data_kutts _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 N2 O4' _chemical_formula_weight 456.52 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.0877(3) _cell_length_b 15.0437(4) _cell_length_c 9.2994(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.757(4) _cell_angle_gamma 90.00 _cell_volume 1180.78(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19957 _cell_measurement_theta_min 2.3450 _cell_measurement_theta_max 30.2060 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63346 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 30.97 _reflns_number_total 3671 _reflns_number_gt 3520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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 compound is not enantionerically pure and crystallizes only by chance in a chiral (Sohncke) space group. In the absence of significant anomalous dispersion, Friedel opposite reflections were merged and the Flack parameter is thus meaningless. The ethyl groups may suffer from libration effects or perhaps slight disorder. ; _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^)+(0.0518P)^2^+0.3181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(9) _chemical_absolute_configuration . _refine_ls_number_reflns 3671 _refine_ls_number_parameters 309 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 N1 N 0.56797(16) 0.67321(9) 0.72096(15) 0.0133(3) Uani 1 1 d . . . N2 N 0.58091(16) 0.64302(10) 0.86252(15) 0.0126(2) Uani 1 1 d . . . C3 C 0.50410(17) 0.57536(11) 0.88247(17) 0.0117(3) Uani 1 1 d . . . C4 C 0.39250(18) 0.52060(10) 0.74799(17) 0.0115(3) Uani 1 1 d . . . C5 C 0.44909(19) 0.53099(11) 0.61180(17) 0.0132(3) Uani 1 1 d . . . H5A H 0.5502 0.4985 0.6362 0.016 Uiso 1 1 calc R . . H5B H 0.3700 0.5036 0.5182 0.016 Uiso 1 1 calc R . . C6 C 0.47327(18) 0.62811(10) 0.57697(17) 0.0126(3) Uani 1 1 d . . . H6 H 0.5383 0.6276 0.5106 0.015 Uiso 1 1 calc R . . C7 C 0.4039(2) 0.42165(11) 0.79357(18) 0.0153(3) Uani 1 1 d . . . C8 C 0.5808(3) 0.29849(14) 0.8698(3) 0.0346(5) Uani 1 1 d . . . H8A H 0.6539 0.2709 0.8260 0.042 Uiso 1 1 calc R . . H8B H 0.4814 0.2636 0.8349 0.042 Uiso 1 1 calc R . . C9 C 0.6531(3) 0.29736(17) 1.0397(3) 0.0393(6) Uani 1 1 d . . . H9A H 0.7465 0.3361 1.0742 0.059 Uiso 1 1 calc R . . H9B H 0.6849 0.2365 1.0754 0.059 Uiso 1 1 calc R . . H9C H 0.5762 0.3187 1.0828 0.059 Uiso 1 1 calc R . . C10 C 0.21624(18) 0.54508(11) 0.69557(18) 0.0137(3) Uani 1 1 d . . . C11 C 0.0204(2) 0.61937(13) 0.7622(2) 0.0216(3) Uani 1 1 d . . . H11A