data_16901 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of the relaxin-like factor ; _BMRB_accession_number 16901 _BMRB_flat_file_name bmr16901.str _Entry_type original _Submission_date 2010-04-26 _Accession_date 2010-04-26 _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 Bullesbach Erika E. . 2 Hass Mathias A.S. . 3 Jensen Malene R. . 4 Hansen Flemming D. . 5 Kristensen Soren M. . 6 Schwabe Christian . . 7 Led Jens J. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 8 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 676 "13C chemical shifts" 48 "15N chemical shifts" 5 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2010-05-19 original author . stop_ _Original_release_date 2010-05-19 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Solution Structure of a Conformationally Restricted Fully Active Derivative of the Human Relaxin-like Factor (dagger) (double dagger).' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 19053253 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Bullesbach Erika E. . 2 Hass Mathias A.S. . 3 Jensen Malene R. . 4 Hansen 'D. Flemming' . . 5 Kristensen Sren M. . 6 Schwabe Christian . . 7 Led Jens J. . stop_ _Journal_abbreviation Biochemistry _Journal_name_full Biochemistry _Journal_volume . _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year 2008 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Human Relaxin-like Factor' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label RLF-A $RLF-A RLF-B $RLF-B 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_RLF-A _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common RLF-A _Molecular_mass 2778.196 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 26 _Mol_residue_sequence ; AAATNPARYCCLSGCTQQDL LTLCPY ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 106 ALA 2 107 ALA 3 108 ALA 4 109 THR 5 110 ASN 6 111 PRO 7 112 ALA 8 113 ARG 9 114 TYR 10 115 CYS 11 116 CYS 12 117 LEU 13 118 SER 14 119 GLY 15 120 CYS 16 121 THR 17 122 GLN 18 123 GLN 19 124 ASP 20 125 LEU 21 126 LEU 22 127 THR 23 128 LEU 24 129 CYS 25 130 PRO 26 131 TYR stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-06-13 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 BMRB 16968 RLF-A_crosslinked 100.00 27 100.00 100.00 1.51e-08 PDB 2H8B "Solution Structure Of Insl3" 96.15 26 100.00 100.00 1.14e-07 PDB 2K6T "Solution Structure Of The Relaxin-Like Factor" 96.15 26 100.00 100.00 1.14e-07 PDB 2K6U "The Solution Structure Of A Conformationally Restricted Fully Active Derivative Of The Human Relaxin-Like Factor (Rlf)" 100.00 27 100.00 100.00 1.51e-08 DBJ BAG63984 "unnamed protein product [Homo sapiens]" 100.00 131 100.00 100.00 9.85e-09 EMBL CAA52017 "Leydig insulin-like hormone [Homo sapiens]" 100.00 101 100.00 100.00 9.03e-09 GB AAB31371 "Ley I-L [Homo sapiens]" 100.00 131 100.00 100.00 9.85e-09 GB AAH32810 "Similar to insulin-like 3 (Leydig cell), partial [Homo sapiens]" 100.00 130 100.00 100.00 1.01e-08 GB AAH53345 "INSL3 protein, partial [Homo sapiens]" 100.00 130 100.00 100.00 1.01e-08 GB AAH71706 "Insulin-like 3 (Leydig cell) [Homo sapiens]" 100.00 131 100.00 100.00 9.85e-09 GB AAI06722 "Insulin-like 3 (Leydig cell) [Homo sapiens]" 100.00 131 100.00 100.00 9.85e-09 REF NP_001171286 "tyrosine-protein kinase JAK3 precursor [Pan troglodytes]" 100.00 131 100.00 100.00 9.09e-09 REF NP_005534 "insulin-like 3 isoform 2 precursor [Homo sapiens]" 100.00 131 100.00 100.00 9.76e-09 REF XP_003275863 "PREDICTED: insulin-like 3 isoform X2 [Nomascus leucogenys]" 100.00 131 100.00 100.00 9.66e-09 REF XP_003915200 "PREDICTED: insulin-like 3 [Papio anubis]" 100.00 131 100.00 100.00 9.46e-09 REF XP_007993939 "PREDICTED: insulin-like 3 [Chlorocebus sabaeus]" 100.00 131 100.00 100.00 9.66e-09 SP P51460 "RecName: Full=Insulin-like 3; AltName: Full=Leydig insulin-like peptide; Short=Ley-I-L; AltName: Full=Relaxin-like factor; Cont" 100.00 131 100.00 100.00 9.76e-09 SP Q5CZK3 "RecName: Full=Insulin-like 3; AltName: Full=Leydig insulin-like peptide; Short=Ley-I-L; AltName: Full=Relaxin-like factor; Cont" 100.00 131 100.00 100.00 9.56e-09 stop_ save_ save_RLF-B _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common RLF-B _Molecular_mass 3528.142 _Mol_thiol_state 'all disulfide bound' _Details . _Residue_count 31 _Mol_residue_sequence ; PTPEMREKLCGHHFVRALVR VCGGPRWSTEA ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 25 PRO 2 26 THR 3 27 PRO 4 28 GLU 5 29 MET 6 30 ARG 7 31 GLU 8 32 LYS 9 33 LEU 10 34 CYS 11 35 GLY 12 36 HIS 13 37 HIS 14 38 PHE 15 39 VAL 16 40 ARG 17 41 ALA 18 42 LEU 19 43 VAL 20 44 ARG 21 45 VAL 22 46 CYS 23 47 GLY 24 48 GLY 25 49 PRO 26 50 ARG 27 51 TRP 28 52 SER 29 53 THR 30 54 GLU 31 55 ALA stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Details $RLF-A Human 9606 Eukaryota Metazoa Homo sapiens 'A chain of synthesized human RLF' $RLF-B Human 9606 Eukaryota Metazoa Homo sapiens 'B chain of synthesized human RLF' 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 _Details $RLF-A 'chemical synthesis' . . . . . 