data_15773 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Analysis of Site-specific Histidine Protonation in Human Prolactin ; _BMRB_accession_number 15773 _BMRB_flat_file_name bmr15773.str _Entry_type original _Submission_date 2008-05-13 _Accession_date 2008-05-13 _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 Tettamanzi 'M. Cristina' . . 2 Keeler Camille . . 3 Meshack Syrus . . 4 Hodsdon Michael E. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 4 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 53 "13C chemical shifts" 34 "15N chemical shifts" 47 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2009-02-23 update BMRB 'complete entry citation' 2008-07-30 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Analysis of Site-specific Histidine Protonation in Human Prolactin' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18652486 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tettamanzi 'M. Cristina' . . 2 Keeler Camille . . 3 Meshack Syrus . . 4 Hodsdon Michael E. . stop_ _Journal_abbreviation Biochemistry _Journal_volume 47 _Journal_issue 33 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8638 _Page_last 8647 _Year 2008 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Human Prolactin' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label hPrl $hPrl 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_hPrl _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common hPrl _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 199 _Mol_residue_sequence ; LPICPGGAARCQVTLRDLFD RAVVLSHYIHNLSSEMFSEF DKRYTHGRGFITKAINSCHT SSLATPEDKEQAQQMNQKDF LSLIVSILRSWNEPLYHLVT EVRGMQEAPEAILSKAVEIE EQTKRLLEGMELIVSQVHPE TKENEIYPVWSGLPSLQMAD EESRLSAYYNLLHCLRRDSH KIDNYLKLLKCRIIHNNNC ; loop_ _Residue_seq_code _Residue_label 1 LEU 2 PRO 3 ILE 4 CYS 5 PRO 6 GLY 7 GLY 8 ALA 9 ALA 10 ARG 11 CYS 12 GLN 13 VAL 14 THR 15 LEU 16 ARG 17 ASP 18 LEU 19 PHE 20 ASP 21 ARG 22 ALA 23 VAL 24 VAL 25 LEU 26 SER 27 HIS 28 TYR 29 ILE 30 HIS 31 ASN 32 LEU 33 SER 34 SER 35 GLU 36 MET 37 PHE 38 SER 39 GLU 40 PHE 41 ASP 42 LYS 43 ARG 44 TYR 45 THR 46 HIS 47 GLY 48 ARG 49 GLY 50 PHE 51 ILE 52 THR 53 LYS 54 ALA 55 ILE 56 ASN 57 SER 58 CYS 59 HIS 60 THR 61 SER 62 SER 63 LEU 64 ALA 65 THR 66 PRO 67 GLU 68 ASP 69 LYS 70 GLU 71 GLN 72 ALA 73 GLN 74 GLN 75 MET 76 ASN 77 GLN 78 LYS 79 ASP 80 PHE 81 LEU 82 SER 83 LEU 84 ILE 85 VAL 86 SER 87 ILE 88 LEU 89 ARG 90 SER 91 TRP 92 ASN 93 GLU 94 PRO 95 LEU 96 TYR 97 HIS 98 LEU 99 VAL 100 THR 101 GLU 102 VAL 103 ARG 104 GLY 105 MET 106 GLN 107 GLU 108 ALA 109 PRO 110 GLU 111 ALA 112 ILE 113 LEU 114 SER 115 LYS 116 ALA 117 VAL 118 GLU 119 ILE 120 GLU 121 GLU 122 GLN 123 THR 124 LYS 125 ARG 126 LEU 127 LEU 128 GLU 129 GLY 130 MET 131 GLU 132 LEU 133 ILE 134 VAL 135 SER 136 GLN 137 VAL 138 HIS 139 PRO 140 GLU 141 THR 142 LYS 143 GLU 144 ASN 145 GLU 146 ILE 147 TYR 148 PRO 149 VAL 150 TRP 151 SER 152 GLY 153 LEU 154 PRO 155 SER 156 LEU 157 GLN 158 MET 159 ALA 160 ASP 161 GLU 162 GLU 