.29 3 19 5 20.71 1.29 3 19 6 6.87 0.52 3 19 7 6.13 0.51 3 19 8 16.57 0.87 3 19 9 0.01 0.33 3 19 10 9.89 0.66 3 20 1 38.40 0.83 3 20 2 20.25 0.70 3 20 3 7.95 0.49 3 20 4 45.49 1.20 3 20 5 1.15 0.43 3 20 6 28.31 0.95 3 20 7 22.68 1.20 3 20 8 1.31 0.49 3 20 9 20.73 0.86 3 21 0 25.35 1.10 3 21 1 2.23 0.35 3 21 2 17.81 0.68 3 21 3 14.94 0.73 3 21 4 1.46 0.41 3 21 5 20.54 0.94 3 21 6 3.21 0.45 3 21 7 9.37 0.73 3 21 8 16.77 0.94 3 22 1 1.30 0.31 3 22 2 1.36 0.34 3 22 3 0.62 0.34 3 22 4 3.59 0.51 3 22 5 0.00 0.36 3 22 6 2.75 0.44 3 22 7 0.44 0.43 3 23 0 0.88 0.45 3 23 1 0.29 0.29 3 23 2 0.25 0.28 3 23 3 2.21 0.47 3 23 4 0.02 0.37 3 23 5 0.38 0.36 3 24 1 7.89 0.56 3 24 2 8.81 0.73 3 24 3 0.94 0.44 4 0 0 699.97 20.04 4 0 1 145.48 1.53 4 0 2 25.53 0.50 4 0 3 148.07 3.44 4 0 4 0.05 0.13 4 0 5 264.68 3.52 4 0 6 114.12 1.53 4 0 7 115.87 1.72 4 0 8 210.43 3.09 4 0 9 4.13 0.36 4 0 10 85.04 1.80 4 0 11 35.59 1.54 4 0 12 24.30 1.07 4 0 13 62.01 1.84 4 0 14 1.41 0.55 4 0 15 31.56 1.40 4 0 16 15.23 1.04 4 1 1 313.52 3.30 4 1 2 26.95 0.30 4 1 3 71.93 0.70 4 1 4 155.52 1.99 4 1 5 0.30 0.12 4 1 6 103.28 1.09 4 1 7 116.13 1.27 4 1 8 10.66 0.31 4 1 9 66.65 0.87 4 1 10 8.89 0.38 4 1 11 38.36 0.80 4 1 12 25.85 0.77 4 1 13 0.50 0.32 4 1 14 26.48 0.86 4 1 15 5.49 0.51 4 1 16 6.45 0.61 4 2 0 7.15 0.20 4 2 1 9.86 0.23 4 2 2 78.53 0.91 4 2 3 28.90 0.45 4 2 4 28.74 0.37 4 2 5 26.46 0.36 4 2 6 4.38 0.19 4 2 7 6.34 0.22 4 2 8 3.45 0.15 4 2 9 0.04 0.15 4 2 10 4.05 0.31 4 2 11 0.99 0.36 4 2 12 0.60 0.28 4 2 13 2.40 0.36 4 2 14 0.62 0.35 4 2 15 2.47 0.43 4 2 16 0.46 0.39 4 3 1 34.49 0.40 4 3 2 27.56 0.37 4 3 3 1.05 0.07 4 3 4 1.02 0.11 4 3 5 0.25 0.08 4 3 6 20.23 0.33 4 3 7 5.79 0.23 4 3 8 0.04 0.15 4 3 9 13.28 0.38 4 3 10 0.02 0.20 4 3 11 3.71 0.30 4 3 12 6.12 0.41 4 3 13 0.02 0.27 4 3 14 1.39 0.38 4 3 15 2.45 0.41 4 3 16 0.11 0.39 4 4 0 240.58 3.49 4 4 1 44.41 0.57 4 4 2 113.02 1.15 4 4 3 142.75 1.50 4 4 4 4.29 0.29 4 4 5 178.69 1.95 4 4 6 20.82 0.37 4 4 7 33.71 0.54 4 4 8 63.09 0.83 4 4 9 0.03 0.17 4 4 10 48.74 0.97 4 4 11 23.17 0.60 4 4 12 8.52 0.42 4 4 13 32.87 0.94 4 4 14 0.39 0.31 4 4 15 14.86 0.72 4 4 16 10.26 0.65 4 5 1 442.72 4.37 4 5 2 123.17 1.45 4 5 3 87.29 1.25 4 5 4 185.87 2.06 4 5 5 6.43 0.37 4 5 6 159.33 1.96 4 5 7 66.34 1.00 4 5 8 13.69 0.65 4 5 9 146.95 1.94 4 5 10 18.59 0.57 4 5 11 32.79 0.81 4 5 12 53.71 1.40 4 5 13 3.69 0.41 4 5 14 33.28 0.96 4 5 15 7.60 0.52 4 5 16 10.58 0.65 4 6 0 168.87 2.82 4 6 1 14.84 0.58 4 6 2 158.87 1.91 4 6 3 111.15 1.37 4 6 4 0.01 0.09 4 6 5 103.07 1.26 4 6 6 17.37 0.48 4 6 7 35.48 0.63 4 6 8 70.83 1.14 4 6 9 0.00 0.18 4 6 10 53.82 0.99 4 6 11 24.12 0.67 4 6 12 8.34 0.46 4 6 13 29.39 1.03 4 6 14 0.35 0.34 4 6 15 14.49 0.71 4 7 1 7.99 0.24 4 7 2 16.51 0.61 4 7 3 10.92 0.29 4 7 4 24.33 0.42 4 7 5 0.10 0.10 4 7 6 16.52 0.35 4 7 7 3.33 0.22 4 7 8 0.58 0.21 4 7 9 7.21 0.34 4 7 10 0.21 0.21 4 7 11 4.57 0.35 4 7 12 3.69 0.35 4 7 13 0.15 0.28 4 7 14 1.04 0.37 4 7 15 0.26 0.39 4 8 0 95.21 2.29 4 8 1 0.40 0.13 4 8 2 23.25 0.38 4 8 3 6.58 0.20 4 8 4 0.69 0.12 4 8 5 1.55 0.16 4 8 6 4.81 0.21 4 8 7 1.70 0.18 4 8 8 2.84 0.24 4 8 9 0.00 0.20 4 8 10 4.37 0.32 4 8 11 3.18 0.31 4 8 12 0.47 0.27 4 8 13 2.02 0.33 4 8 14 0.23 0.37 4 8 15 1.64 0.44 4 9 1 135.70 1.85 4 9 2 41.73 0.65 4 9 3 35.81 0.56 4 9 4 116.16 1.51 4 9 5 4.43 0.21 4 9 6 48.98 0.78 4 9 7 40.98 0.76 4 9 8 7.75 0.36 4 9 9 43.42 0.91 4 9 10 4.06 0.32 4 9 11 25.21 0.69 4 9 12 24.24 0.69 4 9 13 0.00 0.28 4 9 14 17.26 0.80 4 9 15 5.63 0.66 4 10 0 219.89 3.66 4 10 1 36.90 0.66 4 10 2 46.88 0.79 4 10 3 149.89 1.87 4 10 4 2.35 0.17 4 10 5 148.94 2.03 4 10 6 46.48 0.80 4 10 7 49.79 0.93 4 10 8 85.26 1.30 4 10 9 0.00 0.22 4 10 10 59.19 1.21 4 10 11 23.70 0.69 4 10 12 12.25 0.60 4 10 13 41.23 1.04 4 10 14 2.94 0.47 4 11 1 125.14 1.73 4 11 2 44.18 0.75 4 11 3 12.91 0.58 4 11 4 53.44 0.81 4 11 5 1.62 0.20 4 11 6 47.85 0.81 4 11 7 50.19 0.89 4 11 8 7.52 0.43 4 11 9 48.13 0.99 4 11 10 2.46 0.34 4 11 11 28.17 0.82 4 11 12 16.63 0.68 4 11 13 0.50 0.34 4 11 14 16.95 0.74 4 12 0 24.90 0.69 4 12 1 5.00 0.33 4 12 2 2.48 0.17 4 12 3 11.19 0.42 4 12 4 0.88 0.14 4 12 5 5.07 0.29 4 12 6 0.43 0.17 4 12 7 7.33 0.33 4 12 8 4.30 0.29 4 12 9 0.33 0.25 4 12 10 3.95 0.44 4 12 11 0.46 0.29 4 12 12 0.90 0.33 4 12 13 2.13 0.39 4 12 14 0.00 0.37 4 13 1 3.24 0.20 4 13 2 0.03 0.14 4 13 3 1.19 0.22 4 13 4 3.65 0.20 4 13 5 2.58 0.29 4 13 6 6.29 0.34 4 13 7 10.43 0.76 4 13 8 0.05 0.23 4 13 9 4.40 0.43 4 13 10 0.22 0.32 4 13 11 1.22 0.36 4 13 12 3.47 0.41 4 13 13 0.00 0.32 4 14 0 34.75 0.86 4 14 1 5.13 0.27 4 14 2 39.38 0.74 4 14 3 46.99 0.86 4 14 4 1.08 0.21 4 14 5 76.62 1.21 4 14 6 18.42 0.58 4 14 7 8.99 0.45 4 14 8 23.63 0.70 4 14 9 0.00 0.28 4 14 10 22.00 0.84 4 14 11 11.08 0.64 4 14 12 2.69 0.40 4 14 13 15.81 0.72 4 15 1 94.42 1.44 4 15 2 35.26 0.78 4 15 3 46.58 0.86 4 15 4 104.50 1.59 4 15 5 1.37 0.23 4 15 6 46.98 1.09 4 15 7 26.62 0.77 4 15 8 2.95 0.35 4 15 9 38.99 1.08 4 15 10 2.26 0.39 4 15 11 18.55 0.81 4 15 12 24.27 0.85 4 16 0 35.15 0.93 4 16 1 4.04 0.32 4 16 2 39.16 0.77 4 16 3 35.99 1.05 4 16 4 2.59 0.30 4 16 5 51.13 1.18 4 16 6 8.66 0.52 4 16 7 11.49 0.58 4 16 8 21.37 0.90 4 16 9 0.39 0.34 4 16 10 24.58 0.88 4 16 11 8.55 0.62 4 16 12 3.57 0.45 4 17 1 2.82 0.24 4 17 2 3.09 0.38 4 17 3 0.89 0.25 4 17 4 4.64 0.35 4 17 5 0.00 0.25 4 17 6 5.53 0.45 4 17 7 2.40 0.37 4 17 8 0.56 0.32 4 17 9 3.09 0.45 4 17 10 0.00 0.33 4 17 11 1.59 0.43 4 18 0 8.46 0.63 4 18 1 0.00 0.17 4 18 2 4.09 0.35 4 18 3 2.31 0.39 4 18 4 0.00 0.24 4 18 5 0.89 0.31 4 18 6 0.96 0.32 4 18 7 0.28 0.31 4 18 8 1.53 0.39 4 18 9 0.01 0.33 4 18 10 0.01 0.35 4 18 11 0.91 0.42 4 19 1 25.53 1.50 4 19 2 11.11 0.52 4 19 3 4.47 0.37 4 19 4 24.36 1.24 4 19 5 1.13 0.36 4 19 6 14.17 0.70 4 19 7 14.65 0.70 4 19 8 1.57 0.39 4 19 9 17.38 0.96 4 19 10 3.56 0.49 4 20 0 40.36 1.45 4 20 1 7.15 0.45 4 20 2 17.40 0.71 4 20 3 29.05 0.84 4 20 4 1.95 0.45 4 20 5 43.50 1.20 4 20 6 9.91 0.61 4 20 7 12.32 0.67 4 20 8 25.38 0.97 4 20 9 0.00 0.36 4 21 1 20.13 0.79 4 21 2 8.72 0.51 4 21 3 6.86 0.50 4 21 4 21.62 0.98 4 21 5 0.01 0.32 4 21 6 14.91 0.86 4 21 7 12.21 0.84 4 21 8 0.87 0.40 4 22 0 2.34 0.64 4 22 1 1.14 0.31 4 22 2 0.67 0.30 4 22 3 1.03 0.41 4 22 4 0.59 0.35 4 22 5 2.80 0.43 4 22 6 0.38 0.36 4 22 7 1.68 0.81 4 23 1 0.54 0.30 4 23 2 2.62 0.38 4 23 3 0.24 0.40 4 23 4 0.00 0.34 4 23 5 0.00 0.32 4 24 0 15.22 0.98 4 24 1 4.59 0.50 4 24 2 2.35 0.42 5 0 1 289.14 3.51 5 0 2 53.03 1.60 5 0 3 32.45 0.90 5 0 4 275.47 3.97 5 0 5 42.41 1.21 5 0 6 128.85 1.83 5 0 7 153.32 2.31 5 0 8 22.26 0.89 5 0 9 145.89 2.34 5 0 10 26.29 0.84 5 0 11 47.65 1.48 5 0 12 50.05 2.17 5 0 13 2.41 0.77 5 0 14 52.33 1.73 5 0 15 8.06 0.83 5 0 16 11.89 0.99 5 1 0 237.13 3.39 5 1 1 13.96 0.30 5 1 2 90.30 0.96 5 1 3 118.92 1.50 5 1 4 9.60 0.27 5 1 5 156.55 1.56 5 1 6 58.94 0.71 5 1 7 48.81 0.80 5 1 8 68.36 0.88 5 1 9 0.15 0.21 5 1 10 58.31 0.84 5 1 11 19.32 0.66 5 1 12 9.16 0.51 5 1 13 29.43 0.90 5 1 14 1.46 0.38 5 1 15 18.99 1.17 5 1 16 9.23 0.64 5 2 1 33.92 0.50 5 2 2 2.59 0.09 5 2 3 47.85 0.58 5 2 4 66.93 1.18 5 2 5 1.35 0.15 5 2 6 3.97 0.22 5 2 7 2.38 0.15 5 2 8 3.98 0.21 5 2 9 3.23 0.23 5 2 10 0.06 0.22 5 2 11 5.00 0.34 5 2 12 1.46 0.31 5 2 13 0.00 0.31 5 2 14 2.20 0.41 5 2 15 0.47 0.36 5 2 16 0.94 0.41 5 3 0 27.90 0.44 5 3 1 11.74 0.22 5 3 2 2.93 0.15 5 3 3 7.46 0.18 5 3 4 0.82 0.11 5 3 5 21.24 0.42 5 3 6 2.03 0.14 5 3 7 6.66 0.29 5 3 8 13.24 0.33 5 