data_25361 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone 1H and 15N Chemical Shift Assignments for Y171W mutant of Adenylate Kinase in complex with Ap5a for state a ; _BMRB_accession_number 25361 _BMRB_flat_file_name bmr25361.str _Entry_type original _Submission_date 2014-11-21 _Accession_date 2014-11-21 _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 Kovermann Michael . . 2 Wolf-Watz Magnus . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 194 "15N chemical shifts" 194 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-08-21 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 25353 'P177A mutant of Adenylate Kinase' 25357 'Y171W mutant of Adenylate Kinase' 25360 'P177A mutant of Adenylate Kinase in complex with Ap5a' 25362 'Y171W mutant of Adenylate Kinase in complex with Ap5a for state b' stop_ _Original_release_date 2015-08-21 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Structural basis for catalytically restrictive dynamics of a high-energy enzyme state ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26138143 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kovermann Michael . . 2 Aden Jorgen . . 3 Grundstrom Christin . . 4 Sauer-Eriksson Elisabeth . . 5 Sauer Uwe . . 6 Wolf-Watz Magnus . . stop_ _Journal_abbreviation 'Nat. Commun.' _Journal_volume 6 _Journal_issue 7644 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year 2015 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Y171W mutant of Adenylate Kinase in complex with Ap5a for state a' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Adenylate Kinase Y171W' $Adenylate_Kinase_Y171W Ap5a $entity_AP5 stop_ _System_molecular_weight 24326 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'Inhibition of enzymatic activity of Adenylate Kinase by Ap5a' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Adenylate_Kinase_Y171W _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Adenylate_Kinase_Y171W _Molecular_mass . _Mol_thiol_state 'not reported' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 214 _Mol_residue_sequence ; MRIILLGAPGAGKGTQAQFI MEKYGIPQISTGDMLRAAVK SGSELGKQAKDIMDAGKLVT DELVIALVKERIAQEDCRNG FLLDGFPRTIPQADAMKEAG INVDYVLEFDVPDELIVDRI VGRRVHAPSGRVYHVKFNPP KVEGKDDVTGEELTTRKDDQ EETVRKRLVEWHQMTAPLIG YYSKEAEAGNTKYAKVDGTK PVAEVRADLEKILG ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 MET 2 2 ARG 3 3 ILE 4 4 ILE 5 5 LEU 6 6 LEU 7 7 GLY 8 8 ALA 9 9 PRO 10 10 GLY 11 11 ALA 12 12 GLY 13 13 LYS 14 14 GLY 15 15 THR 16 16 GLN 17 17 ALA 18 18 GLN 19 19 PHE 20 20 ILE 21 21 MET 22 22 GLU 23 23 LYS 24 24 TYR 25 25 GLY 26 26 ILE 27 27 PRO 28 28 GLN 29 29 ILE 30 30 SER 31 31 THR 32 32 GLY 33 33 ASP 34 34 MET 35 35 LEU 36 36 ARG 37 37 ALA 38 38 ALA 39 39 VAL 40 40 LYS 41 41 SER 42 42 GLY 43 43 SER 44 44 GLU 45 45 LEU 46 46 GLY 47 47 LYS 48 48 GLN 49 49 ALA 50 50 LYS 51 51 ASP 52 52 ILE 53 53 MET 54 54 ASP 55 55 ALA 56 56 GLY 57 57 LYS 58 58 LEU 59 59 VAL 60 60 THR 61 61 ASP 62 62 GLU 63 63 LEU 64 64 VAL 65 65 ILE 66 66 ALA 67 67 LEU 68 68 VAL 69 69 LYS 70 70 GLU 71 71 ARG 72 72 ILE 73 73 ALA 74 74 GLN 75 75 GLU 76 76 ASP 77 77 CYS 78 78 ARG 79 79 ASN 80 80 GLY 81 81 PHE 82 82 LEU 83 83 LEU 84 84 ASP 85 85 GLY 86 86 PHE 87 87 PRO 88 88 ARG 89 89 THR 90 90 ILE 91 91 PRO 92 92 GLN 93 93 ALA 94 94 ASP 95 95 ALA 96 96 MET 97 97 LYS 98 98 GLU 99 99 ALA 100 100 GLY 101 101 ILE 102 102 ASN 103 103 VAL 104 104 ASP 105 105 TYR 106 106 VAL 107 107 LEU 108 108 GLU 109 109 PHE 110 110 ASP 111 111 VAL 112 112 PRO 113 113 ASP 114 114 GLU 115 115 LEU 116 116 ILE 