H -0.0335 0.6273 0.6490 0.026 Uiso 1 1 calc R . . H11B H 0.0136 0.6761 0.8132 0.026 Uiso 1 1 calc R . . C12 C -0.0604(2) 0.54703(15) 0.8171(3) 0.0299(4) Uani 1 1 d . . . H12A H -0.0607 0.4920 0.7604 0.045 Uiso 1 1 calc R . . H12B H -0.1697 0.5648 0.7984 0.045 Uiso 1 1 calc R . . H12C H -0.0033 0.5371 0.9281 0.045 Uiso 1 1 calc R . . C13 C 0.67220(19) 0.74331(11) 0.72457(19) 0.0139(3) Uani 1 1 d . . . C14 C 0.7659(2) 0.78229(11) 0.86593(19) 0.0163(3) Uani 1 1 d . . . H14 H 0.7562 0.7629 0.9593 0.020 Uiso 1 1 calc R . . C15 C 0.8725(2) 0.84902(12) 0.8696(2) 0.0198(3) Uani 1 1 d . . . H15 H 0.9355 0.8749 0.9660 0.024 Uiso 1 1 calc R . . C16 C 0.8888(2) 0.87878(12) 0.7346(2) 0.0209(3) Uani 1 1 d . . . H16 H 0.9630 0.9241 0.7383 0.025 Uiso 1 1 calc R . . C17 C 0.7947(2) 0.84103(12) 0.5947(2) 0.0197(3) Uani 1 1 d . . . H17 H 0.8048 0.8608 0.5018 0.024 Uiso 1 1 calc R . . C18 C 0.6860(2) 0.77480(12) 0.58811(19) 0.0168(3) Uani 1 1 d . . . H18 H 0.6207 0.7507 0.4909 0.020 Uiso 1 1 calc R . . C19 C 0.54818(18) 0.54789(11) 1.04677(17) 0.0132(3) Uani 1 1 d . . . C20 C 0.4454(2) 0.50230(11) 1.10121(19) 0.0149(3) Uani 1 1 d . . . H20 H 0.3394 0.4911 1.0337 0.018 Uiso 1 1 calc R . . C21 C 0.4979(2) 0.47316(12) 1.25428(19) 0.0178(3) Uani 1 1 d . . . H21 H 0.4277 0.4414 1.2900 0.021 Uiso 1 1 calc R . . C22 C 0.6513(2) 0.49010(13) 1.35480(19) 0.0197(3) Uani 1 1 d . . . H22 H 0.6866 0.4695 1.4587 0.024 Uiso 1 1 calc R . . C23 C 0.7536(2) 0.53736(14) 1.30293(19) 0.0212(3) Uani 1 1 d . . . H23 H 0.8582 0.5505 1.3721 0.025 Uiso 1 1 calc R . . C24 C 0.7030(2) 0.56536(13) 1.15023(19) 0.0188(3) Uani 1 1 d . . . H24 H 0.7740 0.5968 1.1151 0.023 Uiso 1 1 calc R . . C25 C 0.32028(18) 0.67693(11) 0.48591(17) 0.0136(3) Uani 1 1 d . . . C26 C 0.2659(2) 0.74831(12) 0.5464(2) 0.0198(3) Uani 1 1 d . . . H26 H 0.3254 0.7689 0.6480 0.024 Uiso 1 1 calc R . . C27 C 0.1236(2) 0.79016(14) 0.4583(2) 0.0256(4) Uani 1 1 d . . . H27 H 0.0864 0.8387 0.5008 0.031 Uiso 1 1 calc R . . C28 C 0.0366(2) 0.76138(14) 0.3097(2) 0.0260(4) Uani 1 1 d . . . H28 H -0.0604 0.7897 0.2504 0.031 Uiso 1 1 calc R . . C29 C 0.0920(2) 0.69080(14) 0.2478(2) 0.0228(4) Uani 1 1 d . . . H29 H 0.0334 0.6713 0.1452 0.027 Uiso 1 1 calc R . . C30 C 0.2327(2) 0.64850(12) 0.33507(18) 0.0174(3) Uani 1 1 d . . . H30 H 0.2696 0.6000 0.2921 0.021 Uiso 1 1 calc R . . O1 O 0.29722(17) 0.37979(10) 0.80674(16) 0.0241(3) Uani 1 1 d . . . O2 O 0.54701(17) 0.39008(9) 0.81483(16) 0.0246(3) Uani 1 1 d . . . O3 O 0.11930(14) 0.51886(10) 