data_25390 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone 1HN,15N assignments, 15N relaxation data and 3JHNHA coupling constants for the C10A/C13A variant of Hydrogenobacter thermophilus cytochrome c552 ; _BMRB_accession_number 25390 _BMRB_flat_file_name bmr25390.str _Entry_type original _Submission_date 2014-12-11 _Accession_date 2014-12-11 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details ; Backbone 1HN,15N assignments, 15N relaxation data and 3JHNHA coupling constants for the C10A/C13A variant of Hydrogenobacter thermophilus cytochrome c552 ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tozawa Kaeko . . 2 Ferguson Stuart . . 3 Redfield Christina . . 4 Smith Lorna . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 heteronucl_NOE 1 T1_relaxation 1 T2_relaxation 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 75 "15N chemical shifts" 75 "coupling constants" 63 "T1 relaxation values" 68 "T2 relaxation values" 68 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-08-13 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 25389 holo-wt-cytc 6033 ; Assignments for 1H and 15N have been deposited. The chemical shift file being uploaded now has revised 1HN and 15N assignments for residues 3, 4, 36, 51 and 59. ; stop_ _Original_release_date 2015-08-13 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Comparison of the backbone dynamics of wild-type Hydrogenobacter thermophilus cytochrome c(552) and its b-type variant ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 25953310 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tozawa Kaeko . . 2 Ferguson Stuart . . 3 Redfield Christina . . 4 Smith Lorna . . stop_ _Journal_abbreviation 'J. Biomol. NMR' _Journal_volume 62 _Journal_issue 2 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 221 _Page_last 231 _Year 2015 _Details . loop_ _Keyword '15N relaxation' 'c-type cytochrome' heme 'protein dynamics' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name holo-axxa_cytc _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label axxa_cytc $axxa_cytc heme $entity_HEM 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_axxa_cytc _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common axxa_cytc _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 80 _Mol_residue_sequence ; NEQLAKQKGAMAAHDLKAKK VGPAYADVAKKYAGRKDAVD YLAGKIKKGGSGVWGSVPMP PQNVTDAEAKQLAQWILSIK ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 ASN 2 2 GLU 3 3 GLN 4 4 LEU 5 5 ALA 6 6 LYS 7 7 GLN 8 8 LYS 9 9 GLY 10 10 ALA 11 11 MET 12 12 ALA 13 13 ALA 14 14 HIS 15 15 ASP 16 16 LEU 17 17 LYS 18 18 ALA 19 19 LYS 20 20 LYS 21 21 VAL 22 22 GLY 23 23 PRO 24 24 ALA 25 25 