data_50001 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of protein ARR_CleD in complex with c-di-GMP ; _BMRB_accession_number 50001 _BMRB_flat_file_name bmr50001.str _Entry_type original _Submission_date 2019-08-16 _Accession_date 2019-08-16 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'ARR_CleD is the arginine rich region of CleD from Caulobacter crescentus' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Habazettl Judith . . 2 Grzesiek Stephan . . 3 Hee Chee-Seng . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 3 heteronucl_NOE 1 T1_relaxation 1 T2_relaxation 2 S2_parameters 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 245 "13C chemical shifts" 125 "15N chemical shifts" 40 "T1 relaxation values" 30 "T2 relaxation values" 60 "order parameters" 30 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-09-21 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 27990 'apo ARR_CleD' stop_ _Original_release_date 2019-08-21 save_ ############################# # Citation for this entry # ############################# save_citations_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Intercepting second-messenger signaling by rationally designed peptides sequestering c-di-GMP ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 32611811 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Hee Chee-Seng S. . 2 Habazettl Judith . . 3 Schmutz Christoph . . 4 Schirmer Tilman . . 5 Jenal Urs . . 6 Grzesiek Stephan . . stop_ _Journal_abbreviation 'Proc. Natl. Acad. Sci. U.S.A.' _Journal_name_full 'Proceedings of the National Academy of Sciences of the United States of America' _Journal_volume 117 _Journal_issue 29 _Journal_ISSN 1091-6490 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 17211 _Page_last 17220 _Year 2020 _Details . loop_ _Keyword CleD NMR 'bacterial second messenger' biofilm stop_ save_ ################################## # Molecular system description # ################################## save_assembly_1 _Saveframe_category molecular_system _Mol_system_name 'ci-di-GMP in complex with ARR_CleD' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label ARR_CleD $entity_1 'c-di-GMP, 1' $entity_C2E 'c-di-GMP, 2' $entity_C2E stop_ _System_molecular_weight 4164.66 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'The second messenger c-di-GMP is bound as a intercalated dimer to ARR_CleD.' save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 36 _Mol_residue_sequence ; SKPREWVEAVAYVGPDRRRF NSADYKGPRKRKADAS ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 139 SER 2 140 LYS 3 141 PRO 4 142 ARG 5 143 GLU 6 144 TRP 7 145 VAL 8 146 GLU 9 147 ALA 10 148 VAL 11 149 ALA 12 150 TYR 13 151 VAL 14 152 GLY 15 153 PRO 16 154 ASP 17 155 ARG 18 156 ARG 19 157 ARG 20 158 PHE 21 159 ASN 22 160 SER 23 161 ALA 24 162 ASP 25 163 TYR 26 164 LYS 27 165 GLY 28 166 PRO 29 167 ARG 30 168 LYS 31 169 ARG 32 170 LYS 33 171 ALA 34 172 ASP 35 173 ALA 36 174 SER 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 UniProtKB A0A0H3CCM2 'Two component receiver protein' . . . . . stop_ save_ ############# # Ligands # ############# save_C2E _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common "entity_C2E (9,9'-[(2R,3R,3aS,5S,7aR,9R,10R,10aS,12S,14aR)-3,5,10,12-tetrahydroxy-5,12-dioxidooctahydro-2H,7H-difuro[3,2-d:3',2'-j][1,3,7,9,2,8]tetraoxadiphosphacyclododecine-2,9-diyl]bis(2-amino-1,9-dihydro-6H-purin-6-one))" _BMRB_code C2E _PDB_code C2E _Molecular_mass 690.411 _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 P1 P1 P . 0 . ? O2P O2P O . 0 . ? O1P O1P O . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C3' C3' C . 0 . ? O3' O3' O . 0 . ? C2' C2' C . 0 . ? O2' O2' O . 0 . ? C1' C1' C . 0 . ? N9 N9 N . 0 . ? C8 C8 C . 0 . ? N7 N7 N . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? O6 O6 O . 0 . ? N1 N1 N . 0 . ? C2 C2 C . 0 . ? N2 N2 N . 0 . ? N3 N3 N . 0 . ? C4 C4 C . 0 . ? P11 P11 P . 0 . ? O21 O21 O . 0 . ? O11 O11 O . 0 . ? O5A O5A O . 0 . ? C5A C5A C . 0 . ? C4A C4A C . 0 . ? O4A O4A O . 0 . ? C3A C3A C . 0 . ? O3A O3A O . 0 . ? C2A C2A C . 0 . ? O2A O2A O . 0 . ? C1A C1A C . 0 . ? N91 N91 N . 0 . ? C81 C81 C . 0 . ? N71 N71 N . 0 . ? C51 C51 C . 0 . ? C61 C61 C . 0 . ? O61 O61 O . 0 . ? N11 N11 N . 0 . ? C21 C21 C . 0 . ? N21 N21 N . 0 . ? N31 N31 N . 0 . ? C41 C41 C . 0 . ? HO2P HO2P H . 