'human sequence' $RLF-B 'chemical synthesis' . . . . . 'human sequence' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_RLF_H2O _Saveframe_category sample _Sample_type solution _Details '40 mM Na-d4-acetate/NaOD pH 5.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $RLF-A . mM 0.1 1.2 'natural abundance' $RLF-B . mM 0.1 1.2 'natural abundance' Na-d4-acetate/NaOD 40 mM . . 'natural abundance' H2O 92 % . . 'natural abundance' D2O 8 % . . 'natural abundance' stop_ save_ save_RLF_D2O _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $RLF-A 1.2 mM 'natural abundance' $RLF-B 1.2 mM 'natural abundance' Na-d4-acetate/NaOD 40 mM 'natural abundance' D2O 100 % 'natural abundance' stop_ save_ save_15N-RLF_H2O _Saveframe_category sample _Sample_type solution _Details '40 mM d4-actic acid / NaOD pH 5.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $RLF-A . mM 0.2 1.2 [U-15N] $RLF-B . mM 0.2 1.2 [U-15N] 'd4-acetic acid/NaOD' 40 mM . . 'natural abundance' H2O 92 % . . 'natural abundance' D2O 8 % . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CNS _Saveframe_category software _Name CNS _Version 1.1 loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_ARIA _Saveframe_category software _Name ARIA _Version 2 loop_ _Vendor _Address _Electronic_address 'Linge, O'Donoghue and Nilges' ; Institut Pasteur Unit de Bioinformatique Structurale 25-28 rue du Dr Roux F-75724 Paris CEDEX 15 France ; . stop_ loop_ _Task 'NOE assignment' 'structure solution' stop_ _Details 'Ambiguous Restraints for Iterative Assignment' save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3.110 loop_ _Vendor _Address _Electronic_address Goddard 'University of California, San Francisco' . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_PREDITOR _Saveframe_category software _Name PREDITOR _Version . loop_ _Vendor _Address _Electronic_address Wishart 'Department of Biochemistry, University of Alberta, Edmonton, Canada' . stop_ loop_ _Task 'bond angle prediction' stop_ _Details 'Predicting protein torsion angle restraints' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 800 _Details 'with cryo-probe' save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 500 _Details 'with cryo-probe' save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $RLF_D2O save_ save_2D_DQF-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $RLF_D2O save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $RLF_D2O save_ save_2D_1H-1H_TOCSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $RLF_H2O save_ save_2D_1H-13C_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $RLF_D2O save_ save_2D_1H-1H_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_D2O save_ save_2D_1H-1H_NOESY_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_D2O save_ save_2D_1H-1H_NOESY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-1H_NOESY_15 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_H2O save_ save_2D_1H-15N_HSQC_16 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $RLF_H2O save_ save_2D_1H-13C_HSQC_17 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $RLF_D2O save_ ####################### # Sample conditions # ####################### save_1.2_mM_RLF_92%_H2O_8%_D2O-293K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 293 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-296K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 296 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-301K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 301 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-303K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 303 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-306K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 306 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-308K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 308 . K stop_ save_ save_1.2_mM_RLF_92%_H2O_8%_D2O-313K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 313 . K stop_ save_ save_1.2_mM_RLF_100%_D2O-288K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 2.7 0.2 pH temperature 288 . K stop_ save_ save_1.2_mM_RLF_100%_D2O-308K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.1 pH temperature 308 . 