data_n3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H54 N2 O4' _chemical_formula_sum 'C38 H54 N2 O4' _chemical_formula_weight 602.84 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.6101(11) _cell_length_b 6.5900(15) _cell_length_c 27.733(7) _cell_angle_alpha 93.316(9) _cell_angle_beta 94.533(8) _cell_angle_gamma 104.5980(14) _cell_volume 810.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9443 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description laths _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.079 _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+ CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9427 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2743 _reflns_number_gt 2232 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0744P)^2^+0.6478P] 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 2743 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 O1 O 0.5704(3) 0.6039(2) 0.65097(5) 0.0250(4) Uani 1 1 d . . . O2 O 0.9641(3) 0.1237(2) 0.57430(5) 0.0256(4) Uani 1 1 d . . . N1 N 0.7704(4) 0.3657(3) 0.61283(6) 0.0188(4) Uani 1 1 d . . . C1 C 0.6112(5) 0.5207(3) 0.61298(7) 0.0194(5) Uani 1 1 d . . . C2 C 0.5009(4) 0.5766(3) 0.56552(7) 0.0170(5) Uani 1 1 d . . . C3 C 0.5529(4) 0.4722(3) 0.52257(7) 0.0161(4) Uani 1 1 d . . . C4 C 0.7088(4) 0.3143(3) 0.52414(7) 0.0171(5) Uani 1 1 d . . . C5 C 0.8246(5) 0.2575(3) 0.57134(7) 0.0188(5) Uani 1 1 d . . . C6 C 0.3474(5) 0.7303(3) 0.56312(8) 0.0195(5) Uani 1 1 d . . . C7 C 0.7575(5) 0.2154(3) 0.48189(8) 0.0195(5) Uani 1 1 d . . . C8 C 0.8846(5) 0.3113(3) 0.66017(7) 0.0211(5) Uani 1 1 d . . . H8A H 0.9652 0.4420 0.6817 0.025 Uiso 1 1 calc R . . H8B H 1.0529 0.2463 0.6555 0.025 Uiso 1 1 calc R . . C9 C 0.6457(5) 0.1609(3) 0.68500(7) 0.0219(5) Uani 1 1 d . . . H9A H 0.5219 0.2412 0.7015 0.026 Uiso 1 1 calc R . . H9B H 0.5114 0.0582 0.6602 0.026 Uiso 1 1 calc R . . C10 C 0.7869(5) 0.0437(3) 0.72193(7) 0.0210(5) Uani 1 1 d . . . H10A H 0.9223 0.1471 0.7464 0.025 Uiso 1 1 calc R . . H10B H 0.9109 -0.0358 0.7052 0.025 Uiso 1 1 calc R . . C11 C 0.5559(5) -0.1080(3) 0.74769(7) 0.0210(5) Uani 1 1 d . . . H11A H 0.4588 -0.0264 0.7694 0.025 Uiso 1 1 calc R . . H11B H 0.3977 -0.1938 0.7233 0.025 Uiso 1 1 calc R . . C12 C 0.6924(5) -0.2535(3) 0.77729(7) 0.0213(5) Uani 1 1 d . . . H12A H 0.8475 -0.1673 0.8021 0.026 Uiso 1 1 calc R . . H12B H 0.7943 -0.3319 0.7556 0.026 Uiso 1 1 calc R . . C13 C 0.4649(5) -0.4104(3) 0.80249(7) 0.0221(5) Uani 1 1 d . . . H13A H 0.3075 -0.4952 0.7778 0.026 Uiso 1 1 calc R . . H13B H 0.3662 -0.3324 0.8248 0.026 Uiso 1 1 calc R . . C14 C 0.6053(5) -0.5578(3) 0.83112(8) 0.0222(5) Uani 1 1 d . . . H14A H 0.6977 -0.6392 0.8085 0.027 Uiso 1 1 calc R . . H14B H 0.7682 -0.4725 0.8549 0.027 Uiso 1 1 calc R . . C15 C 0.3825(5) -0.7105(3) 0.85804(7) 0.0227(5) Uani 1 1 d . . . H15A H 0.2185 -0.7951 0.8344 0.027 Uiso 1 1 calc R . . H15B H 0.2917 -0.6293 0.8809 0.027 Uiso 1 1 calc R . . C16 C 0.5249(5) -0.8583(3) 0.88611(7) 