TYR 26 26 ALA 27 27 ASP 28 28 VAL 29 29 ALA 30 30 LYS 31 31 LYS 32 32 TYR 33 33 ALA 34 34 GLY 35 35 ARG 36 36 LYS 37 37 ASP 38 38 ALA 39 39 VAL 40 40 ASP 41 41 TYR 42 42 LEU 43 43 ALA 44 44 GLY 45 45 LYS 46 46 ILE 47 47 LYS 48 48 LYS 49 49 GLY 50 50 GLY 51 51 SER 52 52 GLY 53 53 VAL 54 54 TRP 55 55 GLY 56 56 SER 57 57 VAL 58 58 PRO 59 59 MET 60 60 PRO 61 61 PRO 62 62 GLN 63 63 ASN 64 64 VAL 65 65 THR 66 66 ASP 67 67 ALA 68 68 GLU 69 69 ALA 70 70 LYS 71 71 GLN 72 72 LEU 73 73 ALA 74 74 GLN 75 75 TRP 76 76 ILE 77 77 LEU 78 78 SER 79 79 ILE 80 80 LYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_HEM _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 'PROTOPORPHYRIN IX CONTAINING FE' _BMRB_code HEM _PDB_code HEM _Molecular_mass 616.487 _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 CHA CHA C . 0 . ? CHB CHB C . 0 . ? CHC CHC C . 0 . ? CHD CHD C . 0 . ? C1A C1A C . 0 . ? C2A C2A C . 0 . ? C3A C3A C . 0 . ? C4A C4A C . 0 . ? CMA CMA C . 0 . ? CAA CAA C . 0 . ? CBA CBA C . 0 . ? CGA CGA C . 0 . ? O1A O1A O . 0 . ? O2A O2A O . 0 . ? C1B C1B C . 0 . ? C2B C2B C . 0 . ? C3B C3B C . 0 . ? C4B C4B C . 0 . ? CMB CMB C . 0 . ? CAB CAB C . 0 . ? CBB CBB C . 0 . ? C1C C1C C . 0 . ? C2C C2C C . 0 . ? C3C C3C C . 0 . ? C4C C4C C . 0 . ? CMC CMC C . 0 . ? CAC CAC C . 0 . ? CBC CBC C . 0 . ? C1D C1D C . 0 . ? C2D C2D C . 0 . ? C3D C3D C . 0 . ? C4D C4D C . 0 . ? CMD CMD C . 0 . ? CAD CAD C . 0 . ? CBD CBD C . 0 . ? CGD CGD C . 0 . ? O1D O1D O . 0 . ? O2D O2D O . 0 . ? NA NA N . 0 . ? NB NB N . 0 . ? NC NC N . 0 . ? ND ND N . 0 . ? FE FE FE . 0 . ? HHB HHB H . 0 . ? HHC HHC H . 0 . ? HHD HHD H . 0 . ? HMA HMA H . 0 . ? HMAA HMAA H . 0 . ? HMAB HMAB H . 0 . ? HAA HAA H . 0 . ? HAAA HAAA H . 0 . ? HBA HBA H . 0 . ? HBAA HBAA H . 0 . ? HMB HMB H . 0 . ? HMBA HMBA H . 0 . ? HMBB HMBB H . 0 . ? HAB HAB H . 0 . ? HBB HBB H . 0 . ? HBBA HBBA H . 0 . ? HMC HMC H . 0 . ? HMCA HMCA H . 0 . ? HMCB HMCB H . 0 . ? HAC HAC H . 0 . ? HBC HBC H . 0 . ? HBCA HBCA H . 0 . ? HMD HMD H . 0 . ? HMDA HMDA H . 0 . ? HMDB HMDB H . 0 . ? HAD HAD H . 0 . ? HADA HADA H . 0 . ? HBD HBD H . 0 . ? HBDA HBDA H . 0 . ? H2A H2A H . 0 . ? H2D H2D H . 0 . ? HHA HHA 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 CHA C1A ? ? DOUB CHA C4D ? ? SING CHA HHA ? ? SING CHB C4A ? ? DOUB CHB C1B ? ? SING CHB HHB ? ? SING CHC C4B ? ? DOUB CHC C1C ? ? SING CHC HHC ? ? DOUB CHD C4C ? ? SING CHD C1D ? ? SING CHD HHD ? ? DOUB C1A C2A ? ? SING C1A NA ? ? SING C2A C3A ? ? SING C2A CAA ? ? DOUB C3A C4A ? ? SING C3A CMA ? ? SING C4A NA ? ? SING CMA HMA ? ? SING CMA HMAA ? ? SING CMA HMAB ? ? SING CAA CBA ? ? SING CAA HAA ? ? SING CAA HAAA ? ? SING CBA CGA ? ? SING CBA HBA ? ? SING CBA HBAA ? ? DOUB CGA O1A ? ? SING CGA O2A ? ? SING C1B C2B ? ? SING C1B NB ? ? DOUB C2B C3B ? ? SING C2B CMB ? ? SING C3B C4B ? ? SING C3B CAB ? ? DOUB C4B NB ? ? SING CMB HMB ? ? SING CMB HMBA ? ? SING CMB HMBB ? ? DOUB CAB CBB ? ? SING CAB HAB ? ? SING CBB HBB ? ? SING CBB HBBA ? ? SING C1C C2C ? ? SING C1C NC ? ? DOUB C2C C3C ? ? SING C2C CMC ? ? SING C3C C4C ? ? SING C3C CAC ? ? SING C4C NC ? ? SING CMC HMC ? ? SING CMC HMCA ? ? SING CMC HMCB ? ? DOUB CAC CBC ? ? SING CAC HAC ? ? SING CBC HBC ? ? SING CBC HBCA ? ? SING C1D C2D ? ? DOUB C1D ND ? ? DOUB C2D C3D ? ? SING C2D CMD ? ? SING C3D C4D ? ? SING C3D CAD ? ? SING C4D ND ? ? SING CMD HMD ? ? SING CMD HMDA ? ? SING CMD HMDB ? ? SING CAD CBD ? ? SING CAD HAD ? ? SING CAD HADA ? ? SING CBD CGD ? ? SING CBD HBD ? ? SING CBD HBDA ? ? DOUB CGD O1D ? ? SING CGD O2D ? ? SING O2A H2A ? ? SING O2D H2D ? ? SING FE NA ? ? SING FE NB ? ? SING FE NC ? ? SING FE ND ? ? 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 $axxa_cytc aquificales 940 Bacteria . Hydrogenobacter thermophilus 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 $axxa_cytc 'recombinant technology' . Escherichia coli . 'not known' 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 $axxa_cytc . mM 0.4 1 '[U-98% 15N]' 'sodium phosphate' 20 mM . . 'natural abundance' H2O 95 % . . 'natural abundance' D2O 5 % . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ 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_CCPN_Analysis _Saveframe_category software _Name CCPN_Analysis _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Home-built _Model OMEGA _Field_strength 600 _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_15N_T1_experiments_2 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T1 experiments' _Sample_label $sample_1 save_ save_15N_T2_experiments_3 _Saveframe_category NMR_applied_experiment _Experiment_name '15N T2 experiments' _Sample_label $sample_1 save_ save_15N_heteronuclear_NOE_experiment_4 _Saveframe_category NMR_applied_experiment _Experiment_name '15N heteronuclear NOE experiment' _Sample_label $sample_1 save_ save_2D_1H-15N_HMQCJ_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HMQCJ' _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 'ionic strength' 0.08 . M pH 7.1 . 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 water H 1 protons ppm 4.75 internal direct . . . 