0 . ? H5'1 H5'1 H . 0 . ? H5'2 H5'2 H . 0 . ? H4' H4' H . 0 . ? H3' H3' H . 0 . ? H2' H2' H . 0 . ? HO2' HO2' H . 0 . ? H1' H1' H . 0 . ? H8 H8 H . 0 . ? HN1 HN1 H . 0 . ? HN21 HN21 H . 0 . ? HN22 HN22 H . 0 . ? HO21 HO21 H . 0 . ? H511 H511 H . 0 . ? H512 H512 H . 0 . ? H4A H4A H . 0 . ? H3A H3A H . 0 . ? H2A H2A H . 0 . ? HO2A HO2A H . 0 . ? H1A H1A H . 0 . ? H81 H81 H . 0 . ? HN11 HN11 H . 0 . ? HN24 HN24 H . 0 . ? HN23 HN23 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 P1 O2P ? ? DOUB O1P P1 ? ? SING O5' P1 ? ? SING C5' O5' ? ? SING C4' O4' ? ? SING C4' C5' ? ? SING C3' C4' ? ? SING O3' P11 ? ? SING O3' C3' ? ? SING C2' C3' ? ? SING C2' C1' ? ? SING O2' C2' ? ? SING C1' O4' ? ? SING C1' N9 ? ? SING N9 C4 ? ? SING N9 C8 ? ? DOUB C8 N7 ? ? SING C5 N7 ? ? SING C5 C6 ? ? DOUB C6 O6 ? ? SING N1 C6 ? ? SING C2 N1 ? ? SING N2 C2 ? ? DOUB N3 C2 ? ? SING N3 C4 ? ? DOUB C4 C5 ? ? SING P11 O21 ? ? SING P11 O5A ? ? DOUB O11 P11 ? ? SING C5A O5A ? ? SING C5A C4A ? ? SING C4A O4A ? ? SING C4A C3A ? ? SING O4A C1A ? ? SING C3A C2A ? ? SING O3A C3A ? ? SING O3A P1 ? ? SING C2A O2A ? ? SING C1A C2A ? ? SING C1A N91 ? ? SING N91 C41 ? ? DOUB C81 N71 ? ? SING C81 N91 ? ? SING N71 C51 ? ? DOUB C51 C41 ? ? SING C51 C61 ? ? DOUB C61 O61 ? ? SING C61 N11 ? ? SING C21 N11 ? ? SING C21 N21 ? ? DOUB N31 C21 ? ? SING C41 N31 ? ? SING O2P HO2P ? ? SING C5' H5'1 ? ? SING C5' H5'2 ? ? SING C4' H4' ? ? SING C3' H3' ? ? SING C2' H2' ? ? SING O2' HO2' ? ? SING C1' H1' ? ? SING C8 H8 ? ? SING N1 HN1 ? ? SING N2 HN21 ? ? SING N2 HN22 ? ? SING O21 HO21 ? ? SING C5A H511 ? ? SING C5A H512 ? ? SING C4A H4A ? ? SING C3A H3A ? ? SING C2A H2A ? ? SING O2A HO2A ? ? SING C1A H1A ? ? SING C81 H81 ? ? SING N11 HN11 ? ? SING N21 HN24 ? ? SING N21 HN23 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source_1 _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1 'Caulobacter crescentus' 565050 Bacteria . Caulobacter crescentus stop_ save_ ######################### # Experimental source # ######################### save_experimental_source_1 _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_type _Vector_name _Details $entity_1 'recombinant technology' . Escherichia coli BL21 plasmid pET28a pET28a-H6-SUMO-ARR_CleD stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '15N ARR_CleD in complex with c-di-GMP' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1 mM '[U-98% 15N]' $entity_C2E 3 mM 'natural abundance' 'sodium chloride' 100 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' 'sodium azide' 0.02 v/v 'natural abundance' 'magnsesium chloride' 2 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '15N-13C ARR_CleD in complex with c-di-GMP' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1 mM '[U-98% 13C; U-98% 15N]' $entity_C2E 3 mM 'natural abundance' 'sodium chloride' 100 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' 'sodium azide' 0.02 v/v 'natural abundance' 'magnesium chloride' 2 mM 'natural abundance' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details '15N-13C ARR_CleD in complex with c-di-GMP in Phages' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.6 mM '[U-99% 13C; U-99% 15N]' $entity_C2E 1.8 mM 'natural abundance' 'sodium chloride' 66.66 mM 'natural abundance' 'sodium phosphate' 13.33 mM 'natural abundance' 'mgnesium chloride' 1.33 mM 'natural abundance' 'Pf1 phage' 9 mg/mL 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name Bruker _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task 'recording of spectra' stop_ _Details . save_ save_software_3 _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_software_4 _Saveframe_category software _Name MATLAB _Version . loop_ _Vendor _Address _Electronic_address MathWorks . . stop_ loop_ _Task 'fit of relaxation data' stop_ _Details 'Software written for MATLAB in order to fit relaxation data.' save_ save_software_5 _Saveframe_category software _Name ModelFree _Version . loop_ _Vendor _Address _Electronic_address Palmer . . stop_ loop_ _Task 'aanalyze the relaxation data and fits them to different models' stop_ _Details . save_ save_software_6 _Saveframe_category software _Name PIPP _Version . loop_ _Vendor _Address _Electronic_address Garrett . . stop_ loop_ _Task 'peak picking' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'Uniform NMR System' _Field_strength 