data_007-14122 _vrf_RINTA01_007-14122 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: The crystal was of poor quality and small size. This was the best crystal in the sample submitted. The thin edge of the plate morphology produced very week diffraction which contributed to the large Rint value. ; _vrf_PLAT020_007-14122 ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.205 RESPONSE: See resonse to RINTA01 ; _publ_contact_author ; Prof. Scott J. Miller The Department of Chemistry Yale University P. O. Box 208107 New Haven Connecticut 06520 USA. ; _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. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H17 N O2' _chemical_formula_weight 231.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_H-M_alt 'F d d 2' _space_group_name_Hall 'F 2 -2d' _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, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 18.5530(7) _cell_length_b 50.228(4) _cell_length_c 5.1431(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4792.8(4) _cell_formula_units_Z 16 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8825 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 67.6 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.282 _exptl_crystal_F_000 1984 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.685 _shelx_estimated_absorpt_T_min 0.821 _shelx_estimated_absorpt_T_max 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; 'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD' ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_source 'Rotating Anode' _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 31682 _diffrn_reflns_av_unetI/netI 0.0976 _diffrn_reflns_av_R_equivalents 0.2047 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 60 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.520 _diffrn_reflns_theta_max 68.180 _diffrn_reflns_theta_full 67.687 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.955 _diffrn_reflns_point_group_measured_fraction_full 0.957 _reflns_number_total 2101 _reflns_number_gt 1420 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.729 _reflns_Friedel_fraction_max 0.916 _reflns_Friedel_fraction_full 0.922 _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 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: A complete structure solution, refinement and analysis program (2009). J. Appl. Cryst., 42, 339-341. ; _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms were first found in the difference map, then generated geometrically and refined as riding atoms with C-H distances = 0.95- 0.99 \%A and U~iso~(H) = 1.2 times U~eq~(C) for