data_25477 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of oxidized triheme cytochrome PpcA from Geobacter sulfurreducens ; _BMRB_accession_number 25477 _BMRB_flat_file_name bmr25477.str _Entry_type original _Submission_date 2015-02-08 _Accession_date 2015-02-08 _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 Morgado Leonor . . 2 Bruix Marta . . 3 Pokkuluri Raj . . 4 Salgueiro Carlos A. . 5 Turner David L. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 4 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 405 "15N chemical shifts" 63 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-03-29 update BMRB 'update entry citation' 2016-02-08 original author 'original release' stop_ _Original_release_date 2016-02-08 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Redox- and pH-linked conformational changes in triheme cytochrome PpcA from Geobacter sulfurreducens. ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 28062839 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Morgado Leonor . . 2 Bruix Marta . . 3 Pokkuluri Raj . . 4 Salgueiro Carlos A. . 5 Turner David L. . stop_ _Journal_abbreviation 'Biochem. J.' _Journal_name_full 'The Biochemical journal' _Journal_volume 474 _Journal_issue 2 _Journal_ISSN 1470-8728 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 231 _Page_last 246 _Year 2017 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'oxidized triheme cytochrome PpcA' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 'PROTOPORPHYRIN IX CONTAINING FE_1' $entity_HEC 'PROTOPORPHYRIN IX CONTAINING FE_2' $entity_HEC 'PROTOPORPHYRIN IX CONTAINING FE_3' $entity_HEC 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_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 7748.196 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 71 _Mol_residue_sequence ; ADDIVLKAKNGDVKFPHKAH QKAVPDCKKCHEKGPGKIEG FGKEMAHGKGCKGCHEEMKK GPTKCGECHKK ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 ASP 3 ASP 4 ILE 5 VAL 6 LEU 7 LYS 8 ALA 9 LYS 10 ASN 11 GLY 12 ASP 13 VAL 14 LYS 15 PHE 16 PRO 17 HIS 18 LYS 19 ALA 20 HIS 21 GLN 22 LYS 23 ALA 24 VAL 25 PRO 26 ASP 27 CYS 28 LYS 29 LYS 30 CYS 31 HIS 32 GLU 33 LYS 34 GLY 35 PRO 36 GLY 37 LYS 38 ILE 39 GLU 40 GLY 41 PHE 42 GLY 43 LYS 44 GLU 45 MET 46 ALA 47 HIS 48 GLY 49 LYS 50 GLY 51 CYS 52 LYS 53 GLY 54 CYS 55 HIS 56 GLU 57 GLU 58 MET 59 LYS 60 LYS 61 GLY 62 PRO 63 THR 64 LYS 65 CYS 66 GLY 67 GLU 68 CYS 69 HIS 70 LYS 71 LYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_HEC _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common "entity_HEC (HEME C)" _BMRB_code HEC _PDB_code HEC _Molecular_mass 618.503 _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 FE FE FE . 0 . ? CHA CHA C . 0 . ? CHB CHB C . 0 . ? CHC CHC C . 0 . ? CHD CHD C . 0 . ? NA NA N . 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 . ? NB NB N . 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 . ? NC NC N . 