117 117 VAL 118 118 ASP 119 119 ARG 120 120 ILE 121 121 VAL 122 122 GLY 123 123 ARG 124 124 ARG 125 125 VAL 126 126 HIS 127 127 ALA 128 128 PRO 129 129 SER 130 130 GLY 131 131 ARG 132 132 VAL 133 133 TYR 134 134 HIS 135 135 VAL 136 136 LYS 137 137 PHE 138 138 ASN 139 139 PRO 140 140 PRO 141 141 LYS 142 142 VAL 143 143 GLU 144 144 GLY 145 145 LYS 146 146 ASP 147 147 ASP 148 148 VAL 149 149 THR 150 150 GLY 151 151 GLU 152 152 GLU 153 153 LEU 154 154 THR 155 155 THR 156 156 ARG 157 157 LYS 158 158 ASP 159 159 ASP 160 160 GLN 161 161 GLU 162 162 GLU 163 163 THR 164 164 VAL 165 165 ARG 166 166 LYS 167 167 ARG 168 168 LEU 169 169 VAL 170 170 GLU 171 171 TRP 172 172 HIS 173 173 GLN 174 174 MET 175 175 THR 176 176 ALA 177 177 PRO 178 178 LEU 179 179 ILE 180 180 GLY 181 181 TYR 182 182 TYR 183 183 SER 184 184 LYS 185 185 GLU 186 186 ALA 187 187 GLU 188 188 ALA 189 189 GLY 190 190 ASN 191 191 THR 192 192 LYS 193 193 TYR 194 194 ALA 195 195 LYS 196 196 VAL 197 197 ASP 198 198 GLY 199 199 THR 200 200 LYS 201 201 PRO 202 202 VAL 203 203 ALA 204 204 GLU 205 205 VAL 206 206 ARG 207 207 ALA 208 208 ASP 209 209 LEU 210 210 GLU 211 211 LYS 212 212 ILE 213 213 LEU 214 214 GLY stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-11-25 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value BMRB 18683 adenylate_kinase 100.00 214 99.53 100.00 3.36e-151 BMRB 18685 adenylate_kinase 100.00 214 99.53 100.00 3.36e-151 BMRB 18686 adenylate_kinase 100.00 214 99.07 99.53 1.96e-150 BMRB 18687 adenylate_kinase 100.00 214 99.53 100.00 3.36e-151 BMRB 19089 adenylate_kinase_wild_type 100.00 214 99.53 100.00 3.36e-151 BMRB 19090 adenylate_kinase_wild_type 100.00 214 99.53 100.00 3.36e-151 BMRB 19091 adenylate_kinase_wild_type 100.00 214 99.53 100.00 3.36e-151 BMRB 19092 adenylate_kinase_R156K_mutant 100.00 214 99.07 100.00 1.16e-150 BMRB 19093 adenylate_kinase_R156K_mutant 100.00 214 99.07 100.00 1.16e-150 BMRB 25353 Kinase 100.00 214 99.07 99.53 2.80e-150 BMRB 25357 Adenylate_Kinase_Y171W 100.00 214 100.00 100.00 2.28e-152 BMRB 25360 Adenylate_Kinase_P177A 100.00 214 99.07 99.53 2.80e-150 BMRB 25362 Adenylate_Kinase_Y171W 100.00 214 100.00 100.00 2.28e-152 BMRB 4152 "Adenylate kinase" 100.00 214 99.53 100.00 3.36e-151 BMRB 4193 "Adenylate kinase" 100.00 214 99.53 100.00 3.36e-151 BMRB 4350 "Adenylate kinase from E. coli" 100.00 214 99.53 100.00 3.36e-151 PDB 1AKE "Structure Of The Complex Between Adenylate Kinase From Escherichia Coli And The Inhibitor Ap5a Refined At 1.9 Angstroms Resolut" 100.00 214 99.53 100.00 3.36e-151 PDB 1ANK "The Closed Conformation Of A Highly Flexible Protein: The Structure Of E. Cloi Adenylate Kinase With Bound Amp And Amppnp" 100.00 214 99.53 100.00 3.36e-151 PDB 1E4V "Mutant G10v Of Adenylate Kinase From E. Coli, Modified In The Gly-Loop" 100.00 214 99.07 99.53 5.53e-150 PDB 1E4Y "Mutant P9l Of Adenylate Kinase From E. Coli, Modified In The Gly-Loop" 100.00 214 98.60 99.07 9.29e-149 PDB 2ECK "Structure Of Phosphotransferase" 100.00 214 99.53 100.00 3.36e-151 PDB 3HPQ "Crystal Structure Of Wild-Type Adenylate Kinase From E. Coli, In Complex With Ap5a" 100.00 214 99.53 100.00 3.36e-151 PDB 3HPR "Crystal Structure Of V148g Adenylate Kinase From E. Coli, In Complex With Ap5a" 100.00 214 99.07 99.53 6.73e-150 PDB 3X2S "Crystal Structure Of Pyrene-conjugated Adenylate Kinase" 100.00 214 98.13 98.60 1.70e-148 PDB 4AKE "Adenylate Kinase" 100.00 214 99.53 100.00 3.36e-151 PDB 4JZK "Crystal Structure Of Adenylate Kinase Of E. Coli With Adp/amp Bound" 100.00 214 99.53 