CH and CH2 groups and U~iso~(H) = 1.5 times U~eq~(C) for CH3 groups. Atom H8 is semi-freely refining. ; _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^)+(0.0893P)^2^+8.5014P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 430 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.1(5) _chemical_absolute_configuration unk _refine_ls_number_reflns 2101 _refine_ls_number_parameters 158 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2213 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.156 _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_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 C1 C -0.0588(4) -0.11204(12) 0.7903(15) 0.0543(17) Uani 1 1 d . . . . . C2 C -0.0960(4) -0.08528(12) 0.8181(15) 0.0535(17) Uani 1 1 d . . . . . H2 H -0.1104 -0.0833 1.0045 0.064 Uiso 1 1 calc R U . . . C3 C -0.0396(3) -0.06349(11) 0.7590(13) 0.0474(16) Uani 1 1 d . . . . . H3 H -0.0231 -0.0662 0.5758 0.057 Uiso 1 1 calc R U . . . C4 C 0.0262(4) -0.06591(12) 0.9328(14) 0.0526(17) Uani 1 1 d . . . . . H4A H 0.0120 -0.0630 1.1161 0.063 Uiso 1 1 calc R U . . . H4B H 0.0618 -0.0521 0.8852 0.063 Uiso 1 1 calc R U . . . C5 C 0.0604(4) -0.09350(12) 0.9041(16) 0.0591(19) Uani 1 1 d . . . . . H5A H 0.1010 -0.0952 1.0283 0.071 Uiso 1 1 calc R U . . . H5B H 0.0801 -0.0954 0.7262 0.071 Uiso 1 1 calc R U . . . C6 C 0.0060(4) -0.11588(13) 0.9547(17) 0.063(2) Uani 1 1 d . . . . . H6A H 0.0284 -0.1333 0.9146 0.075 Uiso 1 1 calc R U . . . H6B H -0.0080 -0.1159 1.1404 0.075 Uiso 1 1 calc R U . . . O7 O -0.0799(3) -0.12896(10) 0.6373(11) 0.0722(17) Uani 1 1 d . . . . . N8 N -0.0712(3) -0.03685(11) 0.7751(12) 0.0510(15) Uani 1 1 d . . . . . H8 H -0.080(4) -0.0310(14) 0.931(18) 0.061 Uiso 1 1 d . U . . . C9 C -0.0887(3) -0.02257(12) 0.5636(15) 0.0494(16) Uani 1 1 d . . . . . O10 O -0.0760(3) -0.03006(9) 0.3401(10) 0.0538(12) Uani 1 1 d . . . . . C11 C -0.1275(3) 0.00333(11) 0.6082(12) 0.0434(14) Uani 1 1 d . . . . . C12 C -0.1175(4) 0.02365(12) 0.4300(14) 0.0489(16) Uani 1 1 d . . . . . H12 H -0.0846 0.0213 0.2902 0.059 Uiso 1 1 calc R U . . . C13 C -0.1551(4) 0.04740(13) 0.4540(14) 0.0541(17) Uani 1 1 d . . . . . H13 H -0.1471 0.0614 0.3333 0.065 Uiso 1 1 calc R U . . . C14 C -0.2041(4) 0.05061(12) 0.6542(14) 0.0524(17) Uani 1 1 d . . . . . H14 H -0.2308 0.0667 0.6690 0.063 Uiso 1 1 calc R U . . . C15 C -0.2142(4) 0.03038(11) 0.8326(16) 0.0513(16) Uani 1 1 d . . . . . H15 H -0.2476 0.0326 0.9710 0.062 Uiso 1 1 calc R U . . . C16 C -0.1758(3) 0.00669(12) 0.8107(15) 0.0501(15) Uani 1 1 d . . . . . H16 H -0.1826 -0.0071 0.9344 0.060 Uiso 1 1 calc R U . . . C17 C -0.1637(4) -0.08324(14) 