data_16968 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; The Solution Structure of a Conformationally Restricted Fully Active Derivative of the Human Relaxin-like Factor (RLF) ; _BMRB_accession_number 16968 _BMRB_flat_file_name bmr16968.str _Entry_type new _Submission_date 2010-06-01 _Accession_date 2010-06-01 _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 E. . 7 Led Jens J. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 6 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 509 "13C chemical shifts" 58 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2010-06-22 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'The Solution Structure of a Conformationally Restricted Fully Active Derivative of the Human Relaxin-like Factor (RLF)' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 19086273 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_ _Journal_abbreviation Biochemistry _Journal_volume 47 _Journal_issue 50 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 13308 _Page_last 13317 _Year 2008 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Derivative of HRF' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label RLF-A_crosslinked $RLF-A_crosslinked RLF-B_crosslinked $RLF-B_crosslinked 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_crosslinked _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common RLF-A_crosslinked _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 27 _Mol_residue_sequence ; AAATNPARYCCLSGCTQQDL LTLCPYG ; 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 27 132 GLY 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 16901 RLF-A 96.30 26 100.00 100.00 1.56e-08 PDB 2H8B "Solution Structure Of Insl3" 92.59 26 100.00 100.00 1.27e-07 PDB 2K6T "Solution Structure Of The Relaxin-Like Factor" 92.59 26 100.00 100.00 1.27e-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 2.18e-09 DBJ BAG63984 "unnamed protein product [Homo sapiens]" 96.30 131 100.00 100.00 1.03e-08 EMBL CAA52017 "Leydig insulin-like hormone [Homo sapiens]" 96.30 101 100.00 100.00 1.00e-08 GB AAB31371 "Ley I-L [Homo sapiens]" 96.30 131 100.00 100.00 1.03e-08 GB AAH32810 "Similar to insulin-like 3 (Leydig cell), partial [Homo sapiens]" 96.30 130 100.00 100.00 1.10e-08 GB AAH53345 "INSL3 protein, partial [Homo sapiens]" 96.30 130 100.00 100.00 1.06e-08 GB AAH71706 "Insulin-like 3 (Leydig cell) [Homo sapiens]" 96.30 131 100.00 100.00 1.03e-08 GB AAI06722 "Insulin-like 3 (Leydig cell) [Homo sapiens]" 96.30 131 100.00 100.00 1.03e-08 REF NP_001171286 "tyrosine-protein kinase JAK3 precursor [Pan troglodytes]" 96.30 131 100.00 100.00 9.29e-09 REF NP_005534 "insulin-like 3 isoform 2 precursor [Homo sapiens]" 96.30 131 100.00 100.00 1.07e-08 REF XP_003275863 "PREDICTED: insulin-like 3 isoform X2 [Nomascus leucogenys]" 96.30 131 100.00 100.00 1.02e-08 REF XP_003915200 "PREDICTED: insulin-like 3 [Papio anubis]" 96.30 131 100.00 100.00 1.05e-08 REF XP_007993939 "PREDICTED: insulin-like 3 [Chlorocebus sabaeus]" 96.30 131 100.00 100.00 1.06e-08 SP P51460 "RecName: Full=Insulin-like 3; AltName: Full=Leydig insulin-like peptide; Short=Ley-I-L; AltName: Full=Relaxin-like factor; Cont" 96.30 131 100.00 100.00 1.07e-08 SP Q5CZK3 "RecName: Full=Insulin-like 3; AltName: Full=Leydig insulin-like peptide; Short=Ley-I-L; AltName: Full=Relaxin-like factor; Cont" 96.30 131 100.00 100.00 