3 9 0.00 0.15 5 3 10 4.00 0.30 5 3 11 1.16 0.33 5 3 12 1.14 0.30 5 3 13 4.89 0.40 5 3 14 0.00 0.33 5 3 15 1.08 0.40 5 3 16 0.87 0.41 5 4 1 183.56 1.93 5 4 2 99.05 1.13 5 4 3 72.62 0.79 5 4 4 161.39 1.77 5 4 5 1.08 0.13 5 4 6 93.97 1.22 5 4 7 28.92 0.47 5 4 8 5.51 0.25 5 4 9 70.74 1.05 5 4 10 5.50 0.35 5 4 11 19.19 0.60 5 4 12 27.63 0.80 5 4 13 1.16 0.35 5 4 14 23.77 0.76 5 4 15 7.90 0.59 5 4 16 4.79 0.73 5 5 0 299.90 4.62 5 5 1 45.80 0.59 5 5 2 172.70 1.74 5 5 3 196.15 1.88 5 5 4 3.18 0.15 5 5 5 221.57 2.61 5 5 6 32.59 0.53 5 5 7 52.47 0.82 5 5 8 107.04 1.46 5 5 9 0.01 0.19 5 5 10 85.55 1.37 5 5 11 40.26 0.88 5 5 12 12.01 0.58 5 5 13 45.35 1.53 5 5 14 0.62 0.35 5 5 15 21.15 0.85 5 6 1 137.52 1.55 5 6 2 81.81 0.90 5 6 3 16.34 0.24 5 6 4 90.67 1.07 5 6 5 1.66 0.20 5 6 6 106.79 1.38 5 6 7 51.25 0.78 5 6 8 5.05 0.27 5 6 9 71.69 1.10 5 6 10 7.75 0.74 5 6 11 23.80 0.66 5 6 12 28.48 0.73 5 6 13 2.28 0.37 5 6 14 17.98 0.81 5 6 15 3.37 0.51 5 7 0 13.17 0.61 5 7 1 4.81 0.16 5 7 2 18.47 0.30 5 7 3 9.58 0.29 5 7 4 1.39 0.10 5 7 5 21.34 0.44 5 7 6 0.42 0.13 5 7 7 5.20 0.28 5 7 8 7.41 0.29 5 7 9 0.32 0.18 5 7 10 4.81 0.35 5 7 11 0.69 0.25 5 7 12 1.37 0.29 5 7 13 2.78 0.43 5 7 14 0.00 0.34 5 7 15 1.36 0.43 5 8 1 13.74 0.32 5 8 2 3.04 0.23 5 8 3 2.83 0.16 5 8 4 18.66 0.39 5 8 5 1.39 0.14 5 8 6 2.90 0.21 5 8 7 2.05 0.22 5 8 8 2.15 0.23 5 8 9 6.54 0.35 5 8 10 2.21 0.27 5 8 11 2.44 0.30 5 8 12 1.34 0.32 5 8 13 0.00 0.34 5 8 14 1.10 0.41 5 8 15 0.03 0.40 5 9 0 123.69 2.55 5 9 1 4.27 0.20 5 9 2 85.34 1.13 5 9 3 112.21 1.47 5 9 4 4.29 0.19 5 9 5 77.48 1.08 5 9 6 15.96 0.43 5 9 7 28.37 0.60 5 9 8 44.82 0.86 5 9 9 0.00 0.20 5 9 10 30.35 0.79 5 9 11 10.84 0.52 5 9 12 4.83 0.42 5 9 13 20.29 0.84 5 9 14 2.80 0.46 5 9 15 8.97 0.67 5 10 1 167.38 2.07 5 10 2 69.65 1.00 5 10 3 31.21 0.69 5 10 4 135.08 1.68 5 10 5 5.43 0.22 5 10 6 80.34 1.21 5 10 7 74.43 1.20 5 10 8 9.83 0.40 5 10 9 72.25 1.54 5 10 10 7.80 0.49 5 10 11 31.67 0.84 5 10 12 33.06 0.92 5 10 13 0.16 0.33 5 10 14 31.00 1.06 5 11 0 107.18 2.35 5 11 1 9.05 0.41 5 11 2 32.22 0.78 5 11 3 64.28 0.96 5 11 4 0.70 0.14 5 11 5 43.99 0.72 5 11 6 17.43 0.67 5 11 7 43.35 0.87 5 11 8 67.29 1.31 5 11 9 0.01 0.28 5 11 10 31.41 0.92 5 11 11 10.76 0.54 5 11 12 8.15 0.51 5 11 13 17.28 0.73 5 11 14 0.01 0.37 5 12 1 15.45 0.59 5 12 2 5.44 0.25 5 12 3 3.60 0.24 5 12 4 8.58 0.31 5 12 5 0.00 0.14 5 12 6 4.88 0.33 5 12 7 0.99 0.25 5 12 8 4.87 0.39 5 12 9 4.97 0.45 5 12 10 0.43 0.31 5 12 11 2.01 0.38 5 12 12 0.34 0.31 5 12 13 0.00 0.32 5 12 14 1.25 0.44 5 13 0 1.36 0.31 5 13 1 0.71 0.14 5 13 2 1.02 0.16 5 13 3 4.19 0.28 5 13 4 3.92 0.23 5 13 5 5.30 0.48 5 13 6 4.85 0.32 5 13 7 1.98 0.27 5 13 8 7.88 0.58 5 13 9 0.10 0.28 5 13 10 1.50 0.37 5 13 11 1.09 0.36 5 13 12 0.09 0.32 5 13 13 2.16 0.40 5 14 1 52.83 0.93 5 14 2 20.95 0.48 5 14 3 17.69 0.55 5 14 4 57.90 1.18 5 14 5 1.65 0.30 5 14 6 35.60 0.86 5 14 7 22.29 0.65 5 14 8 0.65 0.25 5 14 9 22.85 0.82 5 14 10 1.92 0.39 5 14 11 9.96 0.64 5 14 12 15.10 0.68 5 14 13 0.01 0.34 5 15 0 64.75 1.70 5 15 1 4.60 0.29 5 15 2 88.22 1.53 5 15 3 82.97 1.34 5 15 4 4.41 0.31 5 15 5 79.74 1.62 5 15 6 11.06 0.60 5 15 7 17.54 0.63 5 15 8 34.75 0.86 5 15 9 0.02 0.31 5 15 10 30.50 1.23 5 15 11 11.41 0.68 5 15 12 6.14 0.51 5 16 1 36.31 0.84 5 16 2 18.89 0.63 5 16 3 14.29 0.56 5 16 4 46.10 1.00 5 16 5 0.34 0.27 5 16 6 26.80 0.84 5 16 7 15.13 0.67 5 16 8 2.80 0.36 5 16 9 25.15 0.86 5 16 10 1.85 0.42 5 16 11 11.14 0.70 5 16 12 10.97 0.62 5 17 0 2.54 0.60 5 17 1 0.90 0.24 5 17 2 2.12 0.28 5 17 3 2.21 0.26 5 17 4 0.00 0.24 5 17 5 4.71 0.43 5 17 6 1.48 0.37 5 17 7 1.96 0.32 5 17 8 2.64 0.41 5 17 9 0.08 0.33 5 17 10 2.74 0.45 5 17 11 0.00 0.37 5 18 1 3.49 0.31 5 18 2 1.59 0.31 5 18 3 0.00 0.21 5 18 4 2.15 0.29 5 18 5 0.31 0.29 5 18 6 0.71 0.31 5 18 7 1.22 0.31 5 18 8 0.00 0.30 5 18 9 1.54 0.41 5 18 10 1.15 0.40 5 19 0 29.90 1.11 5 19 1 2.74 0.34 5 19 2 11.56 0.54 5 19 3 18.60 0.63 5 19 4 0.02 0.29 5 19 5 20.72 0.89 5 19 6 7.40 0.66 5 19 7 5.57 0.45 5 19 8 15.74 0.74 5 19 9 0.01 0.36 5 20 1 37.85 0.95 5 20 2 13.88 0.61 5 20 3 14.29 0.61 5 20 4 42.19 1.14 5 20 5 1.54 0.40 5 20 6 18.01 0.81 5 20 7 16.82 0.70 5 20 8 2.75 0.46 5 21 0 17.89 0.96 5 21 1 1.92 0.34 5 21 2 13.63 0.66 5 21 3 14.81 0.64 5 21 4 0.74 0.36 5 21 5 19.58 0.82 5 21 6 4.68 0.51 5 21 7 8.50 1.31 5 22 1 1.33 0.36 5 22 2 0.00 0.28 5 22 3 1.54 0.32 5 22 4 2.28 0.43 5 22 5 0.00 0.34 5 22 6 0.83 0.39 5 23 0 2.19 0.48 5 23 1 1.10 0.35 5 23 2 0.00 0.29 5 23 3 0.26 0.34 5 23 4 0.02 0.35 6 0 0 308.85 6.14 6 0 1 46.26 0.64 6 0 2 91.25 1.23 6 0 3 197.19 3.98 6 0 4 6.95 0.25 6 0 5 213.21 3.35 6 0 6 110.47 1.87 6 0 7 49.47 0.83 6 0 8 114.45 2.30 6 0 9 0.05 0.26 6 0 10 97.47 2.03 6 0 11 33.94 1.22 6 0 12 11.76 0.82 6 0 13 50.63 1.66 6 0 14 4.46 0.67 6 0 15 25.17 1.27 6 1 1 107.61 1.09 6 1 2 67.58 0.84 6 1 3 28.87 0.33 6 1 4 215.01 2.75 6 1 5 12.47 0.68 6 1 6 75.76 0.96 6 1 7 60.11 0.63 6 1 8 14.53 0.36 6 1 9 53.75 0.90 6 1 10 2.02 0.24 6 1 11 33.45 0.86 6 1 12 33.34 0.90 6 1 13 0.27 0.33 6 1 14 29.58 0.92 6 1 15 4.96 0.51 6 2 0 47.03 0.68 6 2 1 0.33 0.05 6 2 2 52.76 0.66 6 2 3 25.07 0.34 6 2 4 13.91 0.24 6 2 5 15.47 0.32 6 2 6 3.93 0.19 6 2 7 1.78 0.15 6 2 8 0.73 0.15 6 2 9 1.46 0.20 6 2 10 8.17 0.35 6 2 11 1.96 0.31 6 2 12 1.10 0.33 6 2 13 2.62 0.42 6 2 14 0.39 0.35 6 2 15 1.85 0.42 6 3 1 1.51 0.09 6 3 2 13.32 0.24 6 3 3 1.36 0.09 6 3 4 22.51 0.41 6 3 5 1.68 0.11 6 3 6 24.52 0.38 6 3 7 6.77 0.28 6 3 8 1.52 0.15 6 3 9 5.96 0.30 6 3 10 0.03 0.25 6 3 11 1.04 0.27 6 3 12 4.59 0.39 6 3 13 0.00 0.31 6 3 14 1.86 0.40 6 3 15 0.04 0.39 6 4 0 193.59 2.82 6 4 1 21.45 0.34 6 4 2 160.90 1.69 6 4 3 99.49 1.48 6 4 4 19.35 0.36 6 4 5 138.73 1.64 6 4 6 14.03 0.39 6 4 7 24.39 0.46 6 4 8 56.41 0.86 6 4 9 0.00 0.17 6 4 10 38.86 0.83 6 4 11 15.80 0.60 6 4 12 5.20 0.42 6 4 13 28.69 0.82 6 4 14 1.29 0.41 6 4 15 8.65 0.66 6 5 1 163.99 1.65 6 5 2 137.33 1.67 6 5 3 55.35 0.75 6 5 4 229.48 2.46 6 5 5 7.81 0.39 6 5 6 117.49 1.44 6 5 7 69.35 1.23 6 5 8 9.49 0.46 6 5 9 113.26 1.59 6 5 10 13.50 0.55 6 5 11 34.55 0.86 6 5 12 45.17 1.30 6 5 13 1.68 0.41 6 5 14 32.37 0.97 6 5 15 8.53 0.66 6 6 0 97.43 1.35 6 6 1 33.73 0.54 6 6 2 48.70 0.87 6 6 3 95.61 1.10 6 6 4 2.23 0.20 6 6 5 127.41 1.50 6 6 6 19.15 0.53 6 6 7 30.14 0.57 6 6 8 65.97 1.04 6 6 9 0.02 0.21 6 6 10 47.12 0.90 6 6 11 16.49 0.58 6 6 12 7.77 0.55 6 6 13 22.03 0.86 6 6 14 0.00 0.48 6 6 15 12.27 0.68 6 7 1 23.15 0.42 6 7 2 3.17 0.17 6 7 3 8.81 0.25 6 7 4 11.56 0.23 6 7 5 0.03 0.11 6 7 6 15.63 0.37 6 7 7 3.86 0.25 6 7 8 0.45 0.17 6 7 9 2.85 0.26 6 7 10 0.00 0.23 6 7 11 3.54 0.36 6 7 12 3.98 0.45 6 7 13 0.67 0.36 6 7 14 2.18 0.46 6 7 15 0.33 0.42 6 8 0 0.28 0.20 6 8 1 0.43 0.10 6 8 2 3.18 0.15 6 8 3 28.15 0.41 6 8 4 0.03 0.09 6 8 5 6.09 0.26 6 8 6 0.70 0.14 6 8 7 5.55 0.26 6 8 8 8.99 0.34 6 8 9 0.25 0.21 6 8 10 3.42 0.39 6 8 11 2.11 0.31 6 8 12 0.00 0.29 6 8 13 0.52 0.37 6 8 14 0.00 0.36 6 8 15 1.70 0.46 6 9 1 114.92 1.65 6 9 2 44.02 0.90 6 9 3 30.66 0.46 6 9 4 85.85 1.20 6 9 5 0.05 0.13 6 9 6 51.67 0.88 6 9 7 36.73 0.74 6 9 8 5.83 0.32 6 9 9 36.14 0.77 6 9 10 5.91 0.48 6 9 11 13.26 0.60 6 9 12 16.24 0.72 6 9 13 0.00 0.35 6 9 14 16.14 0.87 6 10 0 221.40 3.84 6 10 1 17.99 0.78 6 10 2 92.40 1.29 6 10 3 87.87 1.13 6 10 4 5.51 0.21 6 10 5 98.45 1.59 6 10 6 26.68 0.76 6 10 7 47.29 1.01 6 10 8 91.85 1.42 6 10 9 0.45 0.22 6 10 10 41.34 1.09 6 10 11 18.29 0.69 6 10 12 6.91 0.50 6 10 13 30.07 1.34 