1.0 water N 15 protons ppm 118.4 internal 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $CCPN_Analysis stop_ loop_ _Experiment_label '2D 1H-15N HSQC' 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 axxa_cytc _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 GLU H H 7.76 0.01 1 2 2 2 GLU N N 119.48 0.10 1 3 3 3 GLN H H 7.80 0.01 1 4 3 3 GLN N N 119.13 0.10 1 5 4 4 LEU H H 7.81 0.01 1 6 4 4 LEU N N 123.51 0.10 1 7 5 5 ALA H H 7.91 0.01 1 8 5 5 ALA N N 120.99 0.10 1 9 6 6 LYS H H 8.21 0.01 1 10 6 6 LYS N N 118.24 0.10 1 11 7 7 GLN H H 8.44 0.01 1 12 7 7 GLN N N 122.02 0.10 1 13 8 8 LYS H H 8.20 0.01 1 14 8 8 LYS N N 115.23 0.10 1 15 9 9 GLY H H 7.83 0.01 1 16 9 9 GLY N N 107.24 0.10 1 17 10 10 ALA H H 8.51 0.01 1 18 10 10 ALA N N 123.46 0.10 1 19 11 11 MET H H 7.80 0.01 1 20 11 11 MET N N 111.36 0.10 1 21 12 12 ALA H H 7.19 0.01 1 22 12 12 ALA N N 120.91 0.10 1 23 13 13 ALA H H 6.74 0.01 1 24 13 13 ALA N N 118.08 0.10 1 25 14 14 HIS H H 7.10 0.01 1 26 14 14 HIS N N 119.27 0.10 1 27 15 15 ASP H H 7.42 0.01 1 28 15 15 ASP N N 118.87 0.10 1 29 16 16 LEU H H 8.25 0.01 1 30 16 16 LEU N N 120.49 0.10 1 31 17 17 LYS H H 7.95 0.01 1 32 17 17 LYS N N 113.79 0.10 1 33 18 18 ALA H H 8.09 0.01 1 34 18 18 ALA N N 124.67 0.10 1 35 19 19 LYS H H 8.29 0.01 1 36 19 19 LYS N N 122.73 0.10 1 37 20 20 LYS H H 7.37 0.01 1 38 20 20 LYS N N 131.07 0.10 1 39 21 21 VAL H H 7.14 0.01 1 40 21 21 VAL N N 123.47 0.10 1 41 22 22 GLY H H 6.16 0.01 1 42 22 22 GLY N N 104.55 0.10 1 43 24 24 ALA H H 8.31 0.01 1 44 24 24 ALA N N 123.32 0.10 1 45 25 25 TYR H H 7.90 0.01 1 46 25 25 TYR N N 123.08 0.10 1 47 26 26 ALA H H 8.81 0.01 1 48 26 26 ALA N N 120.34 0.10 1 49 27 27 ASP H H 6.76 0.01 1 50 27 27 ASP N N 117.88 0.10 1 51 28 28 VAL H H 7.64 0.01 1 52 28 28 VAL N N 125.08 0.10 1 53 29 29 ALA H H 8.51 0.01 1 54 29 29 ALA N N 121.80 0.10 1 55 30 30 LYS H H 7.35 0.01 1 56 30 30 LYS N N 115.84 0.10 1 57 31 31 LYS H H 7.91 0.01 1 58 31 31 LYS N N 121.28 0.10 1 59 32 32 TYR H H 7.42 0.01 1 60 32 32 TYR N N 113.57 0.10 1 61 33 33 ALA H H 7.38 0.01 1 62 33 33 ALA N N 124.34 0.10 1 63 34 34 GLY H H 8.77 0.01 1 64 34 34 GLY N N 109.43 0.10 1 65 35 35 ARG H H 7.83 0.01 1 66 35 35 ARG N N 122.48 0.10 1 67 36 36 LYS H H 9.23 0.01 1 68 36 36 LYS N N 130.30 0.10 1 69 37 37 ASP H H 8.73 0.01 1 70 37 37 ASP N N 118.36 0.10 1 71 38 38 ALA H H 7.40 0.01 1 72 38 38 ALA N N 121.78 0.10 1 73 39 39 VAL H H 8.41 0.01 1 74 39 39 VAL N N 117.31 0.10 1 75 40 40 ASP H H 7.70 0.01 1 76 40 40 ASP N N 119.88 0.10 1 77 41 41 TYR H H 8.52 0.01 1 78 41 41 TYR N N 121.63 0.10 1 79 42 42 LEU H H 8.74 0.01 1 80 42 42 LEU N N 120.90 0.10 1 81 43 43 ALA H H 8.71 0.01 1 82 43 43 ALA N N 121.79 0.10 1 83 44 44 GLY H H 7.37 0.01 1 84 44 44 GLY N N 103.64 0.10 1 85 45 45 LYS H H 7.13 0.01 1 86 45 45 LYS N N 121.95 0.10 1 87 46 46 ILE H H 7.82 0.01 1 88 46 46 ILE N N 120.87 0.10 1 89 47 47 LYS H H 6.85 0.01 1 90 47 47 LYS N N 114.68 0.10 1 91 48 48 LYS H H 7.88 0.01 1 92 48 48 LYS