9.57e-09 stop_ save_ save_RLF-B_crosslinked _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common RLF-B_crosslinked _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . _Residue_count 27 _Mol_residue_sequence ; PTPEMREKLCGHHFVRALVR VCGGPKW ; 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 LYS 27 51 TRP stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-10 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 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 1.45e-10 stop_ save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bonds _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single disulfide RLF-A_crosslinked 10 CYS SG RLF-A_crosslinked 15 CYS SG single disulfide RLF-A_crosslinked 11 CYS SG RLF-A_crosslinked 10 CYS SG single disulfide RLF-A_crosslinked 24 CYS SG RLF-A_crosslinked 22 CYS SG stop_ 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_crosslinked Human 9606 Eukaryota Metazoa Homo sapiens 'A chain of human RLF C-terminally extended by Gly cross-linked through the C-terminus to the 6-amino group of Lys(50)' $RLF-B_crosslinked Human 9606 Eukaryota Metazoa Homo sapiens 'B chain of human RLF cross-linked through the 6-amino group of Lys(B50) to the carboxyl group of Gly(132) at the terminus of the A chain' 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_crosslinked 'chemical synthesis' . . . . . 'modified human proRLF sequence 106-131' $RLF-B_crosslinked 'chemical synthesis' . . . . . 'modified human proRLF sequence 25-51' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_RLF_crosslinked_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 _Isotopic_labeling $RLF-A_crosslinked 1.2 mM 'natural abundance' $RLF-B_crosslinked 1.2 mM 'natural abundance' 'sodium acetate' 1.2 mM 'natural abundance' Na-d4-acetate/NaOD 40 mM 'natural abundance' H2O 92 % 'natural abundance' D2O 8 % 'natural abundance' stop_ save_ save_RLF_crosslinked_D2O _Saveframe_category sample _Sample_type solution _Details '40 mM Na-d4-acetate/NaOD pH* 5.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $RLF-A_crosslinked 1.2 mM 'natural abundance' $RLF-B_crosslinked 1.2 mM 'natural abundance' 'sodium acetate' 1.2 mM 'natural abundance' Na-d4-acetate/NaOD 40 mM 'natural abundance' D2O 100 % '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 2.1 loop_ _Vendor _Address _Electronic_address 'Linge, O'Donoghue and Nilges' ; Institute Pasteur Unit de Bioinformatique Structurale 25-28 rue du Dr Roux F-75724 Paris CEDEX 15 ; . stop_ loop_ _Task 'structure solution' 'NOE assignment' stop_ _Details 'Ambiguous restraints for interactive assignment' save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3.110 loop_ _Vendor _Address _Electronic_address Goddard 'University of Califormia San Francisco' . stop_ loop_ _Task 'peak picking' 'chemical shift assignment' 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 . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $RLF_crosslinked_D2O save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $RLF_crosslinked_D2O save_ save_2D_1H-1H_TOCSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $RLF_crosslinked_D2O save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $RLF_crosslinked_D2O save_ save_2D_1H-1H_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_crosslinked_D2O save_ save_2D_1H-1H_TOCSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $RLF_crosslinked_H2O save_ save_2D_1H-1H_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $RLF_crosslinked_H2O save_ ####################### # Sample conditions # ####################### save_RLF_crosslinked_H2O_308 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 308 . K pH 5.0 0.1 pH 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 H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_crosslinked_D2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B_crosslinked _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 4.189 0.000 1 2 27 3 PRO HA H 4.406 0.000 1 3 27 3 PRO HB2 H 2.296 0.001 2 4 27 3 PRO HB3 H 1.891 0.000 2 5 27 3 PRO HD2 H 3.836 0.000 2 6 27 3 PRO HD3 H 3.732 0.003 2 7 28 4 GLU HA H 4.272 0.000 1 8 28 4 GLU HB2 H 2.034 0.002 2 9 28 4 GLU HB3 H 1.943 0.000 2 10 29 5 MET HA H 4.409 0.000 1 11 30 6 ARG HA H 4.015 0.002 1 12 30 6 ARG HB2 H 1.557 0.002 2 13 30 6 ARG HB3 H 1.470 0.000 2 14 30 6 ARG HD2 H 3.091 0.000 2 15 30 6 ARG HD3 H 3.050 0.000 2 16 30 6 ARG HG2 H 1.362 0.000 2 17 30 6 ARG HG3 H 1.269 0.003 2 18 31 7 GLU HA H 4.502 0.000 1 19 31 7 GLU HB2 H 1.876 0.000 2 20 32 8 LYS HA H 4.582 0.001 1 21 32 8 LYS HB2 H 1.943 0.000 2 22 32 8 LYS HB3 H 1.724 0.000 2 23 32 8 LYS HD2 H 1.603 0.000 2 24 32 8 LYS HD3 H 1.576 0.000 2 25 32 8 LYS HE2 H 2.833 0.000 2 26 32 8 LYS HE3 H 2.833 0.000 2 27 32 8 LYS HG2 H 1.411 0.002 2 28 32 8 LYS HG3 H 0.988 0.003 2 29 33 9 LEU HA H 4.497 0.002 1 30 33 9 LEU HB2 H 1.807 0.003 2 31 33 9 LEU HB3 H 0.933 0.000 2 32 33 9 LEU HD2 H 0.694 0.002 2 33 33 9 LEU HG H 1.575 0.000 1 34 34 10 CYS HA H 4.937 0.002 1 35 34 10 CYS HB2 H 3.248 0.000 2 36 34 10 CYS HB3 H 2.987 0.000 2 37 35 11 GLY HA2 H 3.991 0.000 2 38 35 11 GLY HA3 H 3.757 0.000 2 39 36 12 HIS HA H 4.384 0.002 1 40 36 12 HIS HB2 H 3.137 0.000 2 41 37 13 HIS HA H 4.255 0.001 1 42 37 13 HIS HB2 H 3.419 0.002 2 43 37 13 HIS HB3 H 3.181 0.002 2 44 38 14 PHE HA H 4.097 0.005 1 45 38 14 PHE HB2 H 3.075 0.004 2 46 38 14 PHE HB3 H 2.925 0.003 2 47 39 15 VAL HA H 3.128 0.001 1 48 39 15 VAL HB H 1.978 0.000 1 49 39 15 VAL HG1 H 1.008 0.000 2 50 39 15 VAL HG2 H 0.834 0.000 2 51 40 16 ARG HA H 3.779 0.000 1 52 40 16 ARG HB3 H 1.672 0.000 2 53 40 16 ARG HD2 H 3.128 0.000 2 54 40 16 ARG HD3 H 3.129 0.000 2 55 41 17 ALA HA H 4.010 0.001 1 56 41 17 ALA HB H 1.392 0.002 1 57 42 18 LEU HA H 3.743 0.002 1 58 42 18 LEU HB2 H 1.250 0.002 2 59 42 18 LEU HB3 H 1.074 0.005 2 60 42 18 LEU HD1 H 0.646 0.002 2 61 42 18 LEU HD2 H 0.537 0.001 2 62 42 18 LEU HG H 1.178 0.002 1 63 43 19 VAL HA H 3.352 0.000 1 64 43 19 VAL HB H 1.941 0.001 1 65 43 19 VAL HG1 H 0.786 0.000 2 66 43 19 VAL HG2 H 0.757 0.000 2 67 44 20 ARG HA H 3.982 0.001 1 68 44 20 ARG HB2 H 1.982 0.000 2 69 44 20 ARG HB3 H 1.859 0.000 2 70 44 20 ARG HD2 H 3.230 0.000 2 71 44 20 ARG HD3 H 3.137 0.000 2 72 45 21 VAL HA H 3.855 0.000 1 73 45 21 VAL HB H 2.023 0.000 1 74 45 21 VAL HG1 H 1.052 0.001 2 75 45 21 VAL HG2 H 0.915 0.002 2 76 47 23 GLY HA2 H 4.053 0.000 2 77 47 23 GLY HA3 H 3.909 0.000 2 78 48 24 GLY HA2 H 4.167 0.003 2 79 48 24 GLY HA3 H 4.005 0.005 2 80 49 25 PRO HA H 4.313 0.001 1 81 49 25 PRO HB2 H 2.121 0.000 2 82 49 25 PRO HB3 H 1.747 0.000 2 83 49 25 PRO HD2 H 3.629 0.002 2 84 49 25 PRO HD3 H 3.548 0.001 2 85 49 25 PRO HG2 H 1.909 0.000 2 86 50 26 LYS HA H 3.993 0.000 1 87 50 26 LYS HB3 H 1.370 0.000 2 88 50 26 LYS HE3 H 2.935 0.000 2 89 51 27 TRP