data_18629 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of H-RasT35S mutant protein in complex with Kobe2601 ; _BMRB_accession_number 18629 _BMRB_flat_file_name bmr18629.str _Entry_type original _Submission_date 2012-08-01 _Accession_date 2012-08-01 _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 Araki Mitsugu . . 2 Tamura Atsuo . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 88 "13C chemical shifts" 77 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-05-20 original BMRB . stop_ _Original_release_date 2012-08-30 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; In silico discovery of small-molecule Ras inhibitors that display antitumor activity by blocking the Ras-effector interaction ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 23630290 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shima Fumi . . 2 Yoshikawa Yoko . . 3 Ye Min . . 4 Araki Mitsugu . . 5 Matsumoto Shigeyuki . . 6 Liao Jingling . . 7 Hu Lizhi . . 8 Sugimoto Takeshi . . 9 Ijiri Yuichi . . 10 Takeda Azusa . . 11 Nishiyama Yuko . . 12 Sato Chie . . 13 Muraoka Shin . . 14 Tamura Atsuo . . 15 Osoda Tsutomu . . 16 Tsuda Ken-ichiro . . 17 Miyakawa Tomoya . . 18 Fukunishi Hiroaki . . 19 Shimada Jiro . . 20 Kumasaka Takashi . . 21 Yamamotog Masaki . . 22 Kataoka Tohru . . stop_ _Journal_abbreviation 'Proc. Natl. Acad. Sci. U. S. A.' _Journal_volume 110 _Journal_issue 20 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8182 _Page_last 8187 _Year 2013 _Details . loop_ _Keyword 'Conformational states' 'GTP-bound form' Ras 'Signaling protein' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'H-RasT35S mutant protein in complex with Kobe2601' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'H-RasT35S mutant protein' $H-RasT35S 'PHOSPHOAMINOPHOSPHONIC ACID-GUANYLATE ESTER' $entity_GNP 'MAGNESIUM ION' $entity_MG KOB $entity_KOB 'water, 1' $entity_HOH 'water, 2' $entity_HOH 'water, 3' $entity_HOH 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_H-RasT35S _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 18861.303 _Mol_thiol_state 'all free' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 166 _Mol_residue_sequence ; MTEYKLVVVGAGGVGKSALT IQLIQNHFVDEYDPSIEDSY RKQVVIDGETCLLDILDTAG QEEYSAMRDQYMRTGEGFLC VFAINNTKSFEDIHQYREQI KRVKDSDDVPMVLVGNKCDL AARTVESRQAQDLARSYGIP YIETSAKTRQGVEDAFYTLV REIRQH ; loop_ _Residue_seq_code _Residue_label 1 MET 2 THR 3 GLU 4 TYR 5 LYS 6 LEU 7 VAL 8 VAL 9 VAL 10 GLY 11 ALA 12 GLY 13 GLY 14 VAL 15 GLY 16 LYS 17 SER 18 ALA 19 LEU 20 THR 21 ILE 22 GLN 23 LEU 24 ILE 25 GLN 26 ASN 27 HIS 28 PHE 