#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012624.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012624 loop_ _publ_author_name 'Thu\'ery, Pierre' 'Asfari, Zouhair' 'Nierlich, Martine' 'Vicens, Jacques' _publ_section_title ; Two triethylammonium ion complexes of monoanionic calix[4]arene ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o223 _journal_page_last o225 _journal_volume 58 _journal_year 2002 _chemical_formula_moiety 'C6 H16 N + , C28 H23 O4 -' _chemical_formula_sum 'C34 H39 N O4' _chemical_formula_weight 525.66 _chemical_name_systematic ; triethylammonium 26,27,28-trihydroxypentacyclo[19.3.1.1^3,7^.1^9,13^.1^15,19^]octacosa- 1(25),3,5,7(28),9,11,13(27),15,17,19(26),21,23-dodecaen-25-olate ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.3531(18) _cell_length_b 10.8710(12) _cell_length_c 13.8210(12) _cell_measurement_reflns_used 15424 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.68 _cell_measurement_theta_min 2.66 _cell_volume 2757.5(5) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material 'SHELXTL and PARST97 (Nardelli, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_av_sigmaI/netI 0.081 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 15424 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 2.66 _diffrn_standards_decay_% none _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 1128 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.23 _refine_diff_density_min -0.25 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 353 _refine_ls_number_reflns 2702 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.100 _refine_ls_R_factor_gt 0.057 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.106 _refine_ls_wR_factor_ref 0.124 _reflns_number_gt 1909 _reflns_number_total 2702 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file dn1006.cif _[local]_cod_data_source_block I _cod_database_code 2012624 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 0.22569(18) 0.7184(3) 0.3797(3) 0.0297(9) Uani d . 1 O H1 0.2470 0.7826 0.3648 0.036 Uiso d R 1 H O2 0.26739(18) 0.9379(3) 0.3475(3) 0.0269(8) Uani d . 1 O H2 0.2323 0.9821 0.3604 0.032 Uiso d R 1 H O3 0.15176(19) 1.0451(3) 0.3858(3) 0.0319(9) Uani d . 1 O O4 0.08297(18) 0.8361(3) 0.4355(3) 0.0301(9) Uani d . 1 O H4 0.1023 0.9013 0.4201 0.036 Uiso d R 1 H C1 0.2195(3) 0.6348(4) 0.5403(4) 0.0240(11) Uani d . 1 C C2 0.2608(3) 0.6838(5) 0.4641(4) 0.0242(11) Uani d . 1 C C3 0.3365(3) 0.6978(4) 0.4707(4) 0.0255(11) Uani d . 1 C C4 0.3714(3) 0.6578(5) 0.5545(4) 0.0278(12) Uani d . 