data_7415 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Evidence of reciprocical reorientation of the catalytic and hemopexin-like domains of full-length MMP-12 ; _BMRB_accession_number 7415 _BMRB_flat_file_name bmr7415.str _Entry_type original _Submission_date 2007-12-03 _Accession_date 2007-12-03 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details ; In this entry are deposited : _ Assignment of FL_MMP12. _ Assignment of hemopexin-like domain. _ RDCs obtained on FL_MMP12. _ R1, R2 and NOE data for catalytic, hemopexin-like domain and full-length protein. ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Bertini Ivano . . 2 Calderone Vito . . 3 Fragai Marco . . 4 Jaiswal Rahul . . 5 Luchinat Claudio . . 6 Melikian Maxime . . 7 Mylonas Efstratios . . 8 Svergun Dmitri I. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count heteronucl_NOE 1 T1_relaxation 1 T2_relaxation 1 stop_ loop_ _Data_type _Data_type_count "T1 relaxation values" 129 "T2 relaxation values" 129 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2011-08-11 update BMRB 'residue name for residue 115 corrected in relaxation save frames' stop_ save_ ############################# # Citation for this entry # ############################# save_citations _Saveframe_category entry_citation _Citation_full . _Citation_title 'Evidence of reciprocal reorientation of the catalytic and hemopexin-like domains of full-length MMP-12' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18465858 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Bertini I. . . 2 Calderone V. . . 3 Fragai M. . . 4 Jaiswal R. . . 5 Luchinat C. . . 6 Melikian M. . . 7 Mylonas E. . . 8 Svergun D. I. . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_volume 130 _Journal_issue 22 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 7011 _Page_last 7022 _Year 2008 _Details . loop_ _Keyword assignment 'matrix metalloproteinase' mobility NMR RDC stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name MMP12_HUMAN _Enzyme_commission_number 3.4.24.65 loop_ _Mol_system_component_name _Mol_label 'Catalytic Domain' $CAT_DOMAIN 'Cadmium ion' $CD stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state complex _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'Active MMP-12 protein composed by a catalytic and a hemopexin-like domain connected by a linker peptide.' save_ ######################## # Monomeric polymers # ######################## save_CAT_DOMAIN _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common CAT_DOMAIN _Molecular_mass . _Mol_thiol_state 'not present' loop_ _Biological_function 'cleavage of the target' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 159 _Mol_residue_sequence ; MGPVWRKHYITYRINNYTPD MNREDVDYAIRKAFQVWSNV TPLKFSKINTGMADILVVFA RGAHGDFHAFDGKGGILAHA FGPGSGIGGDAHFDEDEFWT THSGGTNLFLTAVHEIGHSL GLGHSSDPKAVMFPTYKYVD INTFRLSADDIRGIQSLYG ; loop_ _Residue_seq_code _Residue_label 1 MET 2 GLY 3 PRO 4 VAL 5 TRP 6 ARG 7 LYS 8 HIS 9 TYR 10 ILE 11 THR 12 TYR 13 ARG 14 ILE 15 ASN 16 ASN 17 TYR 18 THR 19 PRO 20 ASP 21 MET 22 ASN 23 ARG 24 GLU 25 ASP 26 VAL 27 ASP 28 TYR 29 ALA 30 ILE 31 ARG 32 LYS 33 ALA 34 PHE 35 GLN 36 VAL 37 TRP 38 SER 39 ASN 40 VAL 41 THR 42 PRO 43 LEU 44 LYS 45 PHE 46 SER 47 