29 VAL 30 ASP 31 GLU 32 TYR 33 ASP 34 PRO 35 SER 36 ILE 37 GLU 38 ASP 39 SER 40 TYR 41 ARG 42 LYS 43 GLN 44 VAL 45 VAL 46 ILE 47 ASP 48 GLY 49 GLU 50 THR 51 CYS 52 LEU 53 LEU 54 ASP 55 ILE 56 LEU 57 ASP 58 THR 59 ALA 60 GLY 61 GLN 62 GLU 63 GLU 64 TYR 65 SER 66 ALA 67 MET 68 ARG 69 ASP 70 GLN 71 TYR 72 MET 73 ARG 74 THR 75 GLY 76 GLU 77 GLY 78 PHE 79 LEU 80 CYS 81 VAL 82 PHE 83 ALA 84 ILE 85 ASN 86 ASN 87 THR 88 LYS 89 SER 90 PHE 91 GLU 92 ASP 93 ILE 94 HIS 95 GLN 96 TYR 97 ARG 98 GLU 99 GLN 100 ILE 101 LYS 102 ARG 103 VAL 104 LYS 105 ASP 106 SER 107 ASP 108 ASP 109 VAL 110 PRO 111 MET 112 VAL 113 LEU 114 VAL 115 GLY 116 ASN 117 LYS 118 CYS 119 ASP 120 LEU 121 ALA 122 ALA 123 ARG 124 THR 125 VAL 126 GLU 127 SER 128 ARG 129 GLN 130 ALA 131 GLN 132 ASP 133 LEU 134 ALA 135 ARG 136 SER 137 TYR 138 GLY 139 ILE 140 PRO 141 TYR 142 ILE 143 GLU 144 THR 145 SER 146 ALA 147 LYS 148 THR 149 ARG 150 GLN 151 GLY 152 VAL 153 GLU 154 ASP 155 ALA 156 PHE 157 TYR 158 THR 159 LEU 160 VAL 161 ARG 162 GLU 163 ILE 164 ARG 165 GLN 166 HIS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_KOB _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 2-(2,4-dinitrophenyl)-N-(4-fluorophenyl)hydrazinecarbothioamide _BMRB_code KOB _PDB_code KOB _Molecular_mass 351.313 _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 C13 C13 C . 0 . ? C12 C12 C . 0 . ? C11 C11 C . 0 . ? F11 F11 F . 0 . ? C10 C10 C . 0 . ? C9 C9 C . 0 . ? C8 C8 C . 0 . ? N8 N8 N . 0 . ? C7 C7 C . 0 . ? S7 S7 S . 0 . ? N7 N7 N . 0 . ? N6 N6 N . 0 . ? C6 C6 C . 0 . ? C5 C5 C . 0 . ? C4 C4 C . 0 . ? C3 C3 C . 0 . ? N3 N3 N . 1 . ? O3B O3B O . -1 . ? O3A O3A O . 0 . ? C2 C2 C . 0 . ? C1 C1 C . 0 . ? N1 N1 N . 1 . ? O1B O1B O . -1 . ? O1A O1A O . 0 . ? HE1 HE1 H . 0 . ? HE2 HE2 H . 0 . ? HD2 HD2 H . 0 . ? HD1 HD1 H . 0 . ? HAD HAD H . 0 . ? HAC HAC H . 0 . ? HAB HAB H . 0 . ? H5 H5 H . 0 . ? H4 H4 H . 0 . ? H2 H2 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 O3B N3 ? ? DOUB O3A N3 ? ? SING N3 C3 ? ? DOUB C3 C2 ? ? SING C3 C4 ? ? SING C2 C1 ? ? DOUB C4 C5 ? ? DOUB O1A N1 ? ? SING C1 N1 ? ? DOUB C1 C6 ? ? SING C5 C6 ? ? SING N1 O1B ? ? SING C6 N6 ? ? DOUB C13 C12 ? ? SING C13 C8 ? ? SING N6 N7 ? ? SING C12 C11 ? ? SING N8 C8 ? ? SING N8 C7 ? ? DOUB C8 C9 ? ? SING N7 C7 ? ? SING C11 F11 ? ? DOUB C11 C10 ? ? DOUB C7 S7 ? ? SING C9 C10 ? ? SING C12 HE2 ? ? SING C10 HE1 ? ? SING C13 HD2 ? ? SING C9 HD1 ? ? SING N8 HAD ? ? SING N7 HAC ? ? SING N6 HAB ? ? SING C5 H5 ? ? SING C4 H4 ? ? SING C2 H2 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ save_GNP _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 'PHOSPHOAMINOPHOSPHONIC ACID-GUANYLATE ESTER' _BMRB_code GNP _PDB_code GNP _Molecular_mass 522.196 _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 PG PG P . 