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 . ? ND ND N . 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 . ? HHA HHA H . 0 . ? HHB HHB H . 0 . ? HHC HHC H . 0 . ? HHD HHD H . 0 . ? HMA1 HMA1 H . 0 . ? HMA2 HMA2 H . 0 . ? HMA3 HMA3 H . 0 . ? HAA1 HAA1 H . 0 . ? HAA2 HAA2 H . 0 . ? HBA1 HBA1 H . 0 . ? HBA2 HBA2 H . 0 . ? H2A H2A H . 0 . ? HMB1 HMB1 H . 0 . ? HMB2 HMB2 H . 0 . ? HMB3 HMB3 H . 0 . ? HAB HAB H . 0 . ? HBB1 HBB1 H . 0 . ? HBB2 HBB2 H . 0 . ? HBB3 HBB3 H . 0 . ? HMC1 HMC1 H . 0 . ? HMC2 HMC2 H . 0 . ? HMC3 HMC3 H . 0 . ? HAC HAC H . 0 . ? HBC1 HBC1 H . 0 . ? HBC2 HBC2 H . 0 . ? HBC3 HBC3 H . 0 . ? HMD1 HMD1 H . 0 . ? HMD2 HMD2 H . 0 . ? HMD3 HMD3 H . 0 . ? HAD1 HAD1 H . 0 . ? HAD2 HAD2 H . 0 . ? HBD1 HBD1 H . 0 . ? HBD2 HBD2 H . 0 . ? H2D H2D 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 FE NA ? ? SING FE NB ? ? SING FE NC ? ? SING FE ND ? ? DOUB CHA C1A ? ? SING CHA C4D ? ? SING CHA HHA ? ? DOUB CHB C4A ? ? SING CHB C1B ? ? SING CHB HHB ? ? DOUB CHC C4B ? ? SING CHC C1C ? ? SING CHC HHC ? ? DOUB CHD C4C ? ? SING CHD C1D ? ? SING CHD HHD ? ? SING NA C1A ? ? SING NA C4A ? ? SING C1A C2A ? ? DOUB C2A C3A ? ? SING C2A CAA ? ? SING C3A C4A ? ? SING C3A CMA ? ? SING CMA HMA1 ? ? SING CMA HMA2 ? ? SING CMA HMA3 ? ? SING CAA CBA ? ? SING CAA HAA1 ? ? SING CAA HAA2 ? ? SING CBA CGA ? ? SING CBA HBA1 ? ? SING CBA HBA2 ? ? DOUB CGA O1A ? ? SING CGA O2A ? ? SING O2A H2A ? ? SING NB C1B ? ? SING NB C4B ? ? DOUB C1B C2B ? ? SING C2B C3B ? ? SING C2B CMB ? ? SING C3B C4B ? ? DOUB C3B CAB ? ? SING CMB HMB1 ? ? SING CMB HMB2 ? ? SING CMB HMB3 ? ? SING CAB CBB ? ? SING CAB HAB ? ? SING CBB HBB1 ? ? SING CBB HBB2 ? ? SING CBB HBB3 ? ? SING NC C1C ? ? SING NC C4C ? ? DOUB C1C C2C ? ? SING C2C C3C ? ? SING C2C CMC ? ? SING C3C C4C ? ? DOUB C3C CAC ? ? SING CMC HMC1 ? ? SING CMC HMC2 ? ? SING CMC HMC3 ? ? SING CAC CBC ? ? SING CAC HAC ? ? SING CBC HBC1 ? ? SING CBC HBC2 ? ? SING CBC HBC3 ? ? SING ND C1D ? ? SING ND C4D ? ? DOUB C1D C2D ? ? SING C2D C3D ? ? SING C2D CMD ? ? DOUB C3D C4D ? ? SING C3D CAD ? ? SING CMD HMD1 ? ? SING CMD HMD2 ? ? SING CMD HMD3 ? ? SING CAD CBD ? ? SING CAD HAD1 ? ? SING CAD HAD2 ? ? SING CBD CGD ? ? SING CBD HBD1 ? ? SING CBD HBD2 ? ? DOUB CGD O1D ? ? SING CGD O2D ? ? SING O2D H2D ? ? 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 $entity_1 'Geobacter sulfurreducens' 35554 Bacteria . Geobacter sulfurreducens 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 $entity_1 'recombinant technology' . Escherichia coli BL21 pCK32 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 $entity_1 2 mM 'natural abundance' H2O 92 % 'natural abundance' D2O 8 % 'natural abundance' 'sodium phosphate' 45 mM 'natural abundance' 'sodium azide' 0.04 % 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 2 mM '[U-100% 15N]' H2O 92 % 'natural abundance' D2O 8 % 'natural abundance' 'sodium