6 10 14 1.47 0.45 6 11 1 43.08 0.79 6 11 2 45.01 0.71 6 11 3 1.42 0.29 6 11 4 59.03 0.86 6 11 5 2.04 0.27 6 11 6 68.95 1.52 6 11 7 51.61 1.30 6 11 8 8.89 0.60 6 11 9 42.67 0.88 6 11 10 4.36 0.47 6 11 11 15.89 1.06 6 11 12 12.79 0.62 6 11 13 0.64 0.39 6 11 14 18.38 0.87 6 12 0 21.00 0.72 6 12 1 0.04 0.14 6 12 2 11.40 0.65 6 12 3 4.49 0.25 6 12 4 2.18 0.21 6 12 5 7.20 0.39 6 12 6 0.22 0.21 6 12 7 4.83 0.48 6 12 8 3.22 0.34 6 12 9 0.36 0.30 6 12 10 3.68 0.44 6 12 11 0.44 0.33 6 12 12 0.75 0.33 6 12 13 0.11 0.38 6 13 1 0.37 0.16 6 13 2 11.21 0.45 6 13 3 2.23 0.21 6 13 4 5.55 0.33 6 13 5 1.45 0.25 6 13 6 6.32 0.39 6 13 7 5.78 0.38 6 13 8 0.02 0.24 6 13 9 2.91 0.40 6 13 10 0.02 0.30 6 13 11 0.28 0.35 6 13 12 2.30 0.40 6 13 13 0.00 0.37 6 14 0 65.64 1.96 6 14 1 7.78 0.39 6 14 2 41.54 0.80 6 14 3 36.64 0.76 6 14 4 2.20 0.27 6 14 5 37.38 0.85 6 14 6 6.04 0.38 6 14 7 11.74 0.52 6 14 8 26.91 0.93 6 14 9 0.01 0.30 6 14 10 14.40 0.70 6 14 11 6.99 0.74 6 14 12 3.62 0.43 6 15 1 84.07 1.89 6 15 2 33.22 0.73 6 15 3 25.09 0.63 6 15 4 76.31 1.88 6 15 5 0.90 0.26 6 15 6 42.55 0.96 6 15 7 23.38 0.72 6 15 8 4.06 0.46 6 15 9 37.80 1.10 6 15 10 3.49 0.44 6 15 11 16.32 0.78 6 15 12 22.57 1.05 6 16 0 37.79 1.21 6 16 1 3.99 0.33 6 16 2 28.92 0.97 6 16 3 35.46 0.85 6 16 4 0.00 0.22 6 16 5 31.25 0.79 6 16 6 5.29 0.52 6 16 7 13.04 0.57 6 16 8 23.73 0.89 6 16 9 0.01 0.34 6 16 10 20.10 1.04 6 16 11 5.80 0.56 6 17 1 3.20 0.30 6 17 2 1.44 0.25 6 17 3 0.60 0.24 6 17 4 3.40 0.33 6 17 5 0.26 0.30 6 17 6 2.66 0.33 6 17 7 0.65 0.30 6 17 8 0.73 0.30 6 17 9 3.09 0.46 6 17 10 0.01 0.33 6 17 11 1.87 0.44 6 18 0 1.33 0.37 6 18 1 0.09 0.22 6 18 2 0.43 0.22 6 18 3 2.47 0.30 6 18 4 0.01 0.22 6 18 5 1.90 0.35 6 18 6 1.11 0.30 6 18 7 0.00 0.26 6 18 8 1.92 0.40 6 18 9 0.05 0.34 6 18 10 1.19 0.41 6 19 1 20.13 0.67 6 19 2 10.48 0.51 6 19 3 3.82 0.36 6 19 4 22.19 0.71 6 19 5 0.91 0.34 6 19 6 10.36 0.62 6 19 7 10.80 0.63 6 19 8 0.80 0.43 6 19 9 14.66 0.77 6 20 0 46.69 1.58 6 20 1 2.19 0.33 6 20 2 29.69 0.85 6 20 3 24.13 0.76 6 20 4 0.73 0.36 6 20 5 30.74 1.01 6 20 6 9.03 0.60 6 20 7 9.37 0.62 6 20 8 19.87 1.37 6 21 1 16.75 0.67 6 21 2 6.42 0.45 6 21 3 4.92 0.42 6 21 4 17.30 0.80 6 21 5 0.38 0.34 6 21 6 15.40 0.76 6 21 7 8.92 0.80 6 22 0 3.93 0.65 6 22 1 0.27 0.29 6 22 2 1.79 0.34 6 22 3 0.92 0.31 6 22 4 0.00 0.32 6 22 5 0.42 0.37 6 23 1 0.72 0.30 6 23 2 0.25 0.29 6 23 3 0.06 0.30 7 0 1 246.08 3.36 7 0 2 174.64 2.56 7 0 3 24.46 0.69 7 0 4 180.15 3.90 7 0 5 4.43 0.33 7 0 6 108.22 1.51 7 0 7 110.43 2.49 7 0 8 11.15 0.96 7 0 9 105.27 3.16 7 0 10 4.39 0.43 7 0 11 49.39 1.57 7 0 12 39.13 1.34 7 0 13 0.20 0.47 7 0 14 40.30 1.53 7 0 15 12.51 1.25 7 1 0 124.24 1.85 7 1 1 15.83 0.33 7 1 2 72.14 1.00 7 1 3 146.27 1.68 7 1 4 1.71 0.20 7 1 5 103.64 1.06 7 1 6 33.51 0.83 7 1 7 40.70 0.62 7 1 8 51.57 0.89 7 1 9 0.57 0.21 7 1 10 47.12 0.84 7 1 11 17.96 0.92 7 1 12 8.40 0.51 7 1 13 33.69 0.93 7 1 14 1.93 0.42 7 1 15 11.95 0.75 7 2 1 48.86 0.57 7 2 2 1.73 0.10 7 2 3 14.77 0.25 7 2 4 15.15 0.30 7 2 5 0.19 0.10 7 2 6 5.28 0.18 7 2 7 3.44 0.20 7 2 8 1.39 0.19 7 2 9 2.84 0.25 7 2 10 0.03 0.19 7 2 11 4.31 0.38 7 2 12 4.43 0.40 7 2 13 0.02 0.30 7 2 14 3.86 0.51 7 2 15 0.31 0.43 7 3 0 0.79 0.12 7 3 1 2.70 0.12 7 3 2 6.52 0.24 7 3 3 16.34 0.28 7 3 4 0.06 0.11 7 3 5 28.64 0.46 7 3 6 0.65 0.13 7 3 7 9.54 0.29 7 3 8 9.18 0.32 7 3 9 0.00 0.17 7 3 10 1.34 0.22 7 3 11 2.09 0.30 7 3 12 0.01 0.29 7 3 13 2.68 0.44 7 3 14 0.00 0.36 7 3 15 0.74 0.43 7 4 1 168.12 1.81 7 4 2 35.55 0.51 7 4 3 82.27 0.97 7 4 4 113.55 1.29 7 4 5 2.12 0.16 7 4 6 60.43 0.82 7 4 7 40.51 0.67 7 4 8 5.12 0.27 7 4 9 47.48 0.76 7 4 10 5.68 0.36 7 4 11 17.64 0.71 7 4 12 25.55 0.79 7 4 13 0.59 0.37 7 4 14 14.15 0.76 7 4 15 4.15 0.54 7 5 0 156.27 2.64 7 5 1 25.17 0.56 7 5 2 125.45 1.33 7 5 3 141.03 1.56 7 5 4 3.97 0.18 7 5 5 158.49 1.80 7 5 6 40.10 0.71 7 5 7 40.27 0.71 7 5 8 118.28 1.50 7 5 9 0.62 0.20 7 5 10 68.16 1.31 7 5 11 30.37 0.90 7 5 12 7.71 0.55 7 5 13 40.24 1.06 7 5 14 0.66 0.37 7 5 15 17.79 0.87 7 6 1 77.24 0.91 7 6 2 54.10 0.84 7 6 3 30.01 0.69 7 6 4 121.24 1.41 7 6 5 7.51 0.51 7 6 6 48.08 0.76 7 6 7 34.37 0.58 7 6 8 8.17 0.55 7 6 9 64.64 1.24 7 6 10 4.46 0.41 7 6 11 24.72 1.03 7 6 12 23.26 0.84 7 6 13 1.04 0.37 7 6 14 17.28 0.78 7 6 15 2.56 0.53 7 7 0 17.55 0.42 7 7 1 2.13 0.11 7 7 2 12.71 0.33 7 7 3 8.87 0.22 7 7 4 1.99 0.18 7 7 5 23.10 0.53 7 7 6 1.97 0.20 7 7 7 2.51 0.23 7 7 8 0.68 0.20 7 7 9 0.47 0.24 7 7 10 3.58 0.36 7 7 11 0.72 0.31 7 7 12 2.31 0.41 7 7 13 3.83 0.47 7 7 14 0.00 0.37 7 8 1 7.67 0.23 7 8 2 9.95 0.32 7 8 3 0.04 0.11 7 8 4 4.71 0.22 7 8 5 0.02 0.15 7 8 6 3.68 0.25 7 8 7 10.64 0.57 7 8 8 0.23 0.19 7 8 9 5.15 0.38 7 8 10 1.32 0.32 7 8 11 1.04 0.34 7 8 12 1.59 0.39 7 8 13 0.00 0.34 7 8 14 2.25 0.47 7 9 0 120.36 1.92 7 9 1 7.75 0.24 7 9 2 69.64 0.91 7 9 3 52.64 0.77 7 9 4 6.89 0.28 7 9 5 67.32 1.09 7 9 6 14.78 0.47 7 9 7 23.74 0.60 7 9 8 42.85 0.87 7 9 9 0.01 0.20 7 9 10 22.43 0.79 7 9 11 12.75 0.76 7 9 12 2.84 0.42 7 9 13 18.15 0.83 7 9 14 0.63 0.41 7 10 1 145.64 1.74 7 10 2 46.85 0.69 7 10 3 36.51 0.68 7 10 4 102.44 1.47 7 10 5 0.87 0.19 7 10 6 80.97 1.79 7 10 7 64.98 1.14 7 10 8 7.19 0.38 7 10 9 58.41 1.09 7 10 10 8.00 0.52 7 10 11 19.42 0.68 7 10 12 19.41 0.82 7 10 13 0.21 0.39 7 10 14 26.35 1.19 7 11 0 37.38 0.92 7 11 1 10.68 0.57 7 11 2 17.17 0.41 7 11 3 57.42 0.87 7 11 4 1.33 0.23 7 11 5 78.82 1.27 7 11 6 16.68 0.50 7 11 7 26.07 0.82 7 11 8 43.86 0.91 7 11 9 0.01 0.21 7 11 10 24.90 1.10 7 11 11 7.91 0.63 7 11 12 4.85 0.48 7 11 13 16.57 0.83 7 12 1 11.13 0.32 7 12 2 0.90 0.16 7 12 3 6.00 0.57 7 12 4 5.60 0.29 7 12 5 0.56 0.33 7 12 6 6.72 0.47 7 12 7 3.64 0.33 7 12 8 0.99 0.25 7 12 9 3.25 0.32 7 12 10 0.01 0.31 7 12 11 1.95 0.40 7 12 12 0.00 0.35 7 12 13 0.41 0.39 7 13 0 1.24 0.30 7 13 1 5.35 0.26 7 13 2 0.00 0.15 7 13 3 7.26 0.30 7 13 4 0.14 0.16 7 13 5 5.08 0.32 7 13 6 1.35 0.23 7 13 7 1.89 0.25 7 13 8 4.33 0.35 7 13 9 0.00 0.24 7 13 10 1.15 0.38 7 13 11 1.55 0.40 7 13 12 0.00 0.35 7 13 13 0.92 0.46 7 14 1 58.65 0.99 7 14 2 22.46 0.52 7 14 3 14.12 0.53 7 14 4 39.47 0.79 7 14 5 1.61 0.26 7 14 6 15.21 0.55 7 14 7 12.09 0.74 7 14 8 3.00 0.33 7 14 9 24.83 0.77 7 14 10 1.88 0.41 7 14 11 7.42 0.61 7 14 12 10.50 0.67 7 15 0 87.86 1.88 7 15 1 8.75 0.37 7 15 2 49.41 0.88 7 15 3 55.36 1.11 7 15 4 0.43 0.22 7 15 5 55.02 1.11 7 15 6 10.34 0.50 7 15 7 18.54 0.67 7 15 8 33.12 0.79 7 15 9 0.03 0.29 7 15 10 27.50 0.99 7 15 11 14.19 0.75 7 16 1 34.98 0.81 7 16 2 15.65 0.66 7 16 3 6.65 0.40 7 16 4 34.64 0.85 7 16 5 1.19 0.33 7 16 6 21.01 0.69 7 16 7 10.58 0.53 7 16 8 2.94 0.34 7 16 9 24.73 0.86 7 16 10 1.88 0.44 7 16 11 11.34 0.72 7 17 0 3.47 0.39 7 17 1 0.90 0.21 7 17 2 1.47 0.26 7 17 3 4.06 0.35 7 17 4 0.10 0.23 7 17 5 2.05 0.36 7 17 6 0.17 0.30 7 17 7 2.95 0.42 7 17 8 2.32 0.33 7 17 9 0.00 0.30 7 17 10 2.32 0.45 7 18 1 1.44 0.24 7 18 2 1.38 0.28 7 18 3 0.07 0.24 7 18 4 1.70 0.29 7 18 5 1.09 0.34 7 18 6 0.13 0.31 7 18 7 2.37 0.41 7 18 8 0.00 0.31 7 18 9 1.68 0.40 7 19 0 21.01 0.83 7 19 1 2.38 0.29 7 19 2 11.19 0.53 7 19 3 16.48 0.63 7 19 4 0.13 0.30 7 19 5 16.66 0.75 7 19 6 5.15 0.50 7 19 7 4.92 0.50 7 19 8 15.84 0.78 7 19 9 0.15 0.36 7 20 1 38.46 0.95 7 20 2 12.12 0.56 7 20 3 8.48 0.57 7 20 4 28.45 0.83 7 20 5 0.17 0.35 7 20 6 22.35 0.88 7 20 7 15.06 0.78 7 20 8 1.62 0.79 7 21 0 18.81 0.98 7 21 1 2.48 0.37 7 21 2 8.52 0.47 7 21 3 15.07 0.66 7 21 4 0.19 0.36 7 21 5 16.93 0.79 7 21 6 