data_27712 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 15N chemical shifts of calmodulin N-terminal lobe in complex with KN-93 ; _BMRB_accession_number 27712 _BMRB_flat_file_name bmr27712.str _Entry_type original _Submission_date 2018-12-04 _Accession_date 2018-12-04 _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 Saad Jamil . . 2 Vlach Jiri . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 90 "15N chemical shifts" 83 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-04-17 update BMRB 'update entry citation' 2019-02-11 original author 'original release' stop_ _Original_release_date 2018-12-04 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; The KN-93 Molecule Inhibits Calcium/Calmodulin-Dependent Protein Kinase II (CaMKII) Activity by Binding to Ca ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30753871 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Wong Melanie H. . 2 Samal Alexandra B. . 3 Lee Mike . . 4 Vlach Jiri . . 5 Novikov Nikolai . . 6 Niedziela-Majka Anita . . 7 Feng Joy Y. . 8 Koltun Dmitry O. . 9 Brendza Katherine M. . 10 Kwon 'Hyock Joo' J. . 11 Schultz Brian E. . 12 Sakowicz Roman . . 13 Saad Jamil S. . 14 Papalia Giuseppe A. . stop_ _Journal_abbreviation 'J. Mol. Biol.' _Journal_name_full 'Journal of molecular biology' _Journal_volume 431 _Journal_issue 7 _Journal_ISSN 1089-8638 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1440 _Page_last 1459 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name CaM-N _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label CaM-N $CaM-N 'Ca, 1' $entity_CA 'Ca, 2' $entity_CA stop_ _System_molecular_weight 8895.7264 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_CaM-N _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common CaM-N _Molecular_mass 8895.7264 _Mol_thiol_state 'not present' _Details calmodulin ############################## # Polymer residue sequence # ############################## _Residue_count 80 _Mol_residue_sequence ; ADQLTEEQIAEFKEAFSLFD KDGDGTITTKELGTVMRSLG QNPTEAELQDMINEVDADGN GTIDFPEFLTMMARKMKDTD ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 ALA 2 2 ASP 3 3 GLN 4 4 LEU 5 5 THR 6 6 GLU 7 7 GLU 8 8 GLN 9 9 ILE 10 10 ALA 11 11 GLU 12 12 PHE 13 13 LYS 14 14 GLU 15 15 ALA 16 16 PHE 17 17 SER 18 18 LEU 19 19 PHE 20 20 ASP 21 21 LYS 22 22 ASP 23 23 GLY 24 24 ASP 25 25 GLY 26 26 THR 27 27 ILE 28 28 THR 29 29 THR 30 30 LYS 31 31 GLU 32 32 LEU 33 33 GLY 34 34 THR 35 35 VAL 36 36 MET 37 37 ARG 38 38 SER 39 39 LEU 40 40 GLY 41 41 GLN 42 42 ASN 43 43 PRO 44 44 THR 45 45 GLU 46 46 ALA 47 47 GLU 48 48 LEU 49 49 GLN 50 50 ASP 51 51 MET 52 52 ILE 53 53 ASN 54 54 GLU 55 55 VAL 56 56 ASP 57 57 ALA 58 58 ASP 59 59 GLY 60 60 ASN 61 61 GLY 62 62 THR 63 63 ILE 64 64 ASP 65 65 PHE 66 66 PRO 67 67 GLU 68 68 PHE 69 69 LEU 70 70 THR 71 71 MET 72 72 MET 73 73 ALA 74 74 ARG 75 75 LYS 76 76 MET 77 77 LYS 78 78 ASP 79 79 THR 80 80 ASP stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . 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 GenBank AAA40864.1 AAA40864.1 . . . . . stop_ save_ ############# # Ligands # ############# save_CA _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 'CALCIUM ION' _BMRB_code CA _PDB_code CA _Molecular_mass 40.078 _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 CA CA CA . 