HB2 H 3.346 0.000 2 90 51 27 TRP HB3 H 3.085 0.000 2 stop_ save_ save_assigned_chem_shift_list_1_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_crosslinked_D2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A_crosslinked _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 4.029 0.000 1 2 106 1 ALA HB H 1.482 0.000 1 3 107 2 ALA HA H 4.221 0.000 1 4 107 2 ALA HB H 1.317 0.000 1 5 108 3 ALA HA H 4.248 0.000 1 6 108 3 ALA HB H 1.281 0.000 1 7 109 4 THR HA H 4.224 0.001 1 8 109 4 THR HB H 4.116 0.001 1 9 109 4 THR HG2 H 1.156 0.000 1 10 110 5 ASN HA H 4.921 0.003 1 11 110 5 ASN HB2 H 2.930 0.000 2 12 111 6 PRO HA H 4.110 0.002 1 13 111 6 PRO HB2 H 2.356 0.003 2 14 111 6 PRO HB3 H 1.914 0.002 2 15 111 6 PRO HD2 H 3.830 0.000 2 16 111 6 PRO HD3 H 3.761 0.000 2 17 111 6 PRO HG2 H 2.018 0.004 2 18 112 7 ALA HB H 1.045 0.000 1 19 113 8 ARG HA H 3.889 0.002 1 20 113 8 ARG HB2 H 1.767 0.000 2 21 113 8 ARG HB3 H 1.688 0.000 2 22 113 8 ARG HG2 H 1.551 0.000 2 23 113 8 ARG HG3 H 1.466 0.000 2 24 114 9 TYR HA H 4.191 0.000 1 25 114 9 TYR HB2 H 3.057 0.000 2 26 114 9 TYR HB3 H 2.969 0.000 2 27 116 11 CYS HA H 4.397 0.000 1 28 116 11 CYS HB2 H 3.548 0.001 2 29 116 11 CYS HB3 H 2.753 0.001 2 30 117 12 LEU HA H 4.145 0.001 1 31 117 12 LEU HG H 1.630 0.000 1 32 118 13 SER HA H 4.466 0.001 1 33 118 13 SER HB2 H 3.495 0.000 2 34 118 13 SER HB3 H 3.079 0.002 2 35 119 14 GLY HA2 H 4.218 0.002 2 36 119 14 GLY HA3 H 3.890 0.002 2 37 120 15 CYS HA H 5.200 0.002 1 38 120 15 CYS HB2 H 3.710 0.001 2 39 120 15 CYS HB3 H 2.595 0.000 2 40 121 16 THR HA H 4.878 0.001 1 41 121 16 THR HB H 4.762 0.001 1 42 121 16 THR HG2 H 1.154 0.001 1 43 122 17 GLN HA H 3.954 0.004 1 44 122 17 GLN HB2 H 2.178 0.003 2 45 122 17 GLN HG2 H 2.412 0.006 2 46 122 17 GLN HG3 H 2.344 0.003 2 47 123 18 GLN HA H 3.963 0.001 1 48 124 19 ASP HA H 4.354 0.001 1 49 124 19 ASP HB2 H 3.212 0.004 2 50 124 19 ASP HB3 H 2.840 0.000 2 51 125 20 LEU HA H 3.970 0.001 1 52 125 20 LEU HB2 H 2.043 0.002 2 53 125 20 LEU HB3 H 1.239 0.001 2 54 125 20 LEU HD1 H 0.795 0.001 2 55 125 20 LEU HD2 H 0.736 0.002 2 56 125 20 LEU HG H 1.875 0.001 1 57 126 21 LEU HA H 4.256 0.000 1 58 126 21 LEU HB2 H 1.775 0.000 2 59 126 21 LEU HB3 H 1.555 0.000 2 60 127 22 THR HA H 4.155 0.000 1 61 127 22 THR HB H 4.374 0.000 1 62 127 22 THR HG2 H 1.401 0.000 1 63 128 23 LEU HA H 4.470 0.000 1 64 128 23 LEU HB2 H 2.147 0.002 2 65 128 23 LEU HB3 H 1.687 0.001 2 66 128 23 LEU HD1 H 1.076 0.001 2 67 128 23 LEU HD2 H 0.890 0.002 2 68 128 23 LEU HG H 1.984 0.000 1 69 129 24 CYS HA H 4.769 0.003 1 70 129 24 CYS HB2 H 3.127 0.000 2 71 129 24 CYS HB3 H 2.811 0.000 2 72 130 25 PRO HD2 H 3.760 0.003 2 73 130 25 PRO HD3 H 3.434 0.000 2 74 131 26 TYR HB2 H 3.076 0.000 2 75 131 26 TYR HB3 H 2.954 0.000 2 76 132 27 GLY HA2 H 3.814 0.000 2 77 132 27 GLY HA3 H 3.616 0.000 2 stop_ save_ save_assigned_chem_shift_list_2_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_crosslinked_H2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B_crosslinked _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 HB H 4.172 0.000 1 3 27 3 PRO HA H 4.387 0.000 1 4 27 3 PRO HB2 H 2.296 0.000 2 5 27 3 PRO HB3 H 1.891 0.000 2 6 27 3 PRO HD2 H 3.818 0.000 2 7 27 3 PRO HD3 H 3.711 0.000 2 8 28 4 GLU H H 8.397 0.001 1 9 28 4 GLU HA H 4.261 0.001 1 10 28 4 GLU HB2 H 2.019 0.000 2 11 28 4 GLU HB3 H 1.919 0.000 2 12 28 4 GLU HG2 H 2.295 