2.59 0.45 7 22 1 2.78 0.36 7 22 2 0.92 0.29 7 22 3 0.34 0.27 7 22 4 0.23 0.35 7 22 5 0.00 0.35 7 23 0 0.45 0.43 7 23 1 0.01 0.28 7 23 2 0.62 0.30 8 0 0 265.19 4.98 8 0 1 29.49 0.55 8 0 2 127.65 1.78 8 0 3 148.06 2.50 8 0 4 2.74 0.21 8 0 5 112.01 2.50 8 0 6 27.91 0.95 8 0 7 76.16 1.33 8 0 8 134.84 2.45 8 0 9 1.62 0.34 8 0 10 57.15 1.38 8 0 11 23.07 1.04 8 0 12 10.76 0.80 8 0 13 34.45 1.80 8 0 14 1.84 0.70 8 0 15 15.92 1.32 8 1 1 155.07 1.51 8 1 2 71.39 1.03 8 1 3 15.36 0.27 8 1 4 79.63 1.14 8 1 5 0.86 0.18 8 1 6 64.24 0.93 8 1 7 43.95 0.73 8 1 8 8.20 0.44 8 1 9 53.88 0.92 8 1 10 5.75 0.36 8 1 11 20.82 0.81 8 1 12 19.96 0.84 8 1 13 0.64 0.39 8 1 14 20.73 1.54 8 1 15 3.74 0.60 8 2 0 31.78 0.59 8 2 1 1.95 0.11 8 2 2 11.64 0.25 8 2 3 13.29 0.37 8 2 4 0.01 0.13 8 2 5 4.89 0.35 8 2 6 1.91 0.15 8 2 7 7.83 0.30 8 2 8 4.47 0.25 8 2 9 0.03 0.18 8 2 10 5.67 0.42 8 2 11 1.67 0.31 8 2 12 1.42 0.38 8 2 13 3.71 0.48 8 2 14 0.04 0.39 8 2 15 1.90 0.55 8 3 1 13.97 0.25 8 3 2 7.58 0.19 8 3 3 6.26 0.20 8 3 4 12.78 0.34 8 3 5 0.52 0.14 8 3 6 12.42 0.28 8 3 7 4.62 0.24 8 3 8 0.03 0.16 8 3 9 1.70 0.23 8 3 10 0.95 0.22 8 3 11 1.77 0.31 8 3 12 2.23 0.39 8 3 13 0.10 0.36 8 3 14 0.72 0.41 8 3 15 1.02 0.44 8 4 0 113.14 2.02 8 4 1 8.49 0.28 8 4 2 88.07 0.99 8 4 3 72.90 0.94 8 4 4 2.48 0.18 8 4 5 90.96 1.13 8 4 6 17.25 0.41 8 4 7 30.37 0.53 8 4 8 54.76 1.02 8 4 9 0.00 0.20 8 4 10 34.51 0.74 8 4 11 16.45 0.65 8 4 12 6.02 0.51 8 4 13 23.23 1.48 8 4 14 0.95 0.43 8 4 15 8.44 0.67 8 5 1 166.22 1.76 8 5 2 66.84 1.03 8 5 3 32.98 0.71 8 5 4 137.73 1.59 8 5 5 12.62 0.33 8 5 6 79.98 1.08 8 5 7 78.48 1.18 8 5 8 9.73 0.39 8 5 9 84.68 1.54 8 5 10 8.92 0.46 8 5 11 33.80 0.97 8 5 12 37.50 1.01 8 5 13 1.26 0.38 8 5 14 29.49 1.01 8 6 0 94.85 1.53 8 6 1 9.40 0.45 8 6 2 64.32 0.78 8 6 3 62.24 0.84 8 6 4 1.34 0.21 8 6 5 73.52 0.99 8 6 6 16.49 0.65 8 6 7 28.89 0.63 8 6 8 61.39 1.05 8 6 9 0.40 0.31 8 6 10 34.10 0.82 8 6 11 12.11 0.64 8 6 12 6.54 0.53 8 6 13 19.68 0.78 8 6 14 0.00 0.36 8 7 1 7.75 0.20 8 7 2 5.53 0.41 8 7 3 6.96 0.27 8 7 4 19.18 0.38 8 7 5 0.00 0.15 8 7 6 8.53 0.32 8 7 7 0.34 0.19 8 7 8 2.10 0.29 8 7 9 5.06 0.37 8 7 10 0.17 0.29 8 7 11 1.47 0.35 8 7 12 1.14 0.37 8 7 13 0.00 0.36 8 7 14 1.21 0.39 8 8 0 13.23 0.45 8 8 1 0.01 0.09 8 8 2 5.95 0.21 8 8 3 0.82 0.14 8 8 4 0.09 0.13 8 8 5 4.77 0.30 8 8 6 7.46 0.32 8 8 7 1.51 0.22 8 8 8 8.03 0.39 8 8 9 0.00 0.23 8 8 10 4.05 0.50 8 8 11 2.78 0.40 8 8 12 0.00 0.33 8 8 13 0.95 0.39 8 8 14 0.00 0.37 8 9 1 75.16 1.00 8 9 2 17.80 0.37 8 9 3 30.30 0.56 8 9 4 77.81 1.12 8 9 5 3.84 0.27 8 9 6 35.32 0.75 8 9 7 29.57 0.67 8 9 8 3.71 0.29 8 9 9 26.75 0.76 8 9 10 3.09 0.47 8 9 11 12.55 0.66 8 9 12 14.49 0.72 8 9 13 0.00 0.37 8 9 14 12.17 0.73 8 10 0 114.30 2.15 8 10 1 11.71 0.37 8 10 2 71.26 1.01 8 10 3 80.98 1.11 8 10 4 6.36 0.28 8 10 5 114.76 1.70 8 10 6 27.45 0.67 8 10 7 22.32 0.81 8 10 8 50.85 0.96 8 10 9 0.00 0.26 8 10 10 42.56 1.15 8 10 11 13.51 0.82 8 10 12 6.42 0.57 8 10 13 27.58 1.01 8 11 1 48.99 0.83 8 11 2 25.00 0.57 8 11 3 17.82 0.93 8 11 4 62.92 0.94 8 11 5 1.02 0.24 8 11 6 31.75 0.73 8 11 7 22.14 0.71 8 11 8 5.57 0.35 8 11 9 34.10 0.89 8 11 10 3.72 0.60 8 11 11 13.33 0.81 8 11 12 11.87 0.69 8 11 13 0.65 0.44 8 12 0 6.66 0.44 8 12 1 0.23 0.16 8 12 2 6.02 0.38 8 12 3 4.52 0.27 8 12 4 0.90 0.18 8 12 5 6.97 0.35 8 12 6 1.50 0.34 8 12 7 2.14 0.27 8 12 8 3.93 0.35 8 12 9 0.00 0.23 8 12 10 2.74 0.43 8 12 11 0.00 0.36 8 12 12 0.84 0.39 8 12 13 1.23 0.43 8 13 1 8.25 0.30 8 13 2 5.45 0.35 8 13 3 0.17 0.18 8 13 4 2.60 0.25 8 13 5 0.04 0.19 8 13 6 0.39 0.22 8 13 7 0.60 0.23 8 13 8 0.01 0.22 8 13 9 2.28 0.31 8 13 10 1.13 0.37 8 13 11 0.02 0.41 8 13 12 0.69 0.40 8 14 0 48.07 1.14 8 14 1 5.92 0.32 8 14 2 23.87 0.61 8 14 3 27.50 0.67 8 14 4 0.71 0.21 8 14 5 35.07 0.87 8 14 6 8.98 0.42 8 14 7 9.27 0.44 8 14 8 19.83 0.70 8 14 9 0.01 0.26 8 14 10 16.59 0.75 8 14 11 7.56 0.60 8 14 12 2.16 0.54 8 15 1 53.79 1.00 8 15 2 25.55 0.64 8 15 3 14.32 0.49 8 15 4 63.94 1.16 8 15 5 2.38 0.33 8 15 6 34.77 0.89 8 15 7 22.48 0.74 8 15 8 3.67 0.35 8 15 9 32.96 0.91 8 15 10 2.91 0.47 8 15 11 14.17 0.77 8 16 0 41.01 1.11 8 16 1 6.17 0.46 8 16 2 15.88 0.70 8 16 3 24.05 0.65 8 16 4 0.46 0.23 8 16 5 26.68 0.76 8 16 6 6.34 0.45 8 16 7 10.44 0.53 8 16 8 17.72 0.71 8 16 9 0.00 0.33 8 16 10 15.28 0.90 8 17 1 3.07 0.39 8 17 2 3.19 0.42 8 17 3 0.13 0.21 8 17 4 1.96 0.28 8 17 5 0.38 0.27 8 17 6 4.10 0.38 8 17 7 0.79 0.32 8 17 8 0.94 0.32 8 17 9 1.81 0.41 8 17 10 0.00 0.41 8 18 0 1.88 0.39 8 18 1 0.16 0.21 8 18 2 0.90 0.25 8 18 3 0.45 0.23 8 18 4 0.10 0.22 8 18 5 0.99 0.30 8 18 6 1.41 0.32 8 18 7 0.31 0.29 8 18 8 2.88 0.40 8 18 9 0.32 0.35 8 19 1 20.98 0.65 8 19 2 8.84 0.54 8 19 3 2.81 0.32 8 19 4 14.94 0.61 8 19 5 0.97 0.32 8 19 6 8.45 0.54 8 19 7 9.50 0.55 8 19 8 1.35 0.40 8 20 0 30.76 1.91 8 20 1 3.26 0.36 8 20 2 18.94 0.70 8 20 3 26.84 0.75 8 20 4 0.62 0.28 8 20 5 26.25 0.87 8 20 6 4.56 0.43 8 20 7 8.75 0.57 8 21 1 14.04 0.64 8 21 2 8.29 0.46 8 21 3 3.71 0.36 8 21 4 14.61 0.68 8 21 5 0.14 0.32 8 22 0 2.73 0.52 8 22 1 0.51 0.29 8 22 2 0.70 0.36 8 22 3 0.93 0.30 9 0 1 232.94 3.27 9 0 2 99.48 1.76 9 0 3 19.65 1.05 9 0 4 119.47 1.80 9 0 5 1.97 0.28 9 0 6 96.25 1.55 9 0 7 53.97 1.23 9 0 8 16.42 0.72 9 0 9 83.27 1.74 9 0 10 12.69 1.03 9 0 11 24.74 1.11 9 0 12 30.45 1.52 9 0 13 1.75 0.67 9 0 14 30.66 1.68 9 1 0 148.15 2.22 9 1 1 15.34 0.35 9 1 2 76.86 0.84 9 1 3 59.04 0.78 9 1 4 4.23 0.30 9 1 5 65.52 0.74 9 1 6 10.29 0.36 9 1 7 36.50 0.62 9 1 8 60.83 1.02 9 1 9 1.29 0.21 9 1 10 35.12 0.80 9 1 11 13.76 0.76 9 1 12 4.24 0.54 9 1 13 17.37 0.91 9 1 14 0.81 0.50 9 2 1 3.47 0.14 9 2 2 2.93 0.14 9 2 3 1.38 0.13 9 2 4 13.37 0.31 9 2 5 1.49 0.20 9 2 6 7.55 0.23 9 2 7 6.03 0.29 9 2 8 2.15 0.25 9 2 9 9.33 0.44 9 2 10 0.50 0.26 9 2 11 1.31 0.31 9 2 12 0.81 0.34 9 2 13 0.02 0.41 9 2 14 1.73 0.52 9 3 0 21.14 0.45 9 3 1 0.23 0.09 9 3 2 18.15 0.34 9 3 3 4.95 0.18 9 3 4 6.51 0.24 9 3 5 13.37 0.40 9 3 6 1.24 0.18 9 3 7 0.02 0.18 9 3 8 1.10 0.21 9 3 9 0.01 0.19 9 3 10 5.66 0.35 9 3 11 2.00 0.33 9 3 12 1.28 0.37 9 3 13 2.66 0.46 9 3 14 0.60 0.47 9 4 1 54.52 0.71 9 4 2 42.38 0.54 9 4 3 13.49 0.34 9 4 4 99.70 1.26 9 4 5 3.68 0.23 9 4 6 56.92 0.88 9 4 7 42.04 0.84 9 4 8 3.15 0.31 9 4 9 34.15 0.72 9 4 10 3.64 0.31 9 4 11 19.63 0.69 9 4 12 16.46 0.73 9 4 13 0.66 0.39 9 4 14 16.13 0.97 9 5 0 128.35 2.05 9 5 1 14.52 0.31 9 5 2 69.21 0.83 9 5 3 101.49 1.19 9 5 4 0.44 0.15 9 5 5 130.05 1.63 9 5 6 31.70 0.88 9 5 7 52.08 1.03 9 5 8 88.36 1.40 9 5 9 0.25 0.25 9 5 10 48.90 0.94 9 5 11 24.11 0.76 9 5 12 7.64 0.55 9 5 13 32.26 1.12 9 5 14 0.86 0.43 9 6 1 90.31 1.07 9 6 2 38.43 0.75 9 6 3 10.97 0.35 9 6 4 60.94 0.82 9 6 5 2.17 0.20 9 6 6 53.71 0.85 9 6 7 32.33 0.65 9 6 8 6.98 0.46 9 6 9 37.26 0.92 9 6 10 3.53 0.35 9 6 11 17.94 0.75 9 6 12 18.30 0.72 9 6 13 0.84 0.36 9 6 14 15.73 0.82 9 7 0 13.52 0.46 9 7 1 2.45 0.21 9 7 2 10.24 0.32 9 7 3 12.83 0.33 9 7 4 0.65 0.13 9 7 5 4.19 0.39 9 7 6 0.16 0.19 9 7 7 3.53 0.26 9 7 8 4.54 0.32 9 7 9 0.01 0.26 9 7 10 2.55 0.40 9 7 11 0.02 0.31 9 7 12 1.90 0.39 9 7 13 2.49 0.42 9 7 14 0.00 0.35 9 8 1 6.56 0.23 9 8 2 0.35 0.14 9 8 3 1.95 0.17 9 8 4 12.05 0.34 9 8 5 8.54 0.38 9 8 6 0.78 0.20 9 8 7 1.62 0.25 9 8 8 0.83 0.24 9 8 9 2.10 0.36 9 8 10 0.00 0.33 9 8 11 2.03 0.38 9 8 12 1.85 0.40 9 8 13 0.00 0.35 9 9 0 58.53 1.15 9 9 1 6.46 0.26 9 9 2 35.05 0.74 9 9 3 44.10 0.71 9 9 4 2.11 0.24 9 9 5 64.51 1.08 9 9 6 17.58 0.53 9 9 7 11.70 