data_nacho4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 N2 O5' _chemical_formula_sum 'C21 H24 N2 O5' _chemical_formula_weight 384.42 _chemical_absolute_configuration syn 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.0655(6) _cell_length_b 8.4614(8) _cell_length_c 46.856(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2008.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4116 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 23.7 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.091 _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 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 14035 _diffrn_reflns_av_R_equivalents 0.1054 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2159 _reflns_number_gt 1182 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0084P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -4(2) _refine_ls_number_reflns 2159 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 0.730 _refine_ls_restrained_S_all 0.730 _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 C1 C 0.7190(8) 0.0063(5) 0.42072(7) 0.0393(10) Uani 1 1 d . . . H1A H 0.8686 0.0814 0.4196 0.047 Uiso 1 1 calc R . . H1B H 0.7839 -0.1000 0.4154 0.047 Uiso 1 1 calc R . . O2 O 0.5101(5) 0.0550(3) 0.40145(5) 0.0317(7) Uani 1 1 d . . . C3 C 0.5936(8) 0.0807(5) 0.37439(8) 0.0290(9) Uani 1 1 d . . . N4 N 0.3875(7) 0.1070(4) 0.35687(6) 0.0303(8) Uani 1 1 d . . . H4 H 0.235(7) 0.096(4) 0.3639(7) 0.023(10) Uiso 1 1 d . . . C5 C 0.4235(8) 0.1405(4) 0.32671(7) 0.0282(9) Uani 1 1 d . . . H5 H 0.6090 0.1141 0.3212 0.034 Uiso 1 1 calc R . . C6 C 0.3765(8) 0.3191(4) 0.32207(8) 0.0271(9) Uani 1 1 d . . . N7 N 0.5922(7) 0.4063(4) 0.31963(7) 0.0296(8) Uani 1 1 d . . . H7 H 0.747(7) 0.372(4) 0.3214(7) 0.031(11) Uiso 1 1 d . . . C8 C 0.5825(8) 0.5783(4) 0.31755(8) 0.0294(9) Uani 1 1 d . . . H8 H 0.3939 0.6120 0.3191 0.035 Uiso 1 1 calc R . . C9 C 0.6854(8) 0.6275(5) 0.28824(9) 0.0366(10) Uani 1 1 d . . . C10 C 0.7383(8) 0.6571(4) 0.34198(7) 0.0348(10) Uani 1 1 d . . . H10A H 0.9267 0.6273 0.3404 0.042 Uiso 1 1 calc R . . H10B H 0.7260 0.7733 0.3400 0.042 Uiso 1 1 calc R . . C11 C 0.6093(8) 0.0033(5) 0.45076(8) 0.0337(10) Uani 1 1 d . . . C12 C 0.7322(8) -0.0927(5) 0.47050(8) 0.0419(11) Uani 1 1 d . . . H12 H 0.8728 -0.1592 0.4646 0.050 Uiso 1 1 calc R . . C13 C 0.6549(9) -0.0938(5) 0.49864(9) 0.0478(12) Uani 1 1 d . . . H13 H 0.7443 -0.1586 0.5121 0.057 Uiso 1 1 calc R . . C14 C 0.4470(9) -0.0002(6) 0.50721(9) 0.0486(12) Uani 1 1 d . . . H14 H 0.3893 -0.0023 0.5265 0.058 Uiso 1 1 calc R . . C15 C 0.3221(9) 0.0973(5) 0.48753(9) 