0.000 2 13 28 4 GLU HG3 H 2.272 0.000 2 14 29 5 MET H H 8.325 0.001 1 15 29 5 MET HA H 4.398 0.003 1 16 29 5 MET HB2 H 2.009 0.000 2 17 29 5 MET HB3 H 1.988 0.003 2 18 29 5 MET HG2 H 2.538 0.001 2 19 29 5 MET HG3 H 2.487 0.003 2 20 30 6 ARG H H 8.382 0.001 1 21 30 6 ARG HA H 3.992 0.000 1 22 30 6 ARG HB2 H 1.539 0.000 2 23 30 6 ARG HB3 H 1.450 0.001 2 24 30 6 ARG HD2 H 3.091 0.000 2 25 30 6 ARG HD3 H 3.050 0.000 2 26 30 6 ARG HE H 7.075 0.000 1 27 30 6 ARG HG2 H 1.347 0.004 2 28 30 6 ARG HG3 H 1.253 0.002 2 29 31 7 GLU H H 7.982 0.005 1 30 31 7 GLU HA H 4.484 0.001 1 31 31 7 GLU HB2 H 1.861 0.004 2 32 31 7 GLU HB3 H 1.813 0.001 2 33 31 7 GLU HG2 H 2.193 0.000 2 34 31 7 GLU HG3 H 2.094 0.000 2 35 32 8 LYS H H 8.663 0.002 1 36 32 8 LYS HA H 4.555 0.000 1 37 32 8 LYS HB2 H 1.923 0.000 2 38 32 8 LYS HB3 H 1.707 0.000 2 39 32 8 LYS HD2 H 1.573 0.000 2 40 32 8 LYS HD3 H 1.553 0.000 2 41 32 8 LYS HE2 H 2.833 0.000 2 42 32 8 LYS HE3 H 2.833 0.000 2 43 32 8 LYS HG2 H 1.397 0.000 2 44 32 8 LYS HG3 H 0.970 0.000 2 45 33 9 LEU H H 7.904 0.002 1 46 33 9 LEU HA H 4.474 0.002 1 47 33 9 LEU HB2 H 1.790 0.003 2 48 33 9 LEU HB3 H 0.933 0.000 2 49 33 9 LEU HD1 H 0.909 0.002 2 50 33 9 LEU HD2 H 0.659 0.002 2 51 33 9 LEU HG H 1.551 0.000 1 52 34 10 CYS H H 8.596 0.001 1 53 34 10 CYS HA H 4.921 0.002 1 54 34 10 CYS HB2 H 3.238 0.000 2 55 34 10 CYS HB3 H 2.968 0.001 2 56 35 11 GLY H H 9.018 0.000 1 57 35 11 GLY HA2 H 3.972 0.000 2 58 35 11 GLY HA3 H 3.769 0.000 2 59 36 12 HIS H H 7.822 0.000 1 60 36 12 HIS HA H 4.384 0.003 1 61 36 12 HIS HB2 H 3.151 0.000 2 62 36 12 HIS HB3 H 3.109 0.000 2 63 36 12 HIS HD2 H 6.998 0.001 1 64 36 12 HIS HE1 H 8.111 0.001 1 65 37 13 HIS H H 7.927 0.002 1 66 37 13 HIS HA H 4.259 0.002 1 67 37 13 HIS HB2 H 3.436 0.001 2 68 37 13 HIS HB3 H 3.201 0.001 2 69 37 13 HIS HD2 H 7.220 0.003 1 70 37 13 HIS HE1 H 8.227 0.000 1 71 38 14 PHE H H 7.050 0.001 1 72 38 14 PHE HA H 4.070 0.003 1 73 38 14 PHE HB2 H 3.055 0.003 2 74 38 14 PHE HB3 H 2.908 0.002 2 75 38 14 PHE HD1 H 6.971 0.000 3 76 38 14 PHE HD2 H 6.971 0.000 3 77 38 14 PHE HE1 H 7.147 0.000 3 78 38 14 PHE HE2 H 7.147 0.000 3 79 39 15 VAL H H 6.992 0.000 1 80 39 15 VAL HA H 3.123 0.002 1 81 39 15 VAL HB H 1.978 0.000 1 82 39 15 VAL HG1 H 1.002 0.000 2 83 39 15 VAL HG2 H 0.843 0.013 2 84 40 16 ARG H H 7.821 0.001 1 85 40 16 ARG HA H 3.772 0.000 1 86 40 16 ARG HB3 H 1.672 0.000 2 87 40 16 ARG HD2 H 3.110 0.000 2 88 40 16 ARG HD3 H 3.111 0.000 2 89 41 17 ALA H H 7.418 0.002 1 90 41 17 ALA HA H 3.991 0.000 1 91 41 17 ALA HB H 1.367 0.001 1 92 42 18 LEU H H 7.764 0.002 1 93 42 18 LEU HA H 3.727 0.001 1 94 42 18 LEU HB2 H 1.247 0.000 2 95 42 18 LEU HB3 H 1.041 0.000 2 96 42 18 LEU HD1 H 0.626 0.001 2 97 42 18 LEU HD2 H 0.525 0.002 2 98 42 18 LEU HG H 1.160 0.000 1 99 43 19 VAL H H 7.954 0.002 1 100 43 19 VAL HA H 3.342 0.000 1 101 43 19 VAL HB H 1.918 0.000 1 102 43 19 VAL HG1 H 0.773 0.001 2 103 43 19 VAL HG2 H 0.745 0.003 2 104 44 20 ARG H H 7.425 0.001 1 105 44 20 ARG HA H 3.970 0.001 1 106 44 20 ARG HB2 H 1.954 0.002 2 107 44 20 ARG HB3 H 1.839 0.002 2 108 44 20 ARG HD2 H 3.215 0.000 2 109 44 20 ARG HD3 H 3.117 0.000 2 110 44 20 ARG HE H 7.187 0.002 1 111 44 20 ARG HG2 H 1.661 0.000 2 112 45 21 VAL H H 8.065 0.000 1 113 45 21 VAL HA H 3.840 0.002 1 114 45 21 VAL HB H 2.001 0.000 1 115 45 21 VAL HG1 H 1.027 0.004 2 116 45 21 VAL HG2 H 0.888 0.002 2 117 46 22 