0.45 9 9 8 26.02 0.67 9 9 9 0.00 0.28 9 9 10 29.01 1.06 9 9 11 8.75 0.56 9 9 12 3.23 0.44 9 9 13 15.81 0.80 9 10 1 86.29 1.23 9 10 2 39.99 0.76 9 10 3 29.67 1.07 9 10 4 102.18 1.48 9 10 5 2.55 0.25 9 10 6 52.01 1.54 9 10 7 37.39 0.81 9 10 8 4.15 0.33 9 10 9 45.44 1.04 9 10 10 4.24 0.52 9 10 11 21.33 0.98 9 10 12 25.17 0.92 9 10 13 0.12 0.38 9 11 0 80.51 1.65 9 11 1 4.45 0.47 9 11 2 55.19 1.14 9 11 3 29.24 0.69 9 11 4 6.39 0.59 9 11 5 42.24 0.85 9 11 6 8.34 0.39 9 11 7 9.57 0.47 9 11 8 23.32 0.66 9 11 9 0.00 0.27 9 11 10 22.47 0.94 9 11 11 5.23 0.59 9 11 12 4.41 0.61 9 12 1 2.87 0.22 9 12 2 1.21 0.26 9 12 3 2.66 0.30 9 12 4 7.01 0.36 9 12 5 1.08 0.26 9 12 6 3.61 0.31 9 12 7 2.23 0.35 9 12 8 2.29 0.30 9 12 9 3.59 0.38 9 12 10 0.00 0.36 9 12 11 2.48 0.50 9 12 12 1.69 0.43 9 13 0 13.05 0.63 9 13 1 0.08 0.17 9 13 2 5.65 0.32 9 13 3 0.25 0.19 9 13 4 2.30 0.32 9 13 5 3.02 0.31 9 13 6 0.00 0.24 9 13 7 0.48 0.25 9 13 8 1.56 0.30 9 13 9 0.79 0.31 9 13 10 0.60 0.44 9 13 11 2.13 0.51 9 13 12 0.00 0.36 9 14 1 28.11 0.69 9 14 2 20.01 0.54 9 14 3 2.79 0.31 9 14 4 30.36 1.01 9 14 5 0.23 0.25 9 14 6 24.54 0.72 9 14 7 17.16 0.65 9 14 8 1.37 0.32 9 14 9 15.89 0.94 9 14 10 1.94 0.49 9 14 11 7.09 0.70 9 15 0 51.77 1.56 9 15 1 9.46 0.41 9 15 2 24.44 0.64 9 15 3 42.44 0.88 9 15 4 0.68 0.24 9 15 5 46.87 1.07 9 15 6 14.32 0.77 9 15 7 11.77 0.59 9 15 8 28.65 0.83 9 15 9 0.02 0.32 9 15 10 24.43 1.11 9 15 11 7.40 1.23 9 16 1 24.22 0.72 9 16 2 11.10 0.62 9 16 3 6.02 0.37 9 16 4 26.97 0.83 9 16 5 0.72 0.29 9 16 6 18.72 0.71 9 16 7 13.82 0.62 9 16 8 2.48 0.38 9 16 9 15.79 0.76 9 16 10 1.08 0.54 9 17 0 5.40 0.54 9 17 1 0.77 0.25 9 17 2 1.80 0.27 9 17 3 1.95 0.28 9 17 4 1.05 0.26 9 17 5 3.85 0.39 9 17 6 0.33 0.28 9 17 7 1.38 0.40 9 17 8 0.76 0.33 9 17 9 0.76 0.37 9 18 1 1.87 0.29 9 18 2 0.90 0.26 9 18 3 0.00 0.22 9 18 4 1.43 0.28 9 18 5 1.41 0.36 9 18 6 0.02 0.27 9 18 7 1.22 0.35 9 18 8 0.00 0.31 9 19 0 19.60 1.25 9 19 1 1.90 0.32 9 19 2 9.41 0.51 9 19 3 11.09 0.52 9 19 4 0.00 0.25 9 19 5 14.58 0.65 9 19 6 3.28 0.42 9 19 7 6.40 0.49 9 20 1 23.74 1.22 9 20 2 11.17 0.58 9 20 3 8.23 0.49 9 20 4 25.49 0.81 9 20 5 0.17 0.32 9 20 6 14.77 0.68 9 21 0 22.72 1.27 9 21 1 3.15 0.57 9 21 2 10.87 0.59 9 21 3 8.70 0.54 9 21 4 2.11 0.39 9 22 1 1.23 0.33 10 0 0 121.93 2.46 10 0 1 14.67 0.67 10 0 2 104.70 1.54 10 0 3 88.05 1.56 10 0 4 9.54 0.54 10 0 5 150.26 3.12 10 0 6 20.36 1.19 10 0 7 48.71 0.98 10 0 8 70.90 1.82 10 0 9 1.22 0.41 10 0 10 43.43 2.53 10 0 11 23.21 1.25 10 0 12 3.14 0.70 10 0 13 32.27 1.77 10 0 14 0.53 0.63 10 1 1 97.88 1.01 10 1 2 27.58 0.53 10 1 3 27.09 0.48 10 1 4 69.22 1.01 10 1 5 1.00 0.19 10 1 6 41.72 0.82 10 1 7 30.07 0.54 10 1 8 6.01 0.37 10 1 9 45.74 1.01 10 1 10 4.88 0.41 10 1 11 11.57 0.54 10 1 12 10.28 0.75 10 1 13 0.92 0.47 10 1 14 15.44 0.94 10 2 0 5.23 0.20 10 2 1 5.17 0.20 10 2 2 0.85 0.12 10 2 3 4.42 0.19 10 2 4 0.12 0.16 10 2 5 6.45 0.32 10 2 6 2.70 0.23 10 2 7 4.93 0.34 10 2 8 12.26 0.43 10 2 9 0.00 0.21 10 2 10 4.83 0.35 10 2 11 0.46 0.33 10 2 12 0.32 0.40 10 2 13 1.63 0.50 10 2 14 0.01 0.43 10 3 1 21.04 0.36 10 3 2 2.39 0.14 10 3 3 10.25 0.27 10 3 4 7.94 0.31 10 3 5 0.04 0.18 10 3 6 0.16 0.16 10 3 7 0.67 0.21 10 3 8 0.63 0.25 10 3 9 3.88 0.34 10 3 10 0.90 0.25 10 3 11 1.97 0.34 10 3 12 1.21 0.46 10 3 13 0.21 0.44 10 3 14 1.83 0.55 10 4 0 43.16 0.84 10 4 1 7.56 0.23 10 4 2 28.28 0.43 10 4 3 73.90 0.98 10 4 4 0.02 0.15 10 4 5 69.17 0.96 10 4 6 20.04 0.44 10 4 7 14.49 0.53 10 4 8 34.48 0.87 10 4 9 0.17 0.23 10 4 10 36.73 0.84 10 4 11 13.83 0.61 10 4 12 5.95 0.53 10 4 13 24.41 1.08 10 4 14 1.65 0.53 10 5 1 87.98 1.04 10 5 2 66.58 0.89 10 5 3 17.32 0.39 10 5 4 148.61 1.74 10 5 5 7.47 0.29 10 5 6 70.69 1.02 10 5 7 42.62 0.85 10 5 8 10.32 0.66 10 5 9 51.97 1.04 10 5 10 4.30 0.33 10 5 11 29.92 0.93 10 5 12 25.81 0.93 10 5 13 0.39 0.48 10 5 14 22.39 1.51 10 6 0 65.70 1.06 10 6 1 7.91 0.43 10 6 2 35.94 0.68 10 6 3 56.71 0.80 10 6 4 2.38 0.38 10 6 5 65.53 0.95 10 6 6 8.97 0.50 10 6 7 28.07 0.85 10 6 8 38.35 0.84 10 6 9 0.02 0.26 10 6 10 22.42 0.64 10 6 11 9.71 0.57 10 6 12 4.07 0.52 10 6 13 12.78 0.72 10 7 1 12.53 0.29 10 7 2 1.90 0.18 10 7 3 3.66 0.24 10 7 4 2.24 0.18 10 7 5 0.80 0.18 10 7 6 4.81 0.37 10 7 7 5.07 0.31 10 7 8 0.38 0.24 10 7 9 3.81 0.41 10 7 10 0.24 0.32 10 7 11 1.74 0.38 10 7 12 0.86 0.36 10 7 13 0.16 0.38 10 8 0 2.69 0.26 10 8 1 1.96 0.16 10 8 2 0.45 0.15 10 8 3 4.64 0.30 10 8 4 0.02 0.12 10 8 5 10.46 0.41 10 8 6 1.18 0.20 10 8 7 3.58 0.30 10 8 8 3.45 0.34 10 8 9 0.00 0.29 10 8 10 1.98 0.38 10 8 11 0.84 0.34 10 8 12 0.00 0.33 10 8 13 0.42 0.36 10 9 1 42.39 0.70 10 9 2 24.14 0.50 10 9 3 10.31 0.39 10 9 4 50.09 0.87 10 9 5 2.81 0.27 10 9 6 25.79 0.87 10 9 7 24.35 0.63 10 9 8 1.03 0.28 10 9 9 28.38 1.12 10 9 10 2.08 0.50 10 9 11 10.85 0.64 10 9 12 12.95 0.97 10 9 13 0.45 0.40 10 10 0 87.82 1.76 10 10 1 7.68 0.36 10 10 2 64.16 1.11 10 10 3 66.28 1.08 10 10 4 0.79 0.25 10 10 5 57.37 1.14 10 10 6 11.87 0.54 10 10 7 20.41 0.90 10 10 8 44.37 1.03 10 10 9 0.33 0.32 10 10 10 32.37 1.16 10 10 11 13.04 0.82 10 10 12 5.76 0.55 10 11 1 82.11 1.34 10 11 2 19.88 0.52 10 11 3 18.47 0.95 10 11 4 26.37 0.61 10 11 5 0.01 0.24 10 11 6 22.23 1.10 10 11 7 12.01 0.55 10 11 8 3.65 0.50 10 11 9 22.86 0.85 10 11 10 0.52 0.40 10 11 11 10.62 0.77 10 11 12 10.31 0.66 10 12 0 4.86 0.50 10 12 1 2.54 0.25 10 12 2 1.67 0.29 10 12 3 5.81 0.41 10 12 4 0.14 0.19 10 12 5 4.76 0.36 10 12 6 2.16 0.31 10 12 7 1.93 0.31 10 12 8 1.54 0.33 10 12 9 0.48 0.39 10 12 10 2.27 0.58 10 12 11 0.00 0.42 10 12 12 1.70 0.55 10 13 1 11.52 0.41 10 13 2 2.47 0.29 10 13 3 0.71 0.22 10 13 4 1.40 0.24 10 13 5 0.48 0.25 10 13 6 1.29 0.30 10 13 7 0.57 0.29 10 13 8 0.00 0.26 10 13 9 1.10 0.43 10 13 10 1.74 0.56 10 13 11 0.01 0.47 10 14 0 16.54 0.78 10 14 1 2.16 0.27 10 14 2 14.28 0.51 10 14 3 28.85 0.87 10 14 4 0.11 0.22 10 14 5 27.40 1.00 10 14 6 4.08 0.39 10 14 7 10.41 0.54 10 14 8 21.68 0.91 10 14 9 0.16 0.34 10 14 10 9.97 0.94 10 15 1 35.59 0.93 10 15 2 16.92 0.74 10 15 3 9.90 0.45 10 15 4 43.42 0.92 10 15 5 0.81 0.30 10 15 6 27.03 0.81 10 15 7 28.41 0.86 10 15 8 2.75 0.44 10 15 9 31.77 1.20 10 15 10 4.16 0.67 10 16 0 28.59 1.10 10 16 1 3.42 0.35 10 16 2 11.87 0.63 10 16 3 18.70 0.61 10 16 4 0.51 0.29 10 16 5 23.53 0.75 10 16 6 5.04 0.43 10 16 7 10.24 0.56 10 16 8 14.85 0.75 10 16 9 0.31 0.44 10 17 1 3.43 0.34 10 17 2 0.51 0.26 10 17 3 1.94 0.39 10 17 4 2.81 0.32 10 17 5 0.50 0.30 10 17 6 2.08 0.35 10 17 7 0.01 0.29 10 17 8 1.55 0.51 10 18 0 1.28 0.40 10 18 1 0.44 0.26 10 18 2 0.29 0.27 10 18 3 1.16 0.27 10 18 4 0.02 0.24 10 18 5 2.04 0.36 10 18 6 0.00 0.30 10 18 7 0.68 0.33 10 19 1 12.73 0.60 10 19 2 7.40 0.47 10 19 3 2.02 0.34 10 19 4 15.51 0.61 10 19 5 0.86 0.34 10 19 6 8.55 0.63 10 20 0 26.86 1.22 10 20 1 2.72 0.37 10 20 2 15.49 0.67 10 20 3 14.54 0.64 10 20 4 0.26 0.31 10 20 5 17.59 1.01 10 21 1 16.14 0.69 10 21 2 2.67 0.37 10 21 3 7.81 1.06 11 0 1 136.15 2.01 11 0 2 62.49 1.19 11 0 3 30.21 0.92 11 0 4 97.07 1.80 11 0 5 0.33 0.26 11 0 6 70.72 1.50 11 0 7 44.52 1.54 11 0 8 5.05 0.85 11 0 9 48.56 1.48 11 0 10 5.47 0.59 11 0 11 20.66 1.07 11 0 12 25.11 1.43 11 0 13 0.53 0.61 11 1 0 68.46 1.16 11 1 1 11.28 0.32 11 1 2 45.11 0.61 11 1 3 27.27 0.52 11 1 4 5.95 0.33 11 1 5 72.72 1.02 11 1 6 20.82 0.56 11 1 7 14.11 0.49 11 1 8 37.54 0.93 11 1 9 0.23 0.37 11 1 10 30.37 0.83 11 1 11 9.21 0.52 11 1 12 2.35 0.50 11 1 13 16.12 0.89 11 2 1 1.47 0.14 11 2 2 