0.57654(14) 0.0208(3) Uani 1 1 d . . . O4 O 0.18642(14) 0.59636(8) 0.79852(14) 0.0160(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0135(6) 0.0150(6) 0.0099(6) 0.0013(5) 0.0024(5) -0.0021(5) N2 0.0116(6) 0.0150(6) 0.0105(6) 0.0008(5) 0.0034(5) 0.0013(5) C3 0.0092(6) 0.0140(7) 0.0101(6) -0.0006(5) 0.0017(5) 0.0006(5) C4 0.0107(6) 0.0115(6) 0.0105(6) 0.0004(5) 0.0020(5) 0.0004(5) C5 0.0144(7) 0.0140(7) 0.0110(6) 0.0009(5) 0.0047(5) 0.0020(5) C6 0.0134(7) 0.0143(7) 0.0093(6) 0.0006(5) 0.0033(5) 0.0008(5) C7 0.0197(8) 0.0134(7) 0.0100(6) -0.0003(5) 0.0020(6) 0.0002(6) C8 0.0440(13) 0.0172(9) 0.0368(12) 0.0060(8) 0.0081(10) 0.0134(9) C9 0.0465(14) 0.0271(11) 0.0332(11) 0.0111(9) 0.0017(10) 0.0035(10) C10 0.0113(6) 0.0141(7) 0.0146(6) 0.0012(5) 0.0036(5) 0.0004(5) C11 0.0129(7) 0.0219(8) 0.0293(9) -0.0025(7) 0.0069(7) 0.0053(6) C12 0.0181(8) 0.0296(10) 0.0460(12) 0.0005(9) 0.0164(8) 0.0028(8) C13 0.0117(7) 0.0131(7) 0.0160(7) 0.0024(5) 0.0042(5) 0.0012(5) C14 0.0166(7) 0.0165(7) 0.0152(7) 0.0002(6) 0.0053(6) -0.0012(6) C15 0.0190(8) 0.0168(7) 0.0214(8) -0.0012(6) 0.0048(6) -0.0049(6) C16 0.0184(8) 0.0159(7) 0.0283(9) 0.0048(7) 0.0085(7) -0.0021(6) C17 0.0193(8) 0.0191(8) 0.0223(8) 0.0085(6) 0.0095(7) 0.0024(6) C18 0.0167(7) 0.0179(7) 0.0156(7) 0.0038(6) 0.0057(6) 0.0018(6) C19 0.0128(7) 0.0151(7) 0.0105(6) -0.0001(5) 0.0031(5) 0.0007(6) C20 0.0143(7) 0.0156(7) 0.0149(7) -0.0010(5) 0.0057(6) -0.0010(6) C21 0.0236(8) 0.0166(7) 0.0169(7) 0.0002(6) 0.0121(6) -0.0002(6) C22 0.0238(8) 0.0230(8) 0.0122(7) 0.0018(6) 0.0065(6) 0.0048(7) C23 0.0156(7) 0.0316(9) 0.0131(7) 0.0006(7) 0.0014(6) 0.0001(7) C24 0.0131(7) 0.0268(9) 0.0146(7) 0.0018(6) 0.0027(6) -0.0030(6) C25 0.0121(7) 0.0150(7) 0.0124(6) 0.0030(5) 0.0031(5) 0.0001(5) C26 0.0175(8) 0.0194(8) 0.0208(8) -0.0023(6) 0.0052(6) 0.0023(6) C27 0.0192(9) 0.0212(9) 0.0352(10) -0.0004(7) 0.0087(7) 0.0060(7) C28 0.0149(8) 0.0271(9) 0.0308(9) 0.0074(8) 0.0022(7) 0.0043(7) C29 0.0164(8) 0.0284(10) 0.0179(8) 0.0054(7) -0.0003(6) 0.0001(7) C30 0.0159(7) 0.0205(7) 0.0133(7) 0.0000(6) 0.0023(6) 0.0012(6) O1 0.0279(7) 0.0192(6) 0.0234(6) 0.0010(5) 0.0073(5) -0.0085(5) O2 0.0261(7) 0.0182(6) 0.0280(7) 0.0066(5) 0.0082(5) 0.0096(5) O3 0.0132(5) 0.0285(7) 0.0160(5) -0.0046(5) 0.0002(4) 0.0007(5) O4 0.0109(5) 0.0162(6) 0.0191(5) -0.0033(4) 0.0036(4) 0.0023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 N2 1.3559(18) . ? N1 C13 1.409(2) . ? N1 C6 1.463(2) . ? N2 C3 1.286(2) . ? C3 C19 1.487(2) . ? C3 C4 1.527(2) . ? C4 