900 _Details 'TCI probe head' save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'Uniform NMR System' _Field_strength 800 _Details 'TXI probe head' save_ save_NMR_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'Uniform NMR System' _Field_strength 600 _Details 'TXI probe head' 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_2D_1H-15N_HSQC_NH2_only_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NH2 only' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_2 save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_3D_HNCO_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_2 save_ save_3D_HNCA_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $sample_2 save_ save_3D_HN(CO)CA_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HN(CO)CA' _Sample_label $sample_2 save_ save_3D_1H-15N_NOESY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ save_3D_1H-15N_TOCSY_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N TOCSY' _Sample_label $sample_1 save_ save_2D_1H-15N_NH2_TOCSY_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N NH2 TOCSY' _Sample_label $sample_1 save_ save_2D_1H-15N_NH2_NOESY_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N NH2 NOESY' _Sample_label $sample_1 save_ save_3D_CBCA(CO)NH_13 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _Sample_label $sample_2 save_ save_3D_CBCANH_14 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCANH' _Sample_label $sample_2 save_ save_3D_C(CO)NH_15 _Saveframe_category NMR_applied_experiment _Experiment_name '3D C(CO)NH' _Sample_label $sample_2 save_ save_3D_HBHA(CO)NH_16 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HBHA(CO)NH' _Sample_label $sample_2 save_ save_2D_1H-15N_NOE_without_saturation_17 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N NOE without saturation' _Sample_label $sample_1 save_ save_2D_1H-15N_NOE_with_saturation_18 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N NOE with saturation' _Sample_label $sample_1 save_ save_3D_1H-15N_t1_interleaved_19 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N t1 interleaved' _Sample_label $sample_1 save_ save_3D_1H-15N_t2_interleaved_20 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N t2 interleaved' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_without_15_decoupling_21 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC without 15 decoupling' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_without_15N_decoupling_22 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC without 15N decoupling' _Sample_label $sample_3 save_ save_2D_HN(CO)CA_without_decoupling_23 _Saveframe_category NMR_applied_experiment _Experiment_name '2D HN(CO)CA without decoupling' _Sample_label $sample_2 save_ save_2D_HN(CO)CA_without_decoupling_24 _Saveframe_category NMR_applied_experiment _Experiment_name '2D HN(CO)CA without decoupling' _Sample_label $sample_3 save_ save_2D_1H-1H_NOESY_25 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_3D_HNCA_26 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $sample_2 save_ save_3D_HNCO_27 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _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' 0.47 . M pH 6.5 0.04 pH pressure 1 . atm temperature 298 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.31 . M pH 6.5 0.04 pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_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 C 13 H ppm 4.7729 internal indirect . . . 0.25144953 water H 1 H ppm 4.7729 internal direct . . . 1 water N 15 H ppm 4.7729 internal indirect . . . 0.10132912 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_chemical_shifts_1_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_1 stop_ loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '3D 1H-15N NOESY' '3D 1H-15N TOCSY' '3D CBCA(CO)NH' '3D CBCANH' '3D C(CO)NH' '3D HBHA(CO)NH' '3D HNCA' '3D HNCO' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name ARR_CleD _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 1 140 2 LYS HA H 4.606 0.000 1 2 140 2 LYS HB2 H 1.698 0.001 2 3 140 2 LYS HB3 H 1.770 0.003 2 4 140 2 LYS HG3 H 1.420 0.000 2 5 141 3 PRO HA H 4.405 0.003 1 6 141 3 PRO HB3 H 2.305 0.002 2 7 141 3 PRO HG3 H 1.952 0.002 2 8 141 3 PRO HD2 H 3.496 0.003 2 9 141 3 PRO HD3 H 3.795 0.003 2 10 141 3 PRO C C 176.823 0.000 1 11 