LYS 48 ILE 49 ASN 50 THR 51 GLY 52 MET 53 ALA 54 ASP 55 ILE 56 LEU 57 VAL 58 VAL 59 PHE 60 ALA 61 ARG 62 GLY 63 ALA 64 HIS 65 GLY 66 ASP 67 PHE 68 HIS 69 ALA 70 PHE 71 ASP 72 GLY 73 LYS 74 GLY 75 GLY 76 ILE 77 LEU 78 ALA 79 HIS 80 ALA 81 PHE 82 GLY 83 PRO 84 GLY 85 SER 86 GLY 87 ILE 88 GLY 89 GLY 90 ASP 91 ALA 92 HIS 93 PHE 94 ASP 95 GLU 96 ASP 97 GLU 98 PHE 99 TRP 100 THR 101 THR 102 HIS 103 SER 104 GLY 105 GLY 106 THR 107 ASN 108 LEU 109 PHE 110 LEU 111 THR 112 ALA 113 VAL 114 HIS 115 GLU 116 ILE 117 GLY 118 HIS 119 SER 120 LEU 121 GLY 122 LEU 123 GLY 124 HIS 125 SER 126 SER 127 ASP 128 PRO 129 LYS 130 ALA 131 VAL 132 MET 133 PHE 134 PRO 135 THR 136 TYR 137 LYS 138 TYR 139 VAL 140 ASP 141 ILE 142 ASN 143 THR 144 PHE 145 ARG 146 LEU 147 SER 148 ALA 149 ASP 150 ASP 151 ILE 152 ARG 153 GLY 154 ILE 155 GLN 156 SER 157 LEU 158 TYR 159 GLY stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_CD _Saveframe_category ligand _Mol_type non-polymer _Name_common 'CD (CADMIUM ION)' _BMRB_code . _PDB_code CD _Molecular_mass 112.411 _Mol_charge 2 _Mol_paramagnetic . _Mol_aromatic no _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Mon Aug 20 19:34:58 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons CD CD CD N 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 $CAT_DOMAIN Human 9606 Eukaryota Metazoa Homo Sapiens 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 $CAT_DOMAIN 'recombinant technology' . Escherichia coli BL21(DE3) pET21a stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details 'pH 6.5, no buffer' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $CAT_DOMAIN . mM '[U-13C; U-15N]' NaCl 300 mM . stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AVANCE _Field_strength 900 _Details 'TCI probe' save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ ############################# # NMR applied experiments # ############################# save_3D_15N-separated_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name 3D_15N-separated_NOESY _Sample_label $sample_1 save_ save_3D_13C-separated_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name 3D_13C-separated_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_1 save_ save_3D_HNCO_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_1 save_ save_3D_HNCA_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $sample_1 save_ save_3D_HN(CO)CA_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _Sample_label $sample_1 save_ save_3D_CBCA(CO)NH_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _Sample_label $sample_1 save_ save_3D_HNCACB_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $sample_1 save_ save_3D_HCCH-TOCSY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $sample_1 save_ save_3D_HBHA(CO)NH_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HBHA(CO)NH' _Sample_label $sample_1 save_ save_3D_HNHA_11 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNHA' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_T1_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T1' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_T2_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T2' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_NOE_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NOE' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_IPAP_15 