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 na indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 na indirect . . . 0.101329118 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_1H-1H_H2O_noesy_308K_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_H2O stop_ _Sample_conditions_label $1.2_mM_RLF_92%_H2O_8%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A _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 1 106 1 ALA HA H 4.006 0.000 1 2 106 1 ALA HB H 1.461 0.000 1 3 107 2 ALA H H 8.457 0.003 1 4 107 2 ALA HA H 4.215 0.000 1 5 107 2 ALA HB H 1.299 0.000 1 6 108 3 ALA H H 8.257 0.000 1 7 108 3 ALA HA H 4.256 0.001 1 8 108 3 ALA HB H 1.278 0.004 1 9 109 4 THR H H 7.971 0.002 1 10 109 4 THR HA H 4.220 0.001 1 11 109 4 THR HB H 4.111 0.001 1 12 109 4 THR HG2 H 1.135 0.003 1 13 110 5 ASN H H 8.294 0.001 1 14 110 5 ASN HA H 4.900 0.000 1 15 110 5 ASN HB2 H 2.883 0.001 2 16 110 5 ASN HB3 H 2.750 0.000 2 17 110 5 ASN HD21 H 7.655 0.002 2 18 110 5 ASN HD22 H 6.937 0.003 2 19 111 6 PRO HA H 4.090 0.002 1 20 111 6 PRO HB2 H 2.297 0.001 2 21 111 6 PRO HB3 H 1.849 0.006 2 22 111 6 PRO HD2 H 3.793 0.000 2 23 111 6 PRO HD3 H 3.783 0.000 2 24 111 6 PRO HG2 H 1.971 0.000 2 25 111 6 PRO HG3 H 1.972 0.000 2 26 112 7 ALA H H 7.883 0.000 1 27 112 7 ALA HB H 1.035 0.003 1 28 113 8 ARG H H 7.420 0.002 1 29 113 8 ARG HA H 3.875 0.003 1 30 113 8 ARG HB2 H 1.672 0.002 2 31 113 8 ARG HB3 H 1.482 0.000 2 32 113 8 ARG HD2 H 3.101 0.000 2 33 113 8 ARG HD3 H 3.101 0.000 2 34 113 8 ARG HE H 6.954 0.000 1 35 113 8 ARG HG2 H 1.423 0.000 2 36 113 8 ARG HG3 H 1.420 0.000 2 37 114 9 TYR H H 8.002 0.001 1 38 114 9 TYR HA H 4.210 0.003 1 39 114 9 TYR HB2 H 3.028 0.000 2 40 114 9 TYR HB3 H 3.029 0.000 2 41 114 9 TYR HD1 H 6.951 0.001 3 42 114 9 TYR HD2 H 6.951 0.001 3 43 114 9 TYR HE1 H 6.773 0.002 3 44 114 9 TYR HE2 H 6.773 0.002 3 45 115 10 CYS H H 8.564 0.003 1 46 115 10 CYS HA H 4.407 0.000 1 47 115 10 CYS HB2 H 3.212 0.003 2 48 115 10 CYS HB3 H 2.827 0.004 2 49 116 11 CYS H H 7.579 0.006 1 50 116 11 CYS HA H 4.389 0.000 1 51 116 11 CYS HB2 H 3.505 0.001 2 52 116 11 CYS HB3 H 2.760 0.000 2 53 117 12 LEU H H 8.066 0.001 1 54 117 12 LEU HA H 4.127 0.000 1 55 117 12 LEU HB2 H 1.642 0.003 2 56 117 12 LEU HB3 H 1.444 0.000 2 57 117 12 LEU HD1 H 0.794 0.000 2 58 117 12 LEU HD2 H 0.795 0.000 2 59 117 12 LEU HG H 1.640 0.000 1 60 118 13 SER H H 8.118 0.001 1 61 118 13 SER HA H 4.468 0.002 1 62 118 13 SER HB2 H 3.520 0.001 2 63 118 13 SER HB3 H 3.114 0.000 2 64 119 14 GLY H H 7.146 0.005 1 65 119 14 GLY HA2 H 4.215 0.001 2 66 119 14 GLY HA3 H 3.898 0.003 2 67 120 15 CYS H H 8.844 0.003 1 68 120 15 CYS HA H 5.178 0.001 1 69 120 15 CYS HB2 H 3.693 0.000 2 70 120 15 CYS HB3 H 2.571 0.000 2 71 121 16 THR H H 9.666 0.002 1 72 121 16 THR HA H 4.858 0.002 1 73 121 16 THR HB H 4.737 0.001 1 74 121 16 THR HG2 H 1.125 0.002 1 75 122 17 GLN H H 8.984 0.001 1 76 122 17 GLN HA H 3.926 0.005 1 77 122 17 GLN HB2 H 2.132 0.001 2 78 122 17 GLN HB3 H 2.068 0.000 2 79 122 17 GLN HE21 H 7.435 0.001 2 80 122 17 GLN HE22 H 6.674 0.002 2 81 122 17 GLN HG2 H 2.397 0.002 2 82 122 17 GLN HG3 H 2.298 0.002 2 83 123 18 GLN H H 8.156 0.001 1 84 123 18 GLN HA H 3.929 0.001 1 85 123 18 GLN HB2 H 2.049 0.001 2 86 123 18 GLN HB3 H 1.966 0.000 2 87 123 18 GLN HE21 H 7.498 0.000 2 88 123 18 GLN HE22 H 6.777 0.002 2 89 123 18 GLN HG2 H 2.418 0.003 2 90 123 18 GLN HG3 H 2.363 0.002 2 91 124 19 ASP H H 7.733 0.002 1 92 124 19 ASP HA H 4.328 0.000 1 93 124 19 ASP HB2 H 3.186 0.003 2 94 124 19 ASP HB3 H 2.784 0.004 2 95 125 20 LEU H H 7.623 0.001 1 96 125 20 LEU HA H 3.950 0.001 1 97 125 20 LEU HB2 H 2.008 0.002 2 98 125 20 LEU HB3 H 1.216 0.005 2 99 125 20 LEU HD1 H 0.769 0.000 2 100 125 20 LEU HD2 H 0.708 0.002 2 101 125 20 LEU HG H 1.836 0.000 1 102 126 21 LEU H H 7.907 0.002 1 103 126 21 LEU HA H 4.187 0.002 1 104 126 21 LEU HB2 H 1.728 0.003 2 105 126 21 LEU HB3 H 1.526 0.003 2 106 126 21 LEU HD1 H 0.846 0.000 2 107 126 21 LEU HD2 H 0.847 0.000 2 108 126 21 LEU HG H 1.631 0.000 1 109 127 22 THR H H 7.436 0.001 1 110 127 22 THR HA H 4.114 