phosphate' 45 mM 'natural abundance' 'sodium azide' 0.04 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TopSpin _Saveframe_category software _Name TopSpin _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_PARADYANA _Saveframe_category software _Name PARADYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Braun and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Avance800 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _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' 100 . mM pH 5.5 . 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 4.8 internal direct . . . 1.0 water N 15 protons ppm 4.8 internal indirect . . . 0.10132918 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_ _Software_label $TopSpin stop_ loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-15N HSQC' 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 entity_1 _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 ALA HA H 5.195 0.011 1 2 1 1 ALA HB H 2.576 0.007 1 3 2 2 ASP H H 10.343 0.008 1 4 2 2 ASP HA H 7.247 0.008 1 5 2 2 ASP HB2 H 4.032 0.003 2 6 2 2 ASP HB3 H 4.489 0.005 2 7 2 2 ASP N N 124.367 0.000 1 8 3 3 ASP H H 9.546 0.005 1 9 3 3 ASP HA H 7.279 0.005 1 10 3 3 ASP HB2 H 3.448 0.006 2 11 3 3 ASP HB3 H 3.486 0.008 2 12 3 3 ASP N N 120.501 0.000 1 13 4 4 ILE H H 10.258 0.005 1 14 4 4 ILE HA H 5.099 0.011 1 15 4 4 ILE HB H 2.727 0.008 1 16 4 4 ILE HG12 H 2.409 0.009 2 17 4 4 ILE HG13 H 4.077 0.010 2 18 4 4 ILE HG2 H 0.845 0.006 1 19 4 4 ILE HD1 H 2.111 0.006 1 20 4 4 ILE N N 123.994 0.000 1 21 5 5 VAL H H 9.384 0.004 1 22 5 5 VAL HA H 4.932 0.012 1 23 5 5 VAL HB H 2.384 0.006 1 24 5 5 VAL HG1 H 1.355 0.007 1 25 5 5 VAL HG2 H 1.485 0.004 1 26 5 5 VAL N N 129.474 0.000 1 27 6 6 LEU H H 9.655 0.005 1 28 6 6 LEU HA H 4.542 0.006 1 29 6 6 LEU HB2 H 1.957 0.007 1 30 6 6 LEU HB3 H 0.840 0.010 1 31 6 6 LEU HG H 1.249 0.005 1 32 6 6 LEU HD1 H -0.612 0.006 1 33 6 6 LEU HD2 H -0.156 0.005 1 34 6 6 LEU N N 132.431 0.000 1 35 7 7 LYS H H 8.556 0.005 1 36 7 7 LYS HA H 4.947 0.008 1 37 7 7 LYS HB2 H 1.768 0.008 2 38 7 7 LYS HB3 H 1.871 0.008 2 39 7 7 LYS HG2 H 1.674 0.005 2 40 7 7 LYS HG3 H 1.644 0.002 2 41 7 7 LYS N N 124.598 0.000 1 42 8 8 ALA H H 10.136 0.010 1 43 8 8 ALA HA H 4.782 0.015 1 44 8 8 ALA HB H 4.325 0.005 1 45 8 8 ALA N N 124.683 0.000 1 46 9 9 LYS H H 10.009 0.006 1 47 9 9 LYS HA H 4.337 0.008 1 48 9 9 LYS HB2 H 1.525 0.009 2 49 9 9 LYS HG2 H 0.974 0.005 2 50 9 9 LYS HG3 H 1.118 0.004 2 51 9 9 LYS HD2 H 1.262 0.007 2 52 9 9 LYS N N 125.212 0.000 1 53 10 10 ASN H H 9.692 0.007 1 54 10 10 ASN HA H 5.107 0.008 1 55 10 10 ASN HB2 H 1.655 0.008 2 56 10 10 ASN HB3 H 2.802 0.007 2 57 10 10 ASN N N 114.864 0.000 1 58 11 11 GLY H H 9.484 0.004 1 59 11 11 GLY HA2 H 5.349 0.008 1 60 11 11 GLY HA3 H 6.962 0.006 1 61 11 11 GLY N N 113.592 0.000 1 62 12 12 ASP H H 10.354 0.006 1 63 12 12 ASP HA H 6.986 0.005 1 64 12 12 ASP HB2 H 3.543 0.008 2 65 