141 3 PRO CA C 63.176 0.024 1 12 141 3 PRO CB C 32.205 0.019 1 13 141 3 PRO CG C 27.305 0.000 1 14 141 3 PRO CD C 50.708 0.000 1 15 142 4 ARG H H 8.515 0.008 1 16 142 4 ARG HA H 4.276 0.011 1 17 142 4 ARG HB2 H 1.791 0.002 2 18 142 4 ARG HB3 H 1.842 0.007 2 19 142 4 ARG HG2 H 1.671 0.000 2 20 142 4 ARG HG3 H 1.717 0.001 2 21 142 4 ARG HD3 H 3.203 0.003 2 22 142 4 ARG C C 176.605 0.000 1 23 142 4 ARG CA C 56.476 0.017 1 24 142 4 ARG CB C 30.856 0.013 1 25 142 4 ARG CG C 27.021 0.000 1 26 142 4 ARG CD C 43.335 0.000 1 27 142 4 ARG N N 119.384 0.030 1 28 143 5 GLU H H 8.740 0.007 1 29 143 5 GLU HA H 4.297 0.011 1 30 143 5 GLU HB2 H 2.003 0.004 2 31 143 5 GLU HB3 H 2.083 0.004 2 32 143 5 GLU HG2 H 2.283 0.002 2 33 143 5 GLU HG3 H 2.301 0.005 2 34 143 5 GLU C C 175.518 0.000 1 35 143 5 GLU CA C 56.856 0.022 1 36 143 5 GLU CB C 30.195 0.005 1 37 143 5 GLU CG C 36.378 0.000 1 38 143 5 GLU N N 119.700 0.049 1 39 144 6 TRP H H 8.365 0.007 1 40 144 6 TRP HA H 4.553 0.004 1 41 144 6 TRP HB2 H 3.105 0.000 1 42 144 6 TRP HB3 H 3.105 0.008 1 43 144 6 TRP HD1 H 7.019 0.003 1 44 144 6 TRP HE1 H 10.090 0.005 1 45 144 6 TRP HE3 H 7.482 0.002 1 46 144 6 TRP HZ2 H 7.340 0.006 1 47 144 6 TRP HZ3 H 7.050 0.001 1 48 144 6 TRP HH2 H 7.167 0.004 1 49 144 6 TRP C C 175.291 0.000 1 50 144 6 TRP CA C 57.317 0.044 1 51 144 6 TRP CB C 30.524 0.065 1 52 144 6 TRP N N 121.416 0.023 1 53 144 6 TRP NE1 N 129.684 0.006 1 54 145 7 VAL H H 8.257 0.009 1 55 145 7 VAL HA H 3.899 0.008 1 56 145 7 VAL HB H 1.687 0.005 1 57 145 7 VAL HG1 H 0.536 0.003 2 58 145 7 VAL HG2 H 0.361 0.003 2 59 145 7 VAL C C 173.843 0.000 1 60 145 7 VAL CA C 61.570 0.014 1 61 145 7 VAL CB C 33.309 0.012 1 62 145 7 VAL CG1 C 20.209 0.000 1 63 145 7 VAL CG2 C 20.209 0.000 1 64 145 7 VAL N N 124.617 0.058 1 65 146 8 GLU H H 8.239 0.007 1 66 146 8 GLU HA H 4.379 0.009 1 67 146 8 GLU HB2 H 1.870 0.006 2 68 146 8 GLU HB3 H 1.983 0.007 2 69 146 8 GLU HG2 H 2.195 0.003 2 70 146 8 GLU HG3 H 2.217 0.004 2 71 146 8 GLU C C 174.469 0.000 1 72 146 8 GLU CA C 55.709 0.007 1 73 146 8 GLU CB C 30.651 0.011 1 74 146 8 GLU CG C 36.350 0.000 1 75 146 8 GLU N N 122.496 0.024 1 76 147 9 ALA H H 8.388 0.008 1 77 147 9 ALA HA H 4.635 0.011 1 78 147 9 ALA HB H 1.444 0.004 1 79 147 9 ALA C C 177.416 0.000 1 80 147 9 ALA CA C 50.967 0.010 1 81 147 9 ALA CB C 20.621 0.013 1 82 147 9 ALA N N 125.711 0.024 1 83 148 10 VAL H H 8.279 0.008 1 84 148 10 VAL HA H 3.788 0.008 1 85 148 10 VAL HB H 2.099 0.008 1 86 148 10 VAL HG1 H 1.006 0.004 2 87 148 10 VAL HG2 H 0.950 0.004 2 88 148 10 VAL C C 177.001 0.000 1 89 148 10 VAL CA C 64.898 0.023 1 90 148 10 VAL CB C 31.896 0.016 1 91 148 10 VAL CG1 C 21.140 0.000 1 92 148 10 VAL CG2 C 21.140 0.000 1 93 148 10 VAL N N 120.171 0.044 1 94 149 11 ALA H H 8.445 0.007 1 95 149 11 ALA HA H 4.395 0.010 1 96 149 11 ALA HB H 1.444 0.006 1 97 149 11 ALA C C 176.993 0.000 1 98 149 11 ALA CA C 52.084 0.029 1 99 149 11 ALA CB C 19.927 0.009 1 100 149 11 ALA N N 122.615 0.025 1 101 150 12 TYR H H 7.360 0.009 1 102 150 12 TYR HA H 4.318 0.013 1 103 150 12 TYR HB2 H 2.994 0.006 1 104 150 12 TYR HB3 H 2.994 0.466 1 105 150 12 TYR HD1 H 6.434 0.004 3 106 150 12 TYR HD2 H 6.434 0.004 3 107 150 12 TYR HE1 H 6.186 0.003 3 108 150 12 TYR HE2 H 6.186 0.003 3 109 150 12 TYR C C 172.200 0.000 1 110 150 12 TYR CA C 59.243 0.006 1 111 150 12 TYR CB C 40.779 0.018 1 112 150 12 TYR N N 119.588 0.031 1 113 151 13 VAL H H 7.206 0.009 1 114 151 13 VAL HA H 4.201 0.004 1 115 151 13 VAL HB H 1.741 0.003 1 116 151 13 VAL HG1 H 0.830 0.003 2 117 151 13 VAL HG2 H 0.796 0.005 2 118 151 13 VAL CA C 59.677 0.075 1 119 151 13 VAL CB C 33.650 0.052 1 120 151 13 VAL CG1 C 20.810 0.000 1 121 151 13 VAL CG2 C 20.810 0.000 1 122 151 13 VAL N N 125.997 0.020 1 123 152 14 GLY H H 7.123 0.003 1 124 152 14 GLY HA3 H 3.447 0.005 2 125 152 14 GLY N N 113.227 0.035 1 126 153 15 PRO HA H 4.299 0.009 1 127 153 15 PRO HB2 H 1.737 0.006 2 128 153 15 PRO HB3 H 2.245 0.006 2 129 153 15 PRO HG2 H 1.942 0.003 2 130 153 15 PRO HG3 H 1.984 0.007 2 131 153 15 PRO HD2 H 3.214 0.001 2 132 153 15 PRO HD3 H 3.310 0.001 2 133 153 15 PRO C C 177.658 0.000 1 134 153 15 PRO CA C 62.189 0.014 1 135 153 15 PRO CB C 32.179 0.011 1 136 153 15 PRO CG C 27.204 0.000 1 137 153 15 PRO CD C 49.250 0.000 1 138 154 16 ASP H H 8.626 0.008 1 139 154 16 ASP HA H 4.057 0.009 