0.001 1 111 127 22 THR HB H 4.315 0.000 1 112 127 22 THR HG2 H 1.369 0.002 1 113 128 23 LEU H H 7.749 0.001 1 114 128 23 LEU HA H 4.369 0.002 1 115 128 23 LEU HB2 H 2.105 0.001 2 116 128 23 LEU HB3 H 1.614 0.001 2 117 128 23 LEU HD1 H 1.030 0.003 2 118 128 23 LEU HD2 H 0.848 0.004 2 119 128 23 LEU HG H 1.902 0.002 1 120 129 24 CYS H H 7.280 0.002 1 121 129 24 CYS HA H 4.708 0.000 1 122 129 24 CYS HB2 H 2.982 0.000 2 123 129 24 CYS HB3 H 2.782 0.000 2 124 130 25 PRO HA H 4.355 0.003 1 125 130 25 PRO HB2 H 1.989 0.000 2 126 130 25 PRO HB3 H 1.836 0.000 2 127 130 25 PRO HD2 H 3.505 0.000 2 128 130 25 PRO HD3 H 3.340 0.000 2 129 130 25 PRO HG2 H 1.643 0.000 2 130 130 25 PRO HG3 H 1.643 0.000 2 131 131 26 TYR H H 7.495 0.001 1 132 131 26 TYR HA H 4.306 0.002 1 133 131 26 TYR HB2 H 2.988 0.002 2 134 131 26 TYR HB3 H 2.836 0.002 2 135 131 26 TYR HD1 H 6.992 0.002 3 136 131 26 TYR HD2 H 6.992 0.002 3 137 131 26 TYR HE1 H 6.712 0.000 3 138 131 26 TYR HE2 H 6.712 0.000 3 stop_ save_ save_1H-1H_H2O_noesy_308K_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_H2O stop_ _Sample_conditions_label $1.2_mM_RLF_92%_H2O_8%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B _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 25 1 PRO HA H 4.429 0.000 1 2 26 2 THR H H 8.560 0.000 1 3 26 2 THR HA H 4.615 0.000 1 4 26 2 THR HB H 4.165 0.000 1 5 26 2 THR HG2 H 1.240 0.000 1 6 27 3 PRO HA H 4.379 0.000 1 7 27 3 PRO HB2 H 2.272 0.000 2 8 27 3 PRO HB3 H 1.871 0.000 2 9 27 3 PRO HD2 H 3.811 0.000 2 10 27 3 PRO HD3 H 3.703 0.000 2 11 28 4 GLU H H 8.396 0.001 1 12 28 4 GLU HA H 4.251 0.000 1 13 28 4 GLU HB2 H 2.014 0.002 2 14 28 4 GLU HB3 H 1.915 0.003 2 15 28 4 GLU HG2 H 2.291 0.001 2 16 28 4 GLU HG3 H 2.261 0.000 2 17 29 5 MET H H 8.308 0.001 1 18 29 5 MET HA H 4.388 0.003 1 19 29 5 MET HB2 H 2.014 0.001 2 20 29 5 MET HB3 H 1.982 0.002 2 21 29 5 MET HG2 H 2.532 0.000 2 22 29 5 MET HG3 H 2.480 0.001 2 23 30 6 ARG H H 8.381 0.002 1 24 30 6 ARG HA H 3.991 0.002 1 25 30 6 ARG HB2 H 1.542 0.000 2 26 30 6 ARG HB3 H 1.462 0.000 2 27 30 6 ARG HD2 H 3.075 0.003 2 28 30 6 ARG HD3 H 3.032 0.003 2 29 30 6 ARG HE H 7.083 0.002 1 30 30 6 ARG HG2 H 1.352 0.000 2 31 30 6 ARG HG3 H 1.255 0.002 2 32 31 7 GLU H H 8.014 0.004 1 33 31 7 GLU HA H 4.491 0.001 1 34 31 7 GLU HB2 H 1.872 0.003 2 35 31 7 GLU HB3 H 1.816 0.000 2 36 31 7 GLU HG2 H 2.181 0.000 2 37 31 7 GLU HG3 H 2.094 0.000 2 38 32 8 LYS H H 8.663 0.002 1 39 32 8 LYS HA H 4.557 0.002 1 40 32 8 LYS HB2 H 1.911 0.001 2 41 32 8 LYS HB3 H 1.708 0.000 2 42 32 8 LYS HD2 H 1.579 0.000 2 43 32 8 LYS HD3 H 1.568 0.000 2 44 32 8 LYS HE2 H 2.830 0.000 2 45 32 8 LYS HE3 H 2.833 0.000 2 46 32 8 LYS HG2 H 1.408 0.000 2 47 32 8 LYS HG3 H 1.003 0.000 2 48 33 9 LEU H H 7.889 0.004 1 49 33 9 LEU HA H 4.468 0.002 1 50 33 9 LEU HB2 H 1.804 0.001 2 51 33 9 LEU HB3 H 0.904 0.003 2 52 33 9 LEU HD1 H 0.902 0.000 2 53 33 9 LEU HD2 H 0.648 0.001 2 54 33 9 LEU HG H 1.559 0.002 1 55 34 10 CYS H H 8.522 0.001 1 56 34 10 CYS HA H 4.922 0.002 1 57 34 10 CYS HB2 H 3.222 0.005 2 58 34 10 CYS HB3 H 2.961 0.001 2 59 35 11 GLY H H 9.106 0.001 1 60 35 11 GLY HA2 H 3.953 0.002 2 61 35 11 GLY HA3 H 3.744 0.004 2 62 36 12 HIS H H 7.891 0.003 1 63 36 12 HIS HA H 4.319 0.002 1 64 36 12 HIS HB2 H 3.076 0.000 2 65 36 12 HIS HB3 H 3.076 0.000 2 66 36 12 HIS HD2 H 6.965 0.007 1 67 36 12 HIS HE1 H 8.074 0.000 1 68 37 13 HIS H H 7.954 0.001 1 69 37 13 HIS HA H 4.257 0.002 1 70 37 13 HIS HB2 H 3.449 0.001 2 71 37 13 HIS HB3 H 3.204 0.003 2 72 37 13 HIS HD2 H 7.220 0.002 1 73 37 13 HIS HE1 H 8.258 0.001 1 74 38 14 PHE H H 7.076 0.002 1 75 38 14 PHE HA H 4.049 0.002 1 76 38 14 PHE HB2 H 3.077 0.006 2 77 38 14 PHE HB3 H 2.918 0.003 2 78 38 14 PHE HD1 H 6.973 0.001 3 79 38 14 PHE HD2 H 6.973 0.001 3 80 38 14 PHE HE1 H 7.137 0.000 3 81 38 14 PHE HE2 H 7.137 0.000 3 82 39 15 VAL H H 7.133 0.004 1 83 39 15 VAL HA H 3.114 0.003 1 84 39 15 VAL HB H 1.989 0.005 1 85 39 15 VAL HG1 H 1.034 0.002 2 86 39 15 VAL HG2 H 0.808 0.001 2 87 40 16 ARG H H 7.871 0.001 1 88 40 16 ARG HA H 3.751 0.002 1 89 40 16 ARG HB2 H 1.729 0.002 2 90 40 16 ARG HB3 H 1.734 0.000 2 91 40 16 ARG HD2 H 3.066 0.000 2 92 40 16 ARG HD3 H 3.045 0.000 2 93 40 16 ARG HE H 6.952 0.000 1 94 40 16 ARG HG2 H 1.634 0.001 2 95 40 16 ARG HG3 H 1.466 0.000 2 96 41 17 ALA H H 7.411 0.002 1 97 41 17 ALA HA H 3.973 0.003 1 98 41 17 ALA HB H 1.348 0.004 1 99 42 18 LEU H H 7.890 0.002 1 100 42 18 LEU HA H 3.716 0.003 1 101 42 