N N 114.42 0.10 1 93 49 49 GLY H H 7.03 0.01 1 94 49 49 GLY N N 109.38 0.10 1 95 50 50 GLY H H 7.38 0.01 1 96 50 50 GLY N N 104.34 0.10 1 97 51 51 SER H H 8.01 0.01 1 98 51 51 SER N N 111.58 0.10 1 99 52 52 GLY H H 7.98 0.01 1 100 52 52 GLY N N 107.49 0.10 1 101 53 53 VAL H H 10.32 0.01 1 102 53 53 VAL N N 128.01 0.10 1 103 54 54 TRP H H 10.49 0.01 1 104 54 54 TRP N N 123.17 0.10 1 105 55 55 GLY H H 8.03 0.01 1 106 55 55 GLY N N 110.40 0.10 1 107 56 56 SER H H 8.85 0.01 1 108 56 56 SER N N 113.52 0.10 1 109 57 57 VAL H H 7.73 0.01 1 110 57 57 VAL N N 126.42 0.10 1 111 59 59 MET H H 8.37 0.01 1 112 59 59 MET N N 122.65 0.10 1 113 62 62 GLN H H 7.17 0.01 1 114 62 62 GLN N N 119.86 0.10 1 115 63 63 ASN H H 8.89 0.01 1 116 63 63 ASN N N 123.85 0.10 1 117 64 64 VAL H H 7.46 0.01 1 118 64 64 VAL N N 115.13 0.10 1 119 65 65 THR H H 9.13 0.01 1 120 65 65 THR N N 114.52 0.10 1 121 66 66 ASP H H 8.89 0.01 1 122 66 66 ASP N N 121.97 0.10 1 123 67 67 ALA H H 8.40 0.01 1 124 67 67 ALA N N 122.04 0.10 1 125 68 68 GLU H H 7.94 0.01 1 126 68 68 GLU N N 120.53 0.10 1 127 69 69 ALA H H 8.88 0.01 1 128 69 69 ALA N N 122.42 0.10 1 129 70 70 LYS H H 7.89 0.01 1 130 70 70 LYS N N 117.83 0.10 1 131 71 71 GLN H H 8.03 0.01 1 132 71 71 GLN N N 120.59 0.10 1 133 72 72 LEU H H 8.91 0.01 1 134 72 72 LEU N N 121.22 0.10 1 135 73 73 ALA H H 8.54 0.01 1 136 73 73 ALA N N 122.46 0.10 1 137 74 74 GLN H H 8.45 0.01 1 138 74 74 GLN N N 115.63 0.10 1 139 75 75 TRP H H 8.05 0.01 1 140 75 75 TRP N N 121.13 0.10 1 141 76 76 ILE H H 8.78 0.01 1 142 76 76 ILE N N 124.51 0.10 1 143 77 77 LEU H H 7.69 0.01 1 144 77 77 LEU N N 114.57 0.10 1 145 78 78 SER H H 7.74 0.01 1 146 78 78 SER N N 116.40 0.10 1 147 79 79 ILE H H 7.13 0.01 1 148 79 79 ILE N N 126.01 0.10 1 149 80 80 LYS H H 7.71 0.01 1 150 80 80 LYS N N 132.75 0.10 1 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details . loop_ _Experiment_label '2D 1H-15N HMQCJ' stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name axxa_cytc _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 2 GLU H 2 GLU HA 5 2 5 0.5 2 3JHNHA 3 GLN H 3 GLN HA 5 2 5 0.5 3 3JHNHA 4 LEU H 4 LEU HA 5 2 5 0.5 4 3JHNHA 5 ALA H 5 ALA HA 5 2 5 0.5 5 3JHNHA 6 LYS H 6 LYS HA 5 2 5 0.5 6 3JHNHA 7 GLN H 7 GLN HA 5 2 5 0.5 7 3JHNHA 8 LYS H 8 LYS HA 7.4 6.9 7.9 0.5 8 3JHNHA 10 ALA H 10 ALA HA 5 2 5 0.5 9 3JHNHA 11 MET H 11 MET HA 7.0 6.5 7.5 0.5 10 3JHNHA 12 ALA H 12 ALA HA 6.5 6.0 7.0 0.5 11 3JHNHA 13 ALA H 13 ALA HA 9.5 9.0 10.0 0.5 12 3JHNHA 14 HIS H 14 HIS HA 9.5 9.0 10.0 0.5 13 3JHNHA 15 ASP H 15 ASP HA 9.3 8.8 9.8 0.5 14 3JHNHA 16 LEU H 16 LEU HA 5 2 5 0.5 15 3JHNHA 17 LYS H 17 LYS HA 9.5 9.0 10.0 0.5 16 3JHNHA 18 ALA H 18 ALA HA 7.8 7.3 