1 140 154 16 ASP HB2 H 2.740 0.008 1 141 154 16 ASP HB3 H 2.880 0.006 1 142 154 16 ASP C C 177.149 0.000 1 143 154 16 ASP CA C 55.955 0.015 1 144 154 16 ASP CB C 40.784 0.008 1 145 154 16 ASP N N 121.935 0.021 1 146 155 17 ARG H H 8.762 0.010 1 147 155 17 ARG HA H 4.006 0.009 1 148 155 17 ARG HB2 H 1.280 0.005 2 149 155 17 ARG HB3 H 2.008 0.005 2 150 155 17 ARG HG2 H 1.526 0.005 1 151 155 17 ARG HG3 H 1.526 0.005 1 152 155 17 ARG HD2 H 2.589 0.001 2 153 155 17 ARG HD3 H 2.654 0.004 2 154 155 17 ARG HE H 5.648 0.007 1 155 155 17 ARG HH21 H 6.376 0.005 1 156 155 17 ARG C C 176.611 0.000 1 157 155 17 ARG CA C 57.048 0.011 1 158 155 17 ARG CB C 31.446 0.016 1 159 155 17 ARG CG C 26.505 0.000 1 160 155 17 ARG CD C 44.397 0.000 1 161 155 17 ARG N N 130.107 0.034 1 162 155 17 ARG NE N 79.463 0.011 1 163 155 17 ARG NH2 N 72.039 0.014 1 164 156 18 ARG H H 8.279 0.008 1 165 156 18 ARG HA H 4.393 0.009 1 166 156 18 ARG HB2 H 1.702 0.004 2 167 156 18 ARG HB3 H 2.082 0.007 2 168 156 18 ARG HG2 H 1.550 0.005 2 169 156 18 ARG HG3 H 1.897 0.004 2 170 156 18 ARG HD2 H 2.938 0.009 2 171 156 18 ARG HD3 H 3.043 0.005 2 172 156 18 ARG HE H 8.816 0.006 1 173 156 18 ARG HH12 H 6.506 0.006 2 174 156 18 ARG HH21 H 7.702 0.003 1 175 156 18 ARG HH22 H 8.037 0.003 1 176 156 18 ARG C C 176.616 0.000 1 177 156 18 ARG CA C 57.155 0.020 1 178 156 18 ARG CB C 29.693 0.015 1 179 156 18 ARG CG C 28.115 0.000 1 180 156 18 ARG CD C 44.323 0.000 1 181 156 18 ARG N N 118.154 0.019 1 182 156 18 ARG NE N 85.962 0.015 1 183 156 18 ARG NH1 N 69.769 0.012 1 184 156 18 ARG NH2 N 74.457 0.019 1 185 157 19 ARG H H 9.817 0.010 1 186 157 19 ARG HA H 4.416 0.013 1 187 157 19 ARG HB2 H 1.646 0.005 2 188 157 19 ARG HB3 H 1.737 0.005 2 189 157 19 ARG HG2 H 1.508 0.006 1 190 157 19 ARG HG3 H 1.508 0.006 1 191 157 19 ARG HD2 H 3.143 0.009 1 192 157 19 ARG HD3 H 3.143 0.009 1 193 157 19 ARG C C 176.113 0.000 1 194 157 19 ARG CA C 55.797 0.012 1 195 157 19 ARG CB C 32.682 0.009 1 196 157 19 ARG CG C 26.422 0.000 1 197 157 19 ARG CD C 43.137 0.000 1 198 157 19 ARG N N 125.718 0.025 1 199 158 20 PHE H H 8.822 0.012 1 200 158 20 PHE HA H 4.713 0.010 1 201 158 20 PHE HB2 H 3.093 0.008 2 202 158 20 PHE HB3 H 3.150 0.005 2 203 158 20 PHE HD1 H 7.287 0.004 3 204 158 20 PHE HD2 H 7.287 0.004 3 205 158 20 PHE HE1 H 7.379 0.004 3 206 158 20 PHE HE2 H 7.379 0.004 3 207 158 20 PHE HZ H 7.329 0.000 1 208 158 20 PHE C C 174.598 0.000 1 209 158 20 PHE CA C 57.658 0.018 1 210 158 20 PHE CB C 40.420 0.009 1 211 158 20 PHE N N 121.640 0.022 1 212 159 21 ASN H H 8.454 0.010 1 213 159 21 ASN HA H 4.763 0.007 1 214 159 21 ASN HB2 H 2.717 0.009 1 215 159 21 ASN HB3 H 2.717 0.009 1 216 159 21 ASN HD21 H 7.603 0.008 1 217 159 21 ASN HD22 H 6.916 0.005 1 218 159 21 ASN C C 174.480 0.000 1 219 159 21 ASN CA C 52.853 0.008 1 220 159 21 ASN CB C 39.396 0.013 1 221 159 21 ASN N N 123.446 0.027 1 222 159 21 ASN ND2 N 113.444 0.086 1 223 160 22 SER H H 8.430 0.008 1 224 160 22 SER HA H 4.478 0.008 1 225 160 22 SER HB2 H 3.904 0.008 2 226 160 22 SER HB3 H 4.009 0.008 2 227 160 22 SER C C 175.484 0.000 1 228 160 22 SER CA C 57.874 0.012 1 229 160 22 SER CB C 64.253 0.010 1 230 160 22 SER N N 118.415 0.029 1 231 161 23 ALA H H 8.678 0.009 1 232 161 23 ALA HA H 4.271 0.010 1 233 161 23 ALA HB H 1.430 0.004 1 234 161 23 ALA C C 177.842 0.000 1 235 161 23 ALA CA C 53.866 0.006 1 236 161 23 ALA CB C 18.868 0.010 1 237 161 23 ALA N N 128.706 0.027 1 238 162 24 ASP H H 8.223 0.008 1 239 162 24 ASP HA H 4.597 0.011 1 240 162 24 ASP HB2 H 2.541 0.009 2 241 162 24 ASP HB3 H 2.696 0.009 2 242 162 24 ASP C C 175.498 0.000 1 243 162 24 ASP CA C 53.837 0.020 1 244 162 24 ASP CB C 40.916 0.045 1 245 162 24 ASP N N 116.677 0.018 1 246 163 25 TYR H H 7.539 0.008 1 247 163 25 TYR HA H 4.362 0.010 1 248 163 25 TYR HB2 H 2.727 0.005 2 249 163 25 TYR HB3 H 3.211 0.008 2 250 163 25 TYR HD1 H 6.758 0.004 3 251 163 25 TYR HD2 H 6.758 0.004 3 252 163 25 TYR HE1 H 6.103 0.002 3 253 163 25 TYR HE2 H 6.103 0.002 3 254 163 25 TYR C C 176.435 0.000 1 255 163 25 TYR CA C 58.902 0.010 1 256 163 25 TYR CB C 38.802 0.010 1 257 163 25 TYR N N 121.445 0.028 1 258 164 26 LYS H H 8.425 0.008 1 259 164 26 LYS HA H 4.267 0.006 1 260 164 26 LYS HB3 H 1.397 0.005 2 261 164 26 LYS HG2 H 1.267 0.005 2 262 164 26 LYS HG3 H 1.343 0.002 2 263 164 26 LYS HD3 H 1.828 