# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_nano _database_code_depnum_ccdc_archive 'CCDC 868566' #TrackingRef 'AP-14g_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 N6 O6' _chemical_formula_weight 528.61 _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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 4.9166(6) _cell_length_b 13.1195(13) _cell_length_c 42.105(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2715.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1606 _cell_measurement_theta_min 2.4757 _cell_measurement_theta_max 29.0427 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_T_min 0.75490 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 5.00 42.50 0.7500 145.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 77.0000 30.0000 50 #__ type_ start__ end____ width___ exp.time_ 2 omega -44.00 68.50 0.7500 145.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 0.0000 -30.0000 150 #__ type_ start__ end____ width___ exp.time_ 3 omega -98.00 -48.50 0.7500 145.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 179.0000 120.0000 66 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10922 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.1072 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 29.11 _reflns_number_total 5632 _reflns_number_gt 3426 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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^)+(0.1133P)^2^+3.5891P] 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 -2(3) _refine_ls_number_reflns 5632 _refine_ls_number_parameters 334 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2792 _refine_ls_wR_factor_gt 0.2379 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.040 _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 N1 N -0.2681(13) 0.5402(4) 0.76456(11) 0.0463(14) Uani 1 1 d . . . N2 N -0.4893(15) 0.5928(7) 0.76419(19) 0.103(3) Uani 1 1 d . . . N3 N -0.4808(15) 0.6571(6) 0.78763(18) 0.097(3) Uani 1 1 d . . . C4 C -0.2443(12) 0.6493(4) 0.80292(12) 0.0347(13) Uani 1 1 d . . . C5 C -0.1076(15) 0.5736(6) 0.78825(17) 0.0582(19) Uani 1 1 d . . . H5 H 0.0680 0.5487 0.7936 0.070 Uiso 1 1 calc R . . C6 C -0.1751(12) 0.7151(4) 0.83048(12) 0.0319(12) Uani 1 1 d . . . H6A H -0.2466 0.7846 0.8266 0.038 Uiso 1 1 calc R . . H6B H 0.0252 0.7200 0.8323 0.038 Uiso 1 1 calc R . . C7 C -0.2903(10) 0.6751(4) 0.86154(11) 0.0252(11) Uani 1 1 d . . . H7 H -0.4915 0.6668 0.8592 0.030 Uiso 1 1 calc R . . C8 C -0.1668(10) 0.5722(4) 0.86925(11) 0.0232(10) Uani 1 1 d . . . N9 N -0.3390(9) 0.4949(3) 0.87413(10) 0.0254(9) Uani 1 1 d . . . H9 H -0.5146 0.5059 0.8720 0.030 Uiso 1 1 calc R . . C10 C -0.2477(11) 0.3934(4) 0.88277(13) 0.0303(12) Uani 1 1 d . B . H10 H -0.0447 0.3912 0.8815 0.036 Uiso 1 1 calc R . . C11 C -0.3645(11) 0.3175(4) 0.85885(15) 0.0342(13) Uani 1 1 d . . . N12 N -0.1812(10) 0.2620(3) 0.84383(13) 0.0424(13) Uani 1 1 d . . . H12 H -0.0085 0.2709 0.8486 0.051 Uiso 1 1 calc R . . C13 C -0.2507(13) 0.1870(4) 0.81989(16) 0.0448(16) Uani 1 1 d . . . H13 H -0.4525 0.1875 0.8170 0.054 Uiso 1 1 calc R . . C14 C -0.1217(18) 0.2157(5) 0.78922(18) 0.059(2) Uani 1 1 d . . . H14A H -0.1426 0.1596 0.7737 0.071 Uiso 1 1 calc R . . H14B H 0.0749 0.2284 0.7924 0.071 Uiso 1 1 calc R . . C15 C -0.265(2) 0.3149(6) 0.7765(2) 0.075(2) Uani 1 1 d . . . H15A H -0.4441 0.2967 0.7674 0.090 Uiso 1 1 calc R . . H15B H -0.2963 0.3623 0.7944 0.090 Uiso 1 1 calc R . . C16 C -0.104(3) 0.3657(6) 0.7525(2) 0.098(4) Uani 1 1 d . . . H16A H -0.0769 0.3181 0.7345 0.118 Uiso 1 1 calc R . . H16B H 0.0775 0.3809 0.7616 0.118 Uiso 1 1 calc R . . C17 C -0.2225(19) 0.4620(5) 0.74009(15) 0.062(2) Uani 1 1 d . . . H17A H -0.0991 0.4901 0.7237 0.074 Uiso 1 1 calc R . . H17B H -0.3981 0.4463 0.7297 0.074 Uiso 1 1 calc R . . N18 N -0.2373(9) 0.7429(3) 0.88794(10) 0.0259(9) Uani 1 1 d . . . H18 H -0.0682 0.7513 0.8943 0.031 Uiso 1 1 calc R . . C19 C -0.4329(11) 0.7930(4) 0.90299(12) 0.0285(12) Uani 1 1 d . . . O20 O -0.6740(7) 0.7902(3) 0.89617(9) 0.0399(10) Uani 1 1 d . . . O21 O -0.3328(9) 0.8485(3) 0.92702(10) 0.0498(12) Uani 1 1 d . . . C22 C -0.5351(17) 0.9064(8) 0.94508(17) 0.083(3) Uani 1 1 d . . . H22A H -0.7147 0.8727 0.9434 0.099 Uiso 1 1 calc R . . H22B H -0.5513 0.9760 0.9362 0.099 Uiso 1 1 calc R . . C23 C -0.4515(15) 0.9118(5) 0.97864(16) 0.0536(18) Uani 1 1 d . . . C24 C -0.245(3) 0.9709(9) 0.98843(19) 0.122(5) Uani 1 1 d . . . H24 H -0.1427 1.0082 0.9733 0.146 Uiso 1 1 calc R . . C25 C -0.181(4) 0.9783(12) 1.0199(2) 0.177(8) Uani 1 1 d . . . H25 H -0.0378 1.0228 1.0261 0.213 Uiso 1 1 calc R . . C26 C -0.310(3) 0.9257(8) 1.0421(3) 0.108(4) Uani 1 1 d . . . H26 H -0.2720 0.9374 1.0639 0.130 Uiso 1 1 calc R . . C27 C -0.475(4) 0.8629(11) 1.0344(2) 0.145(6) Uani 1 1 d . . . H27 H -0.5499 0.8196 1.0502 0.174 Uiso 1 1 calc R . . C28 C -0.564(4) 0.8509(10) 1.0015(3) 0.155(6) Uani 1 1 d . . . H28 H -0.6982 0.8017 0.9960 0.186 Uiso 1 1 calc R . . O29 O 0.0825(7) 0.5620(3) 0.87178(9) 0.0339(9) Uani 1 1 d . . . C30 C -0.3348(16) 0.3671(5) 0.91683(15) 0.0523(17) Uani 1 1 d D . . H30A H -0.5350 0.3593 0.9176 0.063 Uiso 1 1 calc R A 1 H30B H -0.2834 0.4235 0.9312 0.063 Uiso 1 1 calc R A 1 C31 C -0.191(4) 0.2616(8) 0.9289(2) 0.188(9) Uani 1 1 d D B 1 H31 H 0.0120 0.2589 0.9272 0.226 Uiso 1 1 calc R B 1 C32 C -0.310(6) 0.2660(19) 0.9632(4) 0.282 Uiso 1 1 d D B 1 H32A H -0.4782 0.2257 0.9641 0.282 Uiso 1 1 calc R B 1 H32B H -0.3504 0.3369 0.9688 0.282 Uiso 1 1 