data_30163 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Structure of Apo-form Human Tear Lipocalin ; _BMRB_accession_number 30163 _BMRB_flat_file_name bmr30163.str _Entry_type original _Submission_date 2016-08-28 _Accession_date 2016-08-28 _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 Vogel H. J. . 2 Liu Z. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 132 "15N chemical shifts" 132 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-08-22 original BMRB . stop_ _Original_release_date 2016-11-11 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; NMR Structure of Apo-form Human Tear Lipocalin ; _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Vogel H. J. . 2 Liu Z. . . stop_ _Journal_abbreviation . _Journal_volume . _Journal_issue . _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Lipocalin-1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 17453.652 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 158 _Mol_residue_sequence ; HHLLASDEEIQDVSGTWYLK AMTVDREFPEMNLESVTPMT LTTLEGGNLEAKVTMLISGR CQEVKAVLEKTDEPGKYTAD GGKHVAYIIRSHVKDHYIFY SEGELHGKPVRGVKLVGRDP KNNLEALEDFEKAAGARGLS TESILIPRQSETCSPGSD ; loop_ _Residue_seq_code _Residue_label 1 HIS 2 HIS 3 LEU 4 LEU 5 ALA 6 SER 7 ASP 8 GLU 9 GLU 10 ILE 11 GLN 12 ASP 13 VAL 14 SER 15 GLY 16 THR 17 TRP 18 TYR 19 LEU 20 LYS 21 ALA 22 MET 23 THR 24 VAL 25 ASP 26 ARG 27 GLU 28 PHE 29 PRO 30 GLU 31 MET 32 ASN 33 LEU 34 GLU 35 SER 36 VAL 37 THR 38 PRO 39 MET 40 THR 41 LEU 42 THR 43 THR 44 LEU 45 GLU 46 GLY 47 GLY 48 ASN 49 LEU 50 GLU 51 ALA 52 LYS 53 VAL 54 THR 55 MET 56 LEU 57 ILE 58 SER 59 GLY 60 ARG 61 CYS 62 GLN 63 GLU 64 VAL 65 LYS 66 ALA 67 VAL 68 LEU 69 GLU 70 LYS 71 THR 72 ASP 73 GLU 74 PRO 75 GLY 76 LYS 77 TYR 78 THR 79 ALA 80 ASP 81 GLY 82 GLY 83 LYS 84 HIS 85 VAL 86 ALA 87 TYR 88 ILE 89 ILE 90 ARG 91 SER 92 HIS 93 VAL 94 LYS 95 ASP 96 HIS 97 TYR 98 ILE 99 PHE 100 TYR 101 SER 102 GLU 103 GLY 104 GLU 105 LEU 106 HIS 107 GLY 108 LYS 109 PRO 110 VAL 111 ARG 112 GLY 113 VAL 114 LYS 115 LEU 116 VAL 117 GLY 118 ARG 119 ASP 120 PRO 121 LYS 122 ASN 123 ASN 124 LEU 125 GLU 126 ALA 127 LEU 128 GLU 129 ASP 130 PHE 131 GLU 132 LYS 133 ALA 134 ALA 135 GLY 136 ALA 137 ARG 138 GLY 139 LEU 140 SER 141 THR 142 GLU 143 SER 144 ILE 145 LEU 146 ILE 147 PRO 148 ARG 149 GLN 150 SER 151 GLU 152 THR 153 CYS 154 SER 155 PRO 156 GLY 157 SER 158 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 _Gene_mnemonic $entity_1 Human 9606 Eukaryota Metazoa Homo sapiens 'LCN1, VEGP' 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 $entity_1 'recombinant technology' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.0 mM [U-99% 13C; U-99% 15N] Lipocalin, 90 % H2O, 10 % D2O, 50 mM sodium phosphate, 0.04 % sodium azide, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling D2O 10 % 'natural abundance' H2O 90 % 'natural abundance' $entity_1 1.0 mM '[U-99% 13C; U-99% 15N]' 'sodium azide' 0.04 % 'natural abundance' 'sodium phosphate' 50 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name NMRView _Version . loop_ _Vendor _Address _Electronic_address 'Johnson, One Moon Scientific' . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name 'X-PLOR NIH' _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_3D_CBCA(CO)NH_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _Sample_label $sample_1 save_ save_3D_HNCACB_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $sample_1 save_ save_3D_HNCO_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_1 save_ save_3D_HNCACO_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACO' _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 'ionic strength' 50 . mM pH 7.4 . pH pressure 1 . atm temperature 310 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_3 stop_ loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_1 _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 3 3 LEU H H 8.277 . 1 2 3 3 LEU N N 123.087 . 