100.00 3.36e-151 PDB 4X8H "Crystal Structure Of E. Coli Adenylate Kinase P177a Mutant" 100.00 214 99.07 99.53 2.80e-150 PDB 4X8L "Crystal Structure Of E. Coli Adenylate Kinase P177a Mutant In Complex With Inhibitor Ap5a" 100.00 214 99.07 99.53 2.80e-150 PDB 4X8M "Crystal Structure Of E. Coli Adenylate Kinase Y171w Mutant" 100.00 214 100.00 100.00 2.28e-152 PDB 4X8O "Crystal Structure Of E. Coli Adenylate Kinase Y171w Mutant In Complex With Inhibitor Ap5a" 100.00 214 100.00 100.00 2.28e-152 DBJ BAA14303 "adenylate kinase [Escherichia coli K-12]" 50.00 107 99.07 100.00 2.80e-68 DBJ BAB33950 "adenylate kinase [Escherichia coli O157:H7 str. Sakai]" 100.00 214 99.53 100.00 3.36e-151 DBJ BAE76253 "adenylate kinase [Escherichia coli str. K12 substr. W3110]" 100.00 214 99.53 100.00 3.36e-151 DBJ BAG76023 "adenylate kinase [Escherichia coli SE11]" 100.00 214 99.53 100.00 3.36e-151 DBJ BAI23848 "adenylate kinase Adk [Escherichia coli O26:H11 str. 11368]" 100.00 214 99.53 100.00 3.36e-151 EMBL CAA26840 "unnamed protein product [Escherichia coli]" 100.00 214 99.53 100.00 3.36e-151 EMBL CAF33430 "adenylate kinase [Escherichia coli]" 71.96 154 99.35 100.00 1.16e-105 EMBL CAF33431 "adenylate kinase, partial [Escherichia coli]" 71.96 154 99.35 100.00 1.16e-105 EMBL CAF33432 "adenylate kinase, partial [Escherichia coli]" 71.96 154 99.35 100.00 1.16e-105 EMBL CAF33433 "adenylate kinase, partial [Escherichia coli]" 71.96 154 99.35 100.00 1.16e-105 GB AAA23461 "adk ORF [Escherichia coli]" 100.00 214 99.53 100.00 3.36e-151 GB AAB40228 "adenylate kinase [Escherichia coli]" 100.00 233 99.53 100.00 1.35e-151 GB AAC73576 "adenylate kinase [Escherichia coli str. K-12 substr. MG1655]" 100.00 214 99.53 100.00 3.36e-151 GB AAG54823 "adenylate kinase activity; pleiotropic effects on glycerol-3-phosphate acyltransferase activity [Escherichia coli O157:H7 str. " 100.00 214 99.53 100.00 3.36e-151 GB AAM94352 "adenylate kinase [Escherichia coli]" 79.91 171 99.42 100.00 2.88e-119 REF NP_308554 "adenylate kinase [Escherichia coli O157:H7 str. Sakai]" 100.00 214 99.53 100.00 3.36e-151 REF NP_415007 "adenylate kinase [Escherichia coli str. K-12 substr. MG1655]" 100.00 214 99.53 100.00 3.36e-151 REF NP_706367 "adenylate kinase [Shigella flexneri 2a str. 301]" 100.00 214 99.07 99.53 4.07e-150 REF WP_001220233 "MULTISPECIES: adenylate kinase [Proteobacteria]" 100.00 214 99.53 100.00 3.36e-151 REF WP_001220235 "adenylate kinase [Shigella flexneri]" 100.00 214 99.07 99.53 4.07e-150 SP A7ZIN4 "RecName: Full=Adenylate kinase; Short=AK; AltName: Full=ATP-AMP transphosphorylase; AltName: Full=ATP:AMP phosphotransferase; A" 100.00 214 99.53 100.00 3.36e-151 SP A7ZXD2 "RecName: Full=Adenylate kinase; Short=AK; AltName: Full=ATP-AMP transphosphorylase; AltName: Full=ATP:AMP phosphotransferase; A" 100.00 214 99.53 100.00 3.36e-151 SP B1IZC0 "RecName: Full=Adenylate kinase; Short=AK; AltName: Full=ATP-AMP transphosphorylase; AltName: Full=ATP:AMP phosphotransferase; A" 100.00 214 99.53 100.00 3.36e-151 SP B1LJN2 "RecName: Full=Adenylate kinase; Short=AK; AltName: Full=ATP-AMP transphosphorylase; AltName: Full=ATP:AMP phosphotransferase; A" 100.00 214 99.53 100.00 3.36e-151 SP B1XFR1 "RecName: Full=Adenylate kinase; Short=AK; AltName: Full=ATP-AMP transphosphorylase; AltName: Full=ATP:AMP phosphotransferase; A" 100.00 214 99.53 100.00 3.36e-151 stop_ save_ ############# # Ligands # ############# save_AP5 _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common BIS(ADENOSINE)-5'-PENTAPHOSPHATE _BMRB_code AP5 _PDB_code AP5 _Molecular_mass 916.367 _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 PA PA P . 