0.08 0.11 11 2 3 1.93 0.15 11 2 4 5.90 0.31 11 2 5 0.89 0.17 11 2 6 8.95 0.32 11 2 7 10.37 0.45 11 2 8 0.00 0.23 11 2 9 4.17 0.39 11 2 10 0.02 0.27 11 2 11 1.32 0.32 11 2 12 1.34 0.44 11 2 13 0.00 0.42 11 3 0 15.74 0.47 11 3 1 0.37 0.12 11 3 2 5.10 0.21 11 3 3 3.46 0.18 11 3 4 0.65 0.15 11 3 5 2.82 0.24 11 3 6 2.48 0.25 11 3 7 0.86 0.24 11 3 8 3.62 0.33 11 3 9 0.01 0.24 11 3 10 2.81 0.35 11 3 11 1.57 0.45 11 3 12 0.35 0.44 11 3 13 2.10 0.53 11 4 1 45.87 0.68 11 4 2 24.83 0.46 11 4 3 11.89 0.34 11 4 4 63.78 0.93 11 4 5 4.59 0.30 11 4 6 23.94 0.58 11 4 7 29.89 0.71 11 4 8 3.70 0.37 11 4 9 30.81 0.73 11 4 10 4.77 0.42 11 4 11 15.87 0.73 11 4 12 14.41 0.85 11 4 13 0.31 0.45 11 5 0 95.87 1.76 11 5 1 14.64 0.33 11 5 2 48.64 0.76 11 5 3 84.81 1.14 11 5 4 6.05 0.24 11 5 5 94.93 1.23 11 5 6 16.69 0.47 11 5 7 29.67 0.69 11 5 8 56.62 1.16 11 5 9 0.33 0.28 11 5 10 38.32 0.89 11 5 11 17.26 0.80 11 5 12 5.67 0.60 11 5 13 20.79 1.57 11 6 1 49.61 0.94 11 6 2 28.68 0.50 11 6 3 16.38 0.63 11 6 4 75.10 1.07 11 6 5 1.49 0.23 11 6 6 26.48 0.64 11 6 7 17.09 0.51 11 6 8 5.70 0.50 11 6 9 23.88 0.70 11 6 10 1.18 0.27 11 6 11 17.25 0.75 11 6 12 11.45 0.76 11 6 13 0.02 0.43 11 7 0 9.89 0.61 11 7 1 0.02 0.14 11 7 2 4.61 0.29 11 7 3 3.40 0.22 11 7 4 0.28 0.18 11 7 5 5.16 0.31 11 7 6 4.56 0.40 11 7 7 0.11 0.22 11 7 8 0.99 0.29 11 7 9 0.51 0.29 11 7 10 4.69 0.44 11 7 11 1.25 0.34 11 7 12 1.23 0.39 11 7 13 1.66 0.51 11 8 1 4.74 0.25 11 8 2 8.16 0.31 11 8 3 0.31 0.16 11 8 4 4.64 0.26 11 8 5 0.01 0.19 11 8 6 2.14 0.26 11 8 7 1.17 0.26 11 8 8 0.00 0.25 11 8 9 2.39 0.39 11 8 10 0.02 0.32 11 8 11 0.54 0.32 11 8 12 0.57 0.34 11 9 0 46.04 1.16 11 9 1 6.29 0.28 11 9 2 25.72 0.54 11 9 3 29.18 0.59 11 9 4 0.01 0.17 11 9 5 26.05 0.66 11 9 6 7.95 0.44 11 9 7 10.92 0.58 11 9 8 31.25 0.93 11 9 9 0.00 0.30 11 9 10 19.16 0.98 11 9 11 8.23 0.56 11 9 12 3.33 0.43 11 10 1 78.90 1.28 11 10 2 33.17 0.71 11 10 3 11.40 0.55 11 10 4 45.20 0.91 11 10 5 1.15 0.26 11 10 6 43.12 0.97 11 10 7 32.39 0.86 11 10 8 1.99 0.37 11 10 9 35.02 1.17 11 10 10 2.85 0.57 11 10 11 14.47 1.00 11 10 12 22.57 0.90 11 11 0 52.63 1.46 11 11 1 4.52 0.56 11 11 2 35.82 1.03 11 11 3 26.91 0.68 11 11 4 2.41 0.30 11 11 5 35.25 0.88 11 11 6 6.48 0.41 11 11 7 9.96 0.86 11 11 8 16.07 0.70 11 11 9 0.36 0.41 11 11 10 17.99 1.62 11 11 11 4.14 0.69 11 12 1 2.62 0.26 11 12 2 2.93 0.30 11 12 3 0.41 0.22 11 12 4 3.74 0.39 11 12 5 0.01 0.23 11 12 6 4.70 0.39 11 12 7 0.45 0.28 11 12 8 0.59 0.32 11 12 9 1.88 0.47 11 12 10 0.09 0.49 11 12 11 1.70 0.57 11 13 0 2.54 0.44 11 13 1 0.02 0.21 11 13 2 3.12 0.47 11 13 3 1.36 0.24 11 13 4 1.80 0.26 11 13 5 3.73 0.36 11 13 6 0.08 0.26 11 13 7 1.23 0.30 11 13 8 2.43 0.42 11 13 9 0.00 0.37 11 13 10 0.47 0.53 11 14 1 21.85 0.67 11 14 2 11.55 0.46 11 14 3 4.23 0.39 11 14 4 21.54 0.72 11 14 5 0.02 0.26 11 14 6 14.06 0.61 11 14 7 12.90 0.60 11 14 8 0.36 0.31 11 14 9 12.65 0.81 11 14 10 3.08 0.65 11 15 0 42.37 1.58 11 15 1 4.86 0.38 11 15 2 17.59 0.63 11 15 3 30.38 0.81 11 15 4 0.00 0.24 11 15 5 28.85 0.85 11 15 6 8.23 0.50 11 15 7 12.36 0.62 11 15 8 29.45 0.88 11 15 9 0.30 0.43 11 16 1 17.18 1.05 11 16 2 8.19 0.46 11 16 3 5.49 0.53 11 16 4 26.72 0.77 11 16 5 0.07 0.30 11 16 6 14.88 0.67 11 16 7 7.15 0.50 11 16 8 3.51 0.52 11 17 0 5.99 0.74 11 17 1 0.19 0.26 11 17 2 2.57 0.34 11 17 3 2.52 0.34 11 17 4 1.26 0.44 11 17 5 2.05 0.36 11 17 6 0.00 0.30 11 17 7 2.07 0.38 11 18 1 1.46 0.30 11 18 2 1.51 0.32 11 18 3 0.41 0.28 11 18 4 2.60 0.36 11 18 5 0.28 0.32 11 18 6 0.33 0.33 11 19 0 12.63 1.01 11 19 1 1.59 0.33 11 19 2 8.02 0.50 11 19 3 9.80 0.66 11 19 4 0.15 0.29 11 19 5 12.01 0.63 11 20 1 19.80 0.80 11 20 2 7.01 0.51 11 20 3 4.70 0.49 12 0 0 90.36 1.91 12 0 1 6.68 0.73 12 0 2 103.16 2.05 12 0 3 59.31 1.32 12 0 4 6.98 0.65 12 0 5 75.61 1.79 12 0 6 15.96 0.63 12 0 7 23.02 1.31 12 0 8 57.68 2.32 12 0 9 0.28 0.39 12 0 10 34.34 1.43 12 0 11 17.27 0.97 12 0 12 3.47 0.72 12 0 13 20.57 1.55 12 1 1 48.57 0.64 12 1 2 22.66 0.51 12 1 3 11.46 0.38 12 1 4 44.99 0.82 12 1 5 4.09 0.28 12 1 6 34.90 0.74 12 1 7 25.93 1.03 12 1 8 5.04 0.35 12 1 9 33.98 0.88 12 1 10 2.06 0.35 12 1 11 9.64 0.53 12 1 12 10.51 0.76 12 1 13 0.92 0.63 12 2 0 4.58 0.28 12 2 1 2.39 0.18 12 2 2 2.02 0.18 12 2 3 2.13 0.18 12 2 4 0.06 0.17 12 2 5 7.77 0.36 12 2 6 2.54 0.25 12 2 7 1.17 0.25 12 2 8 2.90 0.32 12 2 9 0.15 0.27 12 2 10 4.43 0.41 12 2 11 0.88 0.32 12 2 12 0.04 0.41 12 2 13 1.12 0.50 12 3 1 2.85 0.20 12 3 2 3.68 0.21 12 3 3 0.00 0.15 12 3 4 4.72 0.29 12 3 5 0.11 0.17 12 3 6 3.80 0.26 12 3 7 5.77 0.35 12 3 8 1.57 0.29 12 3 9 2.98 0.38 12 3 10 1.16 0.31 12 3 11 1.18 0.34 12 3 12 0.36 0.44 12 3 13 0.00 0.43 12 4 0 61.00 1.17 12 4 1 5.97 0.27 12 4 2 23.83 0.49 12 4 3 35.92 0.65 12 4 4 0.56 0.21 12 4 5 30.71 0.65 12 4 6 9.78 0.37 12 4 7 18.89 0.57 12 4 8 33.12 0.96 12 4 9 0.44 0.28 12 4 10 19.78 0.72 12 4 11 10.07 0.62 12 4 12 5.47 0.62 12 4 13 14.08 0.89 12 5 1 99.04 1.28 12 5 2 35.64 0.66 12 5 3 26.46 0.61 12 5 4 77.15 1.19 12 5 5 0.58 0.21 12 5 6 34.50 0.70 12 5 7 33.46 0.78 12 5 8 4.40 0.39 12 5 9 34.63 0.89 12 5 10 4.16 0.41 12 5 11 21.04 0.87 12 5 12 20.10 0.97 12 6 0 66.42 1.42 12 6 1 6.64 0.35 12 6 2 28.22 0.86 12 6 3 32.32 0.62 12 6 4 6.92 0.36 12 6 5 43.00 0.86 12 6 6 7.84 0.50 12 6 7 12.38 0.62 12 6 8 24.42 0.76 12 6 9 0.04 0.27 12 6 10 19.96 0.71 12 6 11 6.93 0.65 12 6 12 3.99 0.71 12 7 1 0.81 0.16 12 7 2 0.58 0.17 12 7 3 0.26 0.16 12 7 4 8.90 0.32 12 7 5 1.03 0.21 12 7 6 3.67 0.31 12 7 7 2.94 0.40 12 7 8 1.62 0.33 12 7 9 2.81 0.35 12 7 10 0.98 0.36 12 7 11 0.61 0.42 12 7 12 0.58 0.46 12 8 0 5.80 0.55 12 8 1 0.35 0.16 12 8 2 6.50 0.29 12 8 3 1.38 0.19 12 8 4 0.02 0.16 12 8 5 1.57 0.25 12 8 6 0.02 0.23 12 8 7 1.99 0.31 12 8 8 4.02 0.45 12 8 9 0.03 0.32 12 8 10 0.87 0.37 12 8 11 0.83 0.55 12 8 12 0.00 0.47 12 9 1 30.47 0.65 12 9 2 13.19 0.41 12 9 3 6.47 0.31 12 9 4 29.37 0.63 12 9 5 3.83 0.34 12 9 6 18.27 0.79 12 9 7 17.90 0.71 12 9 8 0.95 0.39 12 9 9 21.27 1.42 12 9 10 2.23 0.43 12 9 11 6.13 0.54 12 10 0 46.07 1.17 12 10 1 3.45 0.29 12 10 2 48.46 0.89 12 10 3 46.38 0.83 12 10 4 0.00 0.20 12 10 5 43.49 0.99 12 10 6 11.00 0.53 12 10 7 13.30 0.66 12 10 8 29.22 1.06 12 10 9 0.27 0.39 12 10 10 26.61 1.09 12 10 11 11.56 0.93 12 11 1 31.43 0.79 12 11 2 17.83 0.63 12 11 3 7.34 0.68 12 11 4 34.24 0.74 12 11 5 1.59 0.31 12 11 6 19.54 0.68 12 11 7 7.13 0.52 12 11 8 6.96 0.52 12 11 9 24.42 1.04 12 11 10 1.50 0.55 12 11 11 5.54 0.77 12 12 0 4.99 0.53 12 12 1 0.94 0.27 12 12 2 3.04 0.31 12 12 3 2.99 0.28 12 12 4 0.17 0.22 12 12 5 2.56 0.34 12 12 6 0.00 0.26 12 12 7 0.96 0.35 12 12 8 1.13 0.37 12 12 9 0.00 0.38 12 12 10 2.02 0.60 12 13 1 3.33 0.31 12 13 2 2.12 0.31 12 13 3 0.50 0.23 12 13 4 3.14 0.31 12 13 5 0.48 0.27 12 13 6 0.00 0.27 12 13 7 0.62 0.34 12 13 8 0.20 0.34 12 13 9 0.12 0.43 12 13 10 0.01 0.48 12 14 0 18.49 0.90 12 14 1 0.45 0.26 12 14 2 17.05 0.61 12 14 3 16.95 0.69 12 14 4 0.31 0.25 12 14 5 15.92 0.65 12 14 6 3.78 0.43 12 14 7 4.72 0.49 12 14 8 13.92 0.73 12 14 9 0.52 0.44 12 15 1 23.71 0.87 12 15 2 10.47 0.52 12 15 3 6.62 0.67 12 15 4 36.25 0.87 12 15 5 1.01 0.33 12 15 6 21.48 0.76 12 15 7 16.60 0.71 12 15 8 1.58 0.41 12 16 0 27.14 1.15 12 16 1 3.49 0.35 12 16 2 11.44 1.01 12 16 3 16.85 0.67 12 16 4 1.35 0.32 12 16 5 15.27 0.67 12 16 6 1.40 0.35 12 16 7 8.83 0.54 12 17 1 3.32 0.37 12 17 2 1.35 0.32 12 17 3 0.64 0.29 12 17 4 0.91 0.32 12 17 5 0.65 0.36 12 17 6 1.69 0.37 12 18 0 3.17 