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC IPAP' _Sample_label $sample_1 save_ save_3D_15N-separated_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name 3D_15N-separated_NOESY _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_13C-separated_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name 3D_13C-separated_NOESY _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNCO_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNCA_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HN(CO)CA_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_CBCA(CO)NH_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNCACB_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HCCH-TOCSY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HBHA(CO)NH_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HBHA(CO)NH' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNHA_11 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNHA' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T1_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T1' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T2_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T2' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_NOE_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NOE' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T1_15 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T1' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T2_16 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T2' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_NOE_17 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NOE' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_18 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNCO_19 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_HNCA_20 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _BMRB_pulse_sequence_accession_number . _Details . save_ save_3D_CBCA(CO)NH_21 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T1_22 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T1' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_T2_23 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC T2' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_NOE_24 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NOE' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D_1H-15N_HSQC_IPAP_25 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC IPAP' _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details '300 mM of NaCl' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 300 . mM pH 7.2 . 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 C 13 'methyl protons' ppm 0.00 . indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 . indirect . . . 0.101329118 stop_ save_ save_heteronuclear_R1_CAT _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 700 _T1_coherence_type NzHz _T1_value_units s-1 _Mol_system_component_name 'Catalytic Domain' _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 6 ARG N 1.021 0.051 2 9 TYR N 0.986 0.049 3 10 ILE N 0.977 0.049 4 11 THR N 1.034 0.052 5 12 TYR N 1.084 0.054 6 13 ARG N 1.054 0.053 7 14 ILE N 1.056 0.053 8 15 ASN N 1.056 0.053 9 16 ASN N 1.157 0.058 10 17 TYR N 0.981 0.049 11 18 THR N 0.998 0.050 12 20 ASP N 1.094 0.055 13 21 MET N 1.051 0.053 14 22 ASN N 1.040 0.052 15 24 GLU N 1.111 0.056 16 25 ASP N 1.025 0.051 17 26 VAL N 1.033 0.052 18 27 ASP N 1.003 0.050 19 28 TYR N 1.040 0.052 20 29 ALA N 0.937 0.047 21 30 ILE N 0.983 0.049 22 31 ARG N 1.007 0.050 23 32 LYS N 1.249 0.062 24 33 ALA N 1.034 0.052 25 34 PHE N 0.979 0.049 26 35 GLN N 1.002 0.050 27 36 VAL N 0.934 0.047 28 37 TRP N 1.027 0.051 29 38 SER N 1.020 0.051 30 39 ASN N 1.052 0.053 31 40 VAL N 0.968 0.048 32 41 THR N 1.023 0.051 33 43 LEU N 1.004 0.050 34 44 LYS N 1.004 0.050 35 45 PHE N 0.960 0.048 36 46 SER N 0.958 0.048 37 47 LYS N 1.080 0.054 38 48 ILE N 1.112 0.056 39 51 GLY N 1.111 0.056 40 52 MET N 1.060 0.053 41 53 ALA N 1.019 0.051 42 55 ILE N 1.017 0.051 43 56 LEU N 1.043 0.052 44 57 VAL N 0.972 0.049 45 58 VAL N 1.005 0.050 46 59 PHE N 0.949 0.047 47 60 ALA N 1.023 0.051 48 61 ARG N 1.075 0.054 49 62 GLY N 1.060 0.053 50 64 HIS N 1.005 0.050 51 69 ALA N 1.078 0.054 52 70 PHE N 1.356 0.068 53 71 ASP N 1.073 0.054 54 72 GLY N 1.086 0.054 55 73 LYS N 1.077 0.054 56 74 GLY N 1.062 0.053 57 75 GLY N 1.114 0.056 58 76 ILE N 1.026 0.051 59 77 LEU N 1.011 0.051 60 78 ALA N 0.976 0.049 61 79 HIS N 1.030 0.052 62 80 ALA N 0.905 0.045 63 82 GLY N 1.062 0.053 64 84 GLY N 1.028 0.051 65 88 GLY N 1.151 0.058 66 89 GLY N 1.088 0.054 67 90 ASP N 1.134 0.057 68 91 ALA N 1.046 0.052 69 92 HIS N 1.005 0.050 70 93 PHE N 1.022 0.051 71 95 GLU N 1.176 0.059 72 96 ASP N 1.062 0.053 73 97 GLU N 1.091 0.055 74 98 PHE N 1.043 0.052 75 99 TRP N 1.101 0.055 76 100 THR N 1.157 0.058 77 101 THR N 1.117 0.056 78 102 HIS N 1.044 0.052 79 105 GLY N 1.139 0.057 80 106 THR N 1.042 0.052 81 107 ASN N 1.031 0.052 82 108 LEU N 1.107 0.055 83 109 PHE N 1.004 0.050 84 110 LEU N 1.023 0.051 85 111 THR N 1.025 0.051 86 112 ALA N 1.076 0.054 87 113 VAL N 0.988 0.049 88 114 HIS N 1.002 0.050 89 115 GLU N 1.020 0.051 90 116 ILE N 1.002 0.050 91 117 GLY N 1.032 0.052 92 118 HIS N 1.056 0.053 93 119 SER N 1.058 0.053 94 120 LEU N 1.007 0.050 95 121 GLY N 1.000 0.050 96 122 LEU N 1.107 0.055 97 123 GLY N 1.095 0.055 98 124 HIS N 0.840 0.042 99 125 SER N 0.983 0.049 100 126 SER N 1.089 0.054 101 127 ASP N 1.096 0.055 102 129 LYS N 1.017 0.051 103 130 ALA N 1.111 0.056 104 131 VAL N 1.016 0.051 105 132 MET N 1.078 0.054 106 133 PHE N 1.153 0.058 107 135 THR N 0.876 0.044 108 136 TYR N 1.046 0.052 109 137 LYS N 1.004 0.050 110 138 TYR N 1.134 0.057 111 139 VAL N 1.034 0.052 112 140 ASP N 1.091 0.055 113 141 ILE N 1.134 0.057 114 142 ASN N 1.125 0.056 115 143 THR N 1.157 0.058 116 144 PHE N 1.121 0.056 117 145 ARG N 1.105 0.055 118 146 LEU N 1.072 0.054 119 147 SER N 1.059 0.053 120 150 ASP N 1.041 0.052 121 151 ILE N 1.009 0.050 122 152 ARG N 0.854 0.043 123 153 GLY N 1.048 0.052 124 154 ILE N 1.056 0.053 125 155 GLN N 1.105 0.055 126 156 SER N 0.967 0.048 127 157 LEU N 0.968 0.048 128 158 TYR N 1.059 0.053 129 159 GLY N 1.089 0.054 stop_ save_ save_heteronuclear_R2_CAT _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 700 _T2_coherence_type NzHz _T2_value_units s-1 _Mol_system_component_name 'Catalytic Domain' _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 6 ARG N 16.70 0.83 . . 