calc R B 1 H32C H -0.1778 0.2380 0.9782 0.282 Uiso 1 1 calc R B 1 C33 C -0.337(5) 0.1762(17) 0.9154(6) 0.282 Uiso 1 1 d D B 1 H33A H -0.2429 0.1126 0.9209 0.282 Uiso 1 1 calc R B 1 H33B H -0.3440 0.1833 0.8923 0.282 Uiso 1 1 calc R B 1 H33C H -0.5220 0.1746 0.9240 0.282 Uiso 1 1 calc R B 1 O35 O -0.6115(8) 0.3112(3) 0.85529(13) 0.0513(12) Uani 1 1 d . . . C36 C -0.1659(12) 0.0810(4) 0.82976(15) 0.0404(14) Uani 1 1 d . . . O37 O -0.2762(10) 0.0049(3) 0.82050(12) 0.0604(13) Uani 1 1 d . . . O38 O 0.0454(9) 0.0808(3) 0.84866(12) 0.0550(13) Uani 1 1 d . . . C39 C 0.1418(17) -0.0175(5) 0.8598(2) 0.066(2) Uani 1 1 d . . . H39A H -0.0142 -0.0615 0.8645 0.098 Uiso 1 1 calc R . . H39B H 0.2507 -0.0081 0.8791 0.098 Uiso 1 1 calc R . . H39C H 0.2538 -0.0494 0.8433 0.098 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 N1 0.067(4) 0.046(3) 0.026(2) -0.005(2) 0.003(3) -0.014(3) N2 0.064(5) 0.145(7) 0.101(6) -0.066(6) -0.048(4) 0.041(5) N3 0.077(5) 0.120(6) 0.095(5) -0.067(5) -0.058(4) 0.049(5) C4 0.043(3) 0.035(3) 0.026(3) 0.010(2) 0.004(3) -0.006(3) C5 0.048(4) 0.064(5) 0.062(4) -0.014(4) -0.009(3) 0.008(4) C6 0.032(3) 0.028(3) 0.036(3) 0.003(2) 0.001(2) -0.007(2) C7 0.021(2) 0.022(2) 0.033(3) -0.005(2) -0.004(2) -0.004(2) C8 0.022(2) 0.026(2) 0.022(2) -0.001(2) -0.001(2) 0.000(2) N9 0.0151(19) 0.0220(19) 0.039(2) 0.0015(19) -0.0040(18) -0.0010(17) C10 0.027(3) 0.018(2) 0.046(3) 0.004(2) -0.008(2) -0.006(2) C11 0.026(3) 0.016(2) 0.060(4) 0.003(3) -0.009(3) 0.002(2) N12 0.022(2) 0.030(2) 0.075(3) -0.013(3) -0.009(2) 0.002(2) C13 0.035(3) 0.025(3) 0.074(4) -0.016(3) -0.015(3) 0.004(3) C14 0.077(5) 0.031(3) 0.070(5) 0.001(3) -0.008(4) 0.004(4) C15 0.099(7) 0.053(4) 0.074(5) -0.007(4) 0.023(5) 0.000(5) C16 0.177(12) 0.060(5) 0.057(5) -0.006(4) 0.007(7) 0.009(7) C17 0.098(6) 0.044(4) 0.042(4) -0.009(3) 0.007(4) -0.010(4) N18 0.0158(19) 0.029(2) 0.033(2) -0.0058(19) -0.0047(18) -0.0024(18) C19 0.031(3) 0.028(3) 0.026(3) 0.000(2) 0.002(2) 0.001(2) O20 0.0188(19) 0.046(2) 0.055(2) -0.009(2) -0.0035(18) 0.0043(19) O21 0.042(2) 0.064(3) 0.043(2) -0.028(2) -0.007(2) 0.014(2) C22 0.062(5) 0.128(8) 0.059(5) -0.049(5) -0.016(4) 0.047(6) C23 0.059(4) 0.054(4) 0.048(4) -0.024(4) 0.004(3) 0.006(4) C24 0.180(12) 0.135(9) 0.049(5) 0.013(5) -0.030(6) -0.090(9) C25 0.28(2) 0.197(14) 0.057(6) 0.006(8) -0.061(9) -0.101(16) C26 0.186(14) 0.076(7) 0.062(6) -0.012(6) -0.005(8) 0.043(9) C27 0.251(19) 0.130(11) 0.052(6) 0.015(7) 0.059(9) -0.036(12) C28 0.227(16) 0.139(11) 0.100(9) -0.017(8) 0.050(10) -0.102(12) O29 0.0194(19) 0.0289(19) 0.053(2) 0.0030(19) -0.0019(17) -0.0026(16) C30 0.064(4) 0.047(4) 0.045(3) 0.014(3) -0.006(3) -0.004(4) C31 0.42(3) 0.097(7) 0.044(5) 0.036(5) -0.019(10) -0.074(14) O35 0.021(2) 