0 . ? O1A O1A O . 0 . ? O2A O2A O . 0 . ? O3A O3A O . 0 . ? PB PB P . 0 . ? O1B O1B O . 0 . ? O2B O2B O . 0 . ? O3B O3B O . 0 . ? PG PG P . 0 . ? O1G O1G O . 0 . ? O2G O2G O . 0 . ? O3G O3G O . 0 . ? PD PD P . 0 . ? O1D O1D O . 0 . ? O2D O2D O . 0 . ? O3D O3D O . 0 . ? PE PE P . 0 . ? O1E O1E O . 0 . ? O2E O2E O . 0 . ? O5F O5F O . 0 . ? C5F C5F C . 0 . ? C4F C4F C . 0 . ? O4F O4F O . 0 . ? C3F C3F C . 0 . ? O3F O3F O . 0 . ? C2F C2F C . 0 . ? O2F O2F O . 0 . ? C1F C1F C . 0 . ? N9A N9A N . 0 . ? C8A C8A C . 0 . ? N7A N7A N . 0 . ? C5A C5A C . 0 . ? C6A C6A C . 0 . ? N6A N6A N . 0 . ? N1A N1A N . 0 . ? C2A C2A C . 0 . ? N3A N3A N . 0 . ? C4A C4A C . 0 . ? O5J O5J O . 0 . ? C5J C5J C . 0 . ? C4J C4J C . 0 . ? O4J O4J O . 0 . ? C3J C3J C . 0 . ? O3J O3J O . 0 . ? C2J C2J C . 0 . ? O2J O2J O . 0 . ? C1J C1J C . 0 . ? N9B N9B N . 0 . ? C8B C8B C . 0 . ? N7B N7B N . 0 . ? C5B C5B C . 0 . ? C6B C6B C . 0 . ? N6B N6B N . 0 . ? N1B N1B N . 0 . ? C2B C2B C . 0 . ? N3B N3B N . 0 . ? C4B C4B C . 0 . ? HOA2 HOA2 H . 0 . ? HOB2 HOB2 H . 0 . ? HOG2 HOG2 H . 0 . ? HOD2 HOD2 H . 0 . ? HOE2 HOE2 H . 0 . ? H51A H51A H . 0 . ? H52A H52A H . 0 . ? H4F H4F H . 0 . ? H3F H3F H . 0 . ? HO3A HO3A H . 0 . ? H2F H2F H . 0 . ? HO2A HO2A H . 0 . ? H1F H1F H . 0 . ? H8A H8A H . 0 . ? H61A H61A H . 0 . ? H62A H62A H . 0 . ? H2A H2A H . 0 . ? H51B H51B H . 0 . ? H52B H52B H . 0 . ? H4J H4J H . 0 . ? H3J H3J H . 0 . ? HO3B HO3B H . 0 . ? H2J H2J H . 0 . ? HO2B HO2B H . 0 . ? H1J H1J H . 0 . ? H8B H8B H . 0 . ? H61B H61B H . 0 . ? H62B H62B H . 0 . ? H2B H2B 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 PA O1A ? ? SING PA O2A ? ? SING PA O3A ? ? SING PA O5F ? ? SING O2A HOA2 ? ? SING O3A PB ? ? DOUB PB O1B ? ? SING PB O2B ? ? SING PB O3B ? ? SING O2B HOB2 ? ? SING O3B PG ? ? DOUB PG O1G ? ? SING PG O2G ? ? SING PG O3G ? ? SING O2G HOG2 ? ? SING O3G PD ? ? DOUB PD O1D ? ? SING PD O2D ? ? SING PD O3D ? ? SING O2D HOD2 ? ? SING O3D PE ? ? DOUB PE O1E ? ? SING PE O2E ? ? SING PE O5J ? ? SING O2E HOE2 ? ? SING O5F C5F ? ? SING C5F C4F ? ? SING C5F H51A ? ? SING C5F H52A ? ? SING C4F O4F ? ? SING C4F C3F ? ? SING C4F H4F ? ? SING O4F C1F ? ? SING C3F O3F ? ? SING C3F C2F ? ? SING C3F H3F ? ? SING O3F HO3A ? ? SING C2F O2F ? ? SING C2F C1F ? ? SING C2F H2F ? ? SING O2F HO2A ? ? SING C1F N9A ? ? SING C1F H1F ? ? SING N9A C8A ? ? SING N9A C4A ? ? DOUB C8A N7A ? ? SING C8A H8A ? ? SING N7A C5A ? ? SING C5A C6A ? ? DOUB C5A C4A ? ? SING C6A N6A ? ? DOUB C6A N1A ? ? SING N6A H61A ? ? SING N6A H62A ? ? SING N1A C2A ? ? DOUB C2A N3A ? ? SING C2A H2A ? ? SING N3A C4A ? ? SING O5J C5J ? ? SING C5J C4J ? ? SING C5J H51B ? ? SING C5J H52B ? ? SING C4J O4J ? ? SING C4J C3J ? ? SING C4J H4J ? ? SING O4J C1J ? ? SING C3J O3J ? ? SING C3J C2J ? ? SING C3J H3J ? ? SING O3J HO3B ? ? SING C2J O2J ? ? SING C2J C1J ? ? SING C2J H2J ? ? SING O2J HO2B ? ? SING C1J N9B ? ? SING C1J H1J ? ? SING N9B C8B ? ? SING N9B C4B ? ? DOUB C8B N7B ? ? SING C8B H8B ? ? SING N7B C5B ? ? SING C5B C6B ? ? DOUB C5B C4B ? ? SING C6B N6B ? ? DOUB C6B N1B ? ? SING N6B H61B ? ? SING N6B H62B ? ? SING N1B C2B ? ? DOUB C2B N3B ? ? SING C2B H2B ? ? SING N3B C4B ? ? 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 $Adenylate_Kinase_Y171W 'E. coli' 562 Bacteria . Escherichia coli 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 $Adenylate_Kinase_Y171W 'recombinant technology' . Escherichia coli . 