2 9 TYR N 16.22 0.81 . . 3 10 ILE N 16.80 0.84 . . 4 11 THR N 17.66 0.88 . . 5 12 TYR N 18.26 0.91 . . 6 13 ARG N 16.85 0.84 . . 7 14 ILE N 16.17 0.81 . . 8 15 ASN N 16.75 0.84 . . 9 16 ASN N 17.26 0.86 . . 10 17 TYR N 15.88 0.79 . . 11 18 THR N 7.86 0.39 . . 12 20 ASP N 17.38 0.87 . . 13 21 MET N 16.65 0.83 . . 14 22 ASN N 16.56 0.83 . . 15 24 GLU N 17.24 0.86 . . 16 25 ASP N 17.67 0.88 . . 17 26 VAL N 17.46 0.87 . . 18 27 ASP N 16.71 0.84 . . 19 28 TYR N 17.25 0.86 . . 20 29 ALA N 20.03 1.00 . . 21 30 ILE N 16.47 0.82 . . 22 31 ARG N 18.34 0.92 . . 23 32 LYS N 18.72 0.94 . . 24 33 ALA N 16.37 0.82 . . 25 34 PHE N 15.16 0.76 . . 26 35 GLN N 17.26 0.86 . . 27 36 VAL N 18.35 0.92 . . 28 37 TRP N 16.30 0.82 . . 29 38 SER N 17.81 0.89 . . 30 39 ASN N 17.22 0.86 . . 31 40 VAL N 16.03 0.80 . . 32 41 THR N 15.79 0.79 . . 33 43 LEU N 14.83 0.74 . . 34 44 LYS N 15.20 0.76 . . 35 45 PHE N 15.74 0.79 . . 36 46 SER N 15.17 0.76 . . 37 47 LYS N 16.27 0.81 . . 38 48 ILE N 16.41 0.82 . . 39 51 GLY N 17.93 0.90 . . 40 52 MET N 17.32 0.87 . . 41 53 ALA N 12.22 0.61 . . 42 55 ILE N 21.54 1.08 . . 43 56 LEU N 16.67 0.83 . . 44 57 VAL N 15.55 0.78 . . 45 58 VAL N 15.82 0.79 . . 46 59 PHE N 15.55 0.78 . . 47 60 ALA N 16.23 0.81 . . 48 61 ARG N 15.90 0.80 . . 49 62 GLY N 19.58 0.98 . . 50 64 HIS N 17.41 0.87 . . 51 69 ALA N 21.34 1.07 . . 52 70 PHE N 14.76 0.74 . . 53 71 ASP N 16.94 0.85 . . 54 72 GLY N 18.11 0.91 . . 55 73 LYS N 17.27 0.86 . . 56 74 GLY N 16.48 0.82 . . 57 75 GLY N 17.90 0.90 . . 58 76 ILE N 16.41 0.82 . . 59 77 LEU N 17.27 0.86 . . 60 78 ALA N 16.42 0.82 . . 61 79 HIS N 17.30 0.87 . . 62 80 ALA N 9.56 0.48 . . 63 82 GLY N 15.98 0.80 . . 64 84 GLY N 16.39 0.82 . . 65 88 GLY N 19.60 0.98 . . 66 89 GLY N 22.46 1.12 . . 67 90 ASP N 16.40 0.82 . . 68 91 ALA N 17.90 0.90 . . 69 92 HIS N 17.36 0.87 . . 70 93 PHE N 16.83 0.84 . . 71 95 GLU N 9.07 0.45 . . 72 96 ASP N 17.84 0.89 . . 73 97 GLU N 18.23 0.91 . . 74 98 PHE N 20.00 1.00 . . 75 99 TRP N 18.85 0.94 . . 76 100 THR N 18.78 0.94 . . 77 101 THR N 17.47 0.87 . . 78 102 HIS N 19.97 1.00 . . 79 105 GLY N 14.41 0.72 . . 80 106 THR N 15.98 0.80 . . 81 107 ASN N 16.84 0.84 . . 82 108 LEU N 17.82 0.89 . . 83 109 PHE N 16.97 0.85 . . 84 110 LEU N 19.29 0.96 . . 85 111 THR N 15.57 0.78 . . 86 112 ALA N 16.49 0.82 . . 87 113 VAL N 17.24 0.86 . . 88 114 HIS N 18.04 0.90 . . 89 115 GLU N 17.18 0.86 . . 90 116 ILE N 17.15 0.86 . . 91 117 GLY N 17.49 0.87 . . 92 118 HIS N 17.43 0.87 . . 93 119 SER N 18.70 0.94 . . 94 120 LEU N 17.11 0.86 . . 95 121 GLY N 17.81 0.89 . . 96 122 LEU N 18.88 0.94 . . 97 123 GLY N 17.66 0.88 . . 98 124 HIS N 12.38 0.62 . . 99 125 SER N 16.31 0.82 . . 100 126 SER N 17.76 0.89 . . 101 127 ASP N 16.92 0.85 . . 102 129 LYS N 16.71 0.84 . . 103 130 ALA N 16.40 0.82 . . 104 131 VAL N 17.25 0.86 . . 105 132 MET N 17.24 0.86 . . 106 133 PHE N 18.28 0.91 . . 107 135 THR N 14.92 0.75 . . 108 136 TYR N 16.33 0.82 . . 109 137 LYS N 15.47 0.77 . . 110 138 TYR N 15.07 0.75 . . 111 139 VAL N 15.04 0.75 . . 112 140 ASP N 15.29 0.76 . . 113 141 ILE N 15.68 0.78 . . 114 142 ASN N 17.72 0.89 . . 115 143 THR N 15.84 0.79 . . 116 144 PHE N 15.47 0.77 . . 117 145 ARG N 14.30 0.72 . . 