0.0480(12) Uani 1 1 d . . . H15 H 0.1806 0.1632 0.4935 0.058 Uiso 1 1 calc R . . C16 C 0.4030(9) 0.0985(5) 0.45939(8) 0.0408(11) Uani 1 1 d . . . H16 H 0.3166 0.1649 0.4460 0.049 Uiso 1 1 calc R . . C21 C 0.6366(9) 0.6096(5) 0.37114(8) 0.0363(10) Uani 1 1 d . . . C22 C 0.4235(9) 0.6851(5) 0.38334(9) 0.0416(11) Uani 1 1 d . . . H22 H 0.3367 0.7672 0.3732 0.050 Uiso 1 1 calc R . . C23 C 0.3338(9) 0.6422(5) 0.41044(10) 0.0509(13) Uani 1 1 d . . . H23 H 0.1871 0.6951 0.4187 0.061 Uiso 1 1 calc R . . C24 C 0.4588(10) 0.5234(6) 0.42503(9) 0.0533(14) Uani 1 1 d . . . H24 H 0.3991 0.4942 0.4435 0.064 Uiso 1 1 calc R . . C25 C 0.6717(9) 0.4459(5) 0.41294(9) 0.0483(12) Uani 1 1 d . . . H25 H 0.7582 0.3636 0.4231 0.058 Uiso 1 1 calc R . . C26 C 0.7582(9) 0.4884(5) 0.38607(8) 0.0427(11) Uani 1 1 d . . . H26 H 0.9027 0.4338 0.3777 0.051 Uiso 1 1 calc R . . O31 O 0.8240(5) 0.0789(3) 0.36714(5) 0.0401(7) Uani 1 1 d . . . C51 C 0.2344(8) 0.0433(4) 0.30862(7) 0.0380(10) Uani 1 1 d . . . H51A H 0.2683 -0.0694 0.3117 0.057 Uiso 1 1 calc R . . H51B H 0.2609 0.0688 0.2884 0.057 Uiso 1 1 calc R . . H51C H 0.0522 0.0679 0.3141 0.057 Uiso 1 1 calc R . . O61 O 0.1515(5) 0.3734(3) 0.32124(6) 0.0457(8) Uani 1 1 d . . . O91 O 0.7286(7) 0.5422(3) 0.26866(6) 0.0608(10) Uani 1 1 d . . . O92 O 0.7107(6) 0.7853(3) 0.28701(6) 0.0509(9) Uani 1 1 d . . . C92 C 0.7921(11) 0.8484(5) 0.25933(8) 0.0626(15) Uani 1 1 d . . . H92A H 0.8027 0.9638 0.2604 0.094 Uiso 1 1 calc R . . H92B H 0.6627 0.8181 0.2448 0.094 Uiso 1 1 calc R . . H92C H 0.9655 0.8054 0.2542 0.094 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 C1 0.035(2) 0.052(2) 0.030(2) 0.003(2) -0.003(2) 0.003(2) O2 0.0242(14) 0.0450(17) 0.0259(15) 0.0053(14) -0.0018(12) -0.0020(12) C3 0.029(2) 0.028(2) 0.030(2) 0.0001(19) 0.000(2) -0.001(2) N4 0.0211(18) 0.043(2) 0.026(2) 0.0047(17) 0.0038(17) -0.004(2) C5 0.027(2) 0.032(2) 0.026(2) 0.0012(18) 0.0030(19) 0.0024(19) C6 0.021(2) 0.032(2) 0.027(2) 0.0014(18) 0.0036(19) 0.000(2) N7 0.0195(18) 0.031(2) 0.038(2) 0.0007(17) 0.0014(17) 0.0010(18) C8 0.026(2) 0.028(2) 0.035(2) -0.0035(19) 0.006(2) 0.001(2) C9 0.034(3) 0.039(3) 0.036(2) 0.003(2) 0.001(2) -0.002(2) C10 0.035(2) 0.032(2) 0.037(2) -0.0060(18) 0.004(2) -0.007(2) C11 0.031(2) 0.038(2) 0.033(2) -0.001(2) -0.002(2) -0.011(2) C12 0.043(3) 0.046(3) 0.037(2) -0.002(2) -0.002(2) 0.006(2) C13 0.050(3) 0.055(3) 0.039(3) 0.007(2) -0.003(2) -0.005(3) C14 0.055(3) 0.058(3) 0.033(3) 0.002(3) 0.003(2) -0.013(3) C15 0.044(3) 0.049(3) 0.050(3) -0.006(2) 0.010(2) 0.003(3) C16 0.046(3) 0.038(3) 0.038(3) 0.000(2) 0.002(2) 0.006(2) C21 