0 . ? O1G O1G O . 0 . ? O2G O2G O . 0 . ? O3G O3G O . 0 . ? N3B N3B N . 0 . ? PB PB P . 0 . ? O1B O1B O . 0 . ? O2B O2B O . 0 . ? O3A O3A O . 0 . ? PA PA P . 0 . ? O1A O1A O . 0 . ? O2A O2A O . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C3' C3' C . 0 . ? O3' O3' O . 0 . ? C2' C2' C . 0 . ? O2' O2' O . 0 . ? C1' C1' C . 0 . ? N9 N9 N . 0 . ? C8 C8 C . 0 . ? N7 N7 N . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? O6 O6 O . 0 . ? N1 N1 N . 0 . ? C2 C2 C . 0 . ? N2 N2 N . 0 . ? N3 N3 N . 0 . ? C4 C4 C . 0 . ? HOG2 HOG2 H . 0 . ? HOG3 HOG3 H . 0 . ? HNB3 HNB3 H . 0 . ? HOB2 HOB2 H . 0 . ? HOA2 HOA2 H . 0 . ? H5'2 H5'2 H . 0 . ? H5'1 H5'1 H . 0 . ? H4' H4' H . 0 . ? H3' H3' H . 0 . ? HO3' HO3' H . 0 . ? H2' H2' H . 0 . ? HO2' HO2' H . 0 . ? H1' H1' H . 0 . ? H8 H8 H . 0 . ? HN1 HN1 H . 0 . ? HN21 HN21 H . 0 . ? HN22 HN22 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 PG O1G ? ? SING PG O2G ? ? SING PG O3G ? ? SING PG N3B ? ? SING O2G HOG2 ? ? SING O3G HOG3 ? ? SING N3B PB ? ? SING N3B HNB3 ? ? DOUB PB O1B ? ? SING PB O2B ? ? SING PB O3A ? ? SING O2B HOB2 ? ? SING O3A PA ? ? DOUB PA O1A ? ? SING PA O2A ? ? SING PA O5' ? ? SING O2A HOA2 ? ? SING O5' C5' ? ? SING C5' C4' ? ? SING C5' H5'2 ? ? SING C5' H5'1 ? ? SING C4' O4' ? ? SING C4' C3' ? ? SING C4' H4' ? ? SING O4' C1' ? ? SING C3' O3' ? ? SING C3' C2' ? ? SING C3' H3' ? ? SING O3' HO3' ? ? SING C2' O2' ? ? SING C2' C1' ? ? SING C2' H2' ? ? SING O2' HO2' ? ? SING C1' N9 ? ? SING C1' H1' ? ? SING N9 C8 ? ? SING N9 C4 ? ? DOUB C8 N7 ? ? SING C8 H8 ? ? SING N7 C5 ? ? SING C5 C6 ? ? DOUB C5 C4 ? ? DOUB C6 O6 ? ? SING C6 N1 ? ? SING N1 C2 ? ? SING N1 HN1 ? ? SING C2 N2 ? ? DOUB C2 N3 ? ? SING N2 HN21 ? ? SING N2 HN22 ? ? SING N3 C4 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ save_MG _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 'MAGNESIUM ION' _BMRB_code MG _PDB_code MG _Molecular_mass 24.305 _Mol_charge 2 _Mol_paramagnetic . _Mol_aromatic no _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons MG MG MG . 2 . ? 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 _Variant $H-RasT35S Human 9606 Eukaryota Metazoa Homo sapiens 'T35S mutation' 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 $H-RasT35S 'recombinant technology' . . . . pGEX-6P-1 $entity_KOB 'chemical synthesis' . . . . . $entity_GNP 'chemical synthesis' . . . . . $entity_MG 'chemical synthesis' . . . . . $entity_HOH 'purified from the natural source' . . . . . 