18 LEU HB2 H 1.379 0.003 2 102 42 18 LEU HB3 H 0.939 0.000 2 103 42 18 LEU HD1 H 0.644 0.005 2 104 42 18 LEU HD2 H 0.642 0.005 2 105 42 18 LEU HG H 1.209 0.000 1 106 43 19 VAL H H 8.032 0.001 1 107 43 19 VAL HA H 3.307 0.002 1 108 43 19 VAL HB H 1.968 0.004 1 109 43 19 VAL HG1 H 0.835 0.003 2 110 43 19 VAL HG2 H 0.722 0.001 2 111 44 20 ARG H H 7.487 0.002 1 112 44 20 ARG HA H 3.936 0.002 1 113 44 20 ARG HB2 H 1.926 0.005 2 114 44 20 ARG HB3 H 1.821 0.000 2 115 44 20 ARG HD2 H 3.191 0.001 2 116 44 20 ARG HD3 H 3.094 0.002 2 117 44 20 ARG HE H 7.217 0.002 1 118 44 20 ARG HG2 H 1.624 0.001 2 119 44 20 ARG HG3 H 1.479 0.001 2 120 45 21 VAL H H 8.053 0.001 1 121 45 21 VAL HA H 3.849 0.001 1 122 45 21 VAL HB H 2.004 0.001 1 123 45 21 VAL HG1 H 1.032 0.002 2 124 45 21 VAL HG2 H 0.895 0.001 2 125 46 22 CYS H H 8.458 0.002 1 126 46 22 CYS HA H 4.699 0.001 1 127 46 22 CYS HB2 H 3.054 0.002 2 128 46 22 CYS HB3 H 2.703 0.003 2 129 47 23 GLY H H 7.825 0.000 1 130 47 23 GLY HA2 H 3.934 0.004 2 131 47 23 GLY HA3 H 3.858 0.004 2 132 48 24 GLY H H 7.834 0.002 1 133 48 24 GLY HA2 H 4.072 0.000 2 134 48 24 GLY HA3 H 3.970 0.000 2 135 49 25 PRO HA H 4.266 0.003 1 136 49 25 PRO HB2 H 2.053 0.000 2 137 49 25 PRO HB3 H 1.644 0.000 2 138 49 25 PRO HD2 H 3.548 0.001 2 139 49 25 PRO HD3 H 3.478 0.001 2 140 49 25 PRO HG2 H 1.872 0.000 2 141 49 25 PRO HG3 H 1.841 0.000 2 142 50 26 ARG H H 8.170 0.001 1 143 50 26 ARG HA H 4.150 0.000 1 144 50 26 ARG HB2 H 1.627 0.002 2 145 50 26 ARG HB3 H 1.555 0.002 2 146 50 26 ARG HD2 H 2.994 0.000 2 147 50 26 ARG HD3 H 2.994 0.000 2 148 50 26 ARG HE H 7.062 0.002 1 149 50 26 ARG HG2 H 1.363 0.000 2 150 50 26 ARG HG3 H 1.363 0.000 2 151 51 27 TRP H H 7.718 0.003 1 152 51 27 TRP HA H 4.593 0.001 1 153 51 27 TRP HB2 H 3.244 0.002 2 154 51 27 TRP HB3 H 3.129 0.004 2 155 51 27 TRP HD1 H 7.166 0.002 1 156 51 27 TRP HE1 H 10.061 0.001 1 157 51 27 TRP HE3 H 7.466 0.001 1 158 51 27 TRP HH2 H 7.033 0.001 1 159 51 27 TRP HZ2 H 7.325 0.002 1 160 51 27 TRP HZ3 H 6.961 0.005 1 161 52 28 SER H H 7.894 0.002 1 162 52 28 SER HA H 4.345 0.003 1 163 52 28 SER HB2 H 3.750 0.001 2 164 52 28 SER HB3 H 3.591 0.001 2 165 53 29 THR H H 7.938 0.001 1 166 53 29 THR HA H 4.277 0.000 1 167 53 29 THR HB H 4.229 0.003 1 168 53 29 THR HG2 H 1.125 0.001 1 169 54 30 GLU H H 8.115 0.001 1 170 54 30 GLU HA H 4.265 0.000 1 171 54 30 GLU HB2 H 2.032 0.001 2 172 54 30 GLU HB3 H 1.848 0.003 2 173 54 30 GLU HG2 H 2.230 0.001 2 174 55 31 ALA H H 7.833 0.001 1 175 55 31 ALA HA H 4.050 0.000 1 176 55 31 ALA HB H 1.265 0.000 1 stop_ save_ save_1H-1H_D2O_noesy_308K_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_D2O stop_ _Sample_conditions_label $1.2_mM_RLF_100%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A _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 1 106 1 ALA HA H 4.004 0.000 1 2 106 1 ALA HB H 1.461 0.000 1 3 107 2 ALA H H 8.436 0.000 1 4 107 2 ALA HA H 4.217 0.000 1 5 107 2 ALA HB H 1.297 0.000 1 6 108 3 ALA H H 8.245 0.000 1 7 108 3 ALA HA H 4.257 0.000 1 8 108 3 ALA HB H 1.277 0.000 1 9 109 4 THR H H 7.952 0.000 1 10 109 4 THR HA H 4.225 0.002 1 11 109 4 THR HB H 4.109 0.003 1 12 109 4 THR HG2 H 1.138 0.001 1 13 110 5 ASN H H 8.331 0.000 1 14 110 5 ASN HA H 4.908 0.001 1 15 110 5 ASN HB2 H 2.878 0.002 2 16 110 5 ASN HB3 H 2.752 0.002 2 17 110 5 ASN HD21 H 6.874 0.000 2 18 110 5 ASN HD22 H 7.630 0.000 2 19 111 6 PRO HA H 4.097 0.002 1 20 111 6 PRO HB2 H 2.297 0.001 2 21 111 6 PRO HB3 H 1.853 0.000 2 22 111 6 PRO HD2 H 3.791 0.000 2 23 111 6 PRO HD3 H 3.791 0.000 2 24 111 6 PRO HG2 H 1.980 0.000 2 25 111 6 PRO HG3 H 1.979 0.000 2 26 112 7 ALA H H 7.813 0.000 1 27 112 7 ALA HB H 1.041 0.000 1 28 113 8 ARG H H 7.451 0.000 1 29 113 8 ARG HA H 3.868 0.002 1 30 113 8 ARG HB2 H 1.675 0.001 2 31 113 8 ARG HB3 H 1.483 0.000 2 32 113 8 ARG HD2 H 3.091 0.000 2 33 113 8 ARG HE H 6.874 0.000 1 34 113 8 ARG HG2 H 1.423 0.000 2 35 113 8 ARG HG3 H 1.420 0.000 2 36 114 9 TYR H H 8.001 0.000 1 37 114 9 TYR HA H 4.226 0.001 1 38 114 9 TYR HB2 H 3.030 0.000 2 39 114 9 TYR HB3 H 3.030 0.000 2 40 114 9 TYR HD1 H 6.954 0.000 3 41 114 9 TYR HD2 H 6.954 0.000 3 42 114 9 TYR HE1 H 6.781 0.000 3 43 114 9 TYR HE2 H 6.781 0.000 3 44 115 10 CYS H H 8.655 0.000 1 45 115 10 CYS HA H 4.407 0.000 1 46 115 10 CYS HB2 H 3.224 0.002 2 47 115 10 CYS HB3 H 2.832 0.002 2 48 116 11 CYS H H 7.488 0.000 1 49 116 11 CYS HA H 4.397 0.000 1 50 116 11 CYS HB2 H 3.506 0.003 2 51 116 11 CYS HB3 