data_30452 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of a ultra-high affinity macrocycle bound to HIV-1 TAR RNA ; _BMRB_accession_number 30452 _BMRB_flat_file_name bmr30452.str _Entry_type original _Submission_date 2018-04-13 _Accession_date 2018-04-13 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shortridge M. D. . 2 Varani G. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 324 "13C chemical shifts" 171 "15N chemical shifts" 11 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-07-19 update BMRB 'update entry citation' 2018-12-04 original author 'original release' stop_ _Original_release_date 2018-08-31 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; An ultra-high affinity ligand of HIV-1 TAR reveals the RNA structure recognized by P-TEFb ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30481318 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shortridge M. D. . 2 Wille P. T. . 3 Jones A. J. . 4 Davidson A. . . 5 Bogdanovic J. . . 6 Arts E. . . 7 Karn J. . . 8 Robinson J. A. . 9 Varani G. . . stop_ _Journal_abbreviation 'Nucleic Acids Res.' _Journal_volume 47 _Journal_issue 3 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1523 _Page_last 1531 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'DAB-VAL-ARG-THR-ARG-LYS-GLY-ARG-ARG-ILE-NOR-ILE-DPR-PRO/RNA Complex' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 entity_2 $entity_2 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 1697.087 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 14 _Mol_residue_sequence ; XVRTRKGRRIXIXP ; loop_ _Residue_seq_code _Residue_label 1 DAB 2 VAL 3 ARG 4 THR 5 ARG 6 LYS 7 GLY 8 ARG 9 ARG 10 ILE 11 4J5 12 ILE 13 DPR 14 PRO stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ save_entity_2 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class RNA _Name_common entity_2 _Molecular_mass 9307.555 _Mol_thiol_state 'not present' _Details . _Residue_count 29 _Mol_residue_sequence ; GGCAGAUCUGAGCCUGGGAG CUCUCUGCC ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 17 G 2 18 G 3 19 C 4 20 A 5 21 G 6 22 A 7 23 U 8 24 C 9 25 U 10 26 G 11 27 A 12 28 G 13 29 C 14 30 C 15 31 U 16 32 G 17 33 G 18 34 G 19 35 A 20 36 G 21 37 C 22 38 U 23 39 C 24 40 U 25 41 C 26 42 U 27 43 G 28 44 C 29 45 C stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_4J5 _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common amino{[(3S)-3-amino-3-carboxypropyl]amino}methaniminium _BMRB_code 4J5 _PDB_code 4J5 _Standard_residue_derivative . _Molecular_mass 161.182 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons OXT OXT O . 0 . ? C C C . 0 . ? N N N . 0 . ? O O O . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? ND ND N . 0 . ? CE CE C . 0 . ? CG CG C . 0 . ? HH11 HH11 H . 