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 _Isotopic_labeling $H-RasT35S 1 mM '[U-98% 13C; U-98% 15N]' $entity_GNP 1 mM 'natural abundance' $entity_MG 8 mM 'natural abundance' 'sodium chloride' 120 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' $entity_KOB 3.8 mM 'natural abundance' D2O 80 % 'natural abundance' DMSO_d6 20 % 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $H-RasT35S 1 mM 'natural abundance' $entity_GNP 1 mM 'natural abundance' $entity_MG 8 mM 'natural abundance' 'sodium chloride' 120 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' $entity_KOB 3.8 mM 'natural abundance' D2O 80 % 'natural abundance' DMSO_d6 20 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CYANA _Saveframe_category software _Name CYANA _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_CNS _Saveframe_category software _Name CNS _Version 1.2 loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'peak picking' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DMX _Field_strength 750 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_3D_1H-13C_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY' _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_2 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' 0.22 . M pH 6.8 . pH pressure 1 . atm temperature 278 . K 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 TSP C 13 'methyl protons' ppm 0.00 external indirect . . . 0.251449530 TSP H 1 'methyl protons' ppm 0.00 external direct . . . 1.000000000 TSP N 15 'methyl protons' ppm 0.00 external indirect . . . 0.101329118 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-13C HSQC' '3D 1H-13C NOESY' '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'H-RasT35S mutant protein' _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 MET HE H 1.946 0.000 2 2 1 1 MET CE C 16.836 0.000 1 3 5 5 LYS HE2 H 2.773 0.000 2 4 5 5 LYS HE3 H 2.773 0.000 2 5 5 5 LYS CE C 41.672 0.000 1 6 6 6 LEU HD1 H 0.657 0.000 2 7 6 6 LEU HD2 H 0.981 0.000 2 8 6 6 LEU CD1 C 23.711 0.000 1 9 6 6 LEU CD2 C 26.648 0.000 1 10 8 8 VAL HG1 H 0.920 0.000 2 11 8 8 VAL HG2 H 0.948 0.000 2 12 8 8 VAL CG1 C 22.341 0.000 1 13 8 8 VAL CG2 C 20.444 0.000 1 14 11 11 ALA HB H 1.607 0.000 2 15 11 11 ALA CB C 19.731 0.000 1 16 18 18 ALA HB H 1.472 0.000 2 17 18 18 ALA CB C 18.620 0.000 1 18 19 19 LEU HD1 H 0.631 0.000 2 19 19 19 LEU CD1 C 26.586 0.000 1 20 20 20 THR HG2 H 0.545 0.000 2 21 20 20 THR CG2 C 22.138 0.000 1 22 21 21 ILE HG2 H 0.677 0.000 2 23 21 21 ILE HD1 H 0.625 