C10 1.536(2) . ? C4 C7 1.541(2) . ? C4 C5 1.541(2) . ? C5 C6 1.530(2) . ? C6 C25 1.522(2) . ? C7 O1 1.200(2) . ? C7 O2 1.329(2) . ? C8 O2 1.462(2) . ? C8 C9 1.469(3) . ? C10 O3 1.1975(19) . ? C10 O4 1.3332(19) . ? C11 O4 1.460(2) . ? C11 C12 1.504(3) . ? C13 C14 1.402(2) . ? C13 C18 1.403(2) . ? C14 C15 1.387(2) . ? C15 C16 1.392(3) . ? C16 C17 1.386(3) . ? C17 C18 1.389(2) . ? C19 C20 1.396(2) . ? C19 C24 1.404(2) . ? C20 C21 1.394(2) . ? C21 C22 1.385(2) . ? C22 C23 1.391(3) . ? C23 C24 1.386(2) . ? C25 C26 1.386(2) . ? C25 C30 1.399(2) . ? C26 C27 1.398(3) . ? C27 C28 1.382(3) . ? C28 C29 1.388(3) . ? C29 C30 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 N1 C13 114.32(13) . . ? N2 N1 C6 122.90(13) . . ? C13 N1 C6 122.07(13) . . ? C3 N2 N1 123.29(14) . . ? N2 C3 C19 114.47(13) . . ? N2 C3 C4 122.70(13) . . ? C19 C3 C4 122.39(14) . . ? C3 C4 C10 115.37(13) . . ? C3 C4 C7 109.84(12) . . ? C10 C4 C7 105.95(13) . . ? C3 C4 C5 107.20(12) . . ? C10 C4 C5 109.95(12) . . ? C7 C4 C5 108.37(13) . . ? C6 C5 C4 112.87(12) . . ? N1 C6 C25 113.06(13) . . ? N1 C6 C5 109.34(12) . . ? C25 C6 C5 113.91(13) . . ? O1 C7 O2 125.49(16) . . ? O1 C7 C4 124.11(16) . . ? O2 C7 C4 110.40(14) . . ? O2 C8 C9 109.84(19) . . ? O3 C10 O4 125.35(15) . . ? O3 C10 C4 122.52(14) . . ? O4 C10 C4 112.11(13) . . ? O4 C11 C12 110.02(15) . . ? C14 C13 C18 118.68(15) . . ? C14 C13 N1 120.27(14) . . ? C18 C13 N1 121.04(15) . . ? C15 C14 C13 120.10(15) . . ? C14 C15 C16 121.19(17) . . ? C17 C16 C15 118.68(16) . . ? C16 C17 C18 121.12(16) . . ? C17 C18 C13 120.20(16) . . ? C20 C19 C24 118.59(14) . . ? C20 C19 C3 123.19(14) . . ? C24 C19 C3 118.16(14) . . ? C21 C20 C19 120.23(15) . . ? C22 C21 C20 120.60(16) . . ? C21 C22 C23 119.69(15) . . ? C24 C23 C22 119.99(16) . . ? C23 C24 C19 120.87(16) . . ? C26 C25 C30 119.20(15) . . ? C26 C25 C6 122.55(14) . . ? C30 C25 C6 118.25(15) . . ? C25 C26 C27 120.20(17) . . ? C28 C27 C26 120.43(18) . . ? C27 C28 C29 119.55(17) . . ? C28 C29 C30 120.32(17) . . ? C29 C30 C25 120.29(17) . . ? C7 O2 C8 117.13(17) . . ? C10 O4 C11 116.01(13) . . ? 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 C13 N1 N2 C3 -174.80(15) . . . . ? C6 N1 N2 C3 -4.2(2) . . . . ? N1 N2 C3 C19 173.94(14) . . . . ? N1 N2 C3 C4 1.4(2) . . . . ? N2 C3 C4 C10 -96.86(17) . . . . ? C19 C3 C4 C10 91.14(17) . . . . ? N2 C3 C4 C7 143.50(15) . . . . ? C19 C3 C4 C7 -28.5(2) . . . . ? N2 C3 C4 C5 26.0(2) . . . . ? C19 C3 C4 C5 -146.04(14) . . . . ? C3 C4 C5 C6 -50.43(16) . . . . ? C10 