163 SER 164 ARG 165 LEU 166 SER 167 ALA 168 TYR 169 TYR 170 ASN 171 LEU 172 LEU 173 HIS 174 CYS 175 LEU 176 ARG 177 ARG 178 ASP 179 SER 180 HIS 181 LYS 182 ILE 183 ASP 184 ASN 185 TYR 186 LEU 187 LYS 188 LEU 189 LEU 190 LYS 191 CYS 192 ARG 193 ILE 194 ILE 195 HIS 196 ASN 197 ASN 198 ASN 199 CYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-10-28 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 1RW5 "Solution Structure Of Human Prolactin" 100.00 199 100.00 100.00 1.44e-145 PDB 2Q98 "X-Ray Structure Of A Prolactin Antagonist" 95.48 191 98.95 98.95 3.13e-135 PDB 3D48 "Crystal Structure Of A Prolactin Receptor Antagonist Bound To The Extracellular Domain Of The Prolactin Receptor" 93.97 188 99.47 99.47 1.28e-133 PDB 3MZG "Crystal Structure Of A Human Prolactin Receptor Antagonist In Complex With The Extracellular Domain Of The Human Prolactin Rece" 92.96 186 99.46 99.46 6.12e-132 PDB 3N06 "A Mutant Human Prolactin Receptor Antagonist H27a In Complex With The Extracellular Domain Of The Human Prolactin Receptor" 92.96 186 98.92 98.92 7.73e-131 PDB 3N0P "A Mutant Human Prolactin Receptor Antagonist H30a In Complex With The Extracellular Domain Of The Human Prolactin Receptor" 92.96 186 98.92 98.92 7.73e-131 PDB 3NCB "A Mutant Human Prolactin Receptor Antagonist H180a In Complex With The Extracellular Domain Of The Human Prolactin Receptor" 92.96 186 98.92 98.92 7.73e-131 PDB 3NCC "A Human Prolactin Receptor Antagonist In Complex With The Mutant Extracellular Domain H188a Of The Human Prolactin Receptor" 92.96 186 99.46 99.46 6.12e-132 PDB 3NCE "A Mutant Human Prolactin Receptor Antagonist H27a In Complex With The Mutant Extracellular Domain H188a Of The Human Prolactin " 92.96 186 98.92 98.92 7.73e-131 PDB 3NCF "A Mutant Human Prolactin Receptor Antagonist H30a In Complex With The Mutant Extracellular Domain H188a Of The Human Prolactin " 92.96 186 98.92 98.92 7.73e-131 PDB 3NPZ "Prolactin Receptor (Prlr) Complexed With The Natural Hormone (Prl)" 100.00 199 100.00 100.00 1.44e-145 DBJ BAA00312 "prolactin PRL precursor [Homo sapiens]" 100.00 217 98.99 99.50 7.11e-144 DBJ BAI46568 "prolactin [synthetic construct]" 100.00 227 100.00 100.00 4.59e-145 EMBL CAA23829 "prolactin [Homo sapiens]" 100.00 227 100.00 100.00 4.59e-145 EMBL CAA25214 "prolactin [Homo sapiens]" 100.00 217 100.00 100.00 1.43e-145 EMBL CAA38264 "prolactin [Homo sapiens]" 100.00 220 100.00 100.00 1.58e-145 GB AAA18471 "prolactin [Macaca mulatta]" 100.00 227 97.99 99.50 1.59e-142 GB AAA60173 "prolactin, partial [Homo sapiens]" 100.00 217 99.50 99.50 2.36e-144 GB AAB70858 "preprolactin, partial [Homo sapiens]" 86.93 191 98.84 98.84 2.86e-122 GB AAH15850 "Prolactin [Homo sapiens]" 100.00 227 100.00 100.00 4.59e-145 GB AAH88370 "Prolactin [Homo sapiens]" 100.00 228 100.00 100.00 3.46e-145 PRF 1005222A prolactin 100.00 217 100.00 100.00 1.43e-145 REF NP_000939 "prolactin precursor [Homo sapiens]" 100.00 227 100.00 100.00 4.59e-145 REF NP_001040593 "prolactin