0.033(2) 0.100(4) -0.010(2) -0.010(2) 0.0008(17) C36 0.030(3) 0.035(3) 0.056(4) -0.007(3) 0.000(3) -0.009(3) O37 0.068(3) 0.038(2) 0.076(3) -0.014(2) -0.005(3) -0.020(3) O38 0.048(3) 0.0226(19) 0.095(4) 0.002(2) -0.016(3) -0.003(2) C39 0.078(5) 0.029(3) 0.089(5) 0.016(4) -0.012(5) -0.001(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 1.288(9) . ? N1 C5 1.345(9) . ? N1 C17 1.471(8) . ? N2 N3 1.299(9) . ? N3 C4 1.333(8) . ? C4 C5 1.349(9) . ? C4 C6 1.486(8) . ? C6 C7 1.519(7) . ? C7 N18 1.448(6) . ? C7 C8 1.515(7) . ? C8 O29 1.238(6) . ? C8 N9 1.338(6) . ? N9 C10 1.451(6) . ? C10 C11 1.528(7) . ? C10 C30 1.536(8) . ? C11 O35 1.227(6) . ? C11 N12 1.320(7) . ? N12 C13 1.449(7) . ? C13 C14 1.487(10) . ? C13 C36 1.509(8) . ? C14 C15 1.574(10) . ? C15 C16 1.445(13) . ? C16 C17 1.487(11) . ? N18 C19 1.326(7) . ? C19 O20 1.220(6) . ? C19 O21 1.341(6) . ? O21 C22 1.464(8) . ? C22 C23 1.473(10) . ? C23 C24 1.341(12) . ? C23 C28 1.367(13) . ? C24 C25 1.368(12) . ? C25 C26 1.322(17) . ? C26 C27 1.201(18) . ? C27 C28 1.463(18) . ? C30 C31 1.635(13) . ? C31 C33 1.446(13) . ? C31 C32 1.562(16) . ? C36 O37 1.202(7) . ? C36 O38 1.309(7) . ? O38 C39 1.452(7) . ? 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 C5 109.3(6) . . ? N2 N1 C17 119.6(6) . . ? C5 N1 C17 131.1(7) . . ? N1 N2 N3 108.2(6) . . ? N2 N3 C4 110.2(6) . . ? N3 C4 C5 105.7(6) . . ? N3 C4 C6 122.2(6) . . ? C5 C4 C6 132.2(6) . . ? N1 C5 C4 106.7(6) . . ? C4 C6 C7 112.7(4) . . ? N18 C7 C8 108.1(4) . . ? N18 C7 C6 112.4(4) . . ? C8 C7 C6 110.1(4) . . ? O29 C8 N9 122.1(5) . . ? O29 C8 C7 120.8(5) . . ? N9 C8 C7 117.1(4) . . ? C8 N9 C10 122.6(4) . . ? N9 C10 C11 108.4(4) . . ? N9 C10 C30 110.7(5) . . ? C11 C10 C30 111.4(5) . . ? O35 C11 N12 125.4(6) . . ? O35 C11 C10 119.8(5) . . ? N12 C11 C10 114.8(5) . . ? C11 N12 C13 123.2(5) . . ? N12 C13 C14 109.4(5) . . ? N12 C13 C36 111.6(5) . . ? C14 C13 C36 110.7(5) . . ? C13 C14 C15 108.3(6) . . ? C16 C15 C14 111.9(8) . . ? C15 C16 C17 115.0(10) . . ? N1 C17 C16 113.9(6) . . ? C19 N18 C7 122.8(4) . . ? O20 C19 N18 125.3(5) . . ? O20 C19 O21 123.4(5) . . ? N18 C19 O21 111.3(5) . . ? C19 O21 C22 115.1(5) . . ? O21 C22 C23 109.5(6) . . ? C24 C23 C28 115.3(9) . . ? C24 C23 C22 122.3(8) . . ? C28 C23 C22 122.2(9) . . ? C23 C24 C25 121.0(11) . . ? C26 C25 C24 122.3(13) . . ? C27 C26 C25 119.6(12) . . ? C26 C27 C28 122.1(12) . . ? C23 C28 C27 118.8(12) . . ? C10 C30 C31 111.0(6) . . ? C33 C31 C32 101.7(17) . . ? C33 C31 C30 108.7(15) . . ? C32 C31 C30 95.3(13) . . ? O37 C36 O38 123.6(6) . . ? O37 C36 C13 123.5(6) . . ? O38 C36 C13 112.9(5) . . ? C36 O38 C39 117.2(5) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.717 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.075