data_19387 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of an intramolecular (3+1) human telomeric G-quadruplex bound to a telomestatin derivative ; _BMRB_accession_number 19387 _BMRB_flat_file_name bmr19387.str _Entry_type original _Submission_date 2013-07-24 _Accession_date 2013-07-24 _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 Chung 'Wan Jun' . . 2 Heddi Brahim . . 3 Tera Masayuki . . 4 Iida Keisuke . . 5 Nagasawa Kazuo . . 6 Phan 'Anh Tuan' . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 240 "31P chemical shifts" 23 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-10-03 update BMRB 'update entry citation' 2013-08-26 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Solution structure of an intramolecular (3 + 1) human telomeric g-quadruplex bound to a telomestatin derivative.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 23909929 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Chung 'Wan Jun' . . 2 Heddi Brahim . . 3 Tera Masayuki . . 4 Iida Keisuke . . 5 Nagasawa Kazuo . . 6 Phan 'Anh Tuan' . . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_name_full 'Journal of the American Chemical Society' _Journal_volume 135 _Journal_issue 36 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 13495 _Page_last 13501 _Year 2013 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'intramolecular (3+1) human telomeric G-quadruplex bound to a telomestatin derivative' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'DNA (5'-D(*TP*TP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*A)-3')' $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') L2H $entity_L2H stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class DNA _Name_common DNA_(5'-D(*TP*TP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*A)-3') _Molecular_mass 7591.945 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 24 _Mol_residue_sequence ; TTGGGTTAGGGTTAGGGTTA GGGA ; loop_ _Residue_seq_code _Residue_label 1 DT 2 DT 3 DG 4 DG 5 DG 6 DT 7 DT 8 DA 9 DG 10 DG 11 DG 12 DT 13 DT 14 DA 15 DG 16 DG 17 DG 18 DT 19 DT 20 DA 21 DG 22 DG 23 DG 24 DA stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_L2H _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common "entity_L2H ((12S,27S)-12,27-bis(4-aminobutyl)-4,30-dimethyl-3,7,14,18,22,29-hexaoxa-11,26,31,32,33,34,35,36-octaazaheptacyclo[26.2.1.1~2,5~.1~6,9~.1~13,16~.1~17,20~.1~21,24~]hexatriaconta-1(30),2(36),4,6(35),8,13(34),15,17(33),19,21(32),23,28(31)-dodecaene-10,25-dione)" _BMRB_code L2H _PDB_code L2H _Molecular_mass 686.675 _Mol_charge 0 _Mol_paramagnetic . _Mol_aromatic yes _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C . 0 . ? C10 C10 C . 0 . ? C11 C11 C . 0 . ? C12 C12 C . 0 . ? C13 C13 C . 0 . ? C14 C14 C . 0 . ? C15 C15 C . 0 . ? C16 C16 C . 0 . ? C17 C17 C . 0 . ? C18 C18 C . 0 . ? C19 C19 C . 0 . ? C2 C2 C . 0 . ? C20 C20 C . 0 . ? C21 C21 C . 0 . ? C22 C22 C . 0 . ? C23 C23 C . 0 . ? C24 C24 C . 0 . ? C25 C25 C . 0 . ? C26 C26 C . 0 . ? C27 C27 C . 0 . ? C28 C28 C . 0 . ? C29 C29 C . 0 . ? C3 C3 C . 