H 2.768 0.003 2 52 117 12 LEU H H 8.051 0.000 1 53 117 12 LEU HA H 4.125 0.002 1 54 117 12 LEU HB2 H 1.643 0.005 2 55 117 12 LEU HB3 H 1.459 0.004 2 56 117 12 LEU HD1 H 0.804 0.000 2 57 117 12 LEU HD2 H 0.788 0.000 2 58 117 12 LEU HG H 1.643 0.002 1 59 118 13 SER H H 8.110 0.000 1 60 118 13 SER HA H 4.476 0.001 1 61 118 13 SER HB2 H 3.526 0.000 2 62 118 13 SER HB3 H 3.150 0.000 2 63 119 14 GLY H H 7.117 0.000 1 64 119 14 GLY HA2 H 4.230 0.002 2 65 119 14 GLY HA3 H 3.909 0.002 2 66 120 15 CYS H H 8.793 0.000 1 67 120 15 CYS HA H 5.185 0.001 1 68 120 15 CYS HB2 H 3.712 0.001 2 69 120 15 CYS HB3 H 2.584 0.000 2 70 121 16 THR H H 9.692 0.000 1 71 121 16 THR HA H 4.869 0.001 1 72 121 16 THR HB H 4.731 0.003 1 73 121 16 THR HG2 H 1.127 0.002 1 74 122 17 GLN H H 8.990 0.000 1 75 122 17 GLN HA H 3.920 0.002 1 76 122 17 GLN HB2 H 2.133 0.005 2 77 122 17 GLN HB3 H 2.079 0.000 2 78 122 17 GLN HE21 H 7.420 0.000 2 79 122 17 GLN HE22 H 6.675 0.000 2 80 122 17 GLN HG2 H 2.396 0.001 2 81 122 17 GLN HG3 H 2.297 0.000 2 82 123 18 GLN H H 8.151 0.000 1 83 123 18 GLN HA H 3.929 0.002 1 84 123 18 GLN HB2 H 2.053 0.001 2 85 123 18 GLN HB3 H 1.966 0.005 2 86 123 18 GLN HE21 H 7.500 0.000 2 87 123 18 GLN HE22 H 6.789 0.000 2 88 123 18 GLN HG2 H 2.411 0.001 2 89 123 18 GLN HG3 H 2.364 0.002 2 90 124 19 ASP H H 7.740 0.000 1 91 124 19 ASP HA H 4.333 0.001 1 92 124 19 ASP HB2 H 3.195 0.001 2 93 124 19 ASP HB3 H 2.785 0.004 2 94 125 20 LEU H H 7.668 0.000 1 95 125 20 LEU HA H 3.959 0.002 1 96 125 20 LEU HB2 H 2.015 0.002 2 97 125 20 LEU HB3 H 1.226 0.003 2 98 125 20 LEU HD1 H 0.768 0.001 2 99 125 20 LEU HD2 H 0.710 0.001 2 100 125 20 LEU HG H 1.834 0.003 1 101 126 21 LEU H H 7.911 0.000 1 102 126 21 LEU HA H 4.184 0.002 1 103 126 21 LEU HB2 H 1.734 0.001 2 104 126 21 LEU HB3 H 1.528 0.001 2 105 126 21 LEU HD1 H 0.835 0.000 2 106 126 21 LEU HD2 H 0.835 0.000 2 107 126 21 LEU HG H 1.633 0.000 1 108 127 22 THR H H 7.464 0.000 1 109 127 22 THR HA H 4.104 0.001 1 110 127 22 THR HB H 4.315 0.000 1 111 127 22 THR HG2 H 1.373 0.000 1 112 128 23 LEU H H 7.763 0.000 1 113 128 23 LEU HA H 4.369 0.001 1 114 128 23 LEU HB2 H 2.117 0.002 2 115 128 23 LEU HB3 H 1.618 0.000 2 116 128 23 LEU HD1 H 1.040 0.002 2 117 128 23 LEU HD2 H 0.860 0.006 2 118 128 23 LEU HG H 1.904 0.002 1 119 129 24 CYS H H 7.367 0.000 1 120 129 24 CYS HA H 4.717 0.000 1 121 129 24 CYS HB2 H 2.968 0.003 2 122 129 24 CYS HB3 H 2.792 0.000 2 123 130 25 PRO HA H 4.344 0.001 1 124 130 25 PRO HB2 H 1.989 0.002 2 125 130 25 PRO HB3 H 1.829 0.000 2 126 130 25 PRO HD2 H 3.505 0.000 2 127 130 25 PRO HD3 H 3.324 0.003 2 128 130 25 PRO HG2 H 1.642 0.002 2 129 130 25 PRO HG3 H 1.646 0.000 2 130 131 26 TYR H H 7.462 0.000 1 131 131 26 TYR HA H 4.299 0.000 1 132 131 26 TYR HB2 H 2.984 0.001 2 133 131 26 TYR HB3 H 2.828 0.001 2 134 131 26 TYR HD1 H 6.984 0.000 3 135 131 26 TYR HD2 H 6.984 0.000 3 136 131 26 TYR HE1 H 6.704 0.000 3 137 131 26 TYR HE2 H 6.704 0.000 3 stop_ save_ save_1H-1H_D2O_noesy_308K_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_D2O stop_ _Sample_conditions_label $1.2_mM_RLF_100%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B _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 26 2 THR H H 8.558 0.000 1 2 26 2 THR HA H 4.615 0.000 1 3 26 2 THR HB H 4.165 0.000 1 4 26 2 THR HG2 H 1.240 0.001 1 5 27 3 PRO HA H 4.380 0.001 1 6 27 3 PRO HB2 H 2.272 0.003 2 7 27 3 PRO HB3 H 1.871 0.003 2 8 27 3 PRO HD2 H 3.811 0.003 2 9 27 3 PRO HD3 H 3.707 0.002 2 10 28 4 GLU H H 8.397 0.000 1 11 28 4 GLU HA H 4.252 0.002 1 12 28 4 GLU HB2 H 2.020 0.004 2 13 28 4 GLU HB3 H 1.917 0.002 2 14 28 4 GLU HG2 H 2.293 0.001 2 15 28 4 GLU HG3 H 2.256 0.000 2 16 29 5 MET H H 8.325 0.000 1 17 29 5 MET HA H 4.391 0.001 1 18 29 5 MET HB2 H 2.009 0.000 2 19 29 5 MET HB3 H 1.975 0.000 2 20 29 5 MET HG2 H 2.536 0.000 2 21 29 5 MET HG3 H 2.481 0.000 2 22 30 6 ARG H H 8.382 0.000 1 23 30 6 ARG HA H 3.999 0.001 1 24 30 6 ARG HB2 H 1.547 0.002 2 25 30 6 ARG HB3 H 1.467 0.002 2 26 30 6 ARG HD2 H 3.075 0.003 2 27 30 6 ARG HD3 H 3.030 0.001 2 28 30 6 ARG HE H 7.075 0.000 1 29 30 6 ARG HG2 H 1.356 0.001 2 30 30 6 ARG HG3 H 1.263 0.002 2 31 31 7 GLU H H 7.982 0.000 1 32 31 7 GLU HA H 4.496 0.001 1 33 31 7 GLU HB2 H 1.875 0.003 2 34 31 7 GLU HB3 H 1.821 0.001 2 35 31 7 GLU HG2 H 2.186 0.001 2 36 31 7 GLU HG3 H 2.106 0.005 2 37 32 8 LYS H H 8.663 0.000 1 38 32 8 LYS HA H 4.566 0.002 1 39 32 8 LYS HB2 H 1.916 0.001 2 40 32 8 LYS HB3 H 1.712 