118 146 LEU N 15.39 0.77 . . 119 147 SER N 16.41 0.82 . . 120 150 ASP N 17.84 0.89 . . 121 151 ILE N 17.32 0.87 . . 122 152 ARG N 17.22 0.86 . . 123 153 GLY N 16.42 0.82 . . 124 154 ILE N 16.08 0.80 . . 125 155 GLN N 18.08 0.90 . . 126 156 SER N 13.24 0.66 . . 127 157 LEU N 16.51 0.83 . . 128 158 TYR N 17.14 0.86 . . 129 159 GLY N 17.72 0.89 . . stop_ save_ save_heteronuclear_noe_CAT _Saveframe_category heteronuclear_NOE _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 700 _Mol_system_component_name 'Catalytic Domain' _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'peak integral' _NOE_reference_value 0 _NOE_reference_description 'NOE ref is obtained after splitting of the spectra generating both NOE ref and NOE.' _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 6 ARG 0.640 0.032 9 TYR 0.730 0.036 10 ILE 0.820 0.041 11 THR 0.750 0.038 12 TYR 0.850 0.043 13 ARG 0.850 0.043 14 ILE 0.780 0.039 15 ASN 0.800 0.040 16 ASN 0.830 0.042 17 TYR 0.840 0.042 18 THR 0.090 0.004 20 ASP 0.840 0.042 21 MET 0.880 0.044 22 ASN 0.660 0.033 24 GLU 0.780 0.039 25 ASP 0.910 0.046 26 VAL 0.970 0.049 27 ASP 0.880 0.044 28 TYR 0.820 0.041 29 ALA 1.040 0.052 30 ILE 0.800 0.040 31 ARG 0.780 0.039 32 LYS 0.750 0.038 33 ALA 0.800 0.040 34 PHE 0.790 0.040 35 GLN 0.830 0.042 36 VAL 0.990 0.050 37 TRP 0.890 0.045 38 SER 0.950 0.048 39 ASN 0.970 0.049 40 VAL 0.840 0.042 41 THR 0.780 0.039 43 LEU 0.620 0.031 44 LYS 0.970 0.049 45 PHE 0.910 0.046 46 SER 0.850 0.043 47 LYS 0.820 0.041 48 ILE 0.890 0.045 53 ALA 0.810 0.041 55 ILE 0.860 0.043 56 LEU 0.940 0.047 57 VAL 0.870 0.044 58 VAL 0.900 0.045 59 PHE 0.770 0.039 60 ALA 0.780 0.039 61 ARG 0.840 0.042 62 GLY 0.860 0.043 64 HIS 1.030 0.052 69 ALA 1.020 0.051 70 PHE 0.740 0.037 71 ASP 0.880 0.044 72 GLY 0.920 0.046 73 LYS 0.610 0.030 74 GLY 0.840 0.042 75 GLY 0.850 0.043 76 ILE 0.830 0.042 77 LEU 0.710 0.035 78 ALA 0.880 0.044 79 HIS 0.810 0.041 80 ALA 0.770 0.039 82 GLY 0.810 0.041 84 GLY 0.900 0.045 88 GLY 0.920 0.046 89 GLY 0.890 0.045 90 ASP 0.780 0.039 91 ALA 0.790 0.040 92 HIS 1.030 0.052 93 PHE 0.990 0.050 95 GLU 0.630 0.032 96 ASP 0.810 0.041 97 GLU 0.840 0.042 98 PHE 0.880 0.044 99 TRP 0.820 0.041 100 THR 0.890 0.045 101 THR 0.860 0.043 102 HIS 0.740 0.037 105 GLY 0.880 0.044 106 THR 0.890 0.045 107 ASN 0.870 0.044 108 LEU 0.860 0.043 109 PHE 0.730 0.036 110 LEU 0.830 0.042 111 THR 0.740 0.037 112 ALA 0.870 0.044 113 VAL 0.740 0.037 114 HIS 0.940 0.047 115 GLU 0.820 0.041 116 ILE 0.810 0.041 117 GLY 0.860 0.043 118 HIS 0.850 0.043 119 SER 0.810 0.041 120 LEU 0.880 0.044 121 GLY 0.750 0.038 122 LEU 0.940 0.047 123 GLY 0.730 0.036 125 SER 0.840 0.042 126 SER 0.960 0.048 127 ASP 0.740 0.037 129 LYS 0.890 0.045 130 ALA 0.710 0.035 131 VAL 0.850 0.043 132 MET 0.800 0.040 133 PHE 0.970 0.049 135 THR 0.660 0.033 136 TYR 0.800 0.040 137 LYS 0.860 0.043 138 TYR 0.760 0.038 139 VAL 0.870 0.044 140 ASP 0.760 0.038 141 ILE 0.760 0.038 142 ASN 0.950 0.048 143 THR 0.730 0.036 144 PHE 0.700 0.035 145 ARG 0.790 0.040 146 LEU 0.680 0.034 147 SER 0.650 0.033 150 ASP 0.750 0.038 151 ILE 0.850 0.043 152 ARG 0.950 0.048 153 GLY 0.830 0.042 154 ILE 0.850 0.043 155 GLN 0.740 0.037 156 SER 0.690 0.034 157 LEU 0.700 0.035 158 TYR 0.870 0.044 159 GLY 0.900 0.045 stop_ save_