0 . ? C30 C30 C . 0 . ? C31 C31 C . 0 . ? C32 C32 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? C7 C7 C . 0 . ? C8 C8 C . 0 . ? C9 C9 C . 0 . ? HA1 HA1 H . 0 . ? HA2 HA2 H . 0 . ? HA2' HA2' H . 0 . ? HA3' HA3' H . 0 . ? HB1 HB1 H . 0 . ? HB1' HB1' H . 0 . ? HB2 HB2 H . 0 . ? HB2' HB2' H . 0 . ? HC1 HC1 H . 0 . ? HC1' HC1' H . 0 . ? HC2 HC2 H . 0 . ? HC2' HC2' H . 0 . ? HD1 HD1 H . 0 . ? HD1' HD1' H . 0 . ? HD2 HD2 H . 0 . ? HD2' HD2' H . 0 . ? HE1 HE1 H . 0 . ? HE1' HE1' H . 0 . ? HE2 HE2 H . 0 . ? HE2' HE2' H . 0 . ? HF HF H . 0 . ? HF' HF' H . 0 . ? HG HG H . 0 . ? HH HH H . 0 . ? HI HI H . 0 . ? HJ HJ H . 0 . ? HK HK H . 0 . ? HL HL H . 0 . ? HM1 HM1 H . 0 . ? HM2 HM2 H . 0 . ? HM3 HM3 H . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? HN3 HN3 H . 0 . ? N1 N1 N . 0 . ? N10 N10 N . 0 . ? N2 N2 N . 0 . ? N3 N3 N . 0 . ? N4 N4 N . 0 . ? N5 N5 N . 0 . ? N6 N6 N . 0 . ? N7 N7 N . 0 . ? N8 N8 N . 0 . ? N9 N9 N . 0 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O6 O6 O . 0 . ? O7 O7 O . 0 . ? O8 O8 O . 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 N10 C20 ? ? DOUB O5 C21 ? ? SING C23 O6 ? ? DOUB C23 C22 ? ? SING C20 C19 ? ? SING C21 C22 ? ? SING C21 N5 ? ? SING O6 C24 ? ? SING C22 N6 ? ? SING C19 C18 ? ? SING O4 C15 ? ? SING O4 C14 ? ? SING C16 C15 ? ? SING C16 N5 ? ? SING C16 C17 ? ? DOUB C15 N4 ? ? DOUB C24 N6 ? ? SING C24 C25 ? ? DOUB C14 C13 ? ? SING N4 C13 ? ? SING C27 C26 ? ? SING C13 C12 ? ? SING C18 C17 ? ? DOUB C25 C26 ? ? SING C25 N7 ? ? SING C26 O7 ? ? SING C12 O3 ? ? DOUB C12 N3 ? ? DOUB N7 C28 ? ? SING O3 C11 ? ? SING O7 C28 ? ? SING N3 C10 ? ? SING C28 C29 ? ? DOUB C11 C10 ? ? SING C10 C9 ? ? SING C29 N8 ? ? DOUB C29 C30 ? ? DOUB C9 N2 ? ? SING C9 O2 ? ? SING C31 C30 ? ? DOUB N8 C32 ? ? SING N2 C7 ? ? SING C30 O8 ? ? SING O2 C8 ? ? DOUB C7 C8 ? ? SING C7 C6 ? ? SING C32 O8 ? ? SING C32 C5 ? ? SING N1 C6 ? ? SING N1 C5 ? ? DOUB C6 O1 ? ? SING C5 C4 ? ? SING C4 C3 ? ? SING C2 C3 ? ? SING C2 C1 ? ? SING N9 C1 ? ? SING C1 HB2 ? ? SING C1 HB1 ? ? SING C2 HC2 ? ? SING C2 HC1 ? ? SING C5 HF ? ? SING C3 HD2 ? ? SING C3 HD1 ? ? SING C20 HB2' ? ? SING C20 HB1' ? ? SING C19 HC2' ? ? SING C19 HC1' ? ? SING C18 HD1' ? ? SING C18 HD2' ? ? SING C23 HL ? ? SING C4 HE1 ? ? SING C4 HE2 ? ? SING C8 HH ? ? SING C17 HE1' ? ? SING C17 HE2' ? ? SING C31 HN3 ? ? SING C31 HN2 ? ? SING C31 HN1 ? ? SING C11 HI ? ? SING C27 HM1 ? ? SING C27 HM3 ? ? SING C27 HM2 ? ? SING C16 HF' ? ? SING C14 HJ ? ? SING N9 HA1 ? ? SING N9 HA2 ? ? SING N10 HA3' ? ? SING N10 HA2' ? ? SING N5 HK ? ? SING N1 HG ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') . . . . . . 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 $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') 'chemical synthesis' . . . . . $entity_L2H 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') . mM 0.2 2 'natural abundance' $entity_L2H . mM 0.2 2 'natural abundance' KPi 20 mM . . 'natural abundance' KCl 70 mM . . 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') . mM 0.2 2 'natural abundance' $entity_L2H . mM 0.2 2 'natural abundance' KPi 20 mM . . 