0.6565(16) 0.064(2) Uani 1 1 d . . . . . H17A H -0.1883 -0.0664 0.6955 0.096 Uiso 1 1 calc R U . . . H17B H -0.1957 -0.0982 0.6974 0.096 Uiso 1 1 calc R U . . . H17C H -0.1510 -0.0838 0.4716 0.096 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 C1 0.067(4) 0.046(3) 0.050(4) 0.001(3) 0.003(4) -0.003(3) C2 0.064(4) 0.046(3) 0.050(4) -0.002(3) -0.001(4) -0.002(3) C3 0.060(4) 0.041(3) 0.041(4) -0.003(3) -0.004(3) 0.007(3) C4 0.065(4) 0.047(3) 0.046(4) -0.002(3) -0.002(4) 0.004(3) C5 0.065(4) 0.055(4) 0.057(5) -0.007(3) -0.005(4) 0.009(3) C6 0.077(5) 0.051(4) 0.060(5) 0.002(3) 0.002(4) 0.006(3) O7 0.080(4) 0.055(3) 0.082(5) -0.015(3) -0.005(3) -0.009(2) N8 0.070(4) 0.043(3) 0.040(4) 0.001(2) 0.002(3) 0.007(2) C9 0.059(4) 0.049(3) 0.039(4) 0.000(3) -0.004(3) -0.005(3) O10 0.067(3) 0.056(2) 0.038(3) -0.006(2) 0.001(2) 0.006(2) C11 0.056(4) 0.039(3) 0.035(3) 0.001(3) 0.002(3) 0.000(2) C12 0.057(4) 0.048(3) 0.042(4) 0.004(3) 0.001(3) 0.002(3) C13 0.067(4) 0.051(4) 0.044(4) 0.006(3) 0.001(4) 0.001(3) C14 0.064(4) 0.043(3) 0.051(4) 0.000(3) -0.003(4) 0.003(3) C15 0.057(4) 0.046(3) 0.050(4) -0.001(3) 0.000(4) 0.002(3) C16 0.058(4) 0.050(3) 0.042(4) -0.001(3) 0.001(4) 0.000(3) C17 0.068(5) 0.062(4) 0.062(5) 0.000(4) -0.007(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O7 1.223(8) . ? C1 C6 1.483(11) . ? C1 C2 1.518(9) . ? C2 C17 1.509(10) . ? C2 C3 1.545(9) . ? C2 H2 1.0000 . ? C3 N8 1.463(7) . ? C3 C4 1.517(9) . ? C3 H3 1.0000 . ? C4 C5 1.532(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.534(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N8 C9 1.343(10) . ? N8 H8 0.87(9) . ? C9 O10 1.232(9) . ? C9 C11 1.504(8) . ? C11 C16 1.384(9) . ? C11 C12 1.384(8) . ? C12 C13 1.387(9) . ? C12 H12 0.9500 . ? C13 C14 1.384(9) . ? C13 H13 0.9500 . ? C14 C15 1.382(9) . ? C14 H14 0.9500 . ? C15 C16 1.392(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 C1 C6 122.4(6) . . ? O7 C1 C2 122.0(7) . . ? C6 C1 C2 115.5(6) . . ? C17 C2 C1 112.7(6) . . ? C17 C2 C3 114.0(5) . . ? C1 C2 C3 107.5(5) . . ? C17 C2 H2 107.4 . . ? C1 C2 H2 107.4 . . ? C3 C2 H2 107.4 . . ? N8 C3 C4 111.2(5) . . ? N8 C3 C2 111.4(5) . . ? C4 C3 C2 111.9(5) . . ? N8 C3 H3 107.4 . . ? C4 C3 H3 107.4 . . ? C2 C3 H3 107.4 . . ? C3 C4 C5 110.5(5) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 112.0(6) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C1 C6 C5 110.0(6) . . ? C1 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? C1 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C9 N8 C3 122.6(6) . . ? C9 N8 H8 121(5) . . ? C3 N8 H8 116(5) . . ? O10 C9 N8 123.1(6) . . ? O10 C9 C11 119.9(6) . . ? N8 C9 C11 