precursor [Macaca mulatta]" 100.00 227 97.99 99.50 1.59e-142 REF NP_001157030 "prolactin precursor [Homo sapiens]" 100.00 227 100.00 100.00 4.59e-145 REF XP_002816520 "PREDICTED: prolactin [Pongo abelii]" 100.00 227 98.99 99.50 3.34e-143 REF XP_003263607 "PREDICTED: prolactin [Nomascus leucogenys]" 100.00 227 99.50 100.00 3.01e-144 SP P01236 "RecName: Full=Prolactin; Short=PRL; Flags: Precursor" 100.00 227 100.00 100.00 4.59e-145 SP P55151 "RecName: Full=Prolactin; Short=PRL; Flags: Precursor" 100.00 227 97.99 99.50 1.59e-142 TPE CDW51382 "TPA: growth hormone A1 [Homo sapiens]" 100.00 228 100.00 100.00 3.46e-145 TPE CDW51392 "TPA: growth hormone A1 [Pongo abelii]" 100.00 228 98.99 99.50 2.41e-143 TPE CDW51397 "TPA: growth hormone A1 [Nomascus leucogenys]" 100.00 228 99.50 100.00 3.08e-144 TPE CDW51400 "TPA: growth hormone A1 [Macaca mulatta]" 100.00 228 97.99 99.50 1.20e-142 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $hPrl Human 9606 Eukaryota Metazoa Homo sapiens stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $hPrl 'recombinant technology' . Escherichia coli . pT7L-hPrl stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details 'pH 5.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $hPrl 0.6 mM '[U-100% 13C; U-100% 15N]' 'potassium phosphate' 25 mM 'natural abundance' 'sodium chloride' 25 mM 'natural abundance' 'sodium azide' 1 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details 'pH 6.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $hPrl 0.6 mM '[U-100% 13C; U-100% 15N]' 'potassium phosphate' 25 mM 'natural abundance' 'sodium chloride' 25 mM 'natural abundance' 'sodium azide' 1 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % . stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details 'pH 7.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $hPrl 0.6 mM '[U-100% 13C; U-100% 15N]' 'potassium phosphate' 25 mM 'natural abundance' 'sodium chloride' 25 mM 'natural abundance' 'sodium azide' 1 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % . stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details 'pH 8.0' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $hPrl 0.6 mM '[U-100% 13C; U-100% 15N]' 'potassium phosphate' 25 mM 'natural abundance' 'sodium chloride' 25 mM 'natural abundance' 'sodium azide' 1 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % . stop_ save_ ############################ # Computer software used # ############################ 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_NMRDraw _Saveframe_category software _Name NMRDraw _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_3 save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_4 save_ save_2D_1H-15N_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_3 save_ save_2D_1H-15N_HSQC_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_4 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' 0.050 . M pH 5.0 . pH pressure 1 . atm temperature 308 . 