12 12 ASP HB3 H 3.836 0.008 2 66 12 12 ASP N N 133.500 0.000 1 67 13 13 VAL H H 10.729 0.004 1 68 13 13 VAL HA H 6.764 0.004 1 69 13 13 VAL HB H 3.384 0.006 1 70 13 13 VAL HG1 H 1.095 0.008 1 71 13 13 VAL HG2 H 6.495 0.007 1 72 13 13 VAL N N 122.888 0.000 1 73 14 14 LYS H H 9.987 0.006 1 74 14 14 LYS HA H 5.074 0.011 1 75 14 14 LYS HB2 H 2.362 0.006 2 76 14 14 LYS HG2 H 1.812 0.007 2 77 14 14 LYS HG3 H 2.067 0.008 2 78 14 14 LYS HD2 H 2.181 0.007 2 79 14 14 LYS HE2 H 3.427 0.005 2 80 14 14 LYS N N 130.045 0.000 1 81 15 15 PHE H H 9.869 0.006 1 82 15 15 PHE HA H 5.815 0.009 1 83 15 15 PHE HB2 H 2.722 0.010 2 84 15 15 PHE HB3 H 3.687 0.009 2 85 15 15 PHE N N 126.228 0.000 1 86 16 16 PRO HA H 7.385 0.007 1 87 16 16 PRO HB2 H 3.260 0.006 2 88 16 16 PRO HB3 H 4.343 0.007 2 89 16 16 PRO HG2 H 2.136 0.009 2 90 16 16 PRO HD2 H 4.518 0.009 2 91 17 17 HIS H H 11.607 0.007 1 92 17 17 HIS HA H 8.377 0.009 1 93 17 17 HIS HB2 H 15.704 0.012 1 94 17 17 HIS HB3 H 11.352 0.016 1 95 17 17 HIS N N 138.291 0.000 1 96 18 18 LYS H H 12.968 0.006 1 97 18 18 LYS HA H 7.447 0.007 1 98 18 18 LYS HB2 H 4.154 0.003 2 99 18 18 LYS HB3 H 4.587 0.007 2 100 18 18 LYS HG2 H 3.064 0.019 2 101 18 18 LYS HG3 H 3.153 0.015 2 102 18 18 LYS HD2 H 3.156 0.015 2 103 18 18 LYS HE2 H 4.069 0.007 2 104 18 18 LYS N N 126.220 0.000 1 105 19 19 ALA H H 10.987 0.005 1 106 19 19 ALA HA H 5.578 0.010 1 107 19 19 ALA HB H 3.019 0.007 1 108 19 19 ALA N N 124.418 0.000 1 109 20 20 HIS H H 12.109 0.008 1 110 20 20 HIS HA H 7.924 0.011 1 111 20 20 HIS HB2 H 9.634 0.011 1 112 20 20 HIS HB3 H 6.070 0.011 1 113 20 20 HIS N N 118.446 0.000 1 114 21 21 GLN H H 9.883 0.006 1 115 21 21 GLN HA H 3.756 0.004 1 116 21 21 GLN HB2 H 2.127 0.004 2 117 21 21 GLN HB3 H 3.464 0.010 2 118 21 21 GLN HG2 H 0.671 0.006 2 119 21 21 GLN HG3 H 4.373 0.002 2 120 21 21 GLN N N 121.637 0.000 1 121 22 22 LYS H H 8.086 0.008 1 122 22 22 LYS HA H 4.448 0.007 1 123 22 22 LYS HB2 H 2.379 0.004 2 124 22 22 LYS HB3 H 2.462 0.003 2 125 22 22 LYS HG2 H 1.797 0.015 2 126 22 22 LYS HD2 H 2.021 0.006 2 127 22 22 LYS HE2 H 3.296 0.012 2 128 22 22 LYS N N 117.108 0.000 1 129 23 23 ALA H H 8.047 0.008 1 130 23 23 ALA HA H 4.376 0.006 1 131 23 23 ALA HB H 2.045 0.008 1 132 23 23 ALA N N 119.728 0.000 1 133 24 24 VAL H H 8.394 0.007 1 134 24 24 VAL HA H 3.824 0.012 1 135 24 24 VAL HB H 1.352 0.011 1 136 24 24 VAL HG1 H -0.377 0.009 1 137 24 24 VAL HG2 H -0.150 0.007 1 138 24 24 VAL N N 118.949 0.000 1 139 25 25 PRO HA H 4.223 0.007 1 140 25 25 PRO HB2 H 1.778 0.008 2 141 25 25 PRO HG2 H 1.708 0.005 2 142 25 25 PRO HD2 H 3.128 0.008 2 143 25 25 PRO HD3 H 3.340 0.006 2 144 26 26 ASP H H 7.169 0.004 1 145 26 26 ASP HA H 4.399 0.006 1 146 26 26 ASP HB2 H 2.280 0.012 2 147 26 26 ASP HB3 H 2.473 0.005 2 148 26 26 ASP N N 118.341 0.000 1 149 27 27 CYS H H 7.468 0.007 1 150 27 27 CYS HA H 2.046 0.005 1 151 27 27 CYS HB2 H 3.230 0.008 2 152 27 27 CYS