117.0(6) . . ? C16 C11 C12 119.7(5) . . ? C16 C11 C9 122.0(5) . . ? C12 C11 C9 118.2(6) . . ? C11 C12 C13 120.5(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.8(6) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.4(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 119.8(6) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C2 C17 H17A 109.5 . . ? C2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 C1 C2 C17 4.9(9) . . . . ? C6 C1 C2 C17 -176.9(6) . . . . ? O7 C1 C2 C3 -121.6(7) . . . . ? C6 C1 C2 C3 56.5(8) . . . . ? C17 C2 C3 N8 52.9(8) . . . . ? C1 C2 C3 N8 178.7(6) . . . . ? C17 C2 C3 C4 178.1(6) . . . . ? C1 C2 C3 C4 -56.1(7) . . . . ? N8 C3 C4 C5 -177.5(6) . . . . ? C2 C3 C4 C5 57.2(7) . . . . ? C3 C4 C5 C6 -54.7(8) . . . . ? O7 C1 C6 C5 122.7(7) . . . . ? C2 C1 C6 C5 -55.4(8) . . . . ? C4 C5 C6 C1 52.8(8) . . . . ? C4 C3 N8 C9 131.4(6) . . . . ? C2 C3 N8 C9 -103.0(7) . . . . ? C3 N8 C9 O10 -4.1(10) . . . . ? C3 N8 C9 C11 174.0(5) . . . . ? O10 C9 C11 C16 144.5(6) . . . . ? N8 C9 C11 C16 -33.7(9) . . . . ? O10 C9 C11 C12 -31.3(9) . . . . ? N8 C9 C11 C12 150.5(6) . . . . ? C16 C11 C12 C13 0.4(9) . . . . ? C9 C11 C12 C13 176.4(6) . . . . ? C11 C12 C13 C14 -1.4(10) . . . . ? C12 C13 C14 C15 1.5(10) . . . . ? C13 C14 C15 C16 -0.6(10) . . . . ? C12 C11 C16 C15 0.5(9) . . . . ? C9 C11 C16 C15 -175.3(6) . . . . ? C14 C15 C16 C11 -0.4(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O10 0.87(9) 2.11(9) 2.927(8) 157(7) 1_556 _refine_diff_density_max 0.259 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.064 _shelxl_version_number 2013-4 _shelx_res_file ; TITL SMC-II-171F 007-14122 CELL 1.54187 18.553 50.2283 5.1431 90 90 90 ZERR 16 0.0007 0.0036 0.0002 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC C H N O UNIT 224 272 16 32 SIZE 0.3 0.2 0.02 TEMP -180 HTAB N8 O10_$1 EQIV $1 +X,+Y,1+Z L.S. 10 BOND $H CONF SHEL 20 0.83 ACTA WGHT 0.089300 8.501400 FVAR 0.21545 C1 1 -0.058827 -0.112038 0.790303 11.00000 0.06736 0.04564 = 0.04975 0.00106 0.00316 -0.00310 C2 1 -0.096019 -0.085280 0.818111 11.00000 0.06428 0.04638 = 0.04991 -0.00246 -0.00065 -0.00160 AFIX 13 H2 2 -0.110402 -0.083309 1.004505 11.00000 -1.20000 AFIX 0 C3 1 -0.039566 -0.063490 0.759019 11.00000 0.05952 0.04134 = 0.04120 -0.00284 -0.00399 0.00696 AFIX 13 H3 2 -0.023063 -0.066151 0.575754 11.00000 -1.20000 AFIX 0 C4 1 0.026190 -0.065909 0.932771 11.00000 0.06455 0.04687 = 0.04643 -0.00237 -0.00182 0.00361 AFIX 23 H4A 2 0.011953 -0.063022 1.116129 11.00000 -1.20000 H4B 2 0.061806 -0.052065 0.885166 11.00000 -1.20000 AFIX 0 C5 1 0.060439 -0.093497 0.904144 11.00000 0.06496 0.05480 = 0.05748 -0.00682 -0.00542 