0.0223(5) Uani 1 1 d . . . H16A H 0.6137 -0.9407 0.8632 0.027 Uiso 1 1 calc R . . H16B H 0.6904 -0.7737 0.9095 0.027 Uiso 1 1 calc R . . C17 C 0.3029(5) -1.0095(3) 0.91348(8) 0.0238(5) Uani 1 1 d . . . H17A H 0.2227 -0.9273 0.9377 0.029 Uiso 1 1 calc R . . H17B H 0.1317 -1.0884 0.8903 0.029 Uiso 1 1 calc R . . C18 C 0.4409(5) -1.1651(3) 0.93925(8) 0.0257(5) Uani 1 1 d . . . H18A H 0.6086 -1.0865 0.9631 0.031 Uiso 1 1 calc R . . H18B H 0.5258 -1.2449 0.9152 0.031 Uiso 1 1 calc R . . C19 C 0.2148(6) -1.3190(4) 0.96540(8) 0.0311(6) Uani 1 1 d . . . H19A H 0.1351 -1.2412 0.9901 0.047 Uiso 1 1 calc R . . H19B H 0.3145 -1.4165 0.9810 0.047 Uiso 1 1 calc R . . H19C H 0.0492 -1.3984 0.9420 0.047 Uiso 1 1 calc R . . H6 H 0.315(5) 0.801(3) 0.5935(8) 0.017(5) Uiso 1 1 d . . . H7 H 0.872(5) 0.111(4) 0.4824(7) 0.020(6) Uiso 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 O1 0.0334(9) 0.0213(8) 0.0217(8) 0.0018(6) 0.0040(6) 0.0094(7) O2 0.0308(9) 0.0221(8) 0.0290(8) 0.0065(6) 0.0030(7) 0.0155(7) N1 0.0201(10) 0.0162(9) 0.0208(9) 0.0046(7) 0.0019(7) 0.0049(8) C1 0.0193(11) 0.0148(10) 0.0236(11) 0.0032(8) 0.0049(8) 0.0024(9) C2 0.0125(10) 0.0113(10) 0.0254(11) 0.0031(8) 0.0032(8) -0.0008(8) C3 0.0117(10) 0.0099(9) 0.0254(11) 0.0041(8) 0.0038(8) -0.0009(8) C4 0.0131(10) 0.0124(10) 0.0254(11) 0.0050(8) 0.0041(8) 0.0009(8) C5 0.0156(11) 0.0132(10) 0.0277(11) 0.0045(8) 0.0036(8) 0.0028(9) C6 0.0195(11) 0.0144(10) 0.0243(11) 0.0011(8) 0.0051(9) 0.0030(9) C7 0.0187(11) 0.0121(10) 0.0282(11) 0.0034(8) 0.0049(9) 0.0038(9) C8 0.0221(11) 0.0208(11) 0.0215(10) 0.0053(8) 0.0005(8) 0.0072(9) C9 0.0241(12) 0.0207(11) 0.0221(11) 0.0060(8) 0.0018(9) 0.0072(10) C10 0.0226(11) 0.0198(11) 0.0221(10) 0.0045(8) 0.0019(8) 0.0081(9) C11 0.0237(12) 0.0191(11) 0.0215(10) 0.0031(8) 0.0026(8) 0.0074(9) C12 0.0219(12) 0.0180(11) 0.0248(11) 0.0053(8) 0.0030(9) 0.0054(9) C13 0.0225(12) 0.0183(11) 0.0260(11) 0.0049(9) 0.0026(9) 0.0057(9) C14 0.0231(12) 0.0179(11) 0.0262(11) 0.0051(9) 0.0048(9) 0.0046(9) C15 0.0239(12) 0.0187(11) 0.0262(11) 0.0060(9) 0.0047(9) 0.0054(10) C16 0.0233(12) 0.0172(11) 0.0257(11) 0.0043(9) 0.0036(9) 0.0031(9) C17 0.0252(12) 0.0197(11) 0.0275(11) 0.0063(9) 0.0043(9) 0.0060(10) C18 0.0287(13) 0.0190(11) 0.0288(11) 0.0067(9) 0.0038(9) 0.0037(10) C19 0.0362(14) 0.0234(12) 0.0332(12) 0.0123(10) 0.0029(10) 0.0050(11) _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 O1 C1 1.209(2) . ? O2 C5 1.218(2) . ? N1 C5 1.391(3) . ? N1 C1 1.399(3) . ? N1 C8 1.473(2) . ? C1 C2 1.474(3) . ? C2 C6 1.376(3) . ? C2 C3 1.408(3) . ? C3 C4 1.407(3) . ? C3 C3 1.409(4) 2_666 ? C4 C7 1.370(3) . ? C4 C5 1.478(3) . ? C6 C7 1.402(3) 2_666 ? C6 H6 0.98(2) . ? C7 C6 1.402(3) 2_666 ? C7 H7 0.97(2) . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.520(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.517(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.522(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.520(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.520(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.521(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 C5 N1 C1 124.81(17) . . ? C5 N1 C8 117.73(17) . . ? C1 N1 C8 117.45(16) . . ? O1 C1 N1 120.17(18) . . ? O1 C1 C2 122.58(19) . . ? N1 C1 C2 117.25(17) . . ? C6 C2 C3 120.01(19) . . ? C6 C2 C1 120.15(18) . . ? C3 C2 C1 119.84(18) . . ? C4 C3 C2 121.00(19) . . ? C4 C3 C3 119.8(2) . 2_666 ? C2 C3 C3 119.2(2) . 2_666 ? C7 C4 C3 119.99(19) . . ? C7 C4 C5 119.95(18) . . ? C3 C4 C5 120.06(18) . . ? O2 C5 N1 120.80(19) . . ? O2 C5 C4 122.17(19) . . ? N1 C5 C4 117.02(17) . . ? C2 C6 C7 120.47(19) . 2_666 ? C2 C6 H6 118.5(13) . . ? C7 C6 H6 121.0(13) 2_666 . ? C4 C7 C6 120.5(2) . 2_666 ? C4 C7 H7 120.8(13) . . ? C6 C7 H7 118.6(12) 2_666 . ? N1 C8 C9 113.28(17) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 111.44(17) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 113.16(17) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C10 112.88(17) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 113.96(17) . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 113.14(17) . . ? C12 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 113.75(18) . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 113.25(18) . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 113.27(18) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 113.30(18) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 112.81(19) . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 C5 N1 C1 O1 178.66(18) . . . . ? C8 N1 C1 O1 -0.4(3) . . . . ? C5 N1 C1 C2 -1.8(3) . . . . ? C8 N1 C1 C2 179.19(17) . . . . ? O1 C1 C2 C6 0.7(3) . . . . ? N1 C1 C2 C6 -178.87(18) . . . . ? O1 C1 C2 C3 -179.30(19) . . . . ? N1 C1 C2 C3 1.2(3) . . . . ? C6 C2 C3 C4 -179.89(18) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C6 C2 C3 C3 0.3(3) . . . 2_666 ? C1 C2 C3 C3 -179.8(2) . . . 2_666 ? C2 C3 C4 C7 -179.80(18) . . . . ? C3 C3 C4 C7 0.1(3) 2_666 . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C3 C3 C4 C5 179.1(2) 2_666 . . . ? C1 N1 C5 O2 -179.62(19) . . . . ? C8 N1 C5 O2 -0.6(3) . . . . ? C1 N1 C5 C4 1.1(3) . . . . ? C8 N1 C5 C4 -179.90(17) . . . . ? C7 C4 C5 O2 0.0(3) . . . . ? C3 C4 C5 O2 -179.02(19) . . . . ? C7 C4 C5 N1 179.26(18) . . . . ? C3 C4 C5 N1 0.3(3) . . . . ? C3 C2 C6 C7 -0.2(3) . . . 2_666 ? C1 C2 C6 C7 179.86(18) . . . 2_666 ? C3 C4 C7 C6 -0.1(3) . . . 2_666 ? C5 C4 C7 C6 -179.14(18) . . . 2_666 ? C5 N1 C8 C9 -98.6(2) . . . . ? C1 N1 C8 C9 80.5(2) . . . . ? N1 C8 C9 C10 157.81(17) . . . . ? C8 C9 C10 C11 179.84(17) . . . . ? C9 C10 C11 C12 169.18(17) . . . . ? C10 C11 C12 C13 -178.63(17) . . . . ? C11 C12 C13 C14 178.82(17) . . . . ? C12 C13 C14 C15 177.91(17) . . . . ? C13 C14 C15 C16 179.43(18) . . . . ? C14 C15 C16 C17 179.37(17) . . . . ? C15 C16 C17 C18 176.83(18) . . . . ? C16 C17 C18 C19 -178.50(18) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.283 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.052