'natural abundance' KCl 70 mM . . 'natural abundance' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') 0.2 mM '[U-99% 13C; U-99% 15N]' $entity_L2H 0.2 mM 'natural abundance' KPi 20 mM 'natural abundance' KCl 70 mM 'natural abundance' stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') 0.2 mM '[U-99% 13C; U-99% 15N]' $entity_L2H 0.2 mM 'natural abundance' KPi 20 mM 'natural abundance' KCl 70 mM 'natural abundance' stop_ save_ save_sample_5 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $DNA_(5'-D(TTGGGTTAGGGTTAGGGTTAGGGA)-3') . mM 0.2 1 '[U-4% 13C]' $entity_L2H . mM 0.2 1 'natural abundance' KPi 20 mM . . 'natural abundance' KCl 70 mM . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_AMBER _Saveframe_category software _Name AMBER _Version . loop_ _Vendor _Address _Electronic_address 'Case, Darden, Cheatham, III, Simmerling, Wang, Duke, Luo, ... and Kollman' . . stop_ loop_ _Task refinement stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'data analysis' 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_X-PLOR_NIH _Saveframe_category software _Name X-PLOR_NIH _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task refinement 'structure solution' stop_ _Details . save_ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 600 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 700 _Details . save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 400 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 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-1H_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_aromatic_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_aromatic_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $sample_5 save_ save_2D_1H-13C_HSQC_aliphatic_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_aliphatic_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_5 save_ save_2D_1H-13C_HSQC_aliphatic_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_4 save_ save_2D_1H-13C_HSQC_aromatic_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $sample_4 save_ save_1D_JRHMBC_13 _Saveframe_category NMR_applied_experiment _Experiment_name '1D JRHMBC' _Sample_label $sample_3 save_ save_2D_1H-31P_HSQC_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-31P HSQC' _Sample_label $sample_2 save_ save_NMR_spectrometer_expt _Saveframe_category NMR_applied_experiment _Experiment_name . _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details '20mM KPi and 70mM KCl' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 310 . K pH 7 . pH pressure 1 . atm 'ionic strength' 90 . mM stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details '20mM KPi and 70mM KCl' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 298 . K pH 7 . pH pressure 1 . atm 'ionic strength' 90 . mM stop_ save_ save_sample_conditions_3 _Saveframe_category sample_conditions _Details '20mM KPi and 20mM KCl' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 298 . K pH 7 . pH pressure 1 . atm 'ionic strength' 40 . mM stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_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 H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS P 31 'methyl protons' ppm 0.00 na indirect . . . 