0 . ? NH1 NH1 N . 0 . ? NH2 NH2 N . 1 . ? H H H . 0 . ? HA HA H . 0 . ? HD HD H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HH12 HH12 H . 0 . ? HH21 HH21 H . 0 . ? HH22 HH22 H . 0 . ? HNA HNA H . 0 . ? HXT HXT H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name DOUB O C ? ? SING CA C ? ? SING C OXT ? ? SING CA N ? ? SING N H ? ? SING N HNA ? ? SING OXT HXT ? ? SING HA CA ? ? SING CA CB ? ? SING HB2 CB ? ? SING CB HB3 ? ? SING CB CG ? ? SING HD ND ? ? SING CE ND ? ? SING ND CG ? ? SING NH1 CE ? ? DOUB CE NH2 ? ? SING CG HG3 ? ? SING CG HG2 ? ? SING HH11 NH1 ? ? SING HH12 NH1 ? ? SING HH22 NH2 ? ? SING NH2 HH21 ? ? stop_ save_ save_chem_comp_DAB _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common '2,4-DIAMINOBUTYRIC ACID' _BMRB_code DAB _PDB_code DAB _Standard_residue_derivative . _Molecular_mass 118.134 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? ND ND N . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD1 HD1 H . 0 . ? HD2 HD2 H . 0 . ? HXT HXT H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N CA ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG ND ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING ND HD1 ? ? SING ND HD2 ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_DPR _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-PROLINE _BMRB_code DPR _PDB_code DPR _Standard_residue_derivative . _Molecular_mass 115.130 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD2 HD2 H . 0 . ? HD3 HD3 H . 0 . ? HXT HXT H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N CA ? ? SING N CD ? ? SING N H ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING CD HD2 ? ? SING CD HD3 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1 . 32630 . . . . $entity_2 . 32630 . . . . stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $entity_1 'recombinant technology' . . . . . $entity_2 'recombinant technology' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details ; 1.7 mM DAB-VAL-ARG-THR-ARG-LYS-GLY-ARG-ARG-ILE-NOR-ILE-DPR-PRO, 1.2 mM RNA (29-MER), 0.01 mM EDTA, 20 mM potassium phosphate, 10 mM sodium chloride, 95% H2O/5% D2O ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.7 mM 'natural abundance' $entity_2 1.2 mM 'natural abundance' EDTA 0.01 mM 'natural abundance' 'potassium phosphate' 20 mM 'natural abundance' 'sodium chloride' 10 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details ; 1.7 mM DAB-VAL-ARG-THR-ARG-LYS-GLY-ARG-ARG-ILE-NOR-ILE-DPR-PRO, 1.2 mM RNA (29-MER), 0.01 mM EDTA, 20 mM potassium phosphate, 10 mM sodium chloride, 100% D2O ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.7 mM 'natural abundance' $entity_2 1.2 mM 'natural abundance' EDTA 0.01 mM 'natural abundance' 'potassium phosphate' 20 mM 