'pEAK-91 vector' 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 $Adenylate_Kinase_Y171W 0.7 mM '[U-100% 15N]' $entity_AP5 3 mM 'natural abundance' 'sodium chloride' 50 mM 'natural abundance' MOPS 30 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . 'Johnson, One Moon Scientific' . . stop_ loop_ _Task collection 'data analysis' processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 850 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.0 . pH pressure 1 . atm temperature 298 . 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 DSS H 1 'methyl protons' ppm 0 na indirect . . . 1 DSS N 15 nitrogen ppm 0 na indirect . . . 0.1013287 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $TOPSPIN stop_ loop_ _Experiment_label '3D 1H-15N NOESY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'Adenylate Kinase Y171W' _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 2 2 ARG H H 9.56078 0.005 . 2 2 2 ARG N N 125.003 0.02 . 3 3 3 ILE H H 8.04852 0.005 . 4 3 3 ILE N N 123.327 0.02 . 5 4 4 ILE H H 8.48809 0.005 . 6 4 4 ILE N N 128.935 0.02 . 7 5 5 LEU H H 8.27592 0.005 . 8 5 5 LEU N N 124.027 0.02 . 9 6 6 LEU H H 9.25496 0.005 . 10 6 6 LEU N N 126.842 0.02 . 11 7 7 GLY H H 9.08923 0.005 . 12 7 7 GLY N N 109.744 0.02 . 13 8 8 ALA H H 8.82122 0.005 . 14 8 8 ALA N N 125.341 0.02 . 15 11 11 ALA H H 7.84545 0.005 . 16 11 11 ALA N N 119.973 0.02 . 17 12 12 GLY H H 8.15846 0.005 . 18 12 12 GLY N N 104.696 0.02 . 19 16 16 GLN H H 7.54629 0.005 . 20 16 16 GLN N N 117.096 0.02 . 21 17 17 ALA H H 9.06535 0.005 . 22 17 17 ALA N N 123.681 0.02 . 23 18 18 GLN H H 7.13483 0.005 . 24 18 18 GLN N N 114.082 0.02 . 25 19 19 PHE H H 6.68905 0.005 . 26 19 19 PHE N N 117.699 0.02 . 27 20 20 ILE H H 7.77089 0.005 . 28 20 20 ILE N N 121.216 0.02 . 29 21 21 MET H H 8.4027 0.005 . 30 21 21 MET N N 119.832 0.02 . 31 22 22 GLU H H 7.39086 0.005 . 32 22 22 GLU N N 118.179 0.02 . 33 23 23 LYS H H 7.91848 0.005 . 34 23 23 LYS N N 118.853 0.02 . 35 24 24 TYR H H 8.108 0.005 . 36 24 24 TYR N N 113.018 0.02 . 37 25 25 GLY H H 7.69394 0.005 . 38 25 25 GLY N N 109.551 0.02 . 39 26 26 ILE H H 6.76879 0.005 . 40 26 26 ILE N N 112.311 0.02 . 41 28 28 GLN H H 7.97937 0.005 . 42 28 28 GLN N N 121.244 0.02 . 43 29 29 ILE H H 9.62632 0.005 . 44 29 29 ILE N N 132.127 0.02 . 45 30 30 SER H H 8.66 0.005 . 46 30 30 SER N N 121.18 0.02 . 47 31 31 THR H H 7.83773 0.005 . 48 31 31 THR N N 118.417 0.02 . 49 32 32 GLY H H 9.89534 0.005 . 50 32 32 GLY N N 111.39 0.02 . 51 33 33 ASP H H 7.97762 0.005 . 52 33 33 ASP N N 122.398 0.02 . 53 34 34 MET H H 8.40156 0.005 . 54 34 34 MET N N 120.155 0.02 . 55 35 35 LEU H H 8.62078 0.005 . 56 35 35 LEU N N 122.035 0.02 . 57 36 36 ARG H H 8.5032 0.005 . 58 36 36 ARG N N 119.115 0.02 . 59 38 38 ALA H H 7.73734 0.005 . 60 38 38 ALA N N 123.224 0.02 . 61 39 39 VAL H H 8.15608 0.005 . 62 39 39 VAL N N 119.545 0.02 . 63 40 40 LYS H H 7.79063 0.005 . 64 40 40 LYS N N 120.522 0.02 . 65 41 41 SER H H 7.95018 0.005 . 66 41 41 SER N N 112.674 0.02 . 67 42 42 GLY H H 7.71232 0.005 . 68 42 42 GLY N N 109.858 0.02 . 69 43 43 SER H H 7.56532 0.005 . 70 43 43 SER N N 114.216 0.02 . 71 44 44 GLU H H 8.84418 0.005 . 72 44 44 GLU N N 121.804 0.02 . 73 45 45 LEU H H 8.13023 0.005 . 74 45 45 LEU N N 120.172 0.02 . 75 46 46 GLY H H 7.72746 0.005 . 76 46 46 GLY N N 107.05 0.02 . 77 47 47 LYS H H 8.23513 0.005 . 78 47 47 LYS N N 120.991 0.02 . 79 48 48 GLN H H 7.58335 0.005 . 80 48 48 GLN N N 116.991 0.02 . 81 49 49 ALA H H 8.14779 0.005 . 82 49 49 ALA N N 119.476 0.02 . 83 50 50 LYS H H 7.89987 0.005 . 84 50 50 LYS N N 118.069 0.02 . 