N N 124.578 0.000 1 153 28 28 LYS H H 8.329 0.006 1 154 28 28 LYS HA H 5.514 0.007 1 155 28 28 LYS HB2 H 2.270 0.008 2 156 28 28 LYS HG2 H 2.014 0.010 2 157 28 28 LYS HG3 H 2.145 0.009 2 158 28 28 LYS HE2 H 3.362 0.001 2 159 28 28 LYS N N 115.097 0.000 1 160 29 29 LYS H H 7.449 0.007 1 161 29 29 LYS HA H 3.787 0.007 1 162 29 29 LYS HB2 H 0.682 0.006 2 163 29 29 LYS HB3 H 1.115 0.006 2 164 29 29 LYS HG2 H 0.495 0.012 2 165 29 29 LYS HE2 H 2.338 0.000 2 166 29 29 LYS HE3 H 2.455 0.008 2 167 29 29 LYS N N 118.552 0.000 1 168 30 30 CYS H H 6.636 0.011 1 169 30 30 CYS HA H 4.399 0.011 1 170 30 30 CYS HB2 H 0.468 0.013 2 171 30 30 CYS HB3 H 1.790 0.024 2 172 30 30 CYS N N 111.091 0.000 1 173 31 31 HIS H H 11.948 0.011 1 174 31 31 HIS HA H 10.231 0.020 1 175 31 31 HIS HB2 H 10.292 0.013 1 176 31 31 HIS HB3 H 12.897 0.011 1 177 31 31 HIS N N 122.497 0.000 1 178 32 32 GLU H H 10.401 0.007 1 179 32 32 GLU HA H 5.147 0.009 1 180 32 32 GLU HB2 H 2.805 0.018 2 181 32 32 GLU HB3 H 2.864 0.007 2 182 32 32 GLU N N 128.508 0.000 1 183 33 33 LYS H H 10.277 0.005 1 184 33 33 LYS HA H 5.304 0.009 1 185 33 33 LYS HB2 H 2.784 0.027 2 186 33 33 LYS HB3 H 2.830 0.031 2 187 33 33 LYS HG2 H 2.021 0.007 2 188 33 33 LYS HG3 H 2.165 0.006 2 189 33 33 LYS HD2 H 2.197 0.000 2 190 33 33 LYS HE2 H 3.383 0.002 2 191 33 33 LYS HE3 H 4.014 0.000 2 192 33 33 LYS N N 117.199 0.000 1 193 34 34 GLY H H 8.997 0.004 1 194 34 34 GLY HA2 H 4.982 0.010 2 195 34 34 GLY HA3 H 5.238 0.007 2 196 34 34 GLY N N 109.000 0.000 1 197 35 35 PRO HA H 6.237 0.015 1 198 35 35 PRO HB2 H -0.786 0.012 2 199 35 35 PRO HB3 H -0.268 0.007 2 200 35 35 PRO HG2 H 1.374 0.006 2 201 35 35 PRO HD2 H 3.735 0.003 2 202 35 35 PRO HD3 H 4.167 0.006 2 203 36 36 GLY HA2 H 1.010 0.004 2 204 36 36 GLY HA3 H 3.934 0.009 2 205 37 37 LYS H H 7.501 0.004 1 206 37 37 LYS HA H 2.806 0.008 1 207 37 37 LYS HB2 H 1.242 0.011 2 208 37 37 LYS HG2 H 0.535 0.003 2 209 37 37 LYS HG3 H 0.766 0.005 2 210 37 37 LYS HD2 H 0.970 0.005 2 211 37 37 LYS N N 118.406 0.000 1 212 38 38 ILE H H 9.561 0.021 1 213 38 38 ILE HA H 5.325 0.006 1 214 38 38 ILE HB H 1.604 0.008 1 215 38 38 ILE HG12 H 4.296 0.005 2 216 38 38 ILE HG2 H 1.445 0.005 1 217 38 38 ILE HD1 H 1.621 0.006 1 218 38 38 ILE N N 128.016 0.000 1 219 39 39 GLU H H 9.317 0.005 1 220 39 39 GLU HA H 4.048 0.007 1 221 39 39 GLU HB2 H 2.164 0.009 2 222 39 39 GLU HG2 H 2.351 0.006 2 223 39 39 GLU HG3 H 2.388 0.005 2 224 39 39 GLU N N 131.257 0.000 1 225 40 40 GLY H H 8.977 0.007 1 226 40 40 GLY HA2 H 3.579 0.007 2 227 40 40 GLY HA3 H 4.038 0.006 2 228 40 40 GLY N N 112.897 0.000 1 229 41 41 PHE H H 7.595 0.007 1 230 41 41 PHE HA H 3.541 0.004 1 231 41 41 PHE HB2 H 2.535 0.007 1 232 41 41 PHE HB3 H 2.174 0.005 1 233 41 41 PHE HD1 H 6.033 0.001 3 234 41 41 PHE HD2 H 6.031 0.006 3 235 41 41 PHE HE1 H 5.013 0.003 3 236 41 41 PHE HE2 H 5.004 0.011 3 237 41 41 PHE HZ H 4.347 0.012 1 238 41 41 PHE N