C4 C5 C6 75.69(16) . . . . ? C7 C4 C5 C6 -168.93(12) . . . . ? N2 N1 C6 C25 106.68(16) . . . . ? C13 N1 C6 C25 -83.48(18) . . . . ? N2 N1 C6 C5 -21.36(19) . . . . ? C13 N1 C6 C5 148.48(14) . . . . ? C4 C5 C6 N1 48.90(17) . . . . ? C4 C5 C6 C25 -78.66(16) . . . . ? C3 C4 C7 O1 114.73(17) . . . . ? C10 C4 C7 O1 -10.5(2) . . . . ? C5 C4 C7 O1 -128.46(17) . . . . ? C3 C4 C7 O2 -65.63(16) . . . . ? C10 C4 C7 O2 169.13(13) . . . . ? C5 C4 C7 O2 51.18(17) . . . . ? C3 C4 C10 O3 166.97(16) . . . . ? C7 C4 C10 O3 -71.28(19) . . . . ? C5 C4 C10 O3 45.6(2) . . . . ? C3 C4 C10 O4 -14.19(19) . . . . ? C7 C4 C10 O4 107.57(14) . . . . ? C5 C4 C10 O4 -135.53(14) . . . . ? N2 N1 C13 C14 -6.7(2) . . . . ? C6 N1 C13 C14 -177.30(15) . . . . ? N2 N1 C13 C18 172.60(14) . . . . ? C6 N1 C13 C18 2.0(2) . . . . ? C18 C13 C14 C15 -1.6(2) . . . . ? N1 C13 C14 C15 177.63(16) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C14 C15 C16 C17 0.7(3) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C13 -1.5(3) . . . . ? C14 C13 C18 C17 2.3(2) . . . . ? N1 C13 C18 C17 -176.95(16) . . . . ? N2 C3 C19 C20 154.27(15) . . . . ? C4 C3 C19 C20 -33.1(2) . . . . ? N2 C3 C19 C24 -28.6(2) . . . . ? C4 C3 C19 C24 144.01(16) . . . . ? C24 C19 C20 C21 -1.5(2) . . . . ? C3 C19 C20 C21 175.58(15) . . . . ? C19 C20 C21 C22 1.0(3) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? C21 C22 C23 C24 -1.6(3) . . . . ? C22 C23 C24 C19 1.0(3) . . . . ? C20 C19 C24 C23 0.6(3) . . . . ? C3 C19 C24 C23 -176.70(17) . . . . ? N1 C6 C25 C26 -9.8(2) . . . . ? C5 C6 C25 C26 115.79(17) . . . . ? N1 C6 C25 C30 169.71(14) . . . . ? C5 C6 C25 C30 -64.67(18) . . . . ? C30 C25 C26 C27 1.2(3) . . . . ? C6 C25 C26 C27 -179.29(17) . . . . ? C25 C26 C27 C28 -0.6(3) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C27 C28 C29 C30 0.9(3) . . . . ? C28 C29 C30 C25 -0.3(3) . . . . ? C26 C25 C30 C29 -0.7(3) . . . . ? C6 C25 C30 C29 179.75(16) . . . . ? O1 C7 O2 C8 -4.7(3) . . . . ? C4 C7 O2 C8 175.62(15) . . . . ? C9 C8 O2 C7 -92.2(2) . . . . ? O3 C10 O4 C11 1.8(2) . . . . ? C4 C10 O4 C11 -177.04(14) . . . . ? C12 C11 O4 C10 85.22(19) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.512 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.045 _iucr_refine_instructions_details ; TITL kutts in P2(1) CELL 0.71073 9.087681 15.043659 9.299439 90.0000 111.7567 90.0000 ZERR 2.00 0.0003 0.0004 0.0003 0.0000 0.004 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 56.00 56.00 4.00 8.00 TEMP -173 SIZE 0.35 0.3 0.12 FMAP 