8.3 0.5 17 3JHNHA 19 LYS H 19 LYS HA 6.2 5.7 6.7 0.5 18 3JHNHA 20 LYS H 20 LYS HA 9.2 8.7 9.7 0.5 19 3JHNHA 21 VAL H 21 VAL HA 9.2 8.7 9.7 0.5 20 3JHNHA 24 ALA H 24 ALA HA 5 2 5 0.5 21 3JHNHA 25 TYR H 25 TYR HA 5 2 5 0.5 22 3JHNHA 26 ALA H 26 ALA HA 5 2 5 0.5 23 3JHNHA 27 ASP H 27 ASP HA 7.2 6.7 7.7 0.5 24 3JHNHA 28 VAL H 28 VAL HA 5 2 5 0.5 25 3JHNHA 29 ALA H 29 ALA HA 5 2 5 0.5 26 3JHNHA 30 LYS H 30 LYS HA 5 2 5 0.5 27 3JHNHA 31 LYS H 31 LYS HA 5 2 5 0.5 28 3JHNHA 32 TYR H 32 TYR HA 9.0 8.5 9.5 0.5 29 3JHNHA 33 ALA H 33 ALA HA 5 2 5 0.5 30 3JHNHA 35 ARG H 35 ARG HA 7.2 6.7 7.7 0.5 31 3JHNHA 37 ASP H 37 ASP HA 8.6 8.1 9.1 0.5 32 3JHNHA 38 ALA H 38 ALA HA 5 2 5 0.5 33 3JHNHA 39 VAL H 39 VAL HA 5 2 5 0.5 34 3JHNHA 40 ASP H 40 ASP HA 5 2 5 0.5 35 3JHNHA 41 TYR H 41 TYR HA 5 2 5 0.5 36 3JHNHA 42 LEU H 42 LEU HA 5 2 5 0.5 37 3JHNHA 43 ALA H 43 ALA HA 5 2 5 0.5 38 3JHNHA 45 LYS H 45 LYS HA 5 2 5 0.5 39 3JHNHA 46 ILE H 46 ILE HA 5 2 5 0.5 40 3JHNHA 47 LYS H 47 LYS HA 5 2 5 0.5 41 3JHNHA 48 LYS H 48 LYS HA 7.3 6.8 7.8 0.5 42 3JHNHA 51 SER H 51 SER HA 6.9 6.4 7.4 0.5 43 3JHNHA 53 VAL H 53 VAL HA 7.9 7.4 8.4 0.5 44 3JHNHA 54 TRP H 54 TRP HA 9.9 9.4 10.4 0.5 45 3JHNHA 57 VAL H 57 VAL HA 7.5 7.0 8.0 0.5 46 3JHNHA 59 MET H 59 MET HA 8.4 7.9 8.9 0.5 47 3JHNHA 62 GLN H 62 GLN HA 9.2 8.7 9.7 0.5 48 3JHNHA 64 VAL H 64 VAL HA 9.6 9.1 10.1 0.5 49 3JHNHA 65 THR H 65 THR HA 7.1 6.6 7.6 0.5 50 3JHNHA 66 ASP H 66 ASP HA 5 2 5 0.5 51 3JHNHA 68 GLU H 68 GLU HA 5 2 5 0.5 52 3JHNHA 69 ALA H 69 ALA HA 5 2 5 0.5 53 3JHNHA 70 LYS H 70 LYS HA 5 2 5 0.5 54 3JHNHA 71 GLN H 71 GLN HA 5 2 5 0.5 55 3JHNHA 72 LEU H 72 LEU HA 5 2 5 0.5 56 3JHNHA 73 ALA H 73 ALA HA 5 2 5 0.5 57 3JHNHA 74 GLN H 74 GLN HA 5 2 5 0.5 58 3JHNHA 75 TRP H 75 TRP HA 5 2 5 0.5 59 3JHNHA 76 ILE H 76 ILE HA 5 2 5 0.5 60 3JHNHA 77 LEU H 77 LEU HA 5 2 5 0.5 61 3JHNHA 78 SER H 78 SER HA 8.0 7.5 8.5 0.5 62 3JHNHA 79 ILE H 79 ILE HA 5.4 4.9 5.9 0.5 63 3JHNHA 80 LYS H 80 LYS HA 8.4 7.9 8.9 0.5 stop_ save_ save_heteronuclear_T1_list_1 _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _T1_coherence_type Sz _T1_value_units ms _Mol_system_component_name axxa_cytc _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 2 GLU N 403.1 21.370 2 3 GLN N 463.5 9.364 3 4 LEU N 456.1 8.128 4 5 ALA N 477.7 7.032 5 6 LYS N 459.3 8.673 6 7 GLN N 441.6 7.986 7 8 LYS N 470.3 12.068 8 9 GLY N 451.4 11.901 9 10 ALA N 449.9 10.185 10 11 MET N 432.1 12.829 11 12 ALA N 427.1 10.965 12 13 ALA N 474.1 17.428 13 14 HIS N 473.6 17.312 14 15 ASP N 490.0 19.132 15 16 LEU N 440.3 9.528 16 17 LYS N 473.1 11.272 17 18 ALA N 541.1 14.244 18 19 LYS N 488.1 21.553 19 20 LYS N 519.2 18.054 20 21 VAL N 516.1 18.005 21 22 GLY N 