0.404808636 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_chem_shift_list_1_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-31P HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_3 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'DNA (5'-D(*TP*TP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*TP*TP*AP*GP*GP*GP*A)-3')' _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 DT H1' H 5.884 0.007 1 2 1 1 DT H2' H 2.097 0.004 1 3 1 1 DT H2'' H 2.364 0.004 1 4 1 1 DT H3' H 4.661 0.025 1 5 1 1 DT H4' H 4.058 0.002 1 6 1 1 DT H5' H 3.576 0.003 1 7 1 1 DT H5'' H 3.623 0.002 1 8 1 1 DT H6 H 7.332 0.005 1 9 1 1 DT H71 H 1.534 0.002 2 10 1 1 DT H72 H 1.534 0.002 2 11 1 1 DT H73 H 1.534 0.002 2 12 2 2 DT H1' H 6.262 0.004 1 13 2 2 DT H2' H 2.405 0.003 1 14 2 2 DT H2'' H 2.634 0.009 1 15 2 2 DT H3' H 4.917 0.023 1 16 2 2 DT H4' H 4.404 0.029 1 17 2 2 DT H5' H 4.052 0.001 1 18 2 2 DT H5'' H 4.110 0.001 1 19 2 2 DT H6 H 7.593 0.002 1 20 2 2 DT H71 H 1.756 0.001 2 21 2 2 DT H72 H 1.756 0.001 2 22 2 2 DT H73 H 1.756 0.001 2 23 2 2 DT P P -0.378 0.001 1 24 3 3 DG H1 H 11.051 0.165 1 25 3 3 DG H1' H 6.000 0.003 1 26 3 3 DG H2' H 2.937 0.005 1 27 3 3 DG H2'' H 3.340 0.002 1 28 3 3 DG H3' H 4.928 0.025 1 29 3 3 DG H4' H 4.529 0.027 1 30 3 3 DG H5' H 4.265 0.004 1 31 3 3 DG H5'' H 4.321 0.003 1 32 3 3 DG H8 H 7.176 0.002 1 33 3 3 DG H21 H 8.068 1.405 2 34 3 3 DG H22 H 8.068 1.405 2 35 3 3 DG P P 0.335 0.001 1 36 4 4 DG H1 H 11.248 0.002 1 37 4 4 DG H1' H 5.745 0.001 1 38 4 4 DG H2' H 2.548 0.002 1 39 4 4 DG H2'' H 2.664 0.002 1 40 4 4 DG H3' H 5.027 0.025 1 41 4 4 DG H4' H 4.310 0.027 1 42 4 4 DG H5' H 4.005 0.002 1 43 4 4 DG H5'' H 4.096 0.003 1 44 4 4 DG H8 H 7.899 0.002 1 45 4 4 DG P P -0.635 0.007 1 46 5 5 DG H1 H 10.808 0.001 1 47 5 5 DG H1' H 6.311 0.000 1 48 5 5 DG H2' H 2.554 0.003 1 49 5 5 DG H2'' H 2.666 0.003 1 50 5 5 DG H3' H 5.060 0.026 1 51 5 5 DG H4' H 4.158 0.028 1 52 5 5 DG H8 H 7.770 0.000 1 53 5 5 DG P P -0.466 0.007 1 54 6 6 DT H1' H 6.449 0.005 1 55 6 6 DT H2' H 2.366 0.003 1 56 6 6 DT H2'' H 2.594 0.004 1 57 6 6 DT H3' H 4.824 0.028 1 58 6 6 DT H4' H 4.490 0.026 1 59 6 6 DT H5' H 4.094 0.002 1 60 6 6 DT H5'' H 4.279 0.004 1 61 6 6 DT H6 H 7.834 0.004 1 62 6 6 DT H71 H 2.007 0.001 2 63 6 6 DT H72 H 2.007 0.001 2 64 6 6 DT H73 H 2.007 0.001 2 65 6 6 DT P P -0.181 0.001 1 66 7 7 DT H1' H 6.460 0.002 1 67 7 7 DT H2' H 2.465 0.004 1 68 7 7 DT H2'' H 2.622 0.003 1 69 7 7 DT H3' H 5.008 0.025 1 70 7 7 DT H4' H 4.411 0.029 1 71 7 7 DT H6 H 7.844 0.005 1 72 7 7 DT H71 H 2.116 0.001 2 73 7 7 DT H72 H 2.116 0.001 2 74 7 7 DT H73 H 2.116 0.001 2 75 7 7 DT P P -0.547 0.000 1 76 8 8 DA H1' H 6.470 0.003 1 77 8 8 DA H2 H 7.958 0.005 1 78 8 8 DA H2' H 2.873 0.003 1 79 8 8 DA H2'' H 3.052 0.003 1 80 8 8 DA H3' H 5.123 0.027 1 81 8 8 DA H4' H 4.518 0.028 1 82 8 8 DA H5' H 4.185 0.001 1 83 8 8 DA