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' 0.052 . M pH 6.0 . pH pressure 1 . atm temperature 308 . K stop_ save_ save_sample_conditions_3 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.064 . M pH 7.0 . pH pressure 1 . atm temperature 308 . K stop_ save_ save_sample_conditions_4 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.082 . M pH 8.0 . pH pressure 1 . atm 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 . indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 . indirect . . . 0.101329118 stop_ save_ ################################### # 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name hPrl _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 27 27 HIS HE1 H 8.512 0.013 1 2 27 27 HIS CE1 C 136.719 0.3 1 3 27 27 HIS HD2 H 7.322 0.001 1 4 27 27 HIS ND1 N 184.105 0.061 1 5 27 27 HIS NE2 N 174.250 0.057 1 6 30 30 HIS HE1 H 7.887 0.022 1 7 30 30 HIS CE1 C 137.554 0.3 1 8 30 30 HIS HD2 H 7.043 0.03 1 9 30 30 HIS ND1 N 186.007 0.3 1 10 30 30 HIS NE2 N 201.282 0.019 1 11 46 46 HIS HE1 H 8.482 0.005 1 12 46 46 HIS CE1 C 136.573 0.3 1 13 46 46 HIS HD2 H 7.170 0.004 1 14 46 46 HIS ND1 N 179.128 0.062 1 15 46 46 HIS NE2 N 174.156 0.037 1 16 59 59 HIS HE1 H 8.707 0.004 1 17 59 59 HIS CE1 C 137.761 0.3 1 18 59 59 HIS ND1 N 185.69 0.3 1 19 59 59 HIS NE2 N 178.265 0.3 1 20 138 138 HIS HE1 H 8.442 0.027 1 21 138 138 HIS CE1 C 137.074 0.3 1 22 138 138 HIS NE2 N 181.439 0.3 1 23 173 173 HIS HE1 H 7.912 0.028 1 24 173 173 HIS CE1 C 138.149 0.3 1 25 173 173 HIS HD2 H 6.727 0.03 1 26 173 173 HIS NE2 N 181.692 0.039 1 27 180 180 HIS HE1 H 8.23 0.018 1 28 180 180 HIS CE1 C 137.425 0.3 1 29 180 180 HIS HD2 H 6.986 0.03 1 30 180 180 HIS ND1 N 199.02 0.3 1 31 180 180 HIS NE2 N 176.471 0.064 1 32 195 195 HIS HE1 H 8.458 0.022 1 33 195 195 HIS NE2 N 181.318 0.3 1 34 195 195 HIS CE1 C 136.886 0.3 1 stop_ save_ save_assigned_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_2 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name hPrl _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 27 27 HIS HE1 H 8.363 0.011 1 2 27 27 HIS CE1 C 137.193 0.3 1 3 27 27 HIS HD2 H 7.271 0.002 1 4 27 27 HIS ND1 N 190.63 0.3 1 5 27 27 HIS NE2 N 177.411 0.038 1 6 30 30 HIS HE1 H 7.679 0.013 1 7 30 30 HIS CE1 C 137.947 0.3 1 8 30 30 HIS HD2 H 6.944 0.003 1 9 30 30 HIS ND1 N 188.126 0.003 1 10 30 30 HIS NE2 N 208.248 0.012 1 11 46 46 HIS HE1 H 8.357 0.013 1 12 46 46 HIS CE1 C 136.972 0.3 1 13 46 46 HIS HD2 H 7.133 0.3 1 14 46 46 HIS ND1 N 185.835 0.015 1 15 46 46 HIS NE2 N 176.525 0.028 1 16 59 59 HIS HD2 H 7.435 0.03 1 17 59 59 HIS HE1 H 8.487 0.02 1 18 59 59 HIS ND1 N 196.948 0.3 1 19 59 59 HIS NE2 N 182.387 0.059 1 20 59 59 HIS CE1 C 138.416 0.3 1 21 97 97 HIS HE1 H 8.253 0.03 1 22 97 97 HIS CE1 C 137.664 0.3 1 23 138 138 HIS HE1 H 8.101 0.021 1 24 138 138 HIS NE2 N 186.576 0.3 1 25 138 138 HIS CE1 C 138.052 0.3 1 26 173 173 HIS HE1 H 7.711 0.011 1 27 173 173 HIS HD2 H 6.705 0.03 1 28 173 173 HIS ND1 N 223.154 0.3 1 29 173 