1 C H4A 0.4216 0.6665 0.5604 0.033 Uiso calc R 1 H C5 0.3316(3) 0.6050(4) 0.6293(4) 0.0279(11) Uani d . 1 C H5A 0.3553 0.5764 0.6844 0.033 Uiso calc R 1 H C6 0.2571(2) 0.5951(4) 0.6217(4) 0.0255(11) Uani d . 1 C H6A 0.2311 0.5607 0.6727 0.031 Uiso calc R 1 H C7 0.3794(3) 0.7612(5) 0.3921(4) 0.0271(12) Uani d . 1 C H7A 0.3553 0.7479 0.3305 0.032 Uiso calc R 1 H H7B 0.4275 0.7247 0.3883 0.032 Uiso calc R 1 H C8 0.3871(3) 0.8990(5) 0.4092(3) 0.0258(12) Uani d . 1 C C9 0.3297(3) 0.9800(5) 0.3869(4) 0.0254(11) Uani d . 1 C C10 0.3387(3) 1.1081(5) 0.4060(4) 0.0268(11) Uani d . 1 C C11 0.4039(3) 1.1493(5) 0.4472(4) 0.0276(12) Uani d . 1 C H11A 0.4102 1.2329 0.4589 0.033 Uiso calc R 1 H C12 0.4593(3) 1.0688(5) 0.4707(4) 0.0322(13) Uani d . 1 C H12A 0.5021 1.0975 0.4990 0.039 Uiso calc R 1 H C13 0.4504(3) 0.9443(5) 0.4516(4) 0.0317(13) Uani d . 1 C H13A 0.4876 0.8899 0.4675 0.038 Uiso calc R 1 H C14 0.2789(3) 1.1987(5) 0.3819(4) 0.0293(12) Uani d . 1 C H14A 0.2568 1.1744 0.3211 0.035 Uiso calc R 1 H H14B 0.3007 1.2791 0.3724 0.035 Uiso calc R 1 H C15 0.2196(3) 1.2099(4) 0.4573(4) 0.0273(12) Uani d . 1 C C16 0.1573(3) 1.1349(4) 0.4558(4) 0.0269(11) Uani d . 1 C C17 0.1019(3) 1.1469(5) 0.5242(4) 0.0243(11) Uani d . 1 C C18 0.1114(3) 1.2341(5) 0.5982(4) 0.0291(12) Uani d . 1 C H18A 0.0754 1.2429 0.6451 0.035 Uiso calc R 1 H C19 0.1728(3) 1.3072(5) 0.6031(4) 0.0330(13) Uani d . 1 C H19A 0.1786 1.3629 0.6535 0.040 Uiso calc R 1 H C20 0.2261(3) 1.2969(5) 0.5320(4) 0.0302(12) Uani d . 1 C H20A 0.2666 1.3482 0.5340 0.036 Uiso calc R 1 H C21 0.0363(3) 1.0626(5) 0.5250(4) 0.0280(12) Uani d . 1 C H21A -0.0048 1.1044 0.5545 0.034 Uiso calc R 1 H H21B 0.0231 1.0413 0.4592 0.034 Uiso calc R 1 H C22 0.0535(3) 0.9475(5) 0.5811(4) 0.0264(12) Uani d . 1 C C23 0.0798(3) 0.8417(5) 0.5344(3) 0.0255(12) Uani d . 1 C C24 0.1014(3) 0.7368(5) 0.5867(4) 0.0262(12) Uani d . 1 C C25 0.0917(3) 0.7361(5) 0.6863(4) 0.0301(13) Uani d . 1 C H25A 0.1037 0.6663 0.7216 0.036 Uiso calc R 1 H C26 0.0640(3) 0.8392(5) 0.7337(4) 0.0336(13) Uani d . 1 C H26A 0.0578 0.8377 0.8005 0.040 Uiso calc R 1 H C27 0.0456(3) 0.9439(5) 0.6818(4) 0.0301(13) Uani d . 1 C H27A 0.0279 1.0126 0.7143 0.036 Uiso calc R 1 H C28 0.1367(3) 0.6287(5) 0.5357(4) 0.0275(12) Uani d . 1 C H28A 0.1214 0.6278 0.4685 0.033 Uiso calc R 1 H H28B 0.1203 0.5529 0.5655 0.033 Uiso calc R 1 H N 0.1534(2) 0.5612(4) 0.2522(3) 0.0303(10) Uani d . 1 N H5 0.1859 0.6081 0.2822 0.036 Uiso d R 1 H C29 0.1884(3) 0.5361(5) 0.1561(4) 0.0368(14) Uani d . 