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 $CaM-N Rat 10116 Eukaryota Metazoa Rattus norvegicus 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 $CaM-N 'recombinant technology' 'Escherichia coli' Escherichia coli BL21 pET28 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_s1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $CaM-N 0.2 mM '[[U-95% 15N]]' KN-93 0.5 mM 'natural abundance' Tris 25 mM 'natural abundance' NaCl 100 mM 'natural abundance' CaCl2 5 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr_Analysis _Saveframe_category software _Name CcpNmr_Analysis _Version 2.4 loop_ _Vendor _Address _Electronic_address CCPN 'Department of Biochemistry, Cambridge CB2 1GA, UK' http://www.ccpn.ac.uk stop_ loop_ _Task analysis stop_ _Details 'The CCPN NMR assignment and data analysis application' save_ save_nmrDraw _Saveframe_category software _Name nmrDraw _Version any loop_ _Vendor _Address _Electronic_address 'F. Delaglio' . . stop_ loop_ _Task 'Spectrum analysis' 'Spectrum display' stop_ _Details . save_ save_nmrPipe _Saveframe_category software _Name nmrPipe _Version any loop_ _Vendor _Address _Electronic_address 'F. Delaglio' . . stop_ loop_ _Task 'Spectrum processing' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_br700 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC/HMQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC/HMQC' _Sample_label $s1 save_ ####################### # Sample conditions # ####################### save_cond1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.110 . M pH 7.000 . pH pressure 1.000 . atm temperature 305.000 . 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 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 na 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $CcpNmr_Analysis stop_ loop_ _Experiment_label '2D 1H-15N HSQC/HMQC' stop_ loop_ _Sample_label $s1 stop_ _Sample_conditions_label $cond1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name CaM-N _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 3 3 GLN H H 8.316 . 1 2 3 3 GLN HE21 H 6.831 . 1 3 3 3 GLN HE22 H 7.539 . 1 4 3 3 GLN N N 119.602 . 1 5 3 3 GLN NE2 N 112.497 0.001 1 6 4 4 LEU H H 8.268 . 1 7 4 4 LEU N N 123.075 . 1 8 5 5 THR H H 8.709 . 1 9 5 5 THR N N 113.013 . 1 10 6 6 GLU H H 9.029 . 1 11 6 6 GLU N N 120.561 . 1 12 7 7 GLU H H 8.736 . 1 13 7 7 GLU N N 119.554 . 1 14 8 8 GLN H H 7.730 . 1 15 8 8 GLN HE21 H 6.749 . 1 16 8 8 GLN HE22 H 7.471 . 1 17 8 8 GLN N N 120.363 . 1 18 8 8 GLN NE2 N 111.309 0.001 1 19 9 9 ILE H H 8.368 . 1 20 9 9 ILE N N 119.491 . 1 21 10 10 ALA H H 8.003 . 1 22 10 10 ALA N N 121.259 . 1 23 11 11 GLU H H 7.782 . 1 24 11 11 GLU N N 119.792 . 1 25 12 12 PHE H H 8.591 . 1 26 12 12 PHE N N 120.208 . 1 27 13 13 LYS H H 9.207 . 1 28 13 13 LYS N N 123.685 . 1 29 14 14 GLU H H 7.816 . 1 30 14 14 GLU N N 120.447 . 1 31 15 15 ALA H H 7.977 . 1 32 15 15 ALA N N 122.572 . 1 33 16 16 PHE H H 8.775 . 1 34 16 16 PHE N N 119.237 . 1 35 17 17 SER H H 7.974 . 1 36 17 17 SER N N 112.792 . 1 37 18 18 LEU H H 7.405 . 1 38 18 18 LEU N N 121.061 . 1 39 19 19 PHE H H 7.193 . 1 40 19 19 PHE N N 114.635 . 1 41 20 20 ASP H H 7.801 . 1 42 20 20 ASP N N 117.278 . 1 43 21 21 LYS H H 7.712 . 1 44 21 21 LYS N N 124.734 . 1 45 22 22 ASP H H 8.079 . 1 46 22 22 ASP N N 114.024 . 1 47 23 23 GLY H H 7.688 . 1 48 23 23 GLY N N 109.313 . 1 49 24 24 ASP H H 8.413 . 1 50 24 24 ASP N N 120.802 . 1 51 25 25 GLY H H 10.636 . 1 52 25 25 GLY N N 113.239 . 1 53 26 26 THR H H 8.171 . 1 54 26 26 THR N N 112.832 . 1 55 27 27 ILE H H 9.860 . 