2 PLAN 10 L.S. 4 MERG 3 ACTA 60 CONF WGHT 0.051800 0.318100 FVAR 8.69962 N1 3 0.567973 0.673215 0.720961 11.00000 0.01347 0.01500 = 0.00990 0.00128 0.00239 -0.00206 N2 3 0.580905 0.643016 0.862515 11.00000 0.01159 0.01504 = 0.01046 0.00076 0.00340 0.00128 C3 1 0.504097 0.575357 0.882466 11.00000 0.00925 0.01398 = 0.01014 -0.00062 0.00172 0.00059 C4 1 0.392499 0.520598 0.747989 11.00000 0.01073 0.01149 = 0.01053 0.00044 0.00205 0.00036 C5 1 0.449094 0.530994 0.611797 11.00000 0.01438 0.01399 = 0.01104 0.00085 0.00467 0.00195 AFIX 23 H5A 2 0.550220 0.498521 0.636191 11.00000 -1.20000 H5B 2 0.370034 0.503601 0.518193 11.00000 -1.20000 AFIX 0 C6 1 0.473274 0.628111 0.576975 11.00000 0.01345 0.01431 = 0.00927 0.00057 0.00330 0.00083 AFIX 13 H6 2 0.538256 0.627580 0.510602 11.00000 -1.20000 AFIX 0 C7 1 0.403895 0.421649 0.793571 11.00000 0.01966 0.01337 = 0.01002 -0.00027 0.00205 0.00017 C8 1 0.580821 0.298491 0.869847 11.00000 0.04399 0.01721 = 0.03685 0.00601 0.00811 0.01335 AFIX 23 H8A 2 0.653881 0.270896 0.826002 11.00000 -1.20000 H8B 2 0.481391 0.263586 0.834881 11.00000 -1.20000 AFIX 0 C9 1 0.653105 0.297356 1.039660 11.00000 0.04654 0.02712 = 0.03315 0.01108 0.00173 0.00350 AFIX 137 H9A 2 0.746492 0.336064 1.074192 11.00000 -1.50000 H9B 2 0.684880 0.236510 1.075360 11.00000 -1.50000 H9C 2 0.576180 0.318738 1.082750 11.00000 -1.50000 AFIX 0 C10 1 0.216241 0.545082 0.695572 11.00000 0.01134 0.01411 = 0.01459 0.00119 0.00358 0.00036 C11 1 0.020416 0.619374 0.762173 11.00000 0.01293 0.02185 = 0.02933 -0.00251 0.00688 0.00530 AFIX 23 H11A 2 -0.033508 0.627290 0.648971 11.00000 -1.20000 H11B 2 0.013604 0.676139 0.813208 11.00000 -1.20000 AFIX 0 C12 1 -0.060370 0.547032 0.817050 11.00000 0.01811 0.02957 = 0.04596 0.00046 0.01636 0.00276 AFIX 137 H12A 2 -0.060736 0.492043 0.760416 11.00000 -1.50000 H12B 2 -0.169686 0.564762 0.798397 11.00000 -1.50000 H12C 2 -0.003332 0.537148 0.928098 11.00000 -1.50000 AFIX 0 C13 1 0.672198 0.743306 0.724572 11.00000 0.01170 0.01307 = 0.01596 0.00240 0.00415 0.00120 C14 1 0.765853 0.782286 0.865929 11.00000 0.01655 0.01647 = 0.01524 0.00017 0.00528 -0.00115 AFIX 43 H14 2 0.756240 0.762947 0.959304 11.00000 -1.20000 AFIX 0 C15 1 0.872487 0.849023 0.869612 11.00000 0.01905 0.01679 = 0.02141 -0.00118 0.00484 -0.00486 AFIX 43 H15 2 0.935499 0.874887 0.966020 11.00000 -1.20000 AFIX 0 C16 1 0.888835 0.878779 0.734616 11.00000 0.01835 0.01589 = 0.02833 0.00480 0.00854 -0.00211 AFIX 43 H16 2 0.963006 0.924058 0.738267 11.00000 -1.20000 AFIX 0 C17 1 0.794727 0.841031 0.594706 11.00000 0.01934 0.01906 = 0.02230 0.00847 0.00948 0.00237 AFIX 43 H17 2 0.804798 0.860813 0.501770 11.00000 -1.20000 AFIX 0 C18 1 0.685993 0.774796 0.588108 11.00000 0.01674 0.01788 = 0.01564 0.00381 0.00571 0.00180 AFIX 43 H18 2 0.620744 0.750728 0.490899 11.00000 -1.20000 AFIX 0 C19 1 0.548175 0.547886 1.046767 11.00000 0.01279 0.01513 = 0.01048 -0.00009 0.00309 0.00071 C20 1 0.445424 0.502299 1.101213 11.00000 0.01434 0.01557 = 0.01491 -0.00103 0.00569 -0.00096 AFIX 43 H20 2 0.339396 0.491105 1.033697 11.00000 -1.20000 AFIX 0 C21 1 0.497858 0.473155 1.254280 11.00000 0.02362 0.01665 = 0.01692 0.00017 0.01209 -0.00024 AFIX 43 H21 2 0.427670 0.441377 1.289972 11.00000 -1.20000 AFIX 0 C22 1 0.651327 0.490099 1.354801 11.00000 0.02377 0.02302 = 0.01216 0.00177 0.00653 0.00477 AFIX 43 H22 2 0.686594 0.469539 1.458709 11.00000 -1.20000 AFIX 0 C23 1 0.753602 0.537361 1.302926 11.00000 0.01560 0.03157 = 0.01307 0.00060 0.00137 0.00014 AFIX 43 H23 2 0.858155 0.550451 1.372145 11.00000 -1.20000 AFIX 0 C24 1 0.702965 0.565360 1.150229 11.00000 0.01310 0.02675 = 0.01459 0.00183 0.00270 -0.00301 AFIX 43 H24 2 0.773960 0.596792 1.115130 11.00000 -1.20000 AFIX 0 C25 1 0.320285 0.676931 0.485908 11.00000 0.01208 0.01496 = 0.01240 0.00304 0.00306 0.00010 C26 1 0.265863 0.748315 0.546368 11.00000 0.01745 0.01939 = 0.02083 -0.00232 0.00524 0.00232 AFIX 43 H26 2 0.325427 0.768877 0.647987 11.00000 -1.20000 AFIX 0 C27 1 0.123595 0.790156 0.458290 11.00000 0.01920 0.02117 = 0.03521 -0.00039 0.00868 0.00601 AFIX 43 H27 2 0.086408 0.838688 0.500795 11.00000 -1.20000 AFIX 0 C28 1 0.036643 0.761383 0.309731 11.00000 0.01488 0.02705 = 0.03078 0.00740 0.00221 0.00426 AFIX 43 H28 2 -0.060360 0.789713 0.250422 11.00000 -1.20000 AFIX 0 C29 1 0.092041 0.690800 0.247796 11.00000 0.01637 0.02838 = 0.01786 0.00540 -0.00029 0.00008 AFIX 43 H29 2 0.033443 0.671348 0.145224 11.00000 -1.20000 AFIX 0 C30 1 0.232694 0.648503 0.335066 11.00000 0.01589 0.02048 = 0.01331 0.00000 0.00231 0.00118 AFIX 43 H30 2 0.269589 0.600046 0.292129 11.00000 -1.20000 AFIX 0 O1 4 0.297221 0.379791 0.806745 11.00000 0.02790 0.01915 = 0.02338 0.00097 0.00729 -0.00852 O2 4 0.547012 0.390080 0.814831 11.00000 0.02605 0.01823 = 0.02805 0.00655 0.00818 0.00964 O3 4 0.119300 0.518863 0.576542 11.00000 0.01322 0.02850 = 0.01603 -0.00456 0.00017 0.00074 O4 4 0.186418 0.596358 0.798522 11.00000 0.01093 0.01623 = 0.01914 -0.00329 0.00365 0.00234 HKLF 4 ; # end of cif file