85 51 51 ASP H H 8.08615 0.005 . 86 51 51 ASP N N 116.194 0.02 . 87 52 52 ILE H H 7.20031 0.005 . 88 52 52 ILE N N 121.219 0.02 . 89 53 53 MET H H 8.20859 0.005 . 90 53 53 MET N N 118.223 0.02 . 91 54 54 ASP H H 8.4545 0.005 . 92 54 54 ASP N N 120.288 0.02 . 93 55 55 ALA H H 7.12595 0.005 . 94 55 55 ALA N N 119.194 0.02 . 95 56 56 GLY H H 7.93473 0.005 . 96 56 56 GLY N N 106.117 0.02 . 97 57 57 LYS H H 7.12797 0.005 . 98 57 57 LYS N N 117.246 0.02 . 99 58 58 LEU H H 8.92448 0.005 . 100 58 58 LEU N N 120.531 0.02 . 101 59 59 VAL H H 8.82789 0.005 . 102 59 59 VAL N N 121.75 0.02 . 103 60 60 THR H H 7.09092 0.005 . 104 60 60 THR N N 118.291 0.02 . 105 61 61 ASP H H 8.8738 0.005 . 106 61 61 ASP N N 126.376 0.02 . 107 62 62 GLU H H 9.29731 0.005 . 108 62 62 GLU N N 116.522 0.02 . 109 63 63 LEU H H 6.90677 0.005 . 110 63 63 LEU N N 117.096 0.02 . 111 64 64 VAL H H 7.07594 0.005 . 112 64 64 VAL N N 115.612 0.02 . 113 65 65 ILE H H 8.79947 0.005 . 114 65 65 ILE N N 119.916 0.02 . 115 66 66 ALA H H 7.07282 0.005 . 116 66 66 ALA N N 119.383 0.02 . 117 68 68 VAL H H 7.75086 0.005 . 118 68 68 VAL N N 119.224 0.02 . 119 69 69 LYS H H 8.29578 0.005 . 120 69 69 LYS N N 118.028 0.02 . 121 70 70 GLU H H 7.27141 0.005 . 122 70 70 GLU N N 116.363 0.02 . 123 71 71 ARG H H 7.38476 0.005 . 124 71 71 ARG N N 120.171 0.02 . 125 72 72 ILE H H 8.13466 0.005 . 126 72 72 ILE N N 111.755 0.02 . 127 73 73 ALA H H 6.79551 0.005 . 128 73 73 ALA N N 121.315 0.02 . 129 74 74 GLN H H 7.12627 0.005 . 130 74 74 GLN N N 116.425 0.02 . 131 75 75 GLU H H 8.89477 0.005 . 132 75 75 GLU N N 121.805 0.02 . 133 76 76 ASP H H 8.40664 0.005 . 134 76 76 ASP N N 117.437 0.02 . 135 77 77 CYS H H 7.59396 0.005 . 136 77 77 CYS N N 117.937 0.02 . 137 78 78 ARG H H 7.64842 0.005 . 138 78 78 ARG N N 121.866 0.02 . 139 79 79 ASN H H 8.36225 0.005 . 140 79 79 ASN N N 115.145 0.02 . 141 80 80 GLY H H 7.31681 0.005 . 142 80 80 GLY N N 107.401 0.02 . 143 81 81 PHE H H 7.48944 0.005 . 144 81 81 PHE N N 109.274 0.02 . 145 82 82 LEU H H 8.657 0.005 . 146 82 82 LEU N N 121.329 0.02 . 147 83 83 LEU H H 9.65231 0.005 . 148 83 83 LEU N N 127.926 0.02 . 149 84 84 ASP H H 8.55888 0.005 . 150 84 84 ASP N N 123.678 0.02 . 151 85 85 GLY H H 8.77455 0.005 . 152 85 85 GLY N N 113.336 0.02 . 153 88 88 ARG H H 8.22472 0.005 . 154 88 88 ARG N N 116.178 0.02 . 155 89 89 THR H H 7.00031 0.005 . 156 89 89 THR N N 107.39 0.02 . 157 90 90 ILE H H 9.67799 0.005 . 158 90 90 ILE N N 123.566 0.02 . 159 92 92 GLN H H 7.11413 0.005 . 160 92 92 GLN N N 115.481 0.02 . 161 93 93 ALA H H 7.47048 0.005 . 162 93 93 ALA N N 123.92 0.02 . 163 94 94 ASP H H 9.09833 0.005 . 164 94 94 ASP N N 120.841 0.02 . 165 95 95 ALA H H 7.88387 0.005 . 166 95 95 ALA N N 122.174 0.02 . 167 96 96 MET H H 7.44638 0.005 . 168 96 96 MET N N 117.15 0.02 . 169 97 97 LYS H H 7.55927 0.005 . 170 97 97 LYS N N 120.763 0.02 . 171 98 98 GLU H H 8.58109 0.005 . 172 98 98 GLU N N 120.873 0.02 . 173 99 99 ALA H H 7.24126 0.005 . 174 99 99 ALA N N 118.177 0.02 . 175 100 100 GLY H H 7.81665 0.005 . 176 100 100 GLY N N 107.869 0.02 . 177 101 101 ILE H H 8.042 0.005 . 178 101 101 ILE N N 122.464 0.02 . 179 102 102 ASN H H 7.95702 0.005 . 180 102 102 ASN N N 124.984 0.02 . 181 103 103 VAL H H 8.79716 0.005 . 182 103 103 VAL N N 113.378 0.02 . 183 105 105 TYR H H 7.46888 0.005 . 184 105 105 TYR N N 114.887 0.02 . 185 106 106 VAL H H 8.70802 0.005 . 186 106 106 VAL N N 123.109 0.02 . 187 107 107 LEU H H 8.45149 0.005 . 188 107 107 LEU N N 124.859 0.02 . 189 108 108 GLU H H 8.72019 0.005 . 