CYS H H 8.488 0.001 1 118 46 22 CYS HA H 4.631 0.000 1 119 46 22 CYS HB2 H 2.987 0.010 2 120 46 22 CYS HB3 H 2.752 0.003 2 121 47 23 GLY H H 7.747 0.000 1 122 47 23 GLY HA2 H 4.042 0.000 2 123 47 23 GLY HA3 H 3.904 0.005 2 124 48 24 GLY H H 7.988 0.001 1 125 48 24 GLY HA2 H 4.152 0.000 2 126 48 24 GLY HA3 H 4.003 0.000 2 127 49 25 PRO HA H 4.296 0.000 1 128 49 25 PRO HB2 H 2.121 0.000 2 129 49 25 PRO HB3 H 1.747 0.000 2 130 49 25 PRO HD2 H 3.609 0.000 2 131 49 25 PRO HD3 H 3.530 0.000 2 132 49 25 PRO HG2 H 1.909 0.000 2 133 50 26 LYS H H 7.996 0.002 1 134 50 26 LYS HA H 3.989 0.000 1 135 50 26 LYS HB2 H 1.443 0.006 2 136 50 26 LYS HB3 H 1.339 0.003 2 137 50 26 LYS HE3 H 2.935 0.000 2 138 50 26 LYS HG3 H 1.004 0.000 2 139 51 27 TRP H H 7.583 0.001 1 140 51 27 TRP HB2 H 3.325 0.002 2 141 51 27 TRP HB3 H 3.075 0.001 2 142 51 27 TRP HD1 H 7.202 0.003 1 143 51 27 TRP HE1 H 9.931 0.000 1 144 51 27 TRP HE3 H 7.574 0.001 1 145 51 27 TRP HH2 H 7.082 0.002 1 146 51 27 TRP HZ2 H 7.372 0.001 1 147 51 27 TRP HZ3 H 7.019 0.000 1 stop_ save_ save_assigned_chem_shift_list_2_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $RLF_crosslinked_H2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A_crosslinked _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 4.029 0.000 1 2 106 1 ALA HB H 1.482 0.000 1 3 107 2 ALA H H 8.436 0.000 1 4 107 2 ALA HA H 4.221 0.000 1 5 107 2 ALA HB H 1.297 0.005 1 6 108 3 ALA H H 8.245 0.002 1 7 108 3 ALA HA H 4.239 0.000 1 8 108 3 ALA HB H 1.267 0.002 1 9 109 4 THR H H 7.952 0.000 1 10 109 4 THR HA H 4.204 0.001 1 11 109 4 THR HB H 4.103 0.000 1 12 109 4 THR HG2 H 1.140 0.000 1 13 110 5 ASN H H 8.331 0.001 1 14 110 5 ASN HA H 4.904 0.001 1 15 110 5 ASN HB2 H 2.917 0.002 2 16 110 5 ASN HB3 H 2.746 0.001 2 17 110 5 ASN HD21 H 6.874 0.000 2 18 110 5 ASN HD22 H 7.630 0.001 2 19 111 6 PRO HA H 4.096 0.000 1 20 111 6 PRO HB2 H 2.335 0.000 2 21 111 6 PRO HB3 H 1.894 0.004 2 22 111 6 PRO HD2 H 3.808 0.002 2 23 111 6 PRO HD3 H 3.745 0.000 2 24 111 6 PRO HG2 H 2.018 0.000 2 25 112 7 ALA H H 7.813 0.003 1 26 112 7 ALA HB H 1.025 0.001 1 27 113 8 ARG H H 7.451 0.001 1 28 113 8 ARG HA H 3.874 0.000 1 29 113 8 ARG HB2 H 1.742 0.002 2 30 113 8 ARG HB3 H 1.672 0.001 2 31 113 8 ARG HE H 6.874 0.001 1 32 113 8 ARG HG2 H 1.540 0.000 2 33 113 8 ARG HG3 H 1.466 0.000 2 34 114 9 TYR H H 8.001 0.003 1 35 114 9 TYR HA H 4.168 0.002 1 36 114 9 TYR HB2 H 3.050 0.000 2 37 114 9 TYR HB3 H 2.957 0.000 2 38 114 9 TYR HD1 H 6.934 0.002 3 39 114 9 TYR HD2 H 6.934 0.002 3 40 114 9 TYR HE1 H 6.769 0.000 3 41 114 9 TYR HE2 H 6.769 0.000 3 42 115 10 CYS H H 8.655 0.003 1 43 115 10 CYS HA H 4.407 0.000 1 44 115 10 CYS HB2 H 3.175 0.002 2 45 115 10 CYS HB3 H 2.754 0.006 2 46 116 11 CYS H H 7.488 0.003 1 47 116 11 CYS HA H 4.377 0.001 1 48 116 11 CYS HB2 H 3.526 0.002 2 49 116 11 CYS HB3 H 2.740 0.001 2 50 117 12 LEU H H 8.051 0.001 1 51 117 12 LEU HA H 4.132 0.000 1 52 117 12 LEU HB2 H 1.646 0.000 2 53 117 12 LEU HB3 H 1.429 0.001 2 54 117 12 LEU HD1 H 0.772 0.000 2 55 117 12 LEU HD2 H 0.772 0.000 2 56 117 12 LEU HG H 1.646 0.000 1 57 118 13 SER H H 8.110 0.002 1 58 118 13 SER HA H 4.449 0.000 1 59 118 13 SER HB2 H 3.490 0.002 2 60 118 13 SER HB3 H 3.082 0.000 2 61 119 14 GLY H H 7.117 0.001 1 62 119 14 GLY HA2 H 4.197 0.008 2 63 119 14 GLY HA3 H 3.878 0.002 2 64 120 15 CYS H H 8.793 0.002 1 65 120 15 CYS HA H 5.175 0.001 1 66 120 