0.51 12 18 1 0.50 0.30 12 18 2 1.42 0.34 12 18 3 0.33 0.29 12 18 4 0.40 0.30 12 18 5 1.40 0.37 12 19 1 12.98 0.70 12 19 2 5.17 0.44 12 19 3 3.00 0.40 13 0 1 99.99 2.02 13 0 2 40.81 1.85 13 0 3 18.48 0.82 13 0 4 51.87 1.20 13 0 5 2.73 0.38 13 0 6 40.11 1.11 13 0 7 26.42 1.11 13 0 8 3.93 0.99 13 0 9 40.37 1.36 13 0 10 2.42 0.49 13 0 11 19.83 1.07 13 0 12 22.63 1.47 13 1 0 32.16 0.93 13 1 1 8.34 0.40 13 1 2 21.78 0.56 13 1 3 33.49 0.74 13 1 4 0.08 0.18 13 1 5 45.20 0.80 13 1 6 10.66 0.43 13 1 7 13.73 0.61 13 1 8 24.57 0.76 13 1 9 0.11 0.28 13 1 10 21.35 0.73 13 1 11 6.55 0.72 13 1 12 3.03 0.55 13 2 1 2.50 0.23 13 2 2 1.79 0.22 13 2 3 2.23 0.24 13 2 4 4.51 0.33 13 2 5 0.83 0.20 13 2 6 4.36 0.28 13 2 7 0.77 0.27 13 2 8 0.24 0.26 13 2 9 3.89 0.40 13 2 10 0.01 0.29 13 2 11 0.57 0.32 13 2 12 1.29 0.45 13 3 0 0.01 0.18 13 3 1 0.06 0.15 13 3 2 0.01 0.15 13 3 3 6.32 0.34 13 3 4 0.01 0.18 13 3 5 7.89 0.40 13 3 6 3.36 0.29 13 3 7 2.23 0.33 13 3 8 2.16 0.32 13 3 9 0.00 0.26 13 3 10 3.44 0.38 13 3 11 1.88 0.37 13 3 12 0.33 0.44 13 4 1 36.38 0.66 13 4 2 17.36 0.42 13 4 3 5.73 0.28 13 4 4 36.49 0.81 13 4 5 0.00 0.20 13 4 6 28.12 0.71 13 4 7 25.74 0.76 13 4 8 1.86 0.33 13 4 9 16.00 0.63 13 4 10 3.05 0.39 13 4 11 11.21 0.65 13 4 12 7.42 0.68 13 5 0 104.88 2.14 13 5 1 6.74 0.29 13 5 2 46.35 0.77 13 5 3 41.33 0.71 13 5 4 5.01 0.33 13 5 5 47.83 0.96 13 5 6 7.92 0.47 13 5 7 24.28 0.81 13 5 8 39.36 1.06 13 5 9 0.23 0.33 13 5 10 23.21 0.79 13 5 11 13.67 0.72 13 5 12 3.19 0.53 13 6 1 51.65 0.85 13 6 2 15.91 0.61 13 6 3 9.46 0.34 13 6 4 32.43 0.67 13 6 5 0.04 0.25 13 6 6 19.15 0.74 13 6 7 15.52 0.80 13 6 8 4.09 0.42 13 6 9 19.03 0.96 13 6 10 2.18 0.42 13 6 11 8.54 1.11 13 6 12 8.88 1.54 13 7 0 2.27 0.35 13 7 1 1.58 0.21 13 7 2 0.00 0.16 13 7 3 5.79 0.28 13 7 4 0.03 0.18 13 7 5 4.07 0.34 13 7 6 1.52 0.29 13 7 7 1.92 0.32 13 7 8 2.41 0.39 13 7 9 0.00 0.31 13 7 10 2.36 0.48 13 7 11 0.48 0.48 13 8 1 6.28 0.31 13 8 2 0.22 0.18 13 8 3 3.42 0.26 13 8 4 3.73 0.25 13 8 5 0.96 0.23 13 8 6 0.66 0.26 13 8 7 0.14 0.25 13 8 8 0.01 0.29 13 8 9 0.49 0.41 13 8 10 0.03 0.44 13 8 11 0.36 0.51 13 9 0 22.97 0.82 13 9 1 5.17 0.31 13 9 2 13.16 0.41 13 9 3 16.95 0.45 13 9 4 0.01 0.17 13 9 5 30.66 0.83 13 9 6 7.06 0.47 13 9 7 7.45 0.45 13 9 8 18.82 0.80 13 9 9 0.00 0.34 13 9 10 12.45 0.76 13 9 11 5.42 0.69 13 10 1 40.02 0.80 13 10 2 21.81 0.61 13 10 3 9.25 0.40 13 10 4 41.98 0.84 13 10 5 1.74 0.33 13 10 6 30.94 0.93 13 10 7 21.05 0.83 13 10 8 2.94 0.51 13 10 9 35.31 1.09 13 10 10 3.95 0.53 13 11 0 26.46 1.03 13 11 1 5.77 0.39 13 11 2 13.28 0.95 13 11 3 14.84 0.64 13 11 4 1.23 0.28 13 11 5 34.24 0.90 13 11 6 7.06 0.53 13 11 7 8.00 0.70 13 11 8 14.32 0.83 13 11 9 0.50 0.43 13 11 10 11.22 0.91 13 12 1 5.09 0.36 13 12 2 0.77 0.27 13 12 3 3.07 0.33 13 12 4 1.17 0.26 13 12 5 0.54 0.30 13 12 6 2.25 0.39 13 12 7 0.56 0.34 13 12 8 0.03 0.39 13 12 9 1.73 0.48 13 13 0 1.18 0.40 13 13 1 0.27 0.25 13 13 2 0.19 0.25 13 13 3 1.82 0.29 13 13 4 0.06 0.24 13 13 5 4.02 0.40 13 13 6 1.53 0.37 13 13 7 0.03 0.33 13 13 8 0.24 0.57 13 13 9 0.00 0.42 13 14 1 19.23 0.68 13 14 2 6.49 0.44 13 14 3 3.76 0.38 13 14 4 15.27 0.77 13 14 5 0.14 0.30 13 14 6 7.91 0.56 13 14 7 8.82 0.60 13 14 8 0.34 0.43 13 15 0 32.66 1.24 13 15 1 4.07 0.39 13 15 2 11.42 0.73 13 15 3 23.26 0.75 13 15 4 0.27 0.30 13 15 5 24.64 0.90 13 15 6 7.21 0.51 13 15 7 5.64 0.53 13 16 1 19.87 0.70 13 16 2 5.68 0.44 13 16 3 7.49 0.49 13 16 4 16.22 0.66 13 16 5 0.16 0.35 13 16 6 8.63 0.56 13 17 0 3.01 0.49 13 17 1 0.70 0.32 13 17 2 2.02 0.35 13 17 3 1.86 0.44 13 17 4 0.76 0.32 13 17 5 1.04 0.39 13 18 1 3.07 0.38 13 18 2 1.06 0.33 13 18 3 0.60 0.32 14 0 0 39.97 1.62 14 0 1 3.93 0.54 14 0 2 52.29 1.57 14 0 3 56.35 1.63 14 0 4 0.20 0.51 14 0 5 52.84 1.35 14 0 6 10.69 0.63 14 0 7 16.39 0.83 14 0 8 36.27 1.28 14 0 9 0.43 0.41 14 0 10 26.99 1.22 14 0 11 8.19 1.35 14 1 1 26.57 0.73 14 1 2 20.93 0.63 14 1 3 7.12 0.41 14 1 4 36.59 0.80 14 1 5 4.11 0.33 14 1 6 21.46 0.64 14 1 7 9.43 0.47 14 1 8 2.88 0.33 14 1 9 23.67 0.77 14 1 10 0.76 0.33 14 1 11 8.35 0.53 14 2 0 8.80 1.39 14 2 1 3.25 0.35 14 2 2 2.68 0.30 14 2 3 2.11 0.25 14 2 4 0.02 0.18 14 2 5 2.02 0.28 14 2 6 0.00 0.22 14 2 7 1.20 0.33 14 2 8 2.67 0.34 14 2 9 0.01 0.27 14 2 10 0.50 0.32 14 2 11 0.10 0.31 14 3 1 0.42 0.19 14 3 2 1.41 0.23 14 3 3 0.01 0.19 14 3 4 7.72 0.41 14 3 5 0.02 0.21 14 3 6 0.72 0.27 14 3 7 1.93 0.36 14 3 8 1.04 0.34 14 3 9 3.96 0.47 14 3 10 2.68 0.42 14 3 11 0.36 0.32 14 4 0 29.10 0.86 14 4 1 1.86 0.26 14 4 2 19.13 0.57 14 4 3 32.76 0.75 14 4 4 0.86 0.24 14 4 5 24.73 0.72 14 4 6 5.52 0.40 14 4 7 9.68 0.56 14 4 8 19.60 0.79 14 4 9 0.00 0.32 14 4 10 17.51 0.80 14 4 11 6.25 0.53 14 5 1 60.50 1.55 14 5 2 20.89 0.57 14 5 3 11.66 0.48 14 5 4 56.42 1.05 14 5 5 0.57 0.24 14 5 6 30.77 0.84 14 5 7 22.07 0.81 14 5 8 4.31 0.46 14 5 9 21.13 0.83 14 5 10 3.95 0.47 14 5 11 12.19 0.81 14 6 0 40.76 1.09 14 6 1 2.37 0.25 14 6 2 20.00 0.51 14 6 3 26.46 0.63 14 6 4 1.30 0.30 14 6 5 23.91 0.71 14 6 6 3.48 0.38 14 6 7 13.44 0.80 14 6 8 19.06 0.79 14 6 9 0.02 0.32 14 6 10 10.95 0.64 14 6 11 5.71 0.63 14 7 1 1.48 0.22 14 7 2 2.42 0.26 14 7 3 0.00 0.18 14 7 4 2.41 0.25 14 7 5 0.00 0.22 14 7 6 1.37 0.31 14 7 7 2.23 0.36 14 7 8 0.90 0.49 14 7 9 3.27 0.47 14 7 10 0.29 0.37 14 8 0 5.22 0.47 14 8 1 2.24 0.25 14 8 2 0.53 0.23 14 8 3 0.02 0.18 14 8 4 0.51 0.20 14 8 5 6.20 0.43 14 8 6 0.01 0.26 14 8 7 0.52 0.30 14 8 8 0.84 0.37 14 8 9 0.01 0.37 14 8 10 0.03 0.41 14 9 1 16.81 0.52 14 9 2 10.94 0.43 14 9 3 4.46 0.40 14 9 4 21.46 0.59 14 9 5 0.34 0.28 14 9 6 17.13 0.66 14 9 7 11.82 0.59 14 9 8 0.33 0.39 14 9 9 15.41 0.85 14 9 10 1.76 0.50 14 10 0 33.34 1.02 14 10 1 5.89 0.36 14 10 2 22.81 0.67 14 10 3 25.78 0.69 14 10 4 0.00 0.21 14 10 5 32.63 0.83 14 10 6 7.46 0.48 14 10 7 11.55 0.65 14 10 8 32.17 1.01 14 10 9 0.29 0.42 14 11 1 19.78 0.76 14 11 2 9.44 0.58 14 11 3 5.12 0.60 14 11 4 18.11 0.70 14 11 5 0.30 0.33 14 11 6 15.79 0.75 14 11 7 7.68 0.52 14 11 8 2.21 0.66 14 11 9 15.81 0.94 14 12 0 6.19 0.60 14 12 1 0.63 0.26 14 12 2 2.94 0.34 14 12 3 0.26 0.26 14 12 4 1.16 0.28 14 12 5 0.97 0.35 14 12 6 0.00 0.31 14 12 7 1.77 0.40 14 12 8 2.38 0.60 14 13 1 1.12 0.29 14 13 2 1.51 0.31 14 13 3 0.01 0.26 14 13 4 2.99 0.36 14 13 5 0.00 0.34 14 13 6 0.05 0.35 14 13 7 0.01 0.34 14 13 8 0.01 0.46 14 14 0 11.21 0.80 14 14 1 0.18 0.28 14 14 2 9.22 0.51 14 14 3 14.90 0.64 14 14 4 0.00 0.28 14 14 5 10.88 0.72 14 14 6 3.98 0.54 14 14 7 2.15 0.43 14 15 1 21.80 0.75 14 15 2 8.99 0.56 14 15 3 6.74 0.49 14 15 4 24.39 0.80 14 15 5 0.46 0.41 14 15 6 11.66 0.77 14 16 0 23.62 1.12 14 16 1 1.25 0.33 14 16 2 10.34 0.64 14 16 3 8.94 0.54 14 16 4 1.39 0.34 14 16 5 10.89 0.67 14 17 1 1.67 0.34 14 17 2 0.82 0.32 14 17 3 0.82 0.32 15 0 1 36.54 1.22 15 0 2 29.03 1.17 15 0 3 8.78 0.69 15 0 4 44.40 2.15 15 0 5 4.95 0.58 15 0 6 28.07 1.17 15 0 7 19.29 1.31 15 0 8 2.05 0.66 15 0 9 31.06 2.78 15 0 10 0.84 0.48 15 1 0 30.36 1.39 15 1 1 4.76 0.43 15 1 2 22.88 0.97 15 1 3 19.04 0.66 15 1 4 0.57 0.27 15 1 5 27.13 0.78 15 1 6 6.48 0.45 15 1 7 4.00 0.44 15 1 8 12.94 0.66 15 1 9 0.56 0.37 15 1 10 14.16 0.72 15 2 1 4.74 0.41 15 2 2 0.78 0.26 15 2 3 3.76 0.34 15 2 4 1.46 0.31 15 2 5 0.04 0.25 15 2 6 2.46 0.32 15 2 7 0.27 0.31 15 2 8 0.00 0.31 15 2 9 1.09 0.37 15 2 10 0.00 0.37 15 3 0 6.27 0.61 15 3 1 0.54 0.32 15 3 2 0.64 0.26 15 3 3 0.94 0.27 15 3 4 1.65 0.27 15 3 5 1.22 0.28 15 3 6 1.32 0.30 15 3 7 0.16 0.31 15 3 