'natural abundance' 'sodium chloride' 10 mM 'natural abundance' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details ; 1.5 mM DAB-VAL-ARG-THR-ARG-LYS-GLY-ARG-ARG-ILE-NOR-ILE-DPR-PRO, 1.0 mM [U-99% 13C; U-99% 15N] RNA (29-MER), 0.01 mM EDTA, 20 mM potassium phosphate, 10 mM sodium chloride, 95% H2O/5% D2O ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.5 mM 'natural abundance' $entity_2 1.0 mM '[U-99% 13C; U-99% 15N]' EDTA 0.01 mM 'natural abundance' 'potassium phosphate' 20 mM 'natural abundance' 'sodium chloride' 10 mM 'natural abundance' stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details ; 1.5 mM DAB-VAL-ARG-THR-ARG-LYS-GLY-ARG-ARG-ILE-NOR-ILE-DPR-PRO, 1.0 mM [U-99% 13C; U-99% 15N] RNA (29-MER), 0.01 mM EDTA, 20 mM potassium phosphate, 10 mM sodium chloride, 100% D2O ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.5 mM 'natural abundance' $entity_2 1.0 mM '[U-99% 13C; U-99% 15N]' EDTA 0.01 mM 'natural abundance' 'potassium phosphate' 20 mM 'natural abundance' 'sodium chloride' 10 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name 'X-PLOR NIH' _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task refinement 'structure calculation' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details 'TCI cryoprobe' save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceII _Field_strength 600 _Details 'TCI cryoprobe' save_ save_NMR_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII _Field_strength 800 _Details 'TCI cryoprobe' save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_3 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_4 save_ save_3D_1H-15N_NOESY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_3 save_ save_3D_1H-13C_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY' _Sample_label $sample_4 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 30 . mM pH 6.5 . pH pressure 1 . atm temperature 277 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 30 . mM pH 6.5 . pH pressure 1 . atm temperature 303 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS C 13 'methyl protons' ppm 0.000 internal indirect . . . 0.25144953 DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.000 internal indirect . . . 0.10132912 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details 'high_temp sample conditions were also used.' loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC' '3D 1H-15N NOESY' '3D 1H-13C NOESY' stop_ loop_ _Sample_label $sample_3 $sample_2 $sample_1 $sample_4 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_2 _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 17 1 G H1 H 12 . . 2 17 1 G H1' H 5.78 . . 3 17 1 G H3' H 4.69 . . 4 17 1 G H4' H 4.53 . . 5 17 1 G H5' H 4.36 . . 6 17 1 G H5'' H 4.21 . . 