0.040(3) 0.034(2) 0.035(2) -0.008(2) -0.002(2) -0.001(2) C22 0.044(3) 0.037(3) 0.044(3) -0.009(2) 0.005(2) -0.001(2) C23 0.044(3) 0.063(3) 0.047(3) -0.014(3) 0.009(3) -0.004(3) C24 0.066(4) 0.062(3) 0.033(3) -0.007(3) 0.007(3) -0.018(3) C25 0.060(3) 0.047(3) 0.038(3) 0.004(2) -0.008(2) -0.005(3) C26 0.045(3) 0.045(3) 0.038(2) -0.006(2) 0.006(2) -0.001(2) O31 0.0216(17) 0.064(2) 0.0343(15) 0.0045(15) 0.0032(12) -0.0020(16) C51 0.041(2) 0.035(2) 0.038(2) -0.0035(19) 0.000(2) -0.004(2) O61 0.0249(17) 0.0305(16) 0.081(2) 0.0105(16) 0.0001(17) 0.0019(14) O91 0.103(3) 0.0395(17) 0.0398(17) -0.0050(15) 0.022(2) 0.0046(19) O92 0.078(3) 0.0337(16) 0.0407(17) 0.0031(14) 0.0145(19) -0.0128(18) C92 0.087(4) 0.057(3) 0.043(3) 0.014(2) 0.009(3) -0.021(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 O2 1.451(4) . ? C1 C11 1.514(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C3 1.354(4) . ? C3 O31 1.216(4) . ? C3 N4 1.347(5) . ? N4 C5 1.453(4) . ? N4 H4 0.85(3) . ? C5 C51 1.521(5) . ? C5 C6 1.545(5) . ? C5 H5 1.0000 . ? C6 O61 1.230(4) . ? C6 N7 1.324(5) . ? N7 C8 1.459(5) . ? N7 H7 0.84(4) . ? C8 C9 1.527(5) . ? C8 C10 1.542(5) . ? C8 H8 1.0000 . ? C9 O91 1.188(4) . ? C9 O92 1.342(4) . ? C10 C21 1.514(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.379(5) . ? C11 C16 1.380(5) . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 C14 1.377(6) . ? C13 H13 0.9500 . ? C14 C15 1.389(6) . ? C14 H14 0.9500 . ? C15 C16 1.381(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.378(5) . ? C21 C26 1.386(5) . ? C22 C23 1.397(6) . ? C22 H22 0.9500 . ? C23 C24 1.371(6) . ? C23 H23 0.9500 . ? C24 C25 1.384(6) . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O92 C92 1.462(4) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 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 O2 C1 C11 108.4(3) . . ? O2 C1 H1A 110.0 . . ? C11 C1 H1A 110.0 . . ? O2 C1 H1B 110.0 . . ? C11 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C3 O2 C1 113.6(3) . . ? O31 C3 N4 125.2(4) . . ? O31 C3 O2 124.0(4) . . ? N4 C3 O2 110.8(3) . . ? C3 N4 C5 121.9(3) . . ? C3 N4 H4 117(2) . . ? C5 N4 H4 121(2) . . ? N4 C5 C51 111.0(3) . . ? N4 C5 C6 108.0(3) . . ? C51 C5 C6 110.7(3) . . ? N4 C5 H5 109.1 . . ? C51 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? O61 C6 N7 123.7(3) . . ? O61 C6 C5 120.9(3) . . ? N7 C6 C5 115.5(3) . . ? C6 N7 C8 122.3(4) . . ? C6 N7 H7 125(3) . . ? C8 N7 H7 112(3) . . ? N7 C8 C9 108.7(3) . . ? N7 C8 C10 111.4(3) . . ? C9 C8 C10 112.0(3) . . ? N7 C8 H8 108.2 . . ? C9 C8 H8 108.2 . . ? C10 C8 H8 108.2 . . ? O91 C9 O92 123.7(4) . . ? O91 