1 C H29A 0.1526 0.4985 0.1138 0.044 Uiso calc R 1 H H29B 0.2026 0.6139 0.1273 0.044 Uiso calc R 1 H C30 0.2537(3) 0.4547(6) 0.1605(6) 0.0552(18) Uani d . 1 C H30A 0.2730 0.4435 0.0965 0.083 Uiso calc R 1 H H30B 0.2401 0.3763 0.1869 0.083 Uiso calc R 1 H H30C 0.2901 0.4918 0.2009 0.083 Uiso calc R 1 H C31 0.0874(3) 0.6412(5) 0.2431(4) 0.0355(14) Uani d . 1 C H31A 0.0637 0.6472 0.3056 0.043 Uiso calc R 1 H H31B 0.0533 0.6030 0.1985 0.043 Uiso calc R 1 H C32 0.1053(3) 0.7695(5) 0.2072(4) 0.0411(15) Uani d . 1 C H32A 0.0612 0.8165 0.2016 0.062 Uiso calc R 1 H H32B 0.1285 0.7642 0.1451 0.062 Uiso calc R 1 H H32C 0.1375 0.8091 0.2523 0.062 Uiso calc R 1 H C33 0.1374(3) 0.4448(5) 0.3092(4) 0.0370(14) Uani d . 1 C H33A 0.1825 0.3996 0.3178 0.044 Uiso calc R 1 H H33B 0.1198 0.4677 0.3729 0.044 Uiso calc R 1 H C34 0.0823(3) 0.3612(6) 0.2627(5) 0.0489(17) Uani d . 1 C H34A 0.0750 0.2901 0.3028 0.073 Uiso calc R 1 H H34B 0.0998 0.3358 0.2003 0.073 Uiso calc R 1 H H34C 0.0370 0.4042 0.2553 0.073 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0279(19) 0.033(2) 0.0286(19) -0.0060(16) -0.0058(17) 0.0042(16) O2 0.0235(19) 0.029(2) 0.0283(18) 0.0032(15) -0.0035(16) -0.0024(16) O3 0.036(2) 0.031(2) 0.0281(19) -0.0019(17) -0.0012(17) -0.0061(17) O4 0.033(2) 0.029(2) 0.028(2) -0.0014(17) 0.0006(16) 0.0003(16) C1 0.025(3) 0.019(2) 0.028(3) 0.003(2) -0.002(2) -0.003(2) C2 0.026(3) 0.023(3) 0.023(3) 0.004(2) -0.004(2) -0.003(2) C3 0.024(3) 0.027(3) 0.026(3) -0.004(2) 0.001(2) -0.002(2) C4 0.023(3) 0.032(3) 0.029(3) 0.004(2) -0.001(2) 0.001(2) C5 0.026(3) 0.025(3) 0.033(3) 0.001(2) -0.008(2) 0.002(2) C6 0.024(3) 0.025(3) 0.028(3) -0.002(2) 0.000(2) -0.005(2) C7 0.022(3) 0.034(3) 0.025(3) 0.009(2) 0.002(2) -0.001(2) C8 0.024(3) 0.034(3) 0.019(3) 0.006(2) 0.005(2) 0.003(2) C9 0.027(3) 0.028(3) 0.022(2) -0.005(2) 0.000(2) 0.001(2) C10 0.029(3) 0.027(3) 0.024(3) 0.002(2) 0.004(2) 0.002(2) C11 0.027(3) 0.030(3) 0.026(3) -0.003(2) 0.001(2) -0.001(2) C12 0.025(3) 0.040(3) 0.032(3) -0.005(2) -0.001(2) -0.002(3) C13 0.022(3) 0.040(3) 0.033(3) -0.001(2) -0.003(2) 0.002(3) C14 0.031(3) 0.032(3) 0.025(3) -0.003(2) 0.002(2) 0.002(2) C15 0.034(3) 0.023(3) 0.025(3) 0.003(2) 0.004(2) 0.003(2) C16 0.036(3) 0.020(3) 0.025(3) 0.001(2) -0.004(2) -0.003(2) C17 0.023(3) 0.022(3) 0.028(3) 0.006(2) -0.004(2) 0.001(2) C18 0.028(3) 0.029(3) 0.030(3) 0.006(2) 0.004(2) 0.003(2) C19 0.045(3) 0.027(3) 0.027(3) 0.002(3) 0.000(3) -0.004(2) C20 0.034(3) 0.020(3) 0.037(3) 0.001(2) -0.001(3) 0.001(2) C21 0.029(3) 