N 121.371 0.000 1 239 42 42 GLY H H 4.698 0.008 1 240 42 42 GLY HA2 H 2.380 0.005 2 241 42 42 GLY HA3 H 3.075 0.003 2 242 43 43 LYS H H 7.221 0.006 1 243 43 43 LYS HA H -0.118 0.009 1 244 43 43 LYS HB2 H -0.438 0.013 2 245 43 43 LYS HB3 H 0.798 0.018 2 246 43 43 LYS HG2 H 3.831 0.027 2 247 43 43 LYS HE2 H 3.007 0.011 2 248 43 43 LYS HE3 H 4.068 0.000 2 249 43 43 LYS N N 121.161 0.000 1 250 44 44 GLU H H 8.811 0.005 1 251 44 44 GLU HA H 6.128 0.010 1 252 44 44 GLU HB2 H 2.512 0.007 2 253 44 44 GLU HB3 H 2.661 0.007 2 254 44 44 GLU HG2 H 3.086 0.008 2 255 44 44 GLU HG3 H 3.168 0.006 2 256 44 44 GLU N N 117.347 0.000 1 257 45 45 MET H H 8.202 0.013 1 258 45 45 MET HA H 4.195 0.007 1 259 45 45 MET HB2 H 0.813 0.009 2 260 45 45 MET HB3 H 1.280 0.012 2 261 45 45 MET HG2 H 1.814 0.013 2 262 45 45 MET HG3 H 2.303 0.010 2 263 45 45 MET N N 119.032 0.000 1 264 46 46 ALA H H 7.585 0.006 1 265 46 46 ALA HA H 1.728 0.007 1 266 46 46 ALA HB H -3.380 0.008 1 267 46 46 ALA N N 120.454 0.000 1 268 47 47 HIS H H 11.691 0.008 1 269 47 47 HIS HA H 8.274 0.011 1 270 47 47 HIS HB2 H 15.250 0.024 2 271 47 47 HIS HB3 H 18.084 0.011 2 272 47 47 HIS N N 118.598 0.000 1 273 48 48 GLY H H 8.572 0.006 1 274 48 48 GLY HA2 H 5.455 0.005 1 275 48 48 GLY HA3 H 4.495 0.013 1 276 48 48 GLY N N 112.155 0.000 1 277 49 49 LYS H H 9.177 0.004 1 278 49 49 LYS HA H 3.317 0.007 1 279 49 49 LYS HB2 H 1.498 0.006 2 280 49 49 LYS HG2 H 1.144 0.007 2 281 49 49 LYS HG3 H 1.267 0.013 2 282 49 49 LYS HD2 H 1.500 0.000 2 283 49 49 LYS N N 126.044 0.000 1 284 50 50 GLY H H 7.684 0.005 1 285 50 50 GLY HA2 H 1.598 0.010 2 286 50 50 GLY HA3 H 1.834 0.007 2 287 50 50 GLY N N 104.401 0.000 1 288 51 51 CYS H H 4.993 0.009 1 289 51 51 CYS HA H -1.919 0.013 1 290 51 51 CYS HB2 H 0.134 0.011 1 291 51 51 CYS HB3 H 0.535 0.010 1 292 52 52 LYS H H 7.729 0.006 1 293 52 52 LYS HA H 5.545 0.009 1 294 52 52 LYS HB2 H 1.599 0.005 2 295 52 52 LYS HB3 H 2.945 0.010 2 296 52 52 LYS HD2 H 2.244 0.002 2 297 52 52 LYS HD3 H 2.467 0.004 2 298 52 52 LYS HE2 H 4.139 0.002 2 299 52 52 LYS N N 121.643 0.000 1 300 53 53 GLY H H 9.306 0.005 1 301 53 53 GLY HA2 H 4.541 0.006 1 302 53 53 GLY HA3 H 3.859 0.004 1 303 53 53 GLY N N 104.830 0.000 1 304 54 54 CYS H H 6.172 0.008 1 305 54 54 CYS HA H 4.415 0.007 1 306 54 54 CYS HB2 H 0.107 0.009 2 307 54 54 CYS HB3 H 1.343 0.007 2 308 54 54 CYS N N 118.874 0.000 1 309 55 55 HIS H H 10.083 0.009 1 310 55 55 HIS HA H 8.557 0.009 1 311 55 55 HIS HB2 H 16.217 0.012 1 312 55 55 HIS HB3 H 19.327 0.010 1 313 55 55 HIS N N 119.047 0.000 1 314 56 56 GLU H H 9.871 0.006 1 315 56 56 GLU HA H 4.780 0.001 1 316 56 56 GLU HB2 H 2.609 0.006 2 317 56 56 GLU HB3 H 2.920 0.013 2 318 56 56 GLU HG3 H 3.334 0.012 2 319 56 56 GLU N N 119.125 0.000 1 320 57 57 GLU H H 8.337 0.006 1 321 57 57 GLU HA H 4.301 0.007 1 322 57 57 GLU HB2 H 2.144 0.008 2 323 57 57 GLU HB3 H 2.307 0.010 2 324 57 57 GLU HG2 H 2.474 