0.003 2 264 164 26 LYS HE3 H 3.090 0.000 2 265 164 26 LYS CA C 54.923 0.000 1 266 164 26 LYS CB C 32.939 0.000 1 267 164 26 LYS N N 128.359 0.024 1 268 165 27 GLY HA2 H 3.254 0.001 2 269 165 27 GLY HA3 H 3.918 0.004 2 270 166 28 PRO HA H 4.173 0.009 1 271 166 28 PRO HB2 H 1.612 0.005 2 272 166 28 PRO HB3 H 2.161 0.006 2 273 166 28 PRO HG2 H 1.881 0.003 2 274 166 28 PRO HG3 H 1.933 0.005 2 275 166 28 PRO HD2 H 3.376 0.003 2 276 166 28 PRO HD3 H 3.416 0.002 2 277 166 28 PRO C C 177.409 0.000 1 278 166 28 PRO CA C 62.933 0.010 1 279 166 28 PRO CB C 31.748 0.019 1 280 166 28 PRO CG C 27.490 0.000 1 281 166 28 PRO CD C 49.316 0.000 1 282 167 29 ARG H H 8.772 0.009 1 283 167 29 ARG HA H 4.216 0.008 1 284 167 29 ARG HB2 H 1.796 0.006 2 285 167 29 ARG HB3 H 1.856 0.006 2 286 167 29 ARG HG2 H 1.471 0.003 1 287 167 29 ARG HG3 H 1.471 0.003 1 288 167 29 ARG HD2 H 3.124 0.002 2 289 167 29 ARG HD3 H 3.208 0.008 2 290 167 29 ARG HE H 7.370 0.006 1 291 167 29 ARG C C 176.744 0.000 1 292 167 29 ARG CA C 56.791 0.024 1 293 167 29 ARG CB C 29.334 0.020 1 294 167 29 ARG CG C 28.046 0.000 1 295 167 29 ARG CD C 43.442 0.000 1 296 167 29 ARG N N 127.463 0.031 1 297 167 29 ARG NE N 85.401 0.039 1 298 168 30 LYS H H 9.223 0.008 1 299 168 30 LYS HA H 4.292 0.012 1 300 168 30 LYS HB2 H 1.347 0.005 2 301 168 30 LYS HB3 H 1.946 0.006 2 302 168 30 LYS HG3 H 1.164 0.007 2 303 168 30 LYS HD2 H 1.476 0.005 2 304 168 30 LYS HD3 H 1.700 0.005 2 305 168 30 LYS HE2 H 2.253 0.002 2 306 168 30 LYS HE3 H 2.555 0.003 2 307 168 30 LYS C C 177.139 0.000 1 308 168 30 LYS CA C 56.386 0.053 1 309 168 30 LYS CB C 33.103 0.007 1 310 168 30 LYS CG C 22.034 0.000 1 311 168 30 LYS CD C 27.984 0.000 1 312 168 30 LYS CE C 38.912 0.000 1 313 168 30 LYS N N 125.168 0.027 1 314 169 31 ARG H H 8.463 0.008 1 315 169 31 ARG HA H 4.555 0.008 1 316 169 31 ARG HB2 H 1.637 0.004 2 317 169 31 ARG HB3 H 2.170 0.005 2 318 169 31 ARG HG2 H 1.703 0.003 2 319 169 31 ARG HG3 H 1.927 0.004 2 320 169 31 ARG HD2 H 2.799 0.008 2 321 169 31 ARG HD3 H 2.897 0.007 2 322 169 31 ARG HE H 8.858 0.004 1 323 169 31 ARG HH21 H 7.488 0.004 1 324 169 31 ARG HH22 H 7.394 0.002 1 325 169 31 ARG C C 180.044 0.000 1 326 169 31 ARG CA C 56.032 0.020 1 327 169 31 ARG CB C 31.045 0.010 1 328 169 31 ARG CG C 27.311 0.000 1 329 169 31 ARG CD C 44.217 0.000 1 330 169 31 ARG N N 117.915 0.024 1 331 169 31 ARG NE N 85.019 0.007 1 332 169 31 ARG NH2 N 72.759 0.011 1 333 170 32 LYS H H 10.003 0.010 1 334 170 32 LYS HA H 4.094 0.008 1 335 170 32 LYS HB2 H 1.875 0.009 2 336 170 32 LYS HB3 H 1.968 0.004 2 337 170 32 LYS HG2 H 1.548 0.007 2 338 170 32 LYS HG3 H 1.595 0.003 2 339 170 32 LYS HD3 H 1.770 0.001 2 340 170 32 LYS HE3 H 3.064 0.002 2 341 170 32 LYS C C 179.528 0.000 1 342 170 32 LYS CA C 59.978 0.006 1 343 170 32 LYS CB C 31.660 0.024 1 344 170 32 LYS CG C 24.516 0.000 1 345 170 32 LYS CD C 28.908 0.000 1 346 170 32 LYS CE C 41.861 0.000 1 347 170 32 LYS N N 129.486 0.036 1 348 171 33 ALA H H 8.331 0.009 1 349 171 33 ALA HA H 4.248 0.010 1 350 171 33 ALA HB H 1.389 0.004 1 351 171 33 ALA C C 178.230 0.000 1 352 171 33 ALA CA C 53.333 0.014 1 353 171 33 ALA CB C 18.941 0.008 1 354 171 33 ALA N N 118.112 0.030 1 355 172 34 ASP H H 7.673 0.011 1 356 172 34 ASP HA H 4.574 0.013 1 357 172 34 ASP HB2 H 2.986 0.007 1 358 172 34 ASP HB3 H 2.727 0.007 1 359 172 34 ASP C C 176.206 0.000 1 360 172 34 ASP CA C 55.757 0.010 1 361 172 34 ASP CB C 41.848 0.010 1 362 172 34 ASP N N 116.593 0.026 1 363 173 35 ALA H H 7.624 0.010 1 364 173 35 ALA HA H 4.423 0.011 1 365 173 35 ALA HB H 1.457 0.007 1 366 173 35 ALA C C 176.629 0.000 1 367 173 35 ALA CA C 52.508 0.021 1 368 173 35 ALA CB C 19.480 0.036 1 369 173 35 ALA N N 123.546 0.024 1 370 174 36 SER H H 7.829 0.009 1 371 174 36 SER HA H 4.271 0.007 1 372 174 36 SER HB2 H 3.850 0.004 1 373 174 36 SER HB3 H 3.850 0.004 1 374 174 36 SER CA C 60.135 0.008 1 375 174 36 SER CB C 65.054 0.000 1 376 174 36 SER N N 121.078 0.054 1 stop_ save_ save_assigned_chemical_shifts_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_1 stop_ loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '3D 1H-15N NOESY' '3D 1H-15N TOCSY' '3D CBCA(CO)NH' '3D CBCANH' '3D C(CO)NH' '3D HBHA(CO)NH' '3D HNCA' '3D HNCO' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name 'c-di-GMP, 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 