7 17 1 G H8 H 8.08 . . 8 17 1 G C1' C 90.84 . . 9 17 1 G C2' C 74.2 . . 10 17 1 G C4' C 83.62 . . 11 17 1 G C5' C 67.43 . . 12 17 1 G C8 C 138.98 . . 13 17 1 G N1 N 147.4 . . 14 17 1 G HO2' H 4.9 . . 15 18 2 G H1 H 13.3 . . 16 18 2 G H1' H 5.87 . . 17 18 2 G H3' H 4.51 . . 18 18 2 G H4' H 4.46 . . 19 18 2 G H5' H 4.23 . . 20 18 2 G H5'' H 4.39 . . 21 18 2 G H8 H 7.59 . . 22 18 2 G H21 H 7.61 . . 23 18 2 G H22 H 6.06 . . 24 18 2 G C1' C 92.97 . . 25 18 2 G C2' C 75.29 . . 26 18 2 G C3' C 73.26 . . 27 18 2 G C4' C 81.72 . . 28 18 2 G C5' C 69.01 . . 29 18 2 G C8 C 136.78 . . 30 18 2 G N1 N 148.2 . . 31 18 2 G HO2' H 4.54 . . 32 19 3 C H1' H 5.5 . . 33 19 3 C H3' H 4.46 . . 34 19 3 C H4' H 4.41 . . 35 19 3 C H5 H 5.21 . . 36 19 3 C H5' H 4.58 . . 37 19 3 C H5'' H 5.22 . . 38 19 3 C H6 H 7.58 . . 39 19 3 C H41 H 8.38 . . 40 19 3 C H42 H 6.84 . . 41 19 3 C C1' C 93.9 . . 42 19 3 C C2' C 75.45 . . 43 19 3 C C3' C 72.03 . . 44 19 3 C C4' C 81.93 . . 45 19 3 C C5 C 97.41 . . 46 19 3 C C5' C 64.63 . . 47 19 3 C C6 C 140.65 . . 48 19 3 C HO2' H 4.57 . . 49 20 4 A H1' H 5.91 . . 50 20 4 A H2 H 6.84 . . 51 20 4 A H4' H 4.49 . . 52 20 4 A H5' H 4.45 . . 53 20 4 A H5'' H 4.47 . . 54 20 4 A H8 H 7.88 . . 55 20 4 A H61 H 7.73 . . 56 20 4 A H62 H 6.23 . . 57 20 4 A C1' C 93.03 . . 58 20 4 A C2 C 152.13 . . 59 20 4 A C2' C 75.99 . . 60 20 4 A C4' C 81.91 . . 61 20 4 A C5' C 65.9 . . 62 20 4 A C8 C 139.28 . . 63 20 4 A HO2' H 4.63 . . 64 21 5 G H1 H 12.52 . . 65 21 5 G H1' H 5.58 . . 66 21 5 G H3' H 4.44 . . 67 21 5 G H4' H 4.43 . . 68 21 5 G H5' H 4.45 . . 69 21 5 G H5'' H 4.03 . . 70 21 5 G H8 H 7.06 . . 71 21 5 G H21 H 7.95 . . 72 21 5 G H22 H 6.04 . . 73 21 5 G C1' C 92.47 . . 74 21 5 G C2' C 75.98 . . 75 21 5 G C3' C 72.31 . . 76 21 5 G C4' C 81.63 . . 77 21 5 G C5' C 65.2 . . 78 21 5 G C8 C 135.4 . . 79 21 5 G N1 N 146.5 . . 80 21 5 G HO2' H 4.37 . . 81 22 6 A H1' H 5.94 . . 82 22 6 A H2 H 7.05 . . 83 22 6 A H3' H 4.63 . . 84 22 6 A H4' H 4.39 . . 85 22 6 A H5' H 4.58 . . 86 22 6 A H5'' H 4.11 . . 87 22 6 A H8 H 7.78 . . 88 22 6 A H61 H 8.09 . . 89 22 6 A H62 H 6.32 . . 90 22 6 A C1' C 92.62 . . 91 22 6 A C2 C 154.02 . . 92 22 6 A C2' C 75.49 . . 93 22 6 A C3' C 72.52 . . 94 22 6 A C4' C 81.79 . . 95 22 6 A C5' C 64.59 . . 96 22 6 A C8 C 138.97 . . 97 22 6 A HO2' H 4.28 . . 98 23 7 U H1' H 5.88 . . 99 23 7 U H3 H 14.16 . . 100 23 7 U H4' H 4.73 . . 101 23 7 U H5 H 4.98 . . 102 23 7 U H5' H 4.51 . . 103 23 7 U H5'' H 4.32 . . 104 23 7 U H6 H 7.83 . . 105 23 7 U C1' C 90.63 . . 106 23 7 U C2' C 75.21 . . 107 23 7 U C4' C 83.7 . . 108 23 7 U C5 C 102.33 . . 109 23 7 U C5' C 70.56 . . 110 23 7 U C6 C 145.09 . . 111 23 7 U N3 N 161.5 . . 112 23 7 U HO2' H 5.05 . . 113 24 8 C H1' H 6.02 . . 114 24 8 C H3' H 4.76 . . 