0.006 2 325 57 57 GLU N N 120.962 0.000 1 326 58 58 MET H H 9.289 0.006 1 327 58 58 MET HA H 4.270 0.006 1 328 58 58 MET HB2 H 2.201 0.012 2 329 58 58 MET HB3 H 2.860 0.007 2 330 58 58 MET HG2 H 2.444 0.004 2 331 58 58 MET N N 114.871 0.000 1 332 59 59 LYS H H 8.157 0.005 1 333 59 59 LYS HA H 4.191 0.002 1 334 59 59 LYS HB2 H 1.994 0.000 2 335 59 59 LYS HB3 H 1.502 0.002 2 336 59 59 LYS HE2 H 3.140 0.003 2 337 59 59 LYS N N 115.252 0.000 1 338 60 60 LYS H H 8.245 0.005 1 339 60 60 LYS HA H 3.865 0.006 1 340 60 60 LYS HB2 H 0.863 0.008 1 341 60 60 LYS HB3 H 0.535 0.008 1 342 60 60 LYS HG2 H 0.870 0.013 2 343 60 60 LYS HG3 H 0.921 0.006 2 344 60 60 LYS HD2 H 1.109 0.008 2 345 60 60 LYS HE2 H 2.542 0.000 2 346 60 60 LYS N N 118.225 0.000 1 347 61 61 GLY H H 6.115 0.006 1 348 61 61 GLY HA2 H -2.601 0.007 2 349 61 61 GLY N N 102.395 0.000 1 350 62 62 PRO HA H 4.514 0.004 1 351 62 62 PRO HB2 H 1.378 0.005 2 352 62 62 PRO HB3 H 1.764 0.012 2 353 62 62 PRO HG2 H -0.233 0.008 2 354 62 62 PRO HD2 H 1.503 0.008 2 355 63 63 THR H H 8.757 0.005 1 356 63 63 THR HA H 4.951 0.008 1 357 63 63 THR HG2 H 2.302 0.006 1 358 63 63 THR N N 111.336 0.000 1 359 64 64 LYS H H 8.034 0.006 1 360 64 64 LYS HA H 4.001 0.010 1 361 64 64 LYS HB2 H 1.094 0.009 2 362 64 64 LYS HB3 H 1.465 0.014 2 363 64 64 LYS HG2 H 1.141 0.003 2 364 64 64 LYS HG3 H 1.249 0.005 2 365 64 64 LYS HD2 H 1.334 0.033 2 366 64 64 LYS HD3 H 1.386 0.022 2 367 64 64 LYS N N 123.633 0.000 1 368 65 65 CYS H H 6.648 0.007 1 369 65 65 CYS HA H -1.385 0.009 1 370 65 65 CYS HB2 H -0.855 0.008 2 371 65 65 CYS HB3 H 1.097 0.008 2 372 65 65 CYS N N 116.426 0.000 1 373 66 66 GLY H H 8.344 0.007 1 374 66 66 GLY HA2 H 3.765 0.007 2 375 66 66 GLY HA3 H 4.964 0.011 2 376 66 66 GLY N N 102.751 0.000 1 377 67 67 GLU H H 6.998 0.006 1 378 67 67 GLU HA H 4.141 0.005 1 379 67 67 GLU HB2 H 1.750 0.006 2 380 67 67 GLU HB3 H 1.533 0.015 2 381 67 67 GLU HG2 H 1.874 0.008 2 382 67 67 GLU HG3 H 1.929 0.008 2 383 67 67 GLU N N 115.893 0.000 1 384 68 68 CYS H H 6.644 0.007 1 385 68 68 CYS HA H 5.542 0.008 1 386 68 68 CYS HB2 H 2.178 0.010 1 387 68 68 CYS HB3 H 3.581 0.013 1 388 68 68 CYS N N 113.306 0.000 1 389 69 69 HIS H H 11.614 0.009 1 390 69 69 HIS HA H 10.514 0.011 1 391 69 69 HIS HB2 H 8.532 0.012 1 392 69 69 HIS HB3 H 11.967 0.012 1 393 69 69 HIS N N 121.421 0.000 1 394 70 70 LYS H H 10.287 0.004 1 395 70 70 LYS HA H 5.834 0.005 1 396 70 70 LYS HB2 H 2.762 0.006 2 397 70 70 LYS HB3 H 2.927 0.005 2 398 70 70 LYS HG2 H 2.237 0.011 2 399 70 70 LYS HD2 H 2.255 0.005 2 400 70 70 LYS HE2 H 3.341 0.005 2 401 70 70 LYS N N 127.268 0.000 1 402 71 71 LYS H H 9.072 0.010 1 403 71 71 LYS HA H 5.007 0.008 1 404 71 71 LYS HB2 H 2.350 0.005 2 405 71 71 LYS HB3 H 2.416 0.003 2 406 71 71 LYS HG2 H 2.084 0.006 2 407 71 71 LYS HD2 H 2.149 0.002 2 408 71 71 LYS HE2 H 3.378 0.001 2 409 71 71 LYS N N 129.872 0.000 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $TopSpin