1 501 1 C2E H1' H 5.704 0.001 1 2 501 1 C2E H1A H 5.545 0.002 1 3 501 1 C2E H2' H 4.887 0.004 1 4 501 1 C2E H2A H 4.473 0.003 1 5 501 1 C2E H3A H 4.788 0.003 1 6 501 1 C2E H4' H 4.489 0.005 1 7 501 1 C2E H4A H 4.364 0.004 1 8 501 1 C2E H5'1 H 4.126 0.002 2 9 501 1 C2E H5'2 H 4.487 0.000 2 10 501 1 C2E H8 H 7.658 0.001 1 11 501 1 C2E H81 H 7.579 0.003 1 12 501 1 C2E H511 H 4.095 0.002 2 13 501 1 C2E H512 H 4.672 0.002 2 14 501 1 C2E HN1 H 11.771 0.002 1 15 501 1 C2E HN11 H 11.636 0.001 1 16 501 1 C2E HN21 H 6.263 0.005 2 17 501 1 C2E HN23 H 6.000 0.003 2 stop_ save_ save_assigned_chemical_shifts_1_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_1 stop_ loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '3D 1H-15N NOESY' '3D 1H-15N TOCSY' '3D CBCA(CO)NH' '3D CBCANH' '3D C(CO)NH' '3D HBHA(CO)NH' '3D HNCA' '3D HNCO' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name 'c-di-GMP, 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 1 502 1 C2E H1' H 5.252 0.002 1 2 502 1 C2E H1A H 4.880 0.007 1 3 502 1 C2E H2' H 4.473 0.003 1 4 502 1 C2E H2A H 5.918 0.003 1 5 502 1 C2E H3' H 4.863 0.006 1 6 502 1 C2E H3A H 4.590 0.006 1 7 502 1 C2E H4' H 4.303 0.004 1 8 502 1 C2E H4A H 4.354 0.023 1 9 502 1 C2E H5'1 H 3.994 0.004 2 10 502 1 C2E H5'2 H 4.667 0.002 2 11 502 1 C2E H8 H 7.353 0.003 1 12 502 1 C2E H81 H 7.450 0.003 1 13 502 1 C2E H511 H 4.074 0.002 2 14 502 1 C2E H512 H 4.422 0.002 2 15 502 1 C2E HN1 H 11.148 0.001 1 16 502 1 C2E HN11 H 13.211 0.001 1 17 502 1 C2E HN21 H 5.853 0.004 2 stop_ save_ save_heteronuclear_T1_list_1 _Saveframe_category T1_relaxation _Details . loop_ _Software_label $software_2 $software_4 $software_5 $software_6 stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600.12282197 _T1_coherence_type Sz _T1_value_units s _Mol_system_component_name ARR_CleD _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 4 ARG N 0.620501 0.00365771 2 5 GLU N 0.548607 0.00475531 3 6 TRP N 0.529633 0.00266486 4 7 VAL N 0.502892 0.0162868 5 8 GLU N 0.508001 0.00606453 6 9 ALA N 0.524411 0.000110003 7 10 VAL N 0.553159 0.0018665 8 11 ALA N 0.517197 0.00545685 9 12 TYR N 0.509918 0.00977661 10 13 VAL N 0.4705 0.00418389 11 14 GLY N 0.452223 0.00525579 12 16 ASP N 0.451162 0.00111951 13 17 ARG N 0.43712 0.000401256 14 18 ARG N 0.428578 0.00332458 15 19 ARG N 0.482323 0.0069558 16 20 PHE N 0.48033 0.00643701 17 21 ASN N 0.530617 0.020103 18 22 SER N 0.564972 0.0112994 19 23 ALA N 0.526343 0.00246563 20 24 ASP N 0.519642 0.000891093 21 25 TYR N 0.510308 0.00218748 22 26 LYS N 0.484332 0.00823367 23 29 ARG N 0.461766 0.00183376 24 30 LYS N 0.475986 0.00928909 25 31 ARG N 0.437292 0.00108998 26 32 LYS N 0.448209 0.00395757 27 33 ALA N 0.441462 0.00304027 28 34 ASP N 0.448189 0.0054035 29 35 ALA N 0.51164 0.00607319 30 36 SER N 1.07666 0.0300231 stop_ save_ save_heteronuclear_T2_list_1 _Saveframe_category T2_relaxation _Details . loop_ _Software_label $software_2 $software_4 $software_5 $software_6 stop_ loop_ _Sample_label $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600.12282197 _T2_coherence_type (S+)+(S-) _T2_value_units s _Mol_system_component_name ARR_CleD _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 4 ARG N 0.310164 0.00154885 . . 2 5 GLU N 0.225657 0.00109481 . . 3 6 TRP N 0.171662 0.000727856 . . 4 7 VAL N 0.0405536 0.00109908 . . 5 8 GLU N 0.250828 0.000578814 . . 6 9 ALA N 0.120953 0.000580793 . . 7 10 VAL N 0.195145 0.000959654 . . 8 11 ALA N 0.0194535 0.0024827 . . 9 12 TYR N 0.115855 0.00408173 . . 10 13 VAL N 0.158428 0.00239952 . . 11 14 GLY N 0.0733622 0.00926459 . . 12 16 ASP N 0.176863 0.00205825 . . 13 17 ARG N 0.195741 0.00176629 . . 14 18 ARG N 0.179337 0.00155984 . . 15 19 ARG N 0.218972 0.000129461 . . 16 20 PHE N 0.203401 0.00143561 . . 17 21 ASN N 0.244481 0.00182899 . . 18 22 SER N 0.243191 0.00238341 . . 19 23 ALA N 0.245652 0.00333104 . . 20 24 ASP N 0.246021 0.00415815 . . 21 25 TYR N 0.218245 0.00214816 . . 22 26 LYS N 0.224215 0.00591204 . . 23 29 ARG N 0.186352 0.00413598 . . 24 30 LYS N 0.220497 0.00246013 . . 25 31 ARG N 0.158316 0.00147375 . . 26 32 LYS N 0.181769 0.000254407 . . 27 33 ALA N 0.170753 0.000769737 . . 28 34 ASP N 0.202996 0.00152468 . . 29 35 ALA N 0.266134 0.00405842 . . 