190 108 108 GLU N N 125.305 0.02 . 191 109 109 PHE H H 9.18015 0.005 . 192 109 109 PHE N N 128.043 0.02 . 193 110 110 ASP H H 8.66958 0.005 . 194 110 110 ASP N N 125.446 0.02 . 195 111 111 VAL H H 7.48286 0.005 . 196 111 111 VAL N N 124.646 0.02 . 197 113 113 ASP H H 8.629 0.005 . 198 113 113 ASP N N 121.398 0.02 . 199 114 114 GLU H H 9.04079 0.005 . 200 114 114 GLU N N 115.014 0.02 . 201 115 115 LEU H H 7.05481 0.005 . 202 115 115 LEU N N 118.575 0.02 . 203 116 116 ILE H H 7.284 0.005 . 204 116 116 ILE N N 119.366 0.02 . 205 117 117 VAL H H 8.00507 0.005 . 206 117 117 VAL N N 118.527 0.02 . 207 118 118 ASP H H 7.80156 0.005 . 208 118 118 ASP N N 116.796 0.02 . 209 119 119 ARG H H 8.02805 0.005 . 210 119 119 ARG N N 119.238 0.02 . 211 120 120 ILE H H 8.1105 0.005 . 212 120 120 ILE N N 117.02 0.02 . 213 121 121 VAL H H 8.36885 0.005 . 214 121 121 VAL N N 116.436 0.02 . 215 122 122 GLY H H 7.12501 0.005 . 216 122 122 GLY N N 104.472 0.02 . 217 123 123 ARG H H 7.55686 0.005 . 218 123 123 ARG N N 122.033 0.02 . 219 124 124 ARG H H 8.33863 0.005 . 220 124 124 ARG N N 128.96 0.02 . 221 125 125 VAL H H 9.25421 0.005 . 222 125 125 VAL N N 116.531 0.02 . 223 126 126 HIS H H 9.07734 0.005 . 224 126 126 HIS N N 125.574 0.02 . 225 127 127 ALA H H 8.94932 0.005 . 226 127 127 ALA N N 129.196 0.02 . 227 129 129 SER H H 6.70367 0.005 . 228 129 129 SER N N 107.534 0.02 . 229 130 130 GLY H H 8.4393 0.005 . 230 130 130 GLY N N 112.907 0.02 . 231 131 131 ARG H H 8.3744 0.005 . 232 131 131 ARG N N 121.951 0.02 . 233 132 132 VAL H H 7.9195 0.005 . 234 132 132 VAL N N 119.076 0.02 . 235 133 133 TYR H H 9.10334 0.005 . 236 133 133 TYR N N 125.104 0.02 . 237 134 134 HIS H H 8.4151 0.005 . 238 134 134 HIS N N 122.155 0.02 . 239 135 135 VAL H H 7.93642 0.005 . 240 135 135 VAL N N 120.155 0.02 . 241 136 136 LYS H H 9.45799 0.005 . 242 136 136 LYS N N 120.022 0.02 . 243 137 137 PHE H H 8.99815 0.005 . 244 137 137 PHE N N 117.944 0.02 . 245 138 138 ASN H H 7.94127 0.005 . 246 138 138 ASN N N 112.992 0.02 . 247 141 141 LYS H H 10.0621 0.005 . 248 141 141 LYS N N 123.919 0.02 . 249 142 142 VAL H H 8.73706 0.005 . 250 142 142 VAL N N 120.646 0.02 . 251 143 143 GLU H H 8.07011 0.005 . 252 143 143 GLU N N 125.558 0.02 . 253 144 144 GLY H H 8.71953 0.005 . 254 144 144 GLY N N 111.619 0.02 . 255 145 145 LYS H H 7.90868 0.005 . 256 145 145 LYS N N 119.444 0.02 . 257 146 146 ASP H H 8.97624 0.005 . 258 146 146 ASP N N 119.838 0.02 . 259 147 147 ASP H H 7.86699 0.005 . 260 147 147 ASP N N 126.982 0.02 . 261 148 148 VAL H H 6.2696 0.005 . 262 148 148 VAL N N 115.248 0.02 . 263 149 149 THR H H 7.43317 0.005 . 264 149 149 THR N N 105.529 0.02 . 265 150 150 GLY H H 7.7663 0.005 . 266 150 150 GLY N N 111.124 0.02 . 267 151 151 GLU H H 7.57196 0.005 . 268 151 151 GLU N N 118.661 0.02 . 269 152 152 GLU H H 8.62242 0.005 . 270 152 152 GLU N N 119.813 0.02 . 271 153 153 LEU H H 7.87889 0.005 . 272 153 153 LEU N N 121.216 0.02 . 273 154 154 THR H H 9.27149 0.005 . 274 154 154 THR N N 113.604 0.02 . 275 155 155 THR H H 8.23506 0.005 . 276 155 155 THR N N 113.601 0.02 . 277 156 156 ARG H H 9.77764 0.005 . 278 156 156 ARG N N 126.856 0.02 . 279 157 157 LYS H H 8.98301 0.005 . 280 157 157 LYS N N 125.492 0.02 . 281 158 158 ASP H H 8.58657 0.005 . 282 158 158 ASP N N 113.194 0.02 . 283 159 159 ASP H H 7.2785 0.005 . 284 159 159 ASP N N 122.489 0.02 . 285 160 160 GLN H H 7.02328 0.005 . 286 160 160 GLN N N 117.487 0.02 . 287 161 161 GLU H H 9.10527 0.005 . 288 161 161 GLU N N 124.9 0.02 . 289 162 162 GLU H H 9.10405 0.005 . 