0.001 2 41 32 8 LYS HD2 H 1.573 0.000 2 42 32 8 LYS HD3 H 1.553 0.000 2 43 32 8 LYS HE2 H 2.830 0.001 2 44 32 8 LYS HE3 H 2.833 0.000 2 45 32 8 LYS HG2 H 1.418 0.002 2 46 32 8 LYS HG3 H 1.015 0.001 2 47 33 9 LEU H H 7.904 0.000 1 48 33 9 LEU HA H 4.457 0.002 1 49 33 9 LEU HB2 H 1.816 0.003 2 50 33 9 LEU HB3 H 0.909 0.002 2 51 33 9 LEU HD1 H 0.906 0.003 2 52 33 9 LEU HD2 H 0.648 0.003 2 53 33 9 LEU HG H 1.566 0.002 1 54 34 10 CYS H H 8.596 0.000 1 55 34 10 CYS HA H 4.927 0.001 1 56 34 10 CYS HB2 H 3.235 0.002 2 57 34 10 CYS HB3 H 2.958 0.000 2 58 35 11 GLY H H 9.018 0.000 1 59 35 11 GLY HA2 H 3.945 0.000 2 60 35 11 GLY HA3 H 3.719 0.000 2 61 36 12 HIS H H 7.822 0.000 1 62 36 12 HIS HA H 4.305 0.001 1 63 36 12 HIS HB2 H 3.072 0.000 2 64 36 12 HIS HB3 H 3.074 0.000 2 65 36 12 HIS HD2 H 6.998 0.000 1 66 36 12 HIS HE1 H 8.111 0.000 1 67 37 13 HIS H H 7.927 0.000 1 68 37 13 HIS HA H 4.260 0.001 1 69 37 13 HIS HB2 H 3.466 0.002 2 70 37 13 HIS HB3 H 3.215 0.001 2 71 37 13 HIS HD2 H 7.220 0.000 1 72 37 13 HIS HE1 H 8.227 0.000 1 73 38 14 PHE H H 7.050 0.000 1 74 38 14 PHE HA H 4.045 0.002 1 75 38 14 PHE HB2 H 3.086 0.006 2 76 38 14 PHE HB3 H 2.918 0.002 2 77 38 14 PHE HD1 H 6.966 0.000 3 78 38 14 PHE HD2 H 6.966 0.000 3 79 38 14 PHE HE1 H 7.140 0.000 3 80 38 14 PHE HE2 H 7.140 0.000 3 81 39 15 VAL H H 6.992 0.000 1 82 39 15 VAL HA H 3.104 0.001 1 83 39 15 VAL HB H 2.004 0.002 1 84 39 15 VAL HG1 H 1.031 0.000 2 85 39 15 VAL HG2 H 0.801 0.000 2 86 40 16 ARG H H 7.821 0.000 1 87 40 16 ARG HA H 3.744 0.002 1 88 40 16 ARG HB2 H 1.733 0.000 2 89 40 16 ARG HB3 H 1.733 0.000 2 90 40 16 ARG HD2 H 3.059 0.001 2 91 40 16 ARG HD3 H 3.032 0.002 2 92 40 16 ARG HG2 H 1.636 0.003 2 93 40 16 ARG HG3 H 1.463 0.000 2 94 41 17 ALA H H 7.418 0.000 1 95 41 17 ALA HA H 3.973 0.002 1 96 41 17 ALA HB H 1.345 0.001 1 97 42 18 LEU H H 7.764 0.000 1 98 42 18 LEU HA H 3.711 0.001 1 99 42 18 LEU HB2 H 1.398 0.001 2 100 42 18 LEU HB3 H 0.935 0.004 2 101 42 18 LEU HD1 H 0.654 0.000 2 102 42 18 LEU HD2 H 0.657 0.001 2 103 42 18 LEU HG H 1.215 0.002 1 104 43 19 VAL H H 7.954 0.000 1 105 43 19 VAL HA H 3.288 0.002 1 106 43 19 VAL HB H 1.967 0.001 1 107 43 19 VAL HG1 H 0.829 0.001 2 108 43 19 VAL HG2 H 0.712 0.002 2 109 44 20 ARG H H 7.425 0.000 1 110 44 20 ARG HA H 3.933 0.001 1 111 44 20 ARG HB2 H 1.927 0.002 2 112 44 20 ARG HB3 H 1.826 0.001 2 113 44 20 ARG HD2 H 3.168 0.002 2 114 44 20 ARG HD3 H 3.094 0.003 2 115 44 20 ARG HE H 7.187 0.000 1 116 44 20 ARG HG2 H 1.624 0.003 2 117 44 20 ARG HG3 H 1.482 0.002 2 118 45 21 VAL H H 8.065 0.000 1 119 45 21 VAL HA H 3.846 0.001 1 120 45 21 VAL HB H 2.012 0.002 1 121 45 21 VAL HG1 H 1.037 0.001 2 122 45 21 VAL HG2 H 0.903 0.001 2 123 46 22 CYS H H 8.488 0.000 1 124 46 22 CYS HA H 4.714 0.002 1 125 46 22 CYS HB2 H 3.048 0.003 2 126 46 22 CYS HB3 H 2.686 0.001 2 127 47 23 GLY H H 7.747 0.000 1 128 47 23 GLY HA2 H 3.909 0.000 2 129 47 23 GLY HA3 H 3.836 0.000 2 130 48 24 GLY H H 7.988 0.000 1 131 48 24 GLY HA2 H 4.089 0.001 2 132 48 24 GLY HA3 H 3.944 0.001 2 133 49 25 PRO HA H 4.269 0.002 1 134 49 25 PRO HB2 H 2.064 0.003 2 135 49 25 PRO HB3 H 1.652 0.001 2 136 49 25 PRO HD2 H 3.559 0.001 2 137 49 25 PRO HD3 H 3.478 0.003 2 138 49 25 PRO HG2 H 1.872 0.001 2 139 49 25 PRO HG3 H 1.845 0.001 2 140 50 26 ARG HA H 4.150 0.001 1 141 50 26 ARG HB2 H 1.629 0.001 2 142 50 26 ARG HB3 H 1.560 0.002 2 143 50 26 ARG HD2 H 2.994 0.000 2 144 50 26 ARG HD3 H 2.994 0.000 2 145 50 26 ARG HG2 H 1.357 0.001 2 146 51 27 TRP H H 7.583 0.000 1 147 51 27 TRP HA H 4.573 0.002 1 148 51 27 TRP HB2 H 3.245 0.002 2 149 51 27 TRP HB3 H 3.131 0.001 2 150 51 27 TRP HD1 H 7.165 0.000 1 151 51 27 TRP HE1 H 9.931 0.000 1 152 51 27 TRP HE3 H 7.447 0.000 1 153 51 27 TRP HH2 H 7.014 0.000 1 154 51 27 TRP HZ2 H 7.311 0.000 1 155 51 27 TRP HZ3 H 6.950 0.000 1 156 52 28 SER HA H 4.322 0.002 1 157 52 28 SER HB2 H 3.743 0.001 2 158 52 28 SER HB3 H 3.560 0.003 2 159 53 29 THR HA H 4.273 0.003 1 160 53 29 THR HB H 4.224 0.000 1 161 53 29 THR HG2 H 1.125 0.002 1 162 54 30 GLU HA H 4.262 0.004 1 163 54 30 GLU HB2 H 2.025 0.000 2 164 54 30 GLU HB3 H 1.850 0.000 2 165 54 30 GLU HG2 H 2.237 0.001 2 166 55 31 ALA HA H 4.044 0.000 1 167 55 31 ALA HB H 1.260 0.000 1 stop_ save_ save_1H-13C_HSQC_308K_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $RLF_D2O stop_ _Sample_conditions_label $1.2_mM_RLF_100%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A _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 