0.00867 AFIX 23 H5A 2 0.100972 -0.095154 1.028286 11.00000 -1.20000 H5B 2 0.080142 -0.095395 0.726220 11.00000 -1.20000 AFIX 0 C6 1 0.006009 -0.115884 0.954695 11.00000 0.07712 0.05081 = 0.05995 0.00224 0.00155 0.00591 AFIX 23 H6A 2 0.028384 -0.133300 0.914599 11.00000 -1.20000 H6B 2 -0.008036 -0.115874 1.140399 11.00000 -1.20000 AFIX 0 O7 4 -0.079946 -0.128961 0.637291 11.00000 0.07959 0.05501 = 0.08211 -0.01538 -0.00510 -0.00880 N8 3 -0.071159 -0.036855 0.775136 11.00000 0.07004 0.04263 = 0.04020 0.00112 0.00184 0.00690 H8 2 -0.079823 -0.030957 0.930955 11.00000 -1.20000 C9 1 -0.088661 -0.022570 0.563568 11.00000 0.05944 0.04928 = 0.03947 0.00039 -0.00428 -0.00527 O10 4 -0.075968 -0.030063 0.340145 11.00000 0.06749 0.05575 = 0.03823 -0.00577 0.00052 0.00568 C11 1 -0.127488 0.003326 0.608223 11.00000 0.05596 0.03882 = 0.03544 0.00054 0.00194 -0.00022 C12 1 -0.117462 0.023650 0.430007 11.00000 0.05708 0.04772 = 0.04204 0.00383 0.00090 0.00176 AFIX 43 H12 2 -0.084590 0.021316 0.290229 11.00000 -1.20000 AFIX 0 C13 1 -0.155062 0.047398 0.454018 11.00000 0.06696 0.05107 = 0.04425 0.00554 0.00143 0.00103 AFIX 43 H13 2 -0.147142 0.061415 0.333347 11.00000 -1.20000 AFIX 0 C14 1 -0.204141 0.050614 0.654239 11.00000 0.06365 0.04254 = 0.05110 -0.00006 -0.00313 0.00309 AFIX 43 H14 2 -0.230825 0.066686 0.669004 11.00000 -1.20000 AFIX 0 C15 1 -0.214215 0.030375 0.832624 11.00000 0.05700 0.04642 = 0.05037 -0.00089 0.00034 0.00249 AFIX 43 H15 2 -0.247575 0.032644 0.970990 11.00000 -1.20000 AFIX 0 C16 1 -0.175766 0.006689 0.810720 11.00000 0.05798 0.04972 = 0.04246 -0.00086 0.00079 0.00029 AFIX 43 H16 2 -0.182640 -0.007129 0.934387 11.00000 -1.20000 AFIX 0 C17 1 -0.163687 -0.083241 0.656478 11.00000 0.06848 0.06222 = 0.06151 -0.00034 -0.00687 -0.00488 AFIX 137 H17A 2 -0.188302 -0.066446 0.695477 11.00000 -1.50000 H17B 2 -0.195675 -0.098190 0.697443 11.00000 -1.50000 H17C 2 -0.151025 -0.083762 0.471558 11.00000 -1.50000 AFIX 0 HKLF 4 REM CMS-II-171F 007-14122 REM R1 = 0.0733 for 1420 Fo > 4sig(Fo) and 0.1070 for all 2101 data REM 158 parameters refined using 1 restraints END WGHT 0.0895 8.4668 REM Highest difference peak 0.259, deepest hole -0.341, 1-sigma level 0.064 Q1 1 -0.0631 -0.0518 0.1929 11.00000 0.05 0.26 Q2 1 -0.0636 -0.0190 0.9274 11.00000 0.05 0.23 Q3 1 -0.1686 0.0265 0.6252 11.00000 0.05 0.23 Q4 1 -0.0703 -0.0046 0.4389 11.00000 0.05 0.23 Q5 1 -0.1326 -0.0163 0.7650 11.00000 0.05 0.21 Q6 1 -0.0917 -0.1487 0.4520 11.00000 0.05 0.21 Q7 1 -0.0713 -0.1304 0.9274 11.00000 0.05 0.20 Q8 1 -0.0464 -0.0864 0.6204 11.00000 0.05 0.20 Q9 1 -0.1822 0.0602 0.2418 11.00000 0.05 0.20 Q10 1 -0.1598 0.0278 