15 CYS HB2 H 3.711 0.009 2 67 120 15 CYS HB3 H 2.564 0.000 2 68 121 16 THR H H 9.692 0.003 1 69 121 16 THR HA H 4.853 0.002 1 70 121 16 THR HB H 4.747 0.004 1 71 121 16 THR HG2 H 1.136 0.002 1 72 122 17 GLN H H 8.990 0.001 1 73 122 17 GLN HA H 3.933 0.000 1 74 122 17 GLN HB2 H 2.154 0.000 2 75 122 17 GLN HB3 H 2.079 0.000 2 76 122 17 GLN HE21 H 7.420 0.002 2 77 122 17 GLN HE22 H 6.675 0.002 2 78 122 17 GLN HG2 H 2.396 0.001 2 79 122 17 GLN HG3 H 2.327 0.004 2 80 123 18 GLN H H 8.151 0.001 1 81 123 18 GLN HA H 3.943 0.000 1 82 123 18 GLN HB2 H 2.057 0.002 2 83 123 18 GLN HB3 H 1.973 0.000 2 84 123 18 GLN HE21 H 7.500 0.001 2 85 123 18 GLN HE22 H 6.789 0.000 2 86 123 18 GLN HG2 H 2.430 0.005 2 87 123 18 GLN HG3 H 2.376 0.002 2 88 124 19 ASP H H 7.740 0.002 1 89 124 19 ASP HA H 4.340 0.002 1 90 124 19 ASP HB2 H 3.191 0.000 2 91 124 19 ASP HB3 H 2.818 0.006 2 92 125 20 LEU H H 7.668 0.002 1 93 125 20 LEU HA H 3.949 0.000 1 94 125 20 LEU HB2 H 2.013 0.000 2 95 125 20 LEU HB3 H 1.239 0.000 2 96 125 20 LEU HD1 H 0.771 0.002 2 97 125 20 LEU HD2 H 0.713 0.002 2 98 125 20 LEU HG H 1.875 0.000 1 99 126 21 LEU H H 7.911 0.002 1 100 126 21 LEU HA H 4.231 0.003 1 101 126 21 LEU HB2 H 1.775 0.000 2 102 126 21 LEU HB3 H 1.555 0.000 2 103 126 21 LEU HD1 H 0.865 0.002 2 104 126 21 LEU HD2 H 0.863 0.004 2 105 126 21 LEU HG H 1.641 0.000 1 106 127 22 THR H H 7.464 0.002 1 107 127 22 THR HA H 4.155 0.000 1 108 127 22 THR HB H 4.373 0.000 1 109 127 22 THR HG2 H 1.378 0.000 1 110 128 23 LEU H H 7.763 0.001 1 111 128 23 LEU HA H 4.446 0.003 1 112 128 23 LEU HB2 H 2.122 0.002 2 113 128 23 LEU HB3 H 1.659 0.004 2 114 128 23 LEU HD1 H 1.050 0.003 2 115 128 23 LEU HD2 H 0.867 0.002 2 116 128 23 LEU HG H 1.956 0.004 1 117 129 24 CYS H H 7.367 0.002 1 118 129 24 CYS HA H 4.730 0.000 1 119 129 24 CYS HB2 H 3.107 0.000 2 120 129 24 CYS HB3 H 2.784 0.000 2 121 130 25 PRO HD2 H 3.735 0.000 2 122 130 25 PRO HD3 H 3.421 0.000 2 123 131 26 TYR H H 7.462 0.000 1 124 131 26 TYR HA H 4.393 0.002 1 125 131 26 TYR HB2 H 3.069 0.010 2 126 131 26 TYR HB3 H 2.937 0.006 2 127 131 26 TYR HD1 H 7.101 0.000 3 128 131 26 TYR HD2 H 7.101 0.000 3 129 131 26 TYR HE1 H 6.816 0.000 3 130 131 26 TYR HE2 H 6.816 0.000 3 131 132 27 GLY H H 8.078 0.001 1 132 132 27 GLY HA2 H 3.801 0.001 2 133 132 27 GLY HA3 H 3.615 0.001 2 stop_ save_ save_assigned_chem_shift_list_3_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $RLF_crosslinked_D2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-B_crosslinked _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 4.446 0.000 1 2 25 1 PRO CA C 62.334 0.000 1 3 26 2 THR HB H 4.184 0.000 1 4 26 2 THR HG2 H 1.261 0.000 1 5 26 2 THR CB C 69.478 0.000 1 6 26 2 THR CG2 C 21.618 0.000 1 7 27 3 PRO HA H 4.394 0.000 1 8 27 3 PRO CA C 63.515 0.000 1 9 28 4 GLU HA H 4.266 0.000 1 10 28 4 GLU CA C 56.309 0.000 1 11 29 5 MET HA H 4.407 0.000 1 12 29 5 MET CA C 55.280 0.000 1 13 30 6 ARG HA H 4.007 0.000 1 14 30 6 ARG CA C 55.754 0.000 1 15 31 7 GLU HA H 4.494 0.000 1 16 31 7 GLU CA C 55.050 0.000 1 17 32 8 LYS HA H 4.570 0.000 1 18 32 8 LYS CA C 56.704 0.000 1 19 33 9 LEU HA H 4.491 0.000 1 20 33 9 LEU CA C 53.209 0.000 1 21 34 10 CYS HA H 4.932 0.000 1 22 34 10 CYS CA C 54.653 0.000 1 23 35 11 GLY HA2 H 3.985 0.000 2 24 35 11 GLY HA3 H 3.811 0.000 2 25 35 11 GLY CA C 46.736 0.004 1 26 36 12 HIS HA H 4.391 0.000 1 27 36 12 HIS CA C 56.518 