290 162 162 GLU N N 116.537 0.02 . 291 163 163 THR H H 7.23915 0.005 . 292 163 163 THR N N 115.603 0.02 . 293 164 164 VAL H H 8.45443 0.005 . 294 164 164 VAL N N 123.694 0.02 . 295 165 165 ARG H H 8.14398 0.005 . 296 165 165 ARG N N 117.822 0.02 . 297 166 166 LYS H H 7.41782 0.005 . 298 166 166 LYS N N 119.777 0.02 . 299 167 167 ARG H H 8.57965 0.005 . 300 167 167 ARG N N 120.002 0.02 . 301 168 168 LEU H H 8.02098 0.005 . 302 168 168 LEU N N 121.121 0.02 . 303 169 169 VAL H H 7.80485 0.005 . 304 169 169 VAL N N 121.047 0.02 . 305 170 170 GLU H H 7.69655 0.005 . 306 170 170 GLU N N 120.056 0.02 . 307 171 171 TRP H H 8.40399 0.005 . 308 171 171 TRP N N 120.791 0.02 . 309 172 172 HIS H H 8.74144 0.005 . 310 172 172 HIS N N 118.509 0.02 . 311 173 173 GLN H H 8.03055 0.005 . 312 173 173 GLN N N 115.703 0.02 . 313 174 174 MET H H 8.55509 0.005 . 314 174 174 MET N N 112.955 0.02 . 315 175 175 THR H H 7.86403 0.005 . 316 175 175 THR N N 116.584 0.02 . 317 176 176 ALA H H 8.11162 0.005 . 318 176 176 ALA N N 124.991 0.02 . 319 178 178 LEU H H 8.59402 0.005 . 320 178 178 LEU N N 117.012 0.02 . 321 179 179 ILE H H 8.04341 0.005 . 322 179 179 ILE N N 122.962 0.02 . 323 180 180 GLY H H 7.63617 0.005 . 324 180 180 GLY N N 109.151 0.02 . 325 181 181 TYR H H 7.54507 0.005 . 326 181 181 TYR N N 122.868 0.02 . 327 182 182 TYR H H 9.001 0.005 . 328 182 182 TYR N N 116.649 0.02 . 329 183 183 SER H H 8.261 0.005 . 330 183 183 SER N N 119.8 0.02 . 331 184 184 LYS H H 7.6817 0.005 . 332 184 184 LYS N N 123.337 0.02 . 333 185 185 GLU H H 7.37949 0.005 . 334 185 185 GLU N N 119.466 0.02 . 335 186 186 ALA H H 8.23562 0.005 . 336 186 186 ALA N N 122.732 0.02 . 337 188 188 ALA H H 7.395 0.005 . 338 188 188 ALA N N 118.565 0.02 . 339 189 189 GLY H H 7.81434 0.005 . 340 189 189 GLY N N 105.29 0.02 . 341 190 190 ASN H H 8.13329 0.005 . 342 190 190 ASN N N 116.787 0.02 . 343 191 191 THR H H 7.43342 0.005 . 344 191 191 THR N N 112.683 0.02 . 345 192 192 LYS H H 7.75513 0.005 . 346 192 192 LYS N N 122.981 0.02 . 347 193 193 TYR H H 8.61801 0.005 . 348 193 193 TYR N N 125.56 0.02 . 349 194 194 ALA H H 8.51518 0.005 . 350 194 194 ALA N N 131.309 0.02 . 351 195 195 LYS H H 8.38916 0.005 . 352 195 195 LYS N N 122.219 0.02 . 353 196 196 VAL H H 9.17997 0.005 . 354 196 196 VAL N N 124.388 0.02 . 355 197 197 ASP H H 8.66987 0.005 . 356 197 197 ASP N N 123.692 0.02 . 357 198 198 GLY H H 8.37025 0.005 . 358 198 198 GLY N N 111.89 0.02 . 359 199 199 THR H H 8.71706 0.005 . 360 199 199 THR N N 111.965 0.02 . 361 200 200 LYS H H 6.31195 0.005 . 362 200 200 LYS N N 122.395 0.02 . 363 202 202 VAL H H 8.15839 0.005 . 364 202 202 VAL N N 122.723 0.02 . 365 203 203 ALA H H 8.81788 0.005 . 366 203 203 ALA N N 118.181 0.02 . 367 204 204 GLU H H 7.3276 0.005 . 368 204 204 GLU N N 118.339 0.02 . 369 205 205 VAL H H 7.89521 0.005 . 370 205 205 VAL N N 121.699 0.02 . 371 206 206 ARG H H 7.70951 0.005 . 372 206 206 ARG N N 118.635 0.02 . 373 207 207 ALA H H 7.1763 0.005 . 374 207 207 ALA N N 120.29 0.02 . 375 208 208 ASP H H 8.03168 0.005 . 376 208 208 ASP N N 121.337 0.02 . 377 209 209 LEU H H 8.29945 0.005 . 378 209 209 LEU N N 121.004 0.02 . 379 210 210 GLU H H 8.2203 0.005 . 380 210 210 GLU N N 119.455 0.02 . 381 211 211 LYS H H 7.39045 0.005 . 382 211 211 LYS N N 117.956 0.02 . 383 212 212 ILE H H 7.23895 0.005 . 384 212 212 ILE N N 119.238 0.02 . 385 213 213 LEU H H 7.88457 0.005 . 386 213 213 LEU N N 117.406 0.02 . 387 214 214 GLY H H 7.62028 0.005 . 388 214 214 GLY N N 112.167 0.02 . stop_ save_