data_20127 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Nociceptin Agonist ; _BMRB_accession_number 20127 _BMRB_flat_file_name bmr20127.str _Entry_type original _Submission_date 2010-08-06 _Accession_date 2010-08-06 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Helically constrained noceceptin receptor agonist peptide' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Fairlie David P. . 2 Hill Tim A. . 3 Harrison Rosemary . . 4 Hoang Huy H. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 structure_coordinate_set 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 68 "coupling constants" 14 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2011-06-02 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Novel Helix-Constrained Nociceptin Derivatives Are Potent Agonists and Antagonists of ERK Phosphorylation and Thermal Analgesia in Mice.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 21067234 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Harrison Rosemary S. . 2 Ruiz-Gomez Gloria . . 3 Hill Timothy A. . 4 Chow Shiao Y. . 5 Shepherd Nicholas E. . 6 Lohman Rink-Jan . . 7 Abbenante Giovanni . . 8 Hoang Huy N. . 9 Fairlie David P. . stop_ _Journal_abbreviation 'J. Med. Chem.' _Journal_name_full 'Journal of medicinal chemistry' _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 2010 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'nociceptin Agonist' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Nociceptin Agonist' $Nociceptin_Agonist stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'Agonist of the nociceptin receptor' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Nociceptin_Agonist _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Nociceptin_Agonist _Molecular_mass . _Mol_thiol_state 'not present' loop_ _Biological_function 'Agonist of the nociceptin receptor' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 15 _Mol_residue_sequence FGGFTKARKDKRKLD loop_ _Residue_seq_code _Residue_label 1 PHE 2 GLY 3 GLY 4 PHE 5 THR 6 LYS 7 ALA 8 ARG 9 LYS 10 ASP 11 LYS 12 ARG 13 LYS 14 LEU 15 ASP 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 $Nociceptin_Agonist . . . . . . 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 $Nociceptin_Agonist 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Nociceptin_Agonist 4 mg 'natural abundance' H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_X-PLOR _Saveframe_category software _Name X-PLOR _Version . loop_ _Vendor _Address _Electronic_address Brunger . . stop_ loop_ _Task 'geometry optimization' refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 288 . K pH 4 . 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 0.0 internal direct . . . 1.000000 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-1H COSY' '2D 1H-1H NOESY' 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 'Nociceptin Agonist' _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 2 2 GLY H H 8.53 0.0035 1 2 2 2 GLY HA2 H 3.81 0.025 1 3 3 3 GLY H H 7.88 0.025 1 4 3 3 GLY HA2 H 3.77 0.025 1 5 4 4 PHE H H 8.29 0.025 1 6 4 4 PHE HA H 4.57 0.0035 1 7 4 4 PHE HB2 H 2.97 0.025 1 8 4 4 PHE HB3 H 2.31 0.0035 1 9 4 4 PHE HD1 H 7.17 0.025 3 10 4 4 PHE HD2 H 7.17 0.025 3 11 4 4 PHE HE1 H 7.27 0.025 3 12 4 4 PHE HE2 H 7.27 0.0035 3 13 5 5 THR H H 7.85 0.0035 1 14 5 5 THR HA H 4.27 0.025 1 15 5 5 THR HB H 4.04 0.025 1 16 5 5 THR HG2 H 1.17 0.0035 1 17 6 6 LYS H H 8.17 0.025 1 18 6 6 LYS HA H 4.01 0.025 1 19 6 6 LYS HB2 H 1.69 0.025 2 20 6 6 LYS HD2 H 2.47 0.025 2 21 6 6 LYS HE2 H 3.58 0.025 2 22 6 6 LYS HG2 H 1.44 0.0035 2 23 6 6 LYS HG3 H 1.08 0.025 2 24 6 6 LYS HZ H 8.04 0.025 1 25 7 7 ALA H H 8.13 0.025 1 26 7 7 ALA HA H 3.99 0.025 1 27 7 7 ALA HB H 1.34 0.025 1 28 8 8 ARG H H 7.67 0.025 1 29 8 8 ARG HA H 3.97 0.025 1 30 8 8 ARG HB2 H 1.74 0.025 2 31 8 8 ARG HD2 H 3.05 0.025 2 32 8 8 ARG HE H 7.07 0.0035 1 33 8 8 ARG HG2 H 1.60 0.025 2 34 8 8 ARG HG3 H 1.49 0.0035 2 35 9 9 LYS H H 8.05 0.025 1 36 9 9 LYS HA H 3.88 0.025 1 37 9 9 LYS HB2 H 1.75 0.0035 2 38 9 9 LYS HG2 H 1.33 0.0035 2 39 10 10 ASP H H 8.69 0.025 1 40 10 10 ASP HA H 4.52 0.025 1 41 10 10 ASP HB2 H 2.59 0.025 2 42 10 10 ASP HB3 H 2.77 0.025 2 43 11 11 LYS H H 7.59 0.025 1 44 11 11 LYS HA H 4.14 0.0035 1 45 11 11 LYS HB2 H 1.86 0.025 2 46 11 11 LYS HD2 H 2.52 0.0035 2 47 11 11 LYS HE2 H 3.54 0.025 2 48 11 11 LYS HG2 H 1.51 0.0035 2 49 11 11 LYS HZ H 7.86 0.025 1 50 12 12 ARG H H 7.82 0.0035 1 51 12 12 ARG HA H 3.97 0.0035 1 52 12 12 ARG HB2 H 1.82 0.025 1 53 12 12 ARG HD2 H 3.10 0.0035 2 54 12 12 ARG HE H 7.16 0.025 1 55 12 12 ARG HG2 H 1.57 0.0035 2 56 12 12 ARG HG3 H 1.67 0.025 2 57 13 13 LYS H H 7.51 0.025 1 58 13 13 LYS HA H 4.01 0.0035 1 59 13 13 LYS HB2 H 1.85 0.0035 2 60 14 14 LEU H H 7.76 0.025 1 61 14 14 LEU HA H 4.03 0.0035 1 62 14 14 LEU HB2 H 1.63 0.025 2 63 14 14 LEU HD1 H 0.8 0.025 2 64 14 14 LEU HG H 1.56 0.025 1 65 15 15 ASP H H 8.18 0.025 1 66 15 15 ASP HA H 4.53 0.025 1 67 15 15 ASP HB2 H 2.58 0.025 2 68 15 15 ASP HB3 H 2.85 0.025 2 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details . loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H NOESY' stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'Nociceptin Agonist' _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 2 GLY H 2 GLY HA2 5.6 . . . 2 3JHNHA 2 GLY H 2 GLY HA3 5.6 . . . 3 3JHNHA 3 GLY H 3 GLY HA2 5.3 . . . 4 3JHNHA 3 GLY H 3 GLY HA3 5.3 . . . 5 3JHNHA 4 PHE H 4 PHE HA 6.3 . . . 6 3JHNHA 5 THR H 5 THR HA 6.0 . . . 7 3JHNHA 7 ALA H 7 ALA HA 2.5 . . . 8 3JHNHA 8 ARG H 8 ARG HA 5.6 . . . 9 3JHNHA 9 LYS H 9 LYS HA 4.9 . . . 10 3JHNHA 10 ASP H 10 ASP HA 5.1 . . . 11 3JHNHA 11 LYS H 11 LYS HA 4.2 . . . 12 3JHNHA 12 ARG H 12 ARG HA 3.6 . . . 13 3JHNHA 13 LYS H 13 LYS HA 5.6 . . . 14 3JHNHA 14 LEU H 14 LEU HA 5.1 . . . stop_ save_