0.029(3) 0.025(3) 0.005(2) 0.001(2) 0.000(2) C22 0.018(2) 0.032(3) 0.029(3) -0.003(2) 0.003(2) 0.001(2) C23 0.027(3) 0.029(3) 0.020(3) -0.002(2) 0.000(2) 0.003(2) C24 0.017(3) 0.030(3) 0.031(3) -0.001(2) 0.001(2) -0.001(2) C25 0.025(3) 0.030(3) 0.035(3) -0.002(2) -0.001(2) 0.006(3) C26 0.031(3) 0.036(3) 0.034(3) 0.002(3) 0.001(3) 0.005(3) C27 0.022(3) 0.036(3) 0.032(3) 0.001(2) 0.005(2) -0.004(3) C28 0.020(3) 0.030(3) 0.033(3) 0.000(2) -0.002(2) -0.001(2) N 0.028(2) 0.033(3) 0.030(2) 0.003(2) -0.004(2) 0.003(2) C29 0.033(3) 0.038(3) 0.039(3) 0.004(3) 0.008(3) 0.005(3) C30 0.042(4) 0.042(4) 0.082(5) 0.013(3) 0.018(3) 0.013(4) C31 0.031(3) 0.044(4) 0.031(3) 0.011(3) -0.005(3) -0.007(3) C32 0.051(4) 0.039(4) 0.033(3) 0.015(3) -0.011(3) 0.001(3) C33 0.040(3) 0.037(3) 0.034(3) -0.007(3) 0.007(3) -0.003(3) C34 0.051(4) 0.039(4) 0.057(4) -0.011(3) 0.011(3) -0.004(3) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 O1 H1 102.7 C9 O2 H2 112.2 C23 O4 H4 103.7 C6 C1 C2 117.2(4) C6 C1 C28 121.1(5) C2 C1 C28 121.7(4) O1 C2 C3 119.2(4) O1 C2 C1 118.9(4) C3 C2 C1 121.9(5) C4 C3 C2 118.5(5) C4 C3 C7 120.1(4) C2 C3 C7 121.3(5) C3 C4 C5 120.4(5) C3 C4 H4A 119.8 C5 C4 H4A 119.8 C6 C5 C4 119.8(5) C6 C5 H5A 120.1 C4 C5 H5A 120.1 C5 C6 C1 122.1(5) C5 C6 H6A 118.9 C1 C6 H6A 118.9 C3 C7 C8 112.8(4) C3 C7 H7A 109.0 C8 C7 H7A 109.0 C3 C7 H7B 109.0 C8 C7 H7B 109.0 H7A C7 H7B 107.8 C13 C8 C9 119.7(5) C13 C8 C7 119.5(5) C9 C8 C7 120.7(4) O2 C9 C8 120.8(4) O2 C9 C10 120.3(4) C8 C9 C10 118.9(5) C11 C10 C9 119.1(5) C11 C10 C14 120.2(5) C9 C10 C14 120.7(5) C12 C11 C10 121.6(5) C12 C11 H11A 119.2 C10 C11 H11A 119.2 C11 C12 C13 119.1(5) C11 C12 H12A 120.5 C13 C12 H12A 120.5 C12 C13 C8 121.6(5) C12 C13 H13A 119.2 C8 C13 H13A 119.2 C10 C14 C15 115.0(4) C10 C14 H14A 108.5 C15 C14 H14A 108.5 C10 C14 H14B 108.5 C15 C14 H14B 108.5 H14A C14 H14B 107.5 C20 C15 C16 118.1(5) C20 C15 C14 120.0(5) C16 C15 C14 122.0(4) O3 C16 C17 119.3(4) O3 C16 C15 118.8(4) C17 C16 C15 122.0(4) C16 C17 C18 117.8(5) C16 C17 C21 121.9(4) C18 C17 C21 120.1(4) C19 C18 C17 121.6(5) C19 C18 H18A 119.2 C17 C18 H18A 119.2 C18 C19 C20 119.6(5) C18 C19 H19A 120.2 C20 C19 H19A 120.2 C19 C20 C15 120.9(5) C19 C20 H20A 119.6 C15 C20 H20A 119.6 C22 C21 C17 109.9(4) C22 C21 H21A 109.7 C17 C21 H21A 109.7 C22 C21 H21B 109.7 C17 C21 H21B 109.7 H21A C21 H21B 108.2 C27 C22 C23 118.0(5) C27 C22 C21 120.9(5) C23 C22 C21 121.1(4) O4 C23 C22 120.7(4) O4 C23 C24 117.7(5) C22 C23 C24 121.6(4) C25 C24 C23 118.5(5) C25 C24 C28 120.8(5) C23 C24 C28 