482.4 18.462 22 24 ALA N 465.0 10.941 23 25 TYR N 441.4 10.796 24 26 ALA N 440.8 8.221 25 27 ASP N 471.3 8.414 26 28 VAL N 453.6 8.665 27 30 LYS N 483.5 7.481 28 31 LYS N 460.1 7.735 29 32 TYR N 483.2 11.828 30 33 ALA N 447.6 5.858 31 35 ARG N 468.8 6.629 32 37 ASP N 440.1 18.533 33 38 ALA N 443.9 5.447 34 39 VAL N 475.6 6.628 35 40 ASP N 504.7 6.802 36 42 LEU N 427.4 10.446 37 43 ALA N 450.3 7.511 38 44 GLY N 467.6 11.233 39 45 LYS N 442.7 9.935 40 46 ILE N 454.2 11.576 41 47 LYS N 457.0 9.343 42 48 LYS N 467.7 11.399 43 49 GLY N 460.1 16.144 44 50 GLY N 468.1 14.505 45 51 SER N 463.0 12.871 46 52 GLY N 462.4 13.248 47 53 VAL N 450.1 24.087 48 54 TRP N 461.1 26.776 49 55 GLY N 478.1 9.496 50 57 VAL N 478.4 11.561 51 59 MET N 463.8 17.049 52 62 GLN N 495.8 14.801 53 64 VAL N 529.8 11.464 54 65 THR N 459.6 10.889 55 67 ALA N 429.0 10.572 56 68 GLU N 466.8 7.766 57 69 ALA N 451.8 8.050 58 70 LYS N 462.1 7.234 59 71 GLN N 465.7 7.497 60 72 LEU N 460.8 9.353 61 73 ALA N 443.6 6.845 62 74 GLN N 471.9 7.692 63 75 TRP N 457.6 9.031 64 76 ILE N 437.1 12.506 65 77 LEU N 467.8 8.401 66 78 SER N 439.2 9.579 67 79 ILE N 431.9 7.488 68 80 LYS N 531.2 9.272 stop_ save_ save_heteronuclear_T2_list_1 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _T2_coherence_type S(+,-) _T2_value_units ms _Mol_system_component_name axxa_cytc _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 2 GLU N 108.7 5.876 0.41 0.21 2 3 GLN N 130.8 2.404 0.00 0.00 3 4 LEU N 135.8 2.266 0.00 0.00 4 5 ALA N 135.1 2.105 0.00 0.00 5 6 LYS N 141.2 2.944 0.00 0.00 6 7 GLN N 133.9 2.739 0.00 0.00 7 8 LYS N 105.6 3.240 0.62 0.11 8 9 GLY N 134.2 4.128 0.00 0.00 9 10 ALA N 127.2 2.753 0.00 0.00 10 11 MET N 140.4 4.350 0.00 0.00 11 12 ALA N 126.0 3.738 0.00 0.00 12 13 ALA N 138.9 5.831 0.00 0.00 13 14 HIS N 134.3 5.643 0.00 0.00 14 15 ASP N 130.1 5.540 0.00 0.00 15 16 LEU N 125.0 3.269 0.00 0.00 16 17 LYS N 140.7 3.710 0.00 0.00 17 18 ALA N 160.3 5.069 0.00 0.00 18 19 LYS N 150.4 8.639 0.00 0.00 19 20 LYS N 148.2 5.758 0.19 0.11 20 21 VAL N 160.6 5.883 0.00 0.00 21 22 GLY N 140.8 6.552 0.00 0.00 22 24 ALA N 132.3 3.399 0.00 0.00 23 25 TYR N 129.4 3.513 0.00 0.00 24 26 ALA N 125.0 2.661 0.00 0.00 25 27 ASP N 135.0 2.896 0.00 0.00 26 28 VAL N 140.3 2.743 0.00 0.00 27 30 LYS N 142.8 2.412 0.00 0.00 28 31 LYS N 132.6 2.556 0.00 0.00 29 32 TYR N 141.9 3.936 0.00 0.00 30 33 ALA N 141.6 2.310 0.00 0.00 31 35 ARG N 126.9 2.002 0.21 0.05 32 37 ASP N 88.9 4.350 1.13 0.21 33 38 ALA N 120.8 1.961 0.00 0.00 34 39 VAL N 135.1 2.040 0.00 0.00 35 40 ASP N 137.8 1.867 0.00 0.00 36 42 LEU N 124.7 3.363 0.00 0.00 37 43 ALA N 124.2 2.495 0.00 0.00 38 44 GLY N 128.6 3.027 0.00 0.00 39 45 LYS N 