1.0100 11.00000 0.05 0.20 Q11 1 -0.0620 -0.0115 0.1831 11.00000 0.05 0.20 Q12 1 -0.0794 0.0250 0.0146 11.00000 0.05 0.19 Q13 1 -0.0516 -0.1450 0.4603 11.00000 0.05 0.19 Q14 1 -0.0780 -0.0315 1.0929 11.00000 0.05 0.19 Q15 1 0.0523 -0.1007 1.3390 11.00000 0.05 0.19 Q16 1 -0.1634 0.0682 0.0296 11.00000 0.05 0.18 Q17 1 -0.1039 0.0043 0.8738 11.00000 0.05 0.18 Q18 1 -0.0812 -0.0585 0.9372 11.00000 0.05 0.18 Q19 1 0.0195 -0.0609 0.5611 11.00000 0.05 0.18 Q20 1 -0.1024 -0.0849 1.0613 11.00000 0.05 0.18 ; _shelx_res_checksum 52866 _shelx_hkl_file ; 0 -4 0 512.62 79.00 0 4 0 384.81 62.11 0 4 0 655.28 97.53 0 4 0 467.99 73.72 0 4 0 603.94 90.42 0 -4 0 645.25 96.21 0 4 0 1113.92 168.23 0 -4 0 692.47 104.26 0 -4 0 591.32 87.75 0 -4 0 515.30 75.95 0 -4 0 629.71 94.00 2 0 0 -0.21 1.15 -2 0 0 0.75 1.05 -2 0 0 -0.24 2.30 2 0 0 0.70 1.48 2 0 0 0.46 2.16 2 0 0 0.99 2.51 2 0 0 -0.36 0.26 -2 0 0 0.12 1.60 -2 0 0 -0.28 2.20 2 0 0 -0.21 1.67 2 2 0 451.64 65.12 -2 -2 0 321.87 46.44 2 2 0 545.59 80.00 2 -2 0 439.33 64.13 2 2 0 323.38 51.05 -2 -2 0 526.68 77.27 -2 -2 0 469.14 69.72 2 2 0 400.25 58.45 -2 -2 0 464.12 68.36 -2 2 0 425.70 60.44 -2 2 0 402.24 56.32 2 -2 0 456.41 66.16 2 -2 0 328.42 49.27 -2 2 0 410.85 59.50 2 -2 0 399.22 61.28 -2 -2 0 425.98 58.61 -2 2 0 466.47 72.34 2 -2 0 366.16 52.26 -2 2 0 399.35 57.20 2 2 0 456.22 67.35 0 6 0 1.33 3.29 0 -6 0 0.26 1.75 0 -6 0 -1.25 1.48 0 6 0 0.12 3.16 0 6 0 1.06 2.04 0 -6 0 -0.11 1.78 0 -6 0 0.44 1.96 0 6 0 0.62 1.62 0 -6 0 0.65 1.98 -2 -4 0 262.34 33.61 2 4 0 227.47 30.86 2 4 0 181.16 26.57 -2 -4 0 196.48 26.54 2 4 0 239.08 36.34 -2 -4 0 208.16 28.19 -2 -4 0 272.48 35.31 2 4 0 292.34 41.50 -2 4 0 246.85 31.31 2 -4 0 278.88 42.53 -2 4 0 274.89 42.77 2 -4 0 237.54 36.18 -2 4 0 206.23 26.62 2 -4 0 222.31 28.47 -2 4 0 223.06 31.68 2 -4 0 224.97 28.09 2 4 0 235.84 31.53 0 -8 0 111.57 17.11 0 -8 0 92.58 14.28 0 8 0 77.92 13.74 0 -8 0 109.75 15.83 0 8 0 108.13 17.99 0 8 0 119.26 18.25 0 -8 0 129.54 18.02 0 8 0 124.55 25.36 0 -8 0 113.16 19.34 2 -6 0 2013.15 545.56 -2 6 0 1310.47 358.09 2 -6 0 1929.18 504.09 -2 6 0 1868.07 505.88 2 -6 0 1547.12 406.45 -2 -6 0 3198.62 841.00 2 -6 0 1642.76 427.64 -2 -6 0 1667.34 437.49 2 6 0 1777.53 486.20 -2 6 0 2471.75 669.08 2 6 0 1842.54 489.34 2 6 0 2069.52 546.00 -2 -6 0 1604.18 424.48 2 6 0 1561.89 417.56 -2 -6 0 2009.35 527.46 -2 6 0 1633.24 426.09 2 -8 0 310.31 59.45 -2 8 0 264.73 45.14 -2 8 0 265.83 48.27 2 -8 0 318.65 57.84 2 -8 0 229.55 34.24 -2 8 0 241.38 37.77 2 8 0 276.87 52.06 2 8 0 280.43 49.78 -2 -8 0 338.67 57.70 2 8 0 302.85 57.11 -2 -8 0 316.81 58.25 2 8 0 231.70 36.24 -2 -8 0 234.46 34.76 2 -8 0 264.34 39.68 -2 8 0 236.48 36.23 -2 -8 0 220.30 33.84 0 10 0 -0.10 3.96 0 -10 0 2.72 5.47 0 -10 0 -0.15 3.97 0 10 0 1.47 5.41 0 -10 0 -0.91 3.81 0 10 0 -2.02 4.19 0 -10 0 -1.82 3.66 0 -10 0 -0.66 4.02 0 10 0 -1.69 7.14 1 -1 -1 3080.62 1115.89 -1 1 -1 3323.36 1240.50 1 -1 -1 3319.21 1248.61 -1 1 -1 3718.77 1446.38 1 -1 -1 3398.61 1388.78 1 -1 -1 3649.89 1348.69 -1 1 -1 3410.28 1245.60 1 1 -1 3386.90 1283.64 1 1 -1 3590.29 1336.52 1 1 -1 3485.05 1249.85 -1 -1 -1 4024.89 1503.13 1 1 -1 3222.27 1190.45 -1 -1 -1 3752.27 1419.58 -1 -1 -1 4161.08 1557.38 -1 -1 -1 3591.33 1357.34 -1 -1 -1 3265.28 1223.01 1 1 -1 3422.10 1287.48 -1 -1 -1 3309.53 1210.75 1 1 -1 3398.75 1446.46 1 -1 -1 3517.58 1333.83 1 -1 -1 3412.74 1307.97 1 1 -1 3321.46 1259.73 -1 1 -1 3149.02 1139.69 1 -1 -1 2737.53 964.00 -1 1 -1 3363.67 1241.19 -1 1 -1 3602.14 1337.38 -1 1 -1 3532.42 1321.40 -1 3 -1 204.91 34.83 -1 -3 -1 264.66 60.96 1 3 -1 203.79 45.17 1 3 -1 251.27 39.74 1 3 -1 184.20 60.61 -1 -3 -1 217.30 46.10 1 3 -1 163.58 17.84 -1 -3 -1 189.41 26.52 1 3 -1 193.88 38.26 -1 3 -1 296.87 51.49 -1 -3 1 156.57 17.66 1 -3 -1 205.04 45.51 -1 3 -1 223.40 51.11 -1 3 -1 212.54 37.85 1 3 1 179.36 22.33 1 -3 -1 181.75 20.29 -1 3 -1 221.11 35.00 -1 3 -1 193.40 21.62 1 -3 -1 209.14 40.79 -1 3 -1 201.23 41.23 1 -3 -1 175.81 26.06 1 -3 -1 201.69 33.03 -1 3 -1 136.84 15.59 1 -3 -1 220.89 50.25 -1 -3 -1 211.97 52.35 1 -3 1 168.51 19.59 1 3 -1 232.36 42.76 1 -3 -1 200.29 38.77 1 3 -1 203.37 32.03 1 3 -1 190.27 37.20 -1 -3 -1 190.50 35.61 -1 3 -1 208.08 28.77 -4 0 0 2041.91 604.22 4 0 0 2246.27 656.45 4 0 0 1762.28 507.62 -4 0 0 2372.35 650.82 4 0 0 1846.26 556.50 -4 0 0 1606.58 462.54 -4 0 0 2018.02 576.36 4 0 0 1331.45 397.32 -4 0 0 1604.43 439.97 -4 2 0 2510.04 812.79 4 -2 0 1780.11 596.31 4 -2 0 2573.91 859.68 -4 -2 0 2431.81 787.60 4 -2 0 2627.70 877.18 4 2 0 2477.21 831.81 4 2 0 2148.30 677.37 4 2 0 2816.74 921.06 -4 2 0 2810.35 920.23 -4 2 0 2333.46 738.31 -4 -2 0 2461.66 773.12 -4 -2 0 2785.52 920.60 -4 -2 0 4593.92 1508.91 4 2 0 2949.75 964.19 -4 2 0 2388.85 775.96 4 2 0 2407.86 781.21 -1 5 1 1669.40 426.99 -1 -5 -1 1649.45 443.10 -1 5 -1 1808.16 516.16 1 5 -1 1571.41 389.27 1 5 -1 1585.08 466.60 1 5 -1 1808.20 498.59 1 5 -1 1726.91 465.95 1 -5 1 1133.04 321.52 -1 -5 -1 1425.17 346.27 1 -5 -1 1588.99 437.87 -1 5 -1 1441.19 411.54 1 -5 -1 1458.16 358.09 1 5 1 1552.75 398.95 1 -5 -1 1622.81 467.17 1 5 -1 1568.86 385.53 1 5 -1 1739.79 506.67 -1 -5 -1 1676.76 499.60 1 5 1 1416.04 353.38 1 5 1 1496.83 429.97 -1 5 -1 1822.53 539.54 1 -5 -1 1446.34 351.13 -1 5 -1 1464.82 358.90 -1 -5 1 1592.85 391.35 -1 5 -1 1616.07 412.85 1 -5 -1 1591.17 469.17 1 