0.000 2 24 21 21 ILE CG2 C 17.585 0.000 1 25 21 21 ILE CD1 C 11.970 0.000 1 26 23 23 LEU HD1 H -0.191 0.000 2 27 23 23 LEU HD2 H 0.617 0.000 2 28 23 23 LEU CD1 C 23.758 0.000 1 29 23 23 LEU CD2 C 22.658 0.000 1 30 24 24 ILE HD1 H 0.479 0.000 2 31 24 24 ILE CD1 C 10.465 0.000 1 32 29 29 VAL HG1 H 0.625 0.000 2 33 29 29 VAL HG2 H 0.712 0.000 2 34 29 29 VAL CG1 C 19.906 0.000 1 35 29 29 VAL CG2 C 21.338 0.000 1 36 36 36 ILE HG2 H 0.899 0.000 2 37 36 36 ILE HD1 H 0.841 0.000 2 38 36 36 ILE CG2 C 17.764 0.000 1 39 36 36 ILE CD1 C 13.453 0.000 1 40 44 44 VAL HG1 H 0.670 0.000 2 41 44 44 VAL CG1 C 19.746 0.000 1 42 45 45 VAL HG1 H 0.647 0.000 2 43 45 45 VAL HG2 H 0.895 0.000 2 44 45 45 VAL CG1 C 20.945 0.000 1 45 45 45 VAL CG2 C 21.018 0.000 1 46 46 46 ILE HG2 H 0.526 0.000 2 47 46 46 ILE CG2 C 16.330 0.000 1 48 50 50 THR HG2 H 1.188 0.000 2 49 50 50 THR CG2 C 22.177 0.000 1 50 52 52 LEU HD1 H 0.773 0.000 2 51 52 52 LEU HD2 H 0.794 0.000 2 52 52 52 LEU CD1 C 24.634 0.000 1 53 52 52 LEU CD2 C 24.836 0.000 1 54 53 53 LEU HD1 H 0.802 0.000 2 55 53 53 LEU CD1 C 25.555 0.000 1 56 55 55 ILE HG2 H 0.873 0.000 2 57 55 55 ILE HD1 H 0.540 0.000 2 58 55 55 ILE CG2 C 19.361 0.000 1 59 55 55 ILE CD1 C 14.679 0.000 1 60 56 56 LEU HD1 H 0.604 0.000 2 61 56 56 LEU HD2 H 0.649 0.000 2 62 56 56 LEU CD1 C 25.728 0.000 1 63 56 56 LEU CD2 C 23.601 0.000 1 64 59 59 ALA HB H 1.469 0.000 2 65 59 59 ALA CB C 20.752 0.000 1 66 66 66 ALA HB H 1.480 0.000 2 67 66 66 ALA CB C 18.209 0.000 1 68 67 67 MET HE H 2.031 0.000 2 69 67 67 MET CE C 16.864 0.000 1 70 70 70 GLN HG2 H 2.361 0.000 2 71 70 70 GLN HG3 H 2.361 0.000 2 72 70 70 GLN CG C 33.530 0.000 1 73 71 71 TYR HD1 H 6.995 0.000 3 74 71 71 TYR HD2 H 6.995 0.000 3 75 71 71 TYR HE1 H 6.647 0.000 3 76 71 71 TYR HE2 H 6.647 0.000 3 77 72 72 MET HE H 2.062 0.000 2 78 72 72 MET CE C 17.831 0.000 1 79 74 74 THR HG2 H 1.280 0.000 2 80 74 74 THR CG2 C 22.002 0.000 1 81 79 79 LEU HD1 H 0.104 0.000 2 82 79 79 LEU HD2 H 0.127 0.000 2 83 79 79 LEU CD1 C 24.864 0.000 1 84 79 79 LEU CD2 C 25.557 0.000 1 85 81 81 VAL HG1 H 0.533 0.000 2 86 81 81 VAL CG1 C 22.770 0.000 1 87 83 83 ALA HB H 1.474 0.000 2 88 83 83 ALA CB C 21.736 0.000 1 89 84 84 ILE HG2 H 0.797 0.000 2 90 84 84 ILE HD1 H 0.775 0.000 2 91 84 84 ILE CG2 C 20.142 0.000 1 92 84 84 ILE CD1 C 15.250 0.000 1 93 87 87 THR HG2 H 1.305 0.000 2 94 87 87 THR CG2 C 22.740 0.000 1 95 93 93 ILE HG2 H 0.968 0.000 2 96 93 93 ILE HD1 H 0.797 0.000 2 97 93 93 ILE CG2 C 17.357 0.000 1 98 93 93 ILE CD1 C 9.138 0.000 1 99 100 100 ILE HG2 H -0.105 0.000 2 100 100 100 ILE HD1 H 0.425 