H5'' H 4.283 0.002 1 84 8 8 DA H8 H 8.551 0.001 1 85 8 8 DA P P 0.504 0.001 1 86 9 9 DG H1 H 11.318 0.140 1 87 9 9 DG H1' H 5.995 0.001 1 88 9 9 DG H2' H 2.988 0.003 1 89 9 9 DG H2'' H 3.444 0.002 1 90 9 9 DG H3' H 5.061 0.036 1 91 9 9 DG H4' H 4.489 0.037 1 92 9 9 DG H8 H 7.428 0.002 1 93 9 9 DG P P -0.044 0.002 1 94 10 10 DG H1 H 11.803 0.001 1 95 10 10 DG H1' H 5.656 0.001 1 96 10 10 DG H2' H 2.626 0.003 2 97 10 10 DG H2'' H 2.626 0.003 2 98 10 10 DG H3' H 5.085 0.028 1 99 10 10 DG H4' H 4.380 0.029 1 100 10 10 DG H5' H 4.272 0.002 1 101 10 10 DG H5'' H 4.332 0.001 1 102 10 10 DG H8 H 8.057 0.001 1 103 10 10 DG P P -0.528 0.001 1 104 11 11 DG H1 H 11.124 0.016 1 105 11 11 DG H1' H 6.282 0.002 1 106 11 11 DG H2' H 2.541 0.003 1 107 11 11 DG H2'' H 2.664 0.006 1 108 11 11 DG H3' H 5.049 0.031 1 109 11 11 DG H4' H 4.518 0.032 1 110 11 11 DG H8 H 7.931 0.003 1 111 11 11 DG P P 0.169 0.004 1 112 12 12 DT H1' H 6.285 0.002 1 113 12 12 DT H2' H 2.420 0.002 1 114 12 12 DT H2'' H 2.506 0.006 1 115 12 12 DT H3' H 4.702 0.029 1 116 12 12 DT H4' H 4.207 0.037 1 117 12 12 DT H6 H 7.614 0.003 1 118 12 12 DT H71 H 1.894 0.004 2 119 12 12 DT H72 H 1.894 0.004 2 120 12 12 DT H73 H 1.894 0.004 2 121 12 12 DT P P 0.239 0.000 1 122 13 13 DT H1' H 5.341 0.003 1 123 13 13 DT H2' H 1.325 0.005 1 124 13 13 DT H2'' H 2.166 0.002 1 125 13 13 DT H3' H 4.482 0.026 1 126 13 13 DT H4' H 3.929 0.027 1 127 13 13 DT H5' H 3.543 0.002 1 128 13 13 DT H5'' H 3.859 0.002 1 129 13 13 DT H6 H 6.547 0.001 1 130 13 13 DT H71 H 1.292 0.001 2 131 13 13 DT H72 H 1.292 0.001 2 132 13 13 DT H73 H 1.292 0.001 2 133 13 13 DT P P -0.104 0.001 1 134 14 14 DA H1' H 6.231 0.001 1 135 14 14 DA H2 H 7.262 0.001 1 136 14 14 DA H2' H 2.202 0.089 1 137 14 14 DA H2'' H 2.383 0.088 1 138 14 14 DA H3' H 4.623 0.030 1 139 14 14 DA H4' H 4.096 0.028 1 140 14 14 DA H5' H 3.468 0.002 2 141 14 14 DA H5'' H 3.468 0.002 2 142 14 14 DA H8 H 7.689 0.001 1 143 14 14 DA P P -1.401 0.006 1 144 15 15 DG H1 H 11.262 0.006 1 145 15 15 DG H1' H 6.099 0.002 1 146 15 15 DG H2' H 3.030 0.003 1 147 15 15 DG H2'' H 3.559 0.002 1 148 15 15 DG H3' H 4.838 0.031 1 149 15 15 DG H4' H 4.455 0.032 1 150 15 15 DG H8 H 7.443 0.002 1 151 15 15 DG P P -0.196 0.001 1 152 16 16 DG H1 H 11.058 0.001 1 153 16 16 DG H1' H 5.819 0.002 1 154 16 16 DG H2' H 2.574 0.005 1 155 16 16 DG H2'' H 2.623 0.007 1 156 16 16 DG H3' H 5.012 0.026 1 157 16 16 DG H4' H 4.242 0.032 1 158 16 16 DG H8 H 7.399 0.004 1 159 16 16 DG P P -0.585 0.005 1 160 17 17 DG H1 H 11.370 0.001 1 161 17 17 DG H1' H 6.027 0.004 1 162 17 17 DG H2' H 2.308 0.005 1 163 17 17 DG H2'' H 2.634 0.010 1 164 17 17 DG H3' H 4.932 0.026 1 165 17 17 DG H4' H 4.409 0.032 1 166 17 17 DG H8 H 8.161 0.002 1 167 17 17 DG H21 H 9.814 0.000 2 168 17 17 DG H22 H 9.814 0.000 2 169 17 17 DG P P -1.171 0.000 1 170 18 18 DT H1' H 6.287 0.003 1 171 18 18 DT H2' H 2.301 0.003 1 172 18 18 DT H2'' H 2.721 0.004 1 173 18 18 DT H3' H 4.824 0.027 1 174 18 18 DT H4' H 4.266 0.032 1 175 18 18 DT H6 H 7.616 0.008 1 176 18 18 DT H71 H 1.914 0.003 2 177 18 18 