173 HIS NE2 N 184.38 0.001 1 30 173 173 HIS CE1 C 138.566 0.3 1 31 180 180 HIS HE1 H 7.987 0.015 1 32 180 180 HIS CE1 C 137.825 0.3 1 33 180 180 HIS HD2 H 6.858 0.001 1 34 180 180 HIS ND1 N 208.671 0.009 1 35 180 180 HIS NE2 N 179.763 0.012 1 36 195 195 HIS HE1 H 8.061 0.02 1 37 195 195 HIS NE2 N 190.021 0.3 1 38 195 195 HIS CE1 C 137.983 0.3 1 stop_ save_ save_assigned_chem_shift_list_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_3 stop_ _Sample_conditions_label $sample_conditions_3 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name hPrl _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 27 27 HIS HE1 H 8.013 0.026 1 2 27 27 HIS CE1 C 138.016 0.3 1 3 27 27 HIS HD2 H 7.127 0.03 1 4 27 27 HIS ND1 N 206.998 0.3 1 5 27 27 HIS NE2 N 188.917 0.01 1 6 30 30 HIS HE1 H 7.484 0.008 1 7 30 30 HIS HD2 H 6.872 0.002 1 8 30 30 HIS ND1 N 187.997 0.069 1 9 30 30 HIS NE2 N 221.177 0.009 1 10 30 30 HIS CE1 C 138.222 0.3 1 11 46 46 HIS HE1 H 7.91 0.027 1 12 46 46 HIS CE1 C 138.012 0.3 1 13 46 46 HIS HD2 H 6.964 0.03 1 14 46 46 HIS ND1 N 210.223 0.3 1 15 46 46 HIS NE2 N 185.471 0.007 1 16 59 59 HIS HE1 H 8.052 0.03 1 17 59 59 HIS CE1 C 139.067 0.3 1 18 97 97 HIS HE1 H 7.886 0.03 1 19 97 97 HIS CE1 C 138.620 0.3 1 20 138 138 HIS HE1 H 7.769 0.019 1 21 138 138 HIS NE2 N 194.929 0.3 1 22 138 138 HIS CE1 C 138.826 0.3 1 23 173 173 HIS HE1 H 7.609 0.03 1 24 173 173 HIS CE1 C 138.683 0.3 1 25 173 173 HIS ND1 N 227.764 0.3 1 26 173 173 HIS NE2 N 185.879 0.3 1 27 180 180 HIS HE1 H 7.698 0.014 1 28 180 180 HIS HD2 H 6.707 0.03 1 29 180 180 HIS ND1 N 221.06 0.044 1 30 180 180 HIS NE2 N 186.117 0.008 1 31 180 180 HIS CE1 C 138.193 0.3 1 32 195 195 HIS HE1 H 7.726 0.014 1 33 195 195 HIS NE2 N 199.851 0.3 1 34 195 195 HIS CE1 C 138.799 0.3 1 stop_ save_ save_assigned_chem_shift_list_4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_4 stop_ _Sample_conditions_label $sample_conditions_4 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name hPrl _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 27 27 HIS HE1 H 7.8 0.001 1 2 27 27 HIS CE1 C 138.681 0.3 1 3 27 27 HIS HD2 H 7.056 0.03 1 4 27 27 HIS ND1 N 214.164 0.3 1 5 27 27 HIS NE2 N 195.558 0.059 1 6 30 30 HIS HE1 H 7.42 0.007 1 7 30 30 HIS CE1 C 138.374 0.3 1 8 30 30 HIS HD2 H 6.856 0.03 1 9 30 30 HIS ND1 N 187.468 0.3 1 10 30 30 HIS NE2 N 226.292 0.091 1 11 46 46 HIS HE1 H 7.695 0.001 1 12 46 46 HIS HD2 H 6.897 0.03 1 13 46 46 HIS ND1 N 220.237 0.3 1 14 46 46 HIS NE2 N 188.941 0.06 1 15 46 46 HIS CE1 C 138.686 0.3 1 16 59 59 HIS HE1 H 7.923 0.03 1 17 59 59 HIS CE1 C 139.305 0.3 1 18 138 138 HIS HE1 H 7.710 0.03 1 19 138 138 HIS CE1 C 139.028 0.3 1 20 173 173 HIS HE1 H 7.580 0.03 1 21 173 173 HIS CE1 C 138.741 0.3 1 22 180 180 HIS HE1 H 7.599 0.004 1 23 180 180 HIS HD2 H 6.665 0.03 1 24 180 180 HIS ND1 N 223.759 0.3 1 25 180 180 HIS NE2 N 188.442 0.035 1 26 180 180 HIS CE1 C 138.361 0.3 1 27 195 195 HIS HE1 H 7.645 0.3 1 28 195 195 HIS CE1 C 139.022 0.3 1 stop_ save_