C9 C8 126.3(4) . . ? O92 C9 C8 110.0(3) . . ? C21 C10 C8 112.4(3) . . ? C21 C10 H10A 109.1 . . ? C8 C10 H10A 109.1 . . ? C21 C10 H10B 109.1 . . ? C8 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 119.3(4) . . ? C12 C11 C1 117.9(4) . . ? C16 C11 C1 122.7(4) . . ? C13 C12 C11 121.2(4) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 119.6(4) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C11 C16 C15 120.0(4) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C22 C21 C26 118.8(4) . . ? C22 C21 C10 121.2(4) . . ? C26 C21 C10 120.0(4) . . ? C21 C22 C23 120.8(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.8(4) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C9 O92 C92 115.3(3) . . ? O92 C92 H92A 109.5 . . ? O92 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? O92 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 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 C11 C1 O2 C3 172.4(3) . . . . ? C1 O2 C3 O31 -6.9(6) . . . . ? C1 O2 C3 N4 172.7(3) . . . . ? O31 C3 N4 C5 -1.5(6) . . . . ? O2 C3 N4 C5 178.9(3) . . . . ? C3 N4 C5 C51 133.9(4) . . . . ? C3 N4 C5 C6 -104.6(4) . . . . ? N4 C5 C6 O61 -77.9(5) . . . . ? C51 C5 C6 O61 43.7(5) . . . . ? N4 C5 C6 N7 101.0(4) . . . . ? C51 C5 C6 N7 -137.4(3) . . . . ? O61 C6 N7 C8 4.1(7) . . . . ? C5 C6 N7 C8 -174.8(3) . . . . ? C6 N7 C8 C9 -115.2(4) . . . . ? C6 N7 C8 C10 120.9(4) . . . . ? N7 C8 C9 O91 10.6(6) . . . . ? C10 C8 C9 O91 134.1(4) . . . . ? N7 C8 C9 O92 -172.1(3) . . . . ? C10 C8 C9 O92 -48.6(5) . . . . ? N7 C8 C10 C21 -58.3(4) . . . . ? C9 C8 C10 C21 179.7(3) . . . . ? O2 C1 C11 C12 156.0(3) . . . . ? O2 C1 C11 C16 -27.7(5) . . . . ? C16 C11 C12 C13 -0.7(7) . . . . ? C1 C11 C12 C13 175.6(4) . . . . ? C11 C12 C13 C14 1.5(7) . . . . ? C12 C13 C14 C15 -1.7(7) . . . . ? C13 C14 C15 C16 1.1(7) . . . . ? C12 C11 C16 C15 0.1(6) . . . . ? C1 C11 C16 C15 -176.1(4) . . . . ? C14 C15 C16 C11 -0.3(7) . . . . ? C8 C10 C21 C22 -83.5(5) . . . . ? C8 C10 C21 C26 96.5(4) . . . . ? C26 C21 C22 C23 1.0(6) . . . . ? C10 C21 C22 C23 -178.9(4) . . . . ? C21 C22 C23 C24 -0.2(6) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 -0.1(6) . . . . ? C24 C25 C26 C21 0.9(6) . . . . ? C22 C21 C26 C25 -1.4(6) . . . . ? C10 C21 C26 C25 178.6(4) . . . . ? O91 C9 O92 C92 1.1(7) . . . . ? C8 C9 O92 C92 -176.3(4) . . . . ? 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 N4 H4 O31 0.85(3) 2.09(3) 2.904(4) 161(3) 1_455 N7 H7 O61 0.84(4) 2.05(4) 2.848(4) 159(3) 1_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.156 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.037