1 106 1 ALA HA H 4.025 0.000 1 2 106 1 ALA HB H 1.480 0.000 1 3 106 1 ALA CA C 51.583 0.000 1 4 106 1 ALA CB C 19.169 0.000 1 5 107 2 ALA HA H 4.237 0.000 1 6 107 2 ALA HB H 1.312 0.000 1 7 107 2 ALA CA C 52.317 0.000 1 8 107 2 ALA CB C 19.095 0.000 1 9 108 3 ALA HA H 4.274 0.000 1 10 108 3 ALA HB H 1.293 0.000 1 11 108 3 ALA CA C 52.239 0.000 1 12 108 3 ALA CB C 19.108 0.000 1 13 109 4 THR HA H 4.231 0.000 1 14 109 4 THR HB H 4.128 0.000 1 15 109 4 THR HG2 H 1.149 0.000 1 16 109 4 THR CA C 61.832 0.000 1 17 109 4 THR CB C 69.551 0.000 1 18 109 4 THR CG2 C 21.544 0.000 1 19 110 5 ASN HA H 4.921 0.000 1 20 110 5 ASN CA C 51.202 0.000 1 21 111 6 PRO HA H 4.113 0.000 1 22 111 6 PRO CA C 64.838 0.000 1 23 112 7 ALA HB H 1.054 0.000 1 24 112 7 ALA CB C 18.160 0.000 1 25 113 8 ARG HA H 3.891 0.000 1 26 113 8 ARG CA C 58.119 0.000 1 27 117 12 LEU HA H 4.136 0.000 1 28 117 12 LEU CA C 56.937 0.000 1 29 120 15 CYS HA H 5.174 0.000 1 30 120 15 CYS CA C 53.484 0.000 1 31 121 16 THR HA H 4.857 0.000 1 32 121 16 THR CA C 59.930 0.000 1 33 122 17 GLN HA H 3.926 0.000 1 34 122 17 GLN CA C 59.899 0.000 1 35 123 18 GLN HA H 3.947 0.000 1 36 123 18 GLN CA C 59.088 0.000 1 37 125 20 LEU HA H 3.961 0.000 1 38 125 20 LEU CA C 57.794 0.000 1 39 126 21 LEU HA H 4.189 0.000 1 40 126 21 LEU CA C 57.271 0.000 1 41 127 22 THR HA H 4.120 0.000 1 42 127 22 THR HB H 4.319 0.000 1 43 127 22 THR HG2 H 1.385 0.000 1 44 127 22 THR CA C 64.242 0.000 1 45 127 22 THR CB C 69.301 0.000 1 46 127 22 THR CG2 C 21.600 0.000 1 47 130 25 PRO HA H 4.359 0.000 1 48 130 25 PRO CA C 63.272 0.000 1 49 131 26 TYR HA H 4.318 0.000 1 50 131 26 TYR CA C 58.821 0.000 1 stop_ save_ save_1H-13C_HSQC_308K_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $RLF_D2O stop_ _Sample_conditions_label $1.2_mM_RLF_100%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B _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 26 2 THR HB H 4.187 0.000 1 2 26 2 THR HG2 H 1.255 0.000 1 3 26 2 THR CB C 69.388 0.000 1 4 26 2 THR CG2 C 21.488 0.000 1 5 27 3 PRO HA H 4.389 0.000 1 6 27 3 PRO CA C 63.394 0.000 1 7 29 5 MET HA H 4.396 0.000 1 8 29 5 MET CA C 55.279 0.000 1 9 30 6 ARG HA H 4.020 0.000 1 10 30 6 ARG CA C 55.773 0.000 1 11 36 12 HIS HA H 4.325 0.000 1 12 36 12 HIS CA C 58.351 0.000 1 13 37 13 HIS HA H 4.266 0.000 1 14 37 13 HIS CA C 58.345 0.000 1 15 38 14 PHE HA H 4.044 0.000 1 16 38 14 PHE CA C 61.270 0.000 1 17 39 15 VAL HA H 3.129 0.000 1 18 39 15 VAL CA C 66.501 0.000 1 19 40 16 ARG HA H 3.758 0.000 1 20 40 16 ARG CA C 59.198 0.000 1 21 41 17 ALA HA H 3.986 0.000 1 22 41 17 ALA HB H 1.353 0.000 1 23 41 17 ALA CA C 54.830 0.000 1 24 41 17 ALA CB C 19.144 0.000 1 25 42 18 LEU HA H 3.718 0.000 1 26 42 18 LEU CA C 57.724 0.000 1 27 43 19 VAL HA H 3.322 0.000 1 28 43 19 VAL CA C 66.247 0.000 1 29 44 20 ARG HA H 3.935 0.000 1 30 44 20 ARG CA C 59.116 0.000 1 31 45 21 VAL HA H 3.860 0.000 1 32 45 21 VAL CA C 65.081 0.000 1 33 49 25 PRO HA H 4.284 0.000 1 34 49 25 PRO CA C 63.480 0.000 1 35 50 26 ARG HA H 4.157 0.000 1 36 50 26 ARG CA C 56.197 0.000 1 37 52 28 SER HA H 4.342 0.000 1 38 52 28 SER CA C 58.332 0.000 1 39 53 29 THR HA H 4.292 0.000 1 40 53 29 THR CA C 61.815 0.000 1 41 54 30 GLU HA H 4.271 0.000 1 42 54 30 GLU CA C 56.259 0.000 1 43 55 31 ALA HA H 4.062 0.000 1 44 55 31 ALA HB H 1.277 0.000 1 45 55 31 ALA CA C 53.645 0.000 1 46 55 31 ALA CB C 20.069 0.000 1 stop_ save_ save_1H-15N_HSQC_noesy_308K_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label $RLF_H2O stop_ _Sample_conditions_label $1.2_mM_RLF_92%_H2O_8%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A _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 1 107 2 ALA H H 8.476 0.000 1 2 107 2 ALA N N 123.655 0.000 1 3 112 7 ALA H H 7.947 0.000 1 4 112 7 ALA HB H 1.077 0.000 1 5 112 7 ALA N N 119.372 0.002 1 6 118 13 SER H H 8.156 0.000 1 7 119 14 GLY H H 7.194 0.000 1 8 119 14 GLY N N 109.053 0.004 1 stop_ save_ save_1H-15N_HSQC_noesy_308K_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label $RLF_H2O stop_ _Sample_conditions_label $1.2_mM_RLF_92%_H2O_8%_D2O-308K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B _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 46 22 CYS H H 8.482 0.000 1 2 47 23 GLY H H 7.883 0.000 1 3 47 23 GLY HA2 H 3.901 0.000 2 4 47 23 GLY HA3 H 3.983 0.000 2 5 47 23 GLY N N 108.185 0.035 1 6 48 24 GLY H H 7.877 0.000 1 7 48 24 GLY N N 108.286 0.009 1 stop_ save_