1 56 27 27 ILE N N 127.283 . 1 57 28 28 THR H H 8.406 . 1 58 28 28 THR N N 116.482 . 1 59 29 29 THR H H 9.094 . 1 60 29 29 THR N N 113.034 . 1 61 30 30 LYS H H 7.669 . 1 62 30 30 LYS N N 120.804 . 1 63 31 31 GLU H H 7.675 . 1 64 31 31 GLU N N 121.694 . 1 65 32 32 LEU H H 8.683 . 1 66 32 32 LEU N N 120.656 . 1 67 33 33 GLY H H 8.672 . 1 68 33 33 GLY N N 105.773 . 1 69 34 34 THR H H 7.933 . 1 70 34 34 THR N N 118.142 . 1 71 35 35 VAL H H 7.670 . 1 72 35 35 VAL N N 122.175 . 1 73 36 36 MET H H 8.551 . 1 74 36 36 MET N N 118.487 . 1 75 37 37 ARG H H 8.485 . 1 76 37 37 ARG N N 119.029 . 1 77 38 38 SER H H 7.929 . 1 78 38 38 SER N N 118.970 . 1 79 39 39 LEU H H 7.397 . 1 80 39 39 LEU N N 120.415 . 1 81 40 40 GLY H H 7.891 . 1 82 40 40 GLY N N 106.915 . 1 83 41 41 GLN H H 7.809 . 1 84 41 41 GLN HE21 H 7.338 . 1 85 41 41 GLN HE22 H 6.708 . 1 86 41 41 GLN N N 118.372 . 1 87 41 41 GLN NE2 N 111.319 0.0 1 88 42 42 ASN H H 8.706 . 1 89 42 42 ASN HD21 H 6.724 . 1 90 42 42 ASN HD22 H 7.524 . 1 91 42 42 ASN N N 116.477 . 1 92 42 42 ASN ND2 N 112.125 0.001 1 93 44 44 THR H H 8.752 . 1 94 44 44 THR N N 112.930 . 1 95 45 45 GLU H H 8.813 . 1 96 45 45 GLU N N 120.779 . 1 97 46 46 ALA H H 8.258 . 1 98 46 46 ALA N N 120.818 . 1 99 47 47 GLU H H 7.688 . 1 100 47 47 GLU N N 118.800 . 1 101 48 48 LEU H H 8.192 . 1 102 48 48 LEU N N 120.371 . 1 103 49 49 GLN H H 8.189 . 1 104 49 49 GLN HE21 H 7.496 . 1 105 49 49 GLN HE22 H 6.911 . 1 106 49 49 GLN N N 118.261 . 1 107 49 49 GLN NE2 N 113.054 0.0 1 108 50 50 ASP H H 8.086 . 1 109 50 50 ASP N N 120.067 . 1 110 51 51 MET H H 7.901 . 1 111 51 51 MET N N 119.405 . 1 112 52 52 ILE H H 7.718 . 1 113 52 52 ILE N N 118.193 . 1 114 53 53 ASN H H 8.658 . 1 115 53 53 ASN HD21 H 7.848 . 1 116 53 53 ASN HD22 H 6.939 . 1 117 53 53 ASN N N 118.026 . 1 118 53 53 ASN ND2 N 111.682 0.0 1 119 54 54 GLU H H 7.590 . 1 120 54 54 GLU N N 116.482 . 1 121 55 55 VAL H H 7.196 . 1 122 55 55 VAL N N 109.832 . 1 123 56 56 ASP H H 7.648 . 1 124 56 56 ASP N N 121.746 . 1 125 57 57 ALA H H 8.301 . 1 126 57 57 ALA N N 131.618 . 1 127 58 58 ASP H H 8.192 . 1 128 58 58 ASP N N 113.781 . 1 129 59 59 GLY H H 7.566 . 1 130 59 59 GLY N N 108.361 . 1 131 60 60 ASN H H 8.105 . 1 132 60 60 ASN HD21 H 7.753 . 1 133 60 60 ASN HD22 H 6.966 . 1 134 60 60 ASN N N 118.637 . 1 135 60 60 ASN ND2 N 115.181 0.001 1 136 61 61 GLY H H 10.620 . 1 137 61 61 GLY N N 113.618 . 1 138 62 62 THR H H 7.671 . 1 139 62 62 THR N N 108.774 . 1 140 63 63 ILE H H 8.899 . 1 141 63 63 ILE N N 124.367 . 1 142 64 64 ASP H H 8.801 . 1 143 64 64 ASP N N 128.220 . 1 144 65 65 PHE H H 8.960 . 1 145 65 65 PHE N N 118.711 . 1 146 67 67 GLU H H 8.084 . 1 147 67 67 GLU N N 117.797 . 1 148 68 68 PHE H H 8.797 . 1 149 68 68 PHE N N 123.864 . 1 150 69 69 LEU H H 8.486 . 1 151 69 69 LEU N N 119.150 . 1 152 70 70 THR H H 7.629 . 1 153 70 70 THR N N 115.489 . 1 154 71 71 MET H H 7.587 . 1 155 71 71 MET N N 121.356 . 1 156 72 72 MET H H 8.000 . 1 157 72 72 MET N N 117.174 . 1 158 73 73 ALA H H 8.215 . 1 159 73 73 ALA N N 121.745 . 1 160 74 74 ARG H H 7.519 . 1 161 74 74 ARG N N 116.687 . 1 162 75 75 LYS H H 7.705 . 1 163 75 75 LYS N N 118.554 . 1 164 76 76 MET H H 7.790 . 1 165 76 76 MET N N 118.568 . 1 166 77 77 LYS H H 7.801 . 1 167 77 77 LYS N N 120.300 . 1 168 78 78 ASP H H 8.225 . 1 169 78 78 ASP N N 121.534 . 1 170 79 79 THR H H 7.942 . 1 171 79 79 THR N N 112.993 . 1 172 80 80 ASP H H 7.983 . 1 173 80 80 ASP N N 128.004 . 1 stop_ save_