8 1.54 0.37 15 3 9 0.00 0.38 15 3 10 2.03 0.43 15 4 1 28.08 0.90 15 4 2 9.34 0.54 15 4 3 5.16 0.36 15 4 4 23.41 0.66 15 4 5 0.01 0.23 15 4 6 13.44 0.57 15 4 7 14.85 0.69 15 4 8 2.85 0.42 15 4 9 15.91 0.73 15 4 10 3.48 0.48 15 5 0 50.50 2.17 15 5 1 4.81 0.43 15 5 2 18.42 0.65 15 5 3 35.08 0.81 15 5 4 1.97 0.29 15 5 5 38.43 0.87 15 5 6 7.41 0.60 15 5 7 16.21 0.73 15 5 8 27.64 0.96 15 5 9 0.33 0.36 15 5 10 16.21 0.80 15 6 1 21.79 0.65 15 6 2 9.50 0.49 15 6 3 5.68 0.40 15 6 4 28.90 0.75 15 6 5 0.52 0.25 15 6 6 13.67 0.61 15 6 7 10.48 0.61 15 6 8 2.14 0.41 15 6 9 10.65 0.66 15 6 10 1.40 0.42 15 7 0 2.97 0.39 15 7 1 0.00 0.20 15 7 2 2.43 0.33 15 7 3 4.31 0.51 15 7 4 0.06 0.23 15 7 5 0.73 0.28 15 7 6 0.52 0.29 15 7 7 0.47 0.33 15 7 8 0.80 0.37 15 7 9 0.00 0.35 15 8 1 1.66 0.25 15 8 2 1.45 0.27 15 8 3 0.39 0.27 15 8 4 1.05 0.28 15 8 5 0.00 0.26 15 8 6 1.14 0.32 15 8 7 0.01 0.33 15 8 8 0.01 0.33 15 8 9 1.18 0.41 15 9 0 23.46 0.88 15 9 1 5.17 0.33 15 9 2 12.64 0.47 15 9 3 9.81 0.48 15 9 4 0.27 0.28 15 9 5 14.38 0.62 15 9 6 2.73 0.36 15 9 7 4.46 0.44 15 9 8 14.84 0.85 15 9 9 0.00 0.41 15 10 1 28.27 0.72 15 10 2 14.22 0.51 15 10 3 4.48 0.39 15 10 4 23.31 0.74 15 10 5 0.33 0.30 15 10 6 24.16 1.07 15 10 7 17.01 1.03 15 10 8 1.20 0.45 15 11 0 17.41 0.90 15 11 1 2.52 0.33 15 11 2 12.18 0.55 15 11 3 10.00 0.56 15 11 4 1.39 0.47 15 11 5 18.62 1.25 15 11 6 3.58 0.45 15 11 7 4.39 0.48 15 11 8 11.06 0.91 15 12 1 1.98 0.33 15 12 2 0.64 0.28 15 12 3 0.78 0.30 15 12 4 0.85 0.32 15 12 5 0.00 0.34 15 12 6 3.17 0.45 15 12 7 0.81 0.34 15 13 0 1.51 0.44 15 13 1 0.00 0.27 15 13 2 0.55 0.28 15 13 3 1.02 0.31 15 13 4 0.00 0.29 15 13 5 0.71 0.42 15 13 6 0.13 0.40 15 14 1 9.42 0.53 15 14 2 5.96 0.46 15 14 3 1.38 0.34 15 14 4 10.22 0.63 15 14 5 0.00 0.40 15 15 0 31.86 1.30 15 15 1 3.06 0.40 15 15 2 9.42 0.62 15 15 3 13.36 0.64 15 15 4 0.88 0.36 15 16 1 11.76 0.74 15 16 2 4.66 0.45 16 0 0 17.38 1.74 16 0 1 3.43 0.60 16 0 2 29.50 1.16 16 0 3 32.74 1.21 16 0 4 0.08 0.37 16 0 5 35.05 1.31 16 0 6 11.28 0.98 16 0 7 8.08 0.87 16 0 8 24.70 1.51 16 0 9 1.20 0.66 16 1 1 26.37 1.03 16 1 2 8.53 0.51 16 1 3 9.88 0.50 16 1 4 17.82 0.65 16 1 5 1.78 0.37 16 1 6 12.87 0.74 16 1 7 7.03 0.61 16 1 8 1.79 0.53 16 1 9 14.68 0.85 16 2 0 2.50 0.65 16 2 1 0.07 0.32 16 2 2 3.80 0.40 16 2 3 0.86 0.28 16 2 4 0.03 0.27 16 2 5 2.99 0.37 16 2 6 0.01 0.32 16 2 7 0.11 0.38 16 2 8 0.46 0.41 16 2 9 0.00 0.40 16 3 1 5.22 0.46 16 3 2 0.60 0.31 16 3 3 0.45 0.31 16 3 4 1.14 0.32 16 3 5 0.00 0.27 16 3 6 0.00 0.30 16 3 7 1.18 0.43 16 3 8 0.74 0.42 16 3 9 1.29 0.41 16 4 0 33.37 1.58 16 4 1 3.16 0.40 16 4 2 8.71 0.55 16 4 3 14.97 0.77 16 4 4 0.92 0.30 16 4 5 13.89 0.62 16 4 6 3.62 0.45 16 4 7 9.36 0.59 16 4 8 12.17 0.68 16 4 9 0.00 0.35 16 5 1 30.28 0.98 16 5 2 12.47 0.67 16 5 3 7.40 0.60 16 5 4 35.97 0.96 16 5 5 0.56 0.27 16 5 6 17.53 0.75 16 5 7 18.60 0.96 16 5 8 1.82 0.40 16 5 9 17.60 0.81 16 6 0 24.33 1.09 16 6 1 1.76 0.38 16 6 2 8.10 0.72 16 6 3 15.82 1.11 16 6 4 1.26 0.33 16 6 5 15.88 0.58 16 6 6 4.79 0.44 16 6 7 4.95 0.49 16 6 8 11.56 0.73 16 6 9 0.30 0.42 16 7 1 2.09 0.38 16 7 2 0.08 0.32 16 7 3 1.37 0.35 16 7 4 2.78 0.37 16 7 5 0.00 0.27 16 7 6 0.66 0.31 16 7 7 0.52 0.36 16 7 8 0.53 0.37 16 8 0 1.96 0.49 16 8 1 0.97 0.29 16 8 2 0.82 0.31 16 8 3 0.02 0.27 16 8 4 0.02 0.27 16 8 5 0.21 0.34 16 8 6 0.40 0.31 16 8 7 0.00 0.34 16 8 8 1.97 0.44 16 9 1 17.76 0.63 16 9 2 6.55 0.47 16 9 3 3.69 0.40 16 9 4 11.08 0.59 16 9 5 0.28 0.35 16 9 6 10.59 0.59 16 9 7 6.18 0.54 16 10 0 15.93 1.02 16 10 1 1.28 0.28 16 10 2 23.72 0.79 16 10 3 24.98 0.91 16 10 4 0.00 0.32 16 10 5 21.82 0.88 16 10 6 4.69 0.55 16 10 7 8.44 0.69 16 11 1 14.34 0.61 16 11 2 5.39 0.47 16 11 3 4.54 0.53 16 11 4 12.57 0.78 16 11 5 0.28 0.39 16 11 6 7.08 0.65 16 12 0 0.66 0.55 16 12 1 0.32 0.29 16 12 2 1.06 0.34 16 12 3 1.43 0.37 16 12 4 0.00 0.36 16 12 5 1.97 0.49 16 13 1 0.68 0.30 16 13 2 0.00 0.28 16 13 3 0.62 0.35 16 13 4 0.63 0.35 16 14 0 8.09 0.74 16 14 1 0.37 0.32 16 14 2 5.05 0.45 16 14 3 9.30 0.60 17 0 1 21.77 1.29 17 0 2 13.37 1.59 17 0 3 5.55 0.81 17 0 4 26.17 1.15 17 0 5 1.89 0.49 17 0 6 24.74 1.46 17 0 7 14.75 1.13 17 0 8 2.81 0.71 17 1 0 21.85 1.28 17 1 1 5.31 0.57 17 1 2 11.33 0.73 17 1 3 7.67 0.56 17 1 4 0.67 0.31 17 1 5 22.32 0.76 17 1 6 4.15 0.52 17 1 7 4.89 0.57 17 1 8 10.56 0.72 17 2 1 1.67 0.42 17 2 2 1.39 0.41 17 2 3 0.46 0.32 17 2 4 0.93 0.35 17 2 5 0.00 0.29 17 2 6 3.39 0.61 17 2 7 0.01 0.39 17 2 8 0.03 0.42 17 3 0 1.88 0.61 17 3 1 0.02 0.35 17 3 2 1.41 0.41 17 3 3 3.28 0.42 17 3 4 0.01 0.30 17 3 5 0.88 0.33 17 3 6 0.67 0.41 17 3 7 0.51 0.43 17 3 8 0.01 0.41 17 4 1 14.78 0.81 17 4 2 6.28 0.52 17 4 3 2.45 0.41 17 4 4 17.46 0.77 17 4 5 0.00 0.33 17 4 6 8.99 0.68 17 4 7 6.60 0.72 17 4 8 1.79 0.49 17 5 0 33.19 1.69 17 5 1 2.96 0.47 17 5 2 11.21 0.65 17 5 3 20.44 1.40 17 5 4 0.78 0.36 17 5 5 19.12 1.65 17 5 6 7.32 0.57 17 5 7 5.56 0.60 17 5 8 16.02 1.28 17 6 1 13.42 0.80 17 6 2 4.99 0.48 17 6 3 2.58 0.41 17 6 4 13.07 0.71 17 6 5 0.55 0.40 17 6 6 7.11 0.55 17 6 7 8.98 0.71 17 7 0 4.62 0.83 17 7 1 0.10 0.33 17 7 2 0.16 0.34 17 7 3 0.79 0.36 17 7 4 0.59 0.37 17 7 5 2.32 0.54 17 7 6 0.01 0.37 17 7 7 1.23 0.38 17 8 1 0.27 0.35 17 8 2 0.00 0.33 17 8 3 0.81 0.36 17 8 4 0.80 0.38 17 8 5 0.08 0.38 17 8 6 0.01 0.36 17 9 0 11.67 1.09 17 9 1 1.44 0.40 17 9 2 9.33 0.64 17 9 3 10.12 0.65 17 9 4 0.00 0.30 17 9 5 11.07 0.69 17 9 6 1.79 0.42 17 10 1 18.19 0.84 17 10 2 9.53 0.64 17 10 3 4.69 0.50 17 10 4 18.75 0.88 17 10 5 0.80 0.39 17 11 0 14.44 1.19 17 11 1 2.17 0.58 17 11 2 8.32 0.69 17 11 3 7.08 0.64 17 11 4 0.12 0.41 17 12 1 0.87 0.42 17 12 2 0.41 0.39 17 12 3 0.01 0.38 18 0 0 17.73 1.84 18 0 1 3.54 0.65 18 0 2 18.67 1.29 18 0 3 18.73 2.07 18 0 4 0.30 0.68 18 0 5 22.67 1.10 18 0 6 3.66 0.75 18 0 7 8.29 2.07 18 1 1 12.51 0.78 18 1 2 7.49 0.60 18 1 3 3.52 0.48 18 1 4 12.36 0.77 18 1 5 0.62 0.35 18 1 6 11.96 0.76 18 1 7 5.57 0.71 18 2 0 3.48 1.13 18 2 1 3.27 0.51 18 2 2 0.40 0.37 18 2 3 0.30 0.38 18 2 4 0.02 0.32 18 2 5 1.75 0.48 18 2 6 0.00 0.38 18 2 7 1.52 0.68 18 3 1 0.63 0.43 18 3 2 0.47 0.38 18 3 3 0.00 0.36 18 3 4 3.24 0.46 18 3 5 0.00 0.38 18 3 6 0.23 0.40 18 4 0 12.64 1.09 18 4 1 0.49 0.39 18 4 2 9.44 0.70 18 4 3 15.05 0.87 18 4 4 0.40 0.37 18 4 5 8.66 0.70 18 4 6 1.69 0.56 18 5 1 17.91 0.91 18 5 2 8.36 0.69 18 5 3 3.47 0.47 18 5 4 18.10 0.89 18 5 5 0.50 0.42 18 5 6 9.82 0.87 18 6 0 16.31 1.25 18 6 1 1.89 0.47 18 6 2 3.55 0.53 18 6 3 9.57 0.63 18 6 4 0.00 0.36 18 6 5 9.26 0.72 18 7 1 1.59 0.45 18 7 2 0.77 0.43 18 7 3 0.35 0.36 18 7 4 0.93 0.39 18 7 5 0.00 0.40 18 8 0 0.49 0.58 18 8 1 0.67 0.42 18 8 2 0.01 0.36 18 8 3 0.08 0.35 18 8 4 0.00 0.40 18 9 1 8.70 0.78 18 9 2 5.02 0.54 18 9 3 2.31 0.46 18 10 0 16.60 1.33 18 10 1 2.10 0.49 18 10 2 11.13 0.69 19 0 1 17.95 2.18 19 0 2 7.15 1.44 19 0 3 7.46 1.53 19 0 4 15.97 1.28 19 1 0 10.08 1.01 19 1 1 3.09 0.52 19 1 2 8.01 0.69 19 1 3 8.02 0.68 19 1 4 0.56 0.40 19 2 1 1.31 0.44 19 2 2 0.81 0.43 19 2 3 0.26 0.39 19 2 4 0.57 0.41 19 3 0 2.51 0.72 19 3 1 0.03 0.38 19 3 2 0.01 0.42 19 3 3 1.60 0.47 19 3 4 0.00 0.41 19 4 1 12.05 0.81 19 4 2 4.05 0.56 19 4 3 2.97 0.53 19 4 4 8.37 0.69 19 5 0 15.28 1.27 19 5 1 1.71 0.47 19 5 2 6.98 0.67 19 5 3 13.68 0.85 19 6 1 6.23 0.64 19 6 2 3.82 0.55 19 7 0 1.07 0.92 19 7 1 0.01 0.38 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 17373 _olex2_submission_special_instructions 'No special instructions were received'