0.000 1 28 37 13 HIS HA H 4.251 0.000 1 29 37 13 HIS CA C 58.506 0.000 1 30 38 14 PHE HA H 4.083 0.000 1 31 38 14 PHE CA C 61.140 0.000 1 32 39 15 VAL HA H 3.121 0.000 1 33 39 15 VAL CA C 66.563 0.000 1 34 40 16 ARG HA H 3.778 0.000 1 35 40 16 ARG CA C 59.028 0.000 1 36 41 17 ALA HA H 4.001 0.000 1 37 41 17 ALA HB H 1.387 0.000 1 38 41 17 ALA CA C 54.911 0.000 1 39 41 17 ALA CB C 19.294 0.000 1 40 42 18 LEU HA H 3.741 0.000 1 41 42 18 LEU CA C 57.751 0.000 1 42 43 19 VAL HA H 3.378 0.000 1 43 43 19 VAL CA C 66.239 0.000 1 44 44 20 ARG HA H 3.994 0.000 1 45 44 20 ARG CA C 57.446 0.000 1 46 45 21 VAL HA H 3.848 0.000 1 47 45 21 VAL CA C 65.079 0.000 1 48 46 22 CYS HA H 4.649 0.000 1 49 46 22 CYS CA C 54.857 0.000 1 50 47 23 GLY HA3 H 3.909 0.000 2 51 47 23 GLY CA C 45.472 0.000 1 52 48 24 GLY HA2 H 4.161 0.000 2 53 48 24 GLY CA C 45.453 0.000 1 54 49 25 PRO HA H 4.297 0.000 1 55 49 25 PRO CA C 63.815 0.000 1 56 51 27 TRP HA H 4.509 0.000 1 57 51 27 TRP CA C 57.116 0.000 1 stop_ save_ save_assigned_chem_shift_list_3_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $RLF_crosslinked_D2O stop_ _Sample_conditions_label $RLF_crosslinked_H2O_308 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name RLF-A_crosslinked _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 4.021 0.000 1 2 106 1 ALA HB H 1.480 0.000 1 3 106 1 ALA CA C 51.546 0.000 1 4 106 1 ALA CB C 19.192 0.000 1 5 107 2 ALA HA H 4.257 0.000 1 6 107 2 ALA HB H 1.308 0.000 1 7 107 2 ALA CA C 52.294 0.000 1 8 107 2 ALA CB C 19.110 0.000 1 9 108 3 ALA HA H 4.236 0.000 1 10 108 3 ALA HB H 1.277 0.000 1 11 108 3 ALA CA C 52.291 0.000 1 12 108 3 ALA CB C 19.065 0.000 1 13 109 4 THR HA H 4.223 0.000 1 14 109 4 THR HB H 4.107 0.000 1 15 109 4 THR CA C 61.946 0.000 1 16 109 4 THR CB C 69.579 0.000 1 17 110 5 ASN HA H 4.917 0.000 1 18 110 5 ASN CA C 51.377 0.000 1 19 111 6 PRO HA H 4.104 0.000 1 20 111 6 PRO CA C 65.103 0.000 1 21 112 7 ALA HB H 1.039 0.000 1 22 112 7 ALA CB C 18.207 0.000 1 23 117 12 LEU HA H 4.141 0.000 1 24 117 12 LEU CA C 56.957 0.000 1 25 118 13 SER HA H 4.459 0.000 1 26 118 13 SER HB2 H 3.494 0.000 2 27 118 13 SER HB3 H 3.075 0.000 2 28 118 13 SER CA C 59.858 0.000 1 29 118 13 SER CB C 63.675 0.007 1 30 119 14 GLY HA2 H 4.217 0.000 2 31 119 14 GLY HA3 H 3.878 0.000 2 32 119 14 GLY CA C 43.938 0.002 1 33 120 15 CYS HA H 5.182 0.000 1 34 120 15 CYS CA C 53.377 0.000 1 35 121 16 THR HA H 4.872 0.000 1 36 121 16 THR HB H 4.756 0.000 1 37 121 16 THR HG2 H 1.151 0.000 1 38 121 16 THR CA C 59.953 0.000 1 39 121 16 THR CB C 71.762 0.000 1 40 121 16 THR CG2 C 21.599 0.000 1 41 122 17 GLN HA H 3.947 0.000 1 42 122 17 GLN CA C 59.982 0.000 1 43 123 18 GLN HA H 3.964 0.000 1 44 123 18 GLN CA C 59.159 0.000 1 45 124 19 ASP HA H 4.350 0.000 1 46 124 19 ASP CA C 57.567 0.000 1 47 125 20 LEU HA H 3.967 0.000 1 48 125 20 LEU CA C 57.907 0.000 1 49 126 21 LEU HA H 4.246 0.000 1 50 126 21 LEU CA C 57.448 0.000 1 51 127 22 THR HA H 4.153 0.000 1 52 127 22 THR HB H 4.367 0.000 1 53 127 22 THR HG2 H 1.389 0.000 1 54 127 22 THR CA C 64.291 0.000 1 55 127 22 THR CB C 69.423 0.000 1 56 127 22 THR CG2 C 21.685 0.000 1 57 128 23 LEU HA H 4.472 0.000 1 58 128 23 LEU CA C 54.602 0.000 1 59 131 26 TYR HA H 4.393 0.000 1 60 131 26 TYR CA C 58.489 0.000 1 61 132 27 GLY HA2 H 3.808 0.000 2 62 132 27 GLY HA3 H 3.616 0.000 2 63 132 27 GLY CA C 45.316 0.008 1 stop_ save_