5 -1 1553.58 501.08 -1 5 1 2611.34 722.45 -1 -5 1 1563.21 396.00 1 -5 -1 1699.07 463.72 -1 5 -1 1307.87 373.72 -1 -5 -1 1597.13 424.96 -1 -5 -1 1953.80 562.94 1 -5 1 1463.98 359.02 -1 -5 -1 1553.56 436.16 -2 10 0 60.41 24.61 2 10 0 53.76 17.24 -2 -10 0 49.59 12.43 -2 10 0 39.62 15.68 2 10 0 57.69 13.00 2 10 0 68.39 19.62 -2 -10 0 50.83 12.14 -2 -10 0 72.35 22.28 -2 10 0 50.10 13.64 2 -10 0 64.72 16.51 2 -10 0 66.02 20.61 -2 10 0 61.38 19.45 -2 -10 0 74.19 24.28 -2 10 0 50.69 10.83 2 -10 0 52.42 16.11 2 -10 0 90.50 31.89 2 10 0 59.60 23.86 4 -4 0 1829.92 547.82 -4 -4 0 1806.93 499.33 4 -4 0 1473.68 421.85 -4 4 0 1868.14 532.47 -4 -4 0 1775.64 509.14 4 -4 0 2466.24 749.52 -4 -4 0 1745.17 504.58 -4 4 0 1680.60 472.48 4 4 0 1629.38 446.35 4 4 0 1931.65 588.99 4 4 0 1775.99 504.21 -4 4 0 1698.38 468.76 4 4 0 2137.64 620.77 -4 -4 0 2415.82 716.86 4 -4 0 1941.37 534.65 4 -4 0 1265.52 372.30 -4 4 0 2848.23 854.08 4 4 0 1690.90 498.84 0 -12 0 1483.40 403.85 0 -12 0 1353.05 343.88 0 -12 0 1297.31 328.68 0 12 0 1609.29 439.54 0 -12 0 1368.99 357.12 0 -12 0 1209.58 306.29 0 12 0 1674.01 475.43 0 12 0 1439.03 388.75 0 12 0 1204.01 304.86 -1 7 1 2728.30 942.22 1 -7 -1 2536.15 806.73 -1 7 -1 2387.30 811.73 1 -7 -1 3477.69 1212.75 -1 -7 1 1840.14 709.22 -1 -7 1 2513.97 803.71 -1 -7 1 2550.67 827.77 1 7 -1 2568.66 838.71 -1 7 -1 2469.14 776.98 -1 7 -1 2671.99 885.54 1 7 1 2488.95 803.31 -1 -7 -1 2786.11 979.01 1 -7 1 2703.37 909.80 1 7 -1 2693.42 844.90 -1 -7 1 2854.38 886.68 1 -7 1 2418.75 825.46 -1 -7 -1 2841.81 943.90 1 7 1 2684.35 876.88 1 -7 -1 2815.22 980.97 1 7 -1 2812.25 983.72 1 7 -1 2706.36 954.98 1 -7 1 2478.43 785.88 1 7 1 2637.12 914.64 -1 -7 -1 2907.88 993.15 1 -7 -1 3197.92 1127.62 -1 7 1 2556.79 807.66 -1 -7 -1 2540.48 806.36 1 -7 1 2324.11 780.15 -1 -7 -1 2398.36 891.55 -1 7 1 2849.81 956.74 -1 7 -1 2836.75 983.49 1 -7 -1 3231.18 1075.49 -1 7 -1 3118.34 1119.83 4 -6 0 3394.87 1295.28 4 -6 0 3491.41 1410.17 -4 6 0 3550.21 1382.74 -4 -6 0 3904.64 1524.58 4 -6 0 3593.71 1423.72 4 -6 0 3395.80 1300.34 4 -6 0 3136.98 1228.92 -4 -6 0 3927.52 1499.41 -4 -6 0 4549.49 1805.04 4 6 0 4454.47 1736.98 4 6 0 3660.40 1414.08 -4 6 0 3504.84 1352.63 -4 6 0 4069.32 1639.79 4 6 0 3779.34 1547.19 4 6 0 3521.27 1343.13 3 -1 1 4377.88 1763.23 3 1 -1 3651.25 1365.72 -3 1 1 6342.85 2528.62 -3 -1 1 3399.74 1291.42 -3 1 -1 3835.89 1553.83 -3 -1 1 3822.25 1568.68 3 -1 -1 2753.37 1216.25 3 1 1 2770.30 1149.44 -3 1 -1 3867.94 1487.18 3 1 1 3837.47 1467.47 3 1 1 3760.53 1426.71 -3 1 -1 4266.46 1702.40 -3 1 -1 4526.77 1812.09 3 1 1 3703.07 1507.21 -3 1 -1 3590.69 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