stop_ loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-15N HSQC' 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 'PROTOPORPHYRIN IX CONTAINING FE_1' _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 1 130 1 HEC HAA1 H 0.862 0.024 2 2 130 1 HEC HAA2 H 3.030 0.013 2 3 130 1 HEC HAB H 0.910 0.005 1 4 130 1 HEC HAC H -4.323 0.009 1 5 130 1 HEC HAD1 H 2.660 0.021 2 6 130 1 HEC HAD2 H 6.713 0.029 2 7 130 1 HEC HBA1 H -0.871 0.016 2 8 130 1 HEC HBA2 H -0.414 0.012 2 9 130 1 HEC HBB1 H 1.146 0.004 1 10 130 1 HEC HBC1 H -3.987 0.007 1 11 130 1 HEC HBD1 H -1.457 0.012 1 12 130 1 HEC HBD2 H -0.312 0.009 1 13 130 1 HEC HHA H 3.714 0.007 1 14 130 1 HEC HHB H -0.713 0.005 1 15 130 1 HEC HHD H -1.521 0.007 1 16 130 1 HEC HMA1 H 15.723 0.011 1 17 130 1 HEC HMB1 H 17.782 0.005 1 18 130 1 HEC HMC1 H 10.407 0.007 1 19 130 1 HEC HMD1 H 20.595 0.017 1 stop_ save_ save_assigned_chem_shift_list_1_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $TopSpin stop_ loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-15N HSQC' 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 'PROTOPORPHYRIN IX CONTAINING FE_2' _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 1 154 1 HEC HAA1 H 3.685 0.010 2 2 154 1 HEC HAA2 H 5.540 0.014 2 3 154 1 HEC HAB H -2.546 0.012 1 4 154 1 HEC HAC H -0.871 0.005 1 5 154 1 HEC HAD1 H 16.042 0.029 2 6 154 1 HEC HAD2 H 19.916 0.006 2 7 154 1 HEC HBA1 H -2.072 0.011 2 8 154 1 HEC HBA2 H -1.969 0.012 2 9 154 1 HEC HBB1 H -2.233 0.008 1 10 154 1 HEC HBC1 H -1.017 0.006 1 11 154 1 HEC HBD1 H -1.753 0.008 2 12 154 1 HEC HBD2 H -0.688 0.008 2 13 154 1 HEC HHA H -1.675 0.005 1 14 154 1 HEC HHB H 8.078 0.005 1 15 154 1 HEC HHC H -3.913 0.027 1 16 154 1 HEC HHD H 11.378 0.004 1 17 154 1 HEC HMA1 H 0.654 0.008 1 18 154 1 HEC HMB1 H 12.145 0.009 1 19 154 1 HEC HMC1 H 18.001 0.006 1 20 154 1 HEC HMD1 H 13.155 0.011 1 stop_ save_ save_assigned_chem_shift_list_1_4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $TopSpin stop_ loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-15N HSQC' 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 'PROTOPORPHYRIN IX CONTAINING FE_3' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 168 1 HEC HAA1 H 2.877 0.013 2 2 168 1 HEC HAA2 H 4.147 0.036 2 3 168 1 HEC HAB H 0.730 0.009 1 4 168 1 HEC HAC H -0.062 0.016 1 5 168 1 HEC HAD1 H 2.435 0.017 2 6 168 1 HEC HAD2 H 6.471 0.011 2 7 168 1 HEC HBA1 H -0.853 0.007 2 8 168 1 HEC HBA2 H -0.257 0.009 2 9 168 1 HEC HBB1 H 2.048 0.006 1 10 168 1 HEC HBC1 H 1.623 0.015 1 11 168 1 HEC HBD1 H 0.126 0.007 1 12 168 1 HEC HBD2 H 0.466 0.009 1 13 168 1 HEC HHA H 0.769 0.006 1 14 168 1 HEC HHB H -1.612 0.002 1 15 168 1 HEC HHC H 2.249 0.005 1 16 168 1 HEC HHD H 1.212 0.003 1 17 168 1 HEC HMA1 H 14.578 0.032 1 18 168 1 HEC HMB1 H 14.484 0.022 1 19 168 1 HEC HMC1 H 10.943 0.006 1 20 168 1 HEC HMD1 H 17.414 0.011 1 stop_ save_