120.7(4) C24 C25 C26 120.6(5) C24 C25 H25A 119.7 C26 C25 H25A 119.7 C27 C26 C25 120.3(5) C27 C26 H26A 119.8 C25 C26 H26A 119.8 C26 C27 C22 120.8(5) C26 C27 H27A 119.6 C22 C27 H27A 119.6 C24 C28 C1 112.0(4) C24 C28 H28A 109.2 C1 C28 H28A 109.2 C24 C28 H28B 109.2 C1 C28 H28B 109.2 H28A C28 H28B 107.9 C31 N C29 112.2(4) C31 N C33 111.8(4) C29 N C33 113.0(4) C31 N H5 104.5 C29 N H5 103.3 C33 N H5 111.5 C30 C29 N 114.6(5) C30 C29 H29A 108.6 N C29 H29A 108.6 C30 C29 H29B 108.6 N C29 H29B 108.6 H29A C29 H29B 107.6 C29 C30 H30A 109.5 C29 C30 H30B 109.5 H30A C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 N C31 C32 112.7(5) N C31 H31A 109.0 C32 C31 H31A 109.0 N C31 H31B 109.0 C32 C31 H31B 109.0 H31A C31 H31B 107.8 C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C34 C33 N 114.3(5) C34 C33 H33A 108.7 N C33 H33A 108.7 C34 C33 H33B 108.7 N C33 H33B 108.7 H33A C33 H33B 107.6 C33 C34 H34A 109.5 C33 C34 H34B 109.5 H34A C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.386(6) O1 O2 2.544(5) O1 N 2.790(6) O1 H1 0.8251 O2 C9 1.346(6) O2 O3 2.478(5) O2 H2 0.8234 O3 C16 1.378(6) O3 O4 2.689(5) O4 C23 1.370(7) O4 H4 0.8213 C1 C6 1.389(7) C1 C2 1.403(7) C1 C28 1.522(7) C2 C3 1.400(6) C3 C4 1.393(7) C3 C7 1.508(7) C4 C5 1.390(7) C4 H4A 0.9300 C5 C6 1.375(6) C5 H5A 0.9300 C6 H6A 0.9300 C7 C8 1.522(7) C7 H7A 0.9700 C7 H7B 0.9700 C8 C13 1.391(7) C8 C9 1.408(7) C9 C10 1.427(7) C10 C11 1.400(7) C10 C14 1.511(7) C11 C12 1.380(7) C11 H11A 0.9300 C12 C13 1.388(7) C12 H12A 0.9300 C13 H13A 0.9300 C14 C15 1.512(7) C14 H14A 0.9700 C14 H14B 0.9700 C15 C20 1.405(7) C15 C16 1.405(7) C16 C17 1.394(7) C17 C18 1.405(7) C17 C21 1.513(7) C18 C19 1.381(7) C18 H18A 0.9300 C19 C20 1.390(7) C19 H19A 0.9300 C20 H20A 0.9300 C21 C22 1.505(7) C21 H21A 0.9700 C21 H21B 0.9700 C22 C27 1.400(7) C22 C23 1.404(7) C23 C24 1.407(7) C24 C25 1.388(7) C24 C28 1.515(7) C25 C26 1.394(7) C25 H25A 0.9300 C26 C27 1.388(7) C26 H26A 0.9300 C27 H27A 0.9300 C28 H28A 0.9700 C28 H28B 0.9700 N C31 1.497(6) N C29 1.501(7) N C33 1.520(7) N H5 0.8872 C29 C30 1.491(7) C29 H29A 0.9700 C29 H29B 0.9700 C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 C31 C32 1.516(8) C31 H31A 0.9700 C31 H31B 0.9700 C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 C34 1.504(8) C33 H33A 0.9700 C33 H33B 0.9700 C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600 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 N H5 O1 0.89 1.95 2.790(6) 158 O1 H1 O2 0.83 1.75 2.544(5) 162 O2 H2 O3 0.82 1.67 2.478(5) 169 O4 H4 O3 0.82 1.87 2.689(5) 177