115 24 8 C H4' H 4.39 . . 116 24 8 C H5 H 6.03 . . 117 24 8 C H6 H 7.83 . . 118 24 8 C C1' C 91.58 . . 119 24 8 C C2' C 75.88 . . 120 24 8 C C3' C 74.86 . . 121 24 8 C C4' C 84.01 . . 122 24 8 C C5 C 99.44 . . 123 24 8 C C6 C 144.15 . . 124 24 8 C HO2' H 4.39 . . 125 25 9 U H1' H 6.09 . . 126 25 9 U H3' H 4.68 . . 127 25 9 U H4' H 4.6 . . 128 25 9 U H5 H 5.91 . . 129 25 9 U H5' H 4.24 . . 130 25 9 U H5'' H 4.17 . . 131 25 9 U H6 H 7.92 . . 132 25 9 U C1' C 90.24 . . 133 25 9 U C2' C 75.83 . . 134 25 9 U C3' C 77.36 . . 135 25 9 U C4' C 85.52 . . 136 25 9 U C5 C 105.43 . . 137 25 9 U C5' C 67.97 . . 138 25 9 U C6 C 144.25 . . 139 25 9 U HO2' H 4.44 . . 140 26 10 G H1 H 12.65 . . 141 26 10 G H1' H 5.94 . . 142 26 10 G H8 H 7.8 . . 143 26 10 G H21 H 8.08 . . 144 26 10 G H22 H 5.87 . . 145 26 10 G C1' C 94.51 . . 146 26 10 G C2' C 75.47 . . 147 26 10 G C8 C 138.02 . . 148 26 10 G N1 N 147.3 . . 149 26 10 G HO2' H 5.01 . . 150 27 11 A H1' H 5.97 . . 151 27 11 A H2 H 7.38 . . 152 27 11 A H2' H 4.65 . . 153 27 11 A H3' H 4.62 . . 154 27 11 A H4' H 4.57 . . 155 27 11 A H5' H 4.68 . . 156 27 11 A H5'' H 4.14 . . 157 27 11 A H8 H 7.88 . . 158 27 11 A H61 H 7.83 . . 159 27 11 A H62 H 6.52 . . 160 27 11 A C1' C 93.24 . . 161 27 11 A C2 C 153.53 . . 162 27 11 A C2' C 75.5 . . 163 27 11 A C3' C 73.26 . . 164 27 11 A C4' C 81.97 . . 165 27 11 A C5' C 65.03 . . 166 27 11 A C8 C 139.73 . . 167 27 11 A HO2' H 6.62 . . 168 28 12 G H1 H 13.72 . . 169 28 12 G H1' H 5.88 . . 170 28 12 G H3' H 4.51 . . 171 28 12 G H4' H 4.46 . . 172 28 12 G H5' H 4.38 . . 173 28 12 G H5'' H 4.24 . . 174 28 12 G H8 H 7.62 . . 175 28 12 G H21 H 8.77 . . 176 28 12 G H22 H 6.38 . . 177 28 12 G C1' C 92.64 . . 178 28 12 G C2' C 75.33 . . 179 28 12 G C3' C 73.27 . . 180 28 12 G C4' C 81.73 . . 181 28 12 G C5' C 69.01 . . 182 28 12 G C8 C 136.04 . . 183 28 12 G N1 N 147.8 . . 184 28 12 G HO2' H 4.54 . . 185 29 13 C H1' H 5.45 . . 186 29 13 C H3' H 4.29 . . 187 29 13 C H5 H 5.14 . . 188 29 13 C H5' H 4.52 . . 189 29 13 C H5'' H 4.02 . . 190 29 13 C H6 H 7.42 . . 191 29 13 C H41 H 8.33 . . 192 29 13 C H42 H 6.87 . . 193 29 13 C C1' C 94.17 . . 194 29 13 C C2' C 75.38 . . 195 29 13 C C3' C 72.16 . . 196 29 13 C C5 C 97.16 . . 197 29 13 C C5' C 64.56 . . 198 29 13 C C6 C 140.37 . . 199 29 13 C HO2' H 4.28 . . 200 30 14 C H1' H 5.66 . . 201 30 14 C H3' H 4.36 . . 202 30 14 C H4' H 4.3 . . 203 30 14 C H5 H 5.47 . . 204 30 14 C H6 H 7.62 . . 205 30 14 C C1' C 93.09 . . 206 30 14 C C2' C 75.97 . . 207 30 14 C C3' C 73.68 . . 208 30 14 C C4' C 82.71 . . 209 30 14 C C5 C 98.23 . . 210 30 14 C C6 C 141.39 . . 211 30 14 C HO2' H 4.35 . . 212 31 15 U H1' H 5.47 . . 213 31 15 U H3' H 4.41 . . 214 31 15 U H4' H 4.19 . . 215 31 15 U H5 H 5.6 . . 216 31 15 U H6 H 7.62 . . 