119.0 3.230 0.00 0.00 40 46 ILE N 123.9 3.219 0.00 0.00 41 47 LYS N 130.7 3.149 0.00 0.00 42 48 LYS N 141.1 3.559 0.00 0.00 43 49 GLY N 137.7 4.691 0.00 0.00 44 50 GLY N 120.9 4.947 0.31 0.12 45 51 SER N 125.4 4.407 0.00 0.00 46 52 GLY N 137.7 4.584 0.00 0.00 47 53 VAL N 137.8 6.825 0.00 0.00 48 54 TRP N 132.0 8.213 0.00 0.00 49 55 GLY N 140.4 3.359 0.00 0.00 50 57 VAL N 135.2 3.891 0.00 0.00 51 59 MET N 128.7 5.629 0.00 0.00 52 62 GLN N 123.0 4.224 0.37 0.12 53 64 VAL N 157.8 4.027 0.00 0.00 54 65 THR N 133.3 3.612 0.00 0.00 55 67 ALA N 101.9 2.894 0.59 0.11 56 68 GLU N 132.8 2.588 0.00 0.00 57 69 ALA N 132.0 2.372 0.00 0.00 58 70 LYS N 134.3 2.176 0.00 0.00 59 71 GLN N 137.8 2.519 0.00 0.00 60 72 LEU N 134.6 3.257 0.00 0.00 61 73 ALA N 133.9 2.356 0.00 0.00 62 74 GLN N 135.8 2.484 0.00 0.00 63 75 TRP N 131.1 3.065 0.00 0.00 64 76 ILE N 131.5 3.841 0.00 0.00 65 77 LEU N 132.7 2.789 0.00 0.00 66 78 SER N 120.9 2.661 0.00 0.00 67 79 ILE N 137.6 2.672 0.00 0.00 68 80 LYS N 174.7 3.052 0.00 0.00 stop_ save_ save_heteronuclear_noe_list_1 _Saveframe_category heteronuclear_NOE _Details . loop_ _Experiment_label '15N heteronuclear NOE experiment' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name axxa_cytc _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'relative intensities' _NOE_reference_value 1.0 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 2 GLU 0.744 0.094 3 GLN 0.748 0.047 4 LEU 0.794 0.036 5 ALA 0.741 0.035 6 LYS 0.641 0.041 7 GLN 0.774 0.038 8 LYS 0.748 0.064 9 GLY 0.841 0.063 10 ALA 0.781 0.047 11 MET 0.863 0.067 12 ALA 0.770 0.058 13 ALA 0.791 0.084 14 HIS 0.716 0.073 15 ASP 0.730 0.084 16 LEU 0.815 0.053 17 LYS 0.735 0.052 18 ALA 0.528 0.056 19 LYS 0.683 0.068 20 LYS 0.500 0.066 21 VAL 0.817 0.082 22 GLY 0.788 0.077 24 ALA 0.767 0.047 25 TYR 0.815 0.054 26 ALA 0.798 0.043 27 ASP 0.828 0.043 28 VAL 0.778 0.044 30 LYS 0.791 0.040 31 LYS 0.744 0.042 32 TYR 0.852 0.060 33 ALA 0.767 0.034 35 ARG 0.773 0.032 37 ASP 0.708 0.065 38 ALA 0.795 0.034 39 VAL 0.782 0.034 40 ASP 0.774 0.031 42 LEU 0.786 0.048 43 ALA 0.769 0.038 44 GLY 0.794 0.052 45 LYS 0.789 0.051 46 ILE 0.779 0.059 47 LYS 0.751 0.050 48 LYS 0.799 0.059 49 GLY 0.835 0.072 50 GLY 0.796 0.055 51 SER 0.755 0.052 52 GLY 0.754 0.056 53 VAL 0.816 0.081 54 TRP 0.795 0.087 55 GLY 0.803 0.043 57 VAL 0.750 0.056 59 MET 0.690 0.056 62 GLN 0.869 0.082 64 VAL 0.677 0.053 65 THR 0.758 0.059 67 ALA 0.791 0.038 68 GLU 0.745 0.038 69 ALA 0.754 0.036 70 LYS 0.769 0.038 71 GLN 0.731 0.039 72 LEU 0.819 0.052 73 ALA 0.768 0.032 74 GLN 0.781 0.043 75 TRP 0.726 0.042 76 ILE 0.818 0.061 77 LEU 0.749 0.043 78 SER 0.816 0.045 79 ILE 0.770 0.044 80 LYS 0.635 0.037 stop_ save_