30 36 SER N 0.507228 0.0103427 . . stop_ save_ save_heteronuclear_Rex_list_1 _Saveframe_category T2_relaxation _Details 'These are the exchange rates derived from fitting the relaxation data with ModelFree.' loop_ _Software_label $software_2 $software_4 $software_5 $software_6 stop_ loop_ _Sample_label $sample_1 $sample_1 $sample_2 $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600.12282197 _T2_coherence_type (S+)+(S-) _T2_value_units s-1 _Mol_system_component_name ARR_CleD _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 4 ARG N . . 0.000 0.000 2 5 GLU N . . 0.000 0.000 3 6 TRP N . . 0.000 0.000 4 7 VAL N . . 10.000 0.699 5 8 GLU N . . 0.000 0.000 6 9 ALA N . . 3.925 0.040 7 10 VAL N . . 0.000 0.000 8 11 ALA N . . 10.000 6.560 9 12 TYR N . . 3.905 0.318 10 13 VAL N . . 0.000 0.000 11 14 GLY N . . 8.451 1.723 12 16 ASP N . . 0.000 0.000 13 17 ARG N . . 0.000 0.000 14 18 ARG N . . 0.000 0.000 15 19 ARG N . . 0.000 0.000 16 20 PHE N . . 0.000 0.000 17 21 ASN N . . 0.000 0.000 18 22 SER N . . 0.000 0.000 19 23 ALA N . . 0.000 0.000 20 24 ASP N . . 0.000 0.000 21 25 TYR N . . 0.000 0.000 22 36 SER N . . 0.000 0.000 23 29 ARG N . . 0.000 0.000 24 30 LYS N . . 0.000 0.000 25 31 ARG N . . 0.000 0.000 26 32 LYS N . . 0.000 0.000 27 33 ALA N . . 0.000 0.000 28 34 ASP N . . 0.000 0.000 29 35 ALA N . . 0.000 0.000 30 36 SER N . . 0.000 0.000 stop_ save_ save_heteronuclear_noe_list_1 _Saveframe_category heteronuclear_NOE _Details . loop_ _Software_label $software_2 $software_4 $software_5 $software_6 stop_ loop_ _Experiment_label '2D 1H-15N NOE without saturation' '2D 1H-15N NOE with saturation' stop_ loop_ _Sample_label . . stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600.12282197 _Mol_system_component_name ARR_CleD _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type Sz _NOE_reference_value . _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 4 ARG -0.0834 0.0047 5 GLU 0.2275 0.0084 6 TRP 0.3853 0.0126 7 VAL 0.4831 0.0268 8 GLU 0.4703 0.0035 9 ALA 0.4782 0.0081 10 VAL 0.4537 0.0068 11 ALA 0.4573 0.0288 12 TYR 0.6012 0.0130 13 VAL 0.6488 0.0047 14 GLY 0.6055 0.0854 16 ASP 0.6637 0.0005 17 ARG 0.7096 0.0056 18 ARG 0.7330 0.0056 19 ARG 0.6568 0.0024 20 PHE 0.5719 0.0061 21 ASN 0.4003 0.0124 22 SER 0.3823 0.0039 23 ALA 0.4473 0.0143 24 ASP 0.4591 0.0032 25 TYR 0.5464 0.0004 26 LYS 0.5597 0.0217 29 ARG 0.6600 0.0080 30 LYS 0.6496 0.0082 31 ARG 0.7312 0.0090 32 LYS 0.6953 0.0047 33 ALA 0.6367 0.0004 34 ASP 0.6542 0.0045 35 ALA 0.4906 0.0040 36 SER -1.0054 0.0012 stop_ save_ save_order_parameter_list_1 _Saveframe_category S2_parameters _Details 'These are the order parameters S2, derived from fitting the relaxation data with ModelFree.' loop_ _Software_label $software_2 $software_4 $software_5 $software_6 stop_ loop_ _Sample_label $sample_1 $sample_1 $sample_2 $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name ARR_CleD _Tau_e_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 4 ARG N . 0.477 0.002 . . . . . . . . . . . . 5 GLU N . 0.654 0.003 . . . . . . . . . . . . 6 TRP N . 0.741 0.003 . . . . . . . . . . . . 7 VAL N . 0.804 0.023 . . . . . . . . . . . . 8 GLU N . 0.600 0.001 . . . . . . . . . . . . 9 ALA N . 0.680 0.001 . . . . . . . . . . . . 10 VAL N . 0.686 0.002 . . . . . . . . . . . . 11 ALA N . 0.768 0.010 . . . . . . . . . . . . 12 TYR N . 0.728 0.014 . . . . . . . . . . . . 13 VAL N . 0.829 0.006 . . . . . . . . . . . . 14 GLY N . 0.816 0.020 . . . . . . . . . . . . 16 ASP N . 0.842 0.002 . . . . . . . . . . . . 17 ARG N . 0.867 0.001 . . . . . . . . . . . . 18 ARG N . 0.871 0.005 . . . . . . . . . . . . 19 ARG N . 0.726 0.000 . . . . . . . . . . . . 20 PHE N . 0.736 0.005 . . . . . . . . . . . . 21 ASN N . 0.558 0.004 . . . . . . . . . . . . 22 SER N . 0.618 0.005 . . . . . . . . . . . . 23 ALA N . 0.671 0.004 . . . . . . . . . . . . 24 ASP N . 0.682 0.001 . . . . . . . . . . . . 25 TYR N . 0.716 0.003 . . . . . . . . . . . . 26 LYS N . 0.736 0.011 . . . . . . . . . . . . 29 ARG N . 0.810 0.004 . . . . . . . . . . . . 30 LYS N . 0.714 0.007 . . . . . . . . . . . . 31 ARG N . 0.879 0.003 . . . . . . . . . . . . 32 LYS N . 0.816 0.001 . . . . . . . . . . . . 33 ALA N . 0.899 0.003 . . . . . . . . . . . . 34 ASP N . 0.797 0.005 . . . . . . . . . . . . 35 ALA N . 0.601 0.006 . . . . . . . . . . . . 36 SER N . 0.225 0.003 . . . . . . . . . . . . stop_ _Tau_s_value_units . save_