217 31 15 U C1' C 92.57 . . 218 31 15 U C2' C 75.52 . . 219 31 15 U C3' C 72.03 . . 220 31 15 U C4' C 83.98 . . 221 31 15 U C5 C 104.53 . . 222 31 15 U C6 C 142.21 . . 223 31 15 U HO2' H 4.19 . . 224 32 16 G H1' H 5.41 . . 225 32 16 G H3' H 4.56 . . 226 32 16 G H4' H 4.1 . . 227 32 16 G H5' H 3.89 . . 228 32 16 G H5'' H 3.99 . . 229 32 16 G H8 H 7.65 . . 230 32 16 G C1' C 89.57 . . 231 32 16 G C2' C 78.15 . . 232 32 16 G C3' C 72.04 . . 233 32 16 G C4' C 85.27 . . 234 32 16 G C5' C 67.73 . . 235 32 16 G C8 C 140.73 . . 236 32 16 G HO2' H 4.56 . . 237 33 17 G H1' H 5.66 . . 238 33 17 G H4' H 4.24 . . 239 33 17 G H8 H 7.32 . . 240 33 17 G C1' C 89.59 . . 241 33 17 G C2' C 75.29 . . 242 33 17 G C4' C 84.98 . . 243 33 17 G C8 C 139.63 . . 244 33 17 G HO2' H 4.7 . . 245 34 18 G H1' H 5.89 . . 246 34 18 G H4' H 4.53 . . 247 34 18 G H8 H 7.9 . . 248 34 18 G C1' C 88.49 . . 249 34 18 G C2' C 75.67 . . 250 34 18 G C4' C 84.7 . . 251 34 18 G C8 C 138.4 . . 252 34 18 G HO2' H 4.86 . . 253 35 19 A H1' H 6.09 . . 254 35 19 A H2 H 8.16 . . 255 35 19 A H3' H 4.88 . . 256 35 19 A H4' H 4.55 . . 257 35 19 A H5' H 4.34 . . 258 35 19 A H8 H 8.43 . . 259 35 19 A C1' C 89.42 . . 260 35 19 A C2 C 155.53 . . 261 35 19 A C2' C 77.12 . . 262 35 19 A C3' C 76.14 . . 263 35 19 A C4' C 85.93 . . 264 35 19 A C5' C 68.32 . . 265 35 19 A C8 C 142.2 . . 266 35 19 A HO2' H 4.9 . . 267 36 20 G H1 H 13.08 . . 268 36 20 G H1' H 5.78 . . 269 36 20 G H3' H 4.48 . . 270 36 20 G H4' H 4.52 . . 271 36 20 G H5' H 4.54 . . 272 36 20 G H5'' H 4.39 . . 273 36 20 G H8 H 7.57 . . 274 36 20 G H21 H 8.77 . . 275 36 20 G H22 H 6.25 . . 276 36 20 G C1' C 92.89 . . 277 36 20 G C3' C 72.14 . . 278 36 20 G C4' C 82.6 . . 279 36 20 G C5' C 64.65 . . 280 36 20 G C8 C 137.01 . . 281 36 20 G N1 N 148.4 . . 282 37 21 C H1' H 5.59 . . 283 37 21 C H4' H 4.44 . . 284 37 21 C H5 H 5.17 . . 285 37 21 C H5' H 4.53 . . 286 37 21 C H5'' H 4.08 . . 287 37 21 C H6 H 7.84 . . 288 37 21 C H41 H 8.79 . . 289 37 21 C H42 H 6.98 . . 290 37 21 C C1' C 94.13 . . 291 37 21 C C2' C 75.38 . . 292 37 21 C C4' C 82.15 . . 293 37 21 C C5 C 96.9 . . 294 37 21 C C5' C 64.47 . . 295 37 21 C C6 C 141.5 . . 296 37 21 C HO2' H 4.52 . . 297 38 22 U H1' H 5.67 . . 298 38 22 U H3 H 14.37 . . 299 38 22 U H3' H 4.41 . . 300 38 22 U H4' H 4.36 . . 301 38 22 U H5 H 5.4 . . 302 38 22 U H5' H 4.5 . . 303 38 22 U H5'' H 4.08 . . 304 38 22 U H6 H 7.71 . . 305 38 22 U C1' C 93.27 . . 306 38 22 U C2' C 75.97 . . 307 38 22 U C3' C 72.8 . . 308 38 22 U C4' C 81.88 . . 309 38 22 U C5 C 103.53 . . 310 38 22 U C5' C 65.08 . . 311 38 22 U C6 C 141.5 . . 312 38 22 U N3 N 162.3 . . 313 38 22 U HO2' H 4.73 . . 314 39 23 C H1' H 5.12 . . 315 39 23 C H3' H 3.9 . . 316 39 23 C H4' H 4.51 . . 317 39 23 C H5 H 5.55 . . 318 39 23 C H5' H 4.23 . . 319 39 23 C H5'' H 4.06 . . 320 39 23 C H6 H 7.44 . . 321 39 23 C H41 H 8.43 . . 322 39 23 C H42 H 7.22 . . 323 39 23 C C1' C 95.54 . . 324 39 23 C C2' C 75.62 . . 325 39 23 C C3' C 73.92 . . 326 39 23 C C4' C 82.98 . . 327 39 23 C C5 C 98.89 . . 328 39 23 C C5' C 68.48 . . 329 39 23 C C6 C 140.84 . . 330 39 23 C HO2' H 4.44 . . 331 40 24 U H1' H 5.43 . . 332 40 24 U H3 H 13.91 . . 333 40 24 U H3' H 4.47 . . 334 40 24 U H4' H 4.32 . . 335 40 24 U H5 H 5.39 . . 336 40 24 U H5' H 4.53 . . 337 40 24 U H5'' H 4.02 . . 338 40 24 U H6 H 7.9 . . 339 40 24 U C1' C 93.88 . . 340 40 24 U C2' C 74.83 . . 341 40 24 U C3' C 71.78 . . 342 40 24 U C4' C 82.24 . . 343 40 24 U C5 C 102.69 . . 344 40 24 U C5' C 64.07 . . 345 40 24 U C6 C 141.88 . . 346 40 24 U N3 N 162.2 . . 347 40 24 U HO2' H 4.31 . . 348 41 25 C H1' H 5.42 . . 349 41 25 C H3' H 4.45 . . 350 41 25 C H5 H 5.61 . . 351 41 25 C H6 H 7.9 . . 352 41 25 C H41 H 8.37 . . 353 41 25 C H42 H 7.05 . . 354 41 25 C C1' C 93.8 . . 355 41 25 C C2' C 75.37 . . 356 41 25 C C3' C 71.96 . . 357 41 25 C C5 C 96.96 . . 358 41 25 C C6 C 141.94 . . 359 41 25 C HO2' H 4.22 . . 360 42 26 U H1' H 5.42 . . 361 42 26 U H3 H 13.56 . . 362 42 26 U H3' H 4.47 . . 363 42 26 U H4' H 4.57 . . 364 42 26 U H5 H 5.32 . . 365 42 26 U H6 H 7.84 . . 366 42 26 U C1' C 93.64 . . 367 42 26 U C2' C 75.34 . . 368 42 26 U C3' C 71.9 . . 369 42 26 U C4' C 82 . . 370 42 26 U C5 C 103.35 . . 371 42 26 U C6 C 141.8 . . 372 42 26 U N3 N 162.1 . . 373 42 26 U HO2' H 4.53 . . 374 43 27 G H1 H 12.44 . . 375 43 27 G H1' H 5.72 . . 376 43 27 G H3' H 4.56 . . 377 43 27 G H4' H 4.44 . . 378 43 27 G H8 H 7.71 . . 379 43 27 G H21 H 8.11 . . 380 43 27 G H22 H 5.98 . . 381 43 27 G C1' C 92.89 . . 382 43 27 G C2' C 75.35 . . 383 43 27 G C3' C 72.8 . . 384 43 27 G C4' C 81.93 . . 385 43 27 G C8 C 136.38 . . 386 43 27 G N1 N 147.5 . . 387 43 27 G HO2' H 4.45 . . 388 44 28 C H1' H 5.45 . . 389 44 28 C H3' H 4.4 . . 390 44 28 C H5 H 5.15 . . 391 44 28 C H6 H 7.63 . . 392 44 28 C H41 H 8.47 . . 393 44 28 C H42 H 6.85 . . 394 44 28 C C1' C 94.29 . . 395 44 28 C C2' C 75.69 . . 396 44 28 C C3' C 72.05 . . 397 44 28 C C5 C 96.98 . . 398 44 28 C C6 C 141.23 . . 399 44 28 C HO2' H 4.19 . . 400 45 29 C H1' H 5.73 . . 401 45 29 C H3' H 4.14 . . 402 45 29 C H4' H 4.12 . . 403 45 29 C H5 H 5.47 . . 404 45 29 C H5' H 4.43 . . 405 45 29 C H5'' H 4 . . 406 45 29 C H6 H 7.63 . . 407 45 29 C C1' C 92.77 . . 408 45 29 C C2' C 77.56 . . 409 45 29 C C3' C 69.68 . . 410 45 29 C C4' C 83.43 . . 411 45 29 C C5 C 98.23 . . 412 45 29 C C5' C 65.1 . . 413 45 29 C C6 C 141.88 . . 414 45 29 C HO2' H 3.96 . . stop_ save_ save_assigned_chemical_shifts_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC' '3D 1H-15N NOESY' '3D 1H-13C NOESY' stop_ loop_ _Sample_label $sample_3 $sample_2 $sample_1 $sample_4 stop_ _Sample_conditions_label $sample_conditions_2 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_1 _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 1 DAB H H 7.7 . . 2 1 1 DAB HA H 4.551 . . 3 1 1 DAB HB2 H 2.11 . . 4 1 1 DAB HB3 H 2.17 . . 5 1 1 DAB HD1 H 7.97 . . 6 1 1 DAB HD2 H 7.97 . . 7 1 1 DAB HD3 H 7.97 . . 8 1 1 DAB HG2 H 2.85 . . 9 1 1 DAB HG3 H 3.02 . . 10 2 2 VAL H H 8.71 . . 11 2 2 VAL HA H 4.875 . . 12 2 2 VAL HB H 1.92 . . 13 2 2 VAL HG1 H 0.72 . . 14 3 3 ARG H H 8.57 . . 15 3 3 ARG HA H 4.75 . . 16 3 3 ARG HB2 H 1.987 . . 17 3 3 ARG HB3 H 1.689 . . 18 3 3 ARG HG2 H 1.512 . . 19 3 3 ARG HG3 H 1.459 . . 20 3 3 ARG HE H 7.13 . . 21 4 4 THR H H 7.94 . . 22 4 4 THR HA H 5.02 . . 23 4 4 THR HB H 3.925 . . 24 4 4 THR HG2 H 0.98 . . 25 5 5 ARG H H 8.98 . . 26 5 5 ARG HA H 4.36 . . 27 5 5 ARG HB3 H 1.685 . . 28 5 5 ARG HG2 H 1.185 . . 29 5 5 ARG HG3 H 1.28 . . 30 5 5 ARG HD2 H 3.065 . . 31 5 5 ARG HE H 6.52 . . 32 6 6 LYS H H 9.54 . . 33 6 6 LYS HA H 3.72 . . 34 6 6 LYS HB2 H 1.777 . . 35 6 6 LYS HG2 H 1.305 . . 36 6 6 LYS HG3 H 1.215 . . 37 6 6 LYS HD2 H 1.616 . . 38 6 6 LYS HD3 H 1.524 . . 39 6 6 LYS HE2 H 2.944 . . 40 6 6 LYS HE3 H 2.944 . . 41 6 6 LYS HZ H 7.56 . . 42 7 7 GLY H H 8.77 . . 43 7 7 GLY HA2 H 4.1 . . 44 7 7 GLY HA3 H 3.483 . . 45 8 8 ARG H H 7.75 . . 46 8 8 ARG HA H 4.52 . . 47 8 8 ARG HB2 H 1.841 . . 48 8 8 ARG HB3 H 1.752 . . 49 8 8 ARG HG2 H 1.573 . . 50 8 8 ARG HG3 H 1.545 . . 51 8 8 ARG HD2 H 2.935 . . 52 8 8 ARG HE H 7.18 . . 53 9 9 ARG H H 8.72 . . 54 9 9 ARG HA H 4.69 . . 55 9 9 ARG HB2 H 1.718 . . 56 9 9 ARG HB3 H 1.602 . . 57 9 9 ARG HG2 H 1.492 . . 58 9 9 ARG HD2 H 3.06 . . 59 10 10 ILE H H 8.89 . . 60 10 10 ILE HA H 4.479 . . 61 10 10 ILE HB H 1.627 . . 62 10 10 ILE HG12 H 1.225 . . 63 10 10 ILE HG13 H 1.225 . . 64 10 10 ILE HG2 H 0.7599 . . 65 10 10 ILE HD1 H 0.6637 . . 66 11 11 4J5 H H 8.72 . . 67 11 11 4J5 HA H 4.74 . . 68 11 11 4J5 HB2 H 1.999 . . 69 11 11 4J5 HB3 H 1.934 . . 70 11 11 4J5 HD H 6.79 . . 71 11 11 4J5 HG2 H 2.951 . . 72 11 11 4J5 HG3 H 2.866 . . 73 12 12 ILE H H 8.64 . . 74 12 12 ILE HA H 4.86 . . 75 12 12 ILE HB H 1.699 . . 76 12 12 ILE HG12 H 1.245 . . 77 12 12 ILE HG13 H 1.071 . . 78 12 12 ILE HG2 H 0.8056 . . 79 12 12 ILE HD1 H 0.6893 . . 80 13 13 DPR HA H 4.541 . . 81 13 13 DPR HB2 H 2.324 . . 82 13 13 DPR HB3 H 2.121 . . 83 13 13 DPR HD2 H 3.91 . . 84 13 13 DPR HD3 H 3.443 . . 85 13 13 DPR HG2 H 2.066 . . 86 13 13 DPR HG3 H 1.888 . . 87 14 14 PRO HA H 4.327 . . 88 14 14 PRO HB2 H 2.301 . . 89 14 14 PRO HB3 H 2.114 . . 90 14 14 PRO HG2 H 2.042 . . 91 14 14 PRO HD2 H 3.971 . . 92 14 14 PRO HD3 H 3.748 . . stop_ save_