DT H72 H 1.914 0.003 2 178 18 18 DT H73 H 1.914 0.003 2 179 18 18 DT P P 0.230 0.001 1 180 19 19 DT H1' H 5.888 0.002 1 181 19 19 DT H2' H 1.515 0.004 1 182 19 19 DT H2'' H 1.756 0.005 1 183 19 19 DT H3' H 4.741 0.024 1 184 19 19 DT H4' H 4.161 0.030 1 185 19 19 DT H5' H 4.011 0.005 1 186 19 19 DT H5'' H 4.048 0.006 1 187 19 19 DT H6 H 7.395 0.003 1 188 19 19 DT H71 H 1.588 0.002 2 189 19 19 DT H72 H 1.588 0.002 2 190 19 19 DT H73 H 1.588 0.002 2 191 19 19 DT P P -0.168 0.003 1 192 20 20 DA H1' H 6.556 0.007 1 193 20 20 DA H2 H 8.149 0.002 1 194 20 20 DA H2' H 2.851 0.003 2 195 20 20 DA H2'' H 2.851 0.003 2 196 20 20 DA H3' H 5.098 0.029 1 197 20 20 DA H4' H 4.698 0.030 1 198 20 20 DA H8 H 8.557 0.004 1 199 20 20 DA P P -0.432 0.000 1 200 21 21 DG H1 H 11.226 0.001 1 201 21 21 DG H1' H 6.045 0.003 1 202 21 21 DG H2' H 3.000 0.004 1 203 21 21 DG H2'' H 3.833 0.004 1 204 21 21 DG H3' H 5.057 0.029 1 205 21 21 DG H4' H 4.525 0.030 1 206 21 21 DG H8 H 7.367 0.004 1 207 21 21 DG P P -0.020 0.001 1 208 22 22 DG H1 H 11.058 0.000 1 209 22 22 DG H1' H 5.816 0.001 1 210 22 22 DG H2' H 2.564 0.002 1 211 22 22 DG H2'' H 2.755 0.002 1 212 22 22 DG H3' H 5.043 0.029 1 213 22 22 DG H4' H 4.415 0.032 1 214 22 22 DG H8 H 8.012 0.002 1 215 22 22 DG P P -0.654 0.000 1 216 23 23 DG H1 H 10.484 0.001 1 217 23 23 DG H1' H 5.824 0.003 1 218 23 23 DG H2' H 2.174 0.002 1 219 23 23 DG H2'' H 2.555 0.007 1 220 23 23 DG H3' H 4.925 0.027 1 221 23 23 DG H4' H 4.405 0.033 1 222 23 23 DG H8 H 7.350 0.003 1 223 23 23 DG P P -0.581 0.000 1 224 24 24 DA H1' H 6.155 0.001 1 225 24 24 DA H2 H 7.553 0.002 1 226 24 24 DA H2' H 2.450 0.002 1 227 24 24 DA H2'' H 2.720 0.004 1 228 24 24 DA H3' H 4.716 0.004 1 229 24 24 DA H4' H 4.220 0.031 1 230 24 24 DA H5' H 4.150 0.001 2 231 24 24 DA H5'' H 4.150 0.001 2 232 24 24 DA H8 H 7.947 0.001 1 233 24 24 DA P P -0.390 0.001 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-31P HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_3 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name L2H _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 25 1 L2H HB1 H 2.860 0.002 2 2 25 1 L2H HB1' H 2.832 0.010 2 3 25 1 L2H HB2 H 2.860 0.002 2 4 25 1 L2H HB2' H 2.832 0.010 2 5 25 1 L2H HC1 H 1.541 0.005 1 6 25 1 L2H HC1' H 1.631 0.003 2 7 25 1 L2H HC2 H 1.608 0.007 1 8 25 1 L2H HC2' H 1.631 0.003 2 9 25 1 L2H HD1 H 0.934 0.004 1 10 25 1 L2H HD1' H 0.965 0.004 1 11 25 1 L2H HD2 H 1.343 0.005 1 12 25 1 L2H HD2' H 1.366 0.003 1 13 25 1 L2H HE1 H 1.843 0.003 1 14 25 1 L2H HE1' H 1.920 0.002 1 15 25 1 L2H HE2 H 2.122 0.007 1 16 25 1 L2H HE2' H 1.966 0.005 1 17 25 1 L2H HF H 4.845 0.002 1 18 25 1 L2H HF' H 4.293 0.004 1 19 25 1 L2H HG H 7.721 0.003 1 20 25 1 L2H HH H 7.506 0.001 1 21 25 1 L2H HI H 8.052 0.001 1 22 25 1 L2H HJ H 8.484 0.002 1 23 25 1 L2H HK H 7.795 0.001 1 24 25 1 L2H HL H 7.845 0.001 1 25 25 1 L2H HM1 H 2.305 0.003 2 26 25 1 L2H HM2 H 2.305 0.003 2 27 25 1 L2H HM3 H 2.305 0.003 2 28 25 1 L2H HN1 H 2.400 0.001 2 29 25 1 L2H HN2 H 2.400 0.001 2 30 25 1 L2H HN3 H 2.400 0.001 2 stop_ save_