0.000 2 101 100 100 ILE CG2 C 17.745 0.000 1 102 100 100 ILE CD1 C 15.850 0.000 1 103 103 103 VAL HG1 H 0.995 0.000 2 104 103 103 VAL CG1 C 21.700 0.000 1 105 109 109 VAL HG1 H 0.755 0.000 2 106 109 109 VAL HG2 H 0.985 0.000 2 107 109 109 VAL CG1 C 21.286 0.000 1 108 109 109 VAL CG2 C 21.109 0.000 1 109 111 111 MET HE H 1.847 0.000 2 110 111 111 MET CE C 17.254 0.000 1 111 112 112 VAL HG1 H 0.748 0.000 2 112 112 112 VAL HG2 H 0.785 0.000 2 113 112 112 VAL CG1 C 21.808 0.000 1 114 112 112 VAL CG2 C 22.493 0.000 1 115 113 113 LEU HD1 H 1.096 0.000 2 116 113 113 LEU HD2 H 1.386 0.000 2 117 113 113 LEU CD1 C 27.674 0.000 1 118 113 113 LEU CD2 C 25.368 0.000 1 119 114 114 VAL HG1 H 0.607 0.000 2 120 114 114 VAL HG2 H 0.692 0.000 2 121 114 114 VAL CG1 C 23.147 0.000 1 122 114 114 VAL CG2 C 23.355 0.000 1 123 120 120 LEU HD1 H 0.836 0.000 2 124 120 120 LEU CD1 C 22.310 0.000 1 125 121 121 ALA HB H 1.434 0.000 2 126 121 121 ALA CB C 19.105 0.000 1 127 122 122 ALA HB H 1.319 0.000 2 128 122 122 ALA CB C 17.275 0.000 1 129 125 125 VAL HG1 H -0.145 0.000 2 130 125 125 VAL CG1 C 19.113 0.000 1 131 130 130 ALA HB H 0.861 0.000 2 132 130 130 ALA CB C 18.613 0.000 1 133 133 133 LEU HD1 H 0.470 0.000 2 134 133 133 LEU HD2 H 0.502 0.000 2 135 133 133 LEU CD1 C 26.145 0.000 1 136 133 133 LEU CD2 C 22.860 0.000 1 137 134 134 ALA HB H 1.724 0.000 2 138 134 134 ALA CB C 18.088 0.000 1 139 139 139 ILE HD1 H 0.888 0.000 2 140 139 139 ILE CD1 C 15.271 0.000 1 141 142 142 ILE HG2 H 0.675 0.000 2 142 142 142 ILE HD1 H 0.718 0.000 2 143 142 142 ILE CG2 C 17.724 0.000 1 144 142 142 ILE CD1 C 13.844 0.000 1 145 146 146 ALA HB H 1.559 0.000 2 146 146 146 ALA CB C 18.722 0.000 1 147 148 148 THR HG2 H 1.046 0.000 2 148 148 148 THR CG2 C 21.022 0.000 1 149 155 155 ALA HB H 1.099 0.000 2 150 155 155 ALA CB C 17.352 0.000 1 151 158 158 THR HG2 H 1.190 0.000 2 152 158 158 THR CG2 C 21.396 0.000 1 153 160 160 VAL HG1 H 0.064 0.000 2 154 160 160 VAL HG2 H 0.713 0.000 2 155 160 160 VAL CG1 C 19.916 0.000 1 156 160 160 VAL CG2 C 23.731 0.000 1 157 163 163 ILE HG2 H 1.071 0.000 2 158 163 163 ILE HD1 H 0.631 0.000 2 159 163 163 ILE CG2 C 17.926 0.000 1 160 163 163 ILE CD1 C 15.634 0.000 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' '3D 1H-13C NOESY' '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'PHOSPHOAMINOPHOSPHONIC ACID-GUANYLATE ESTER' _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 1 203 1 KOB H1 H 7.102 0.008 1 2 203 1 KOB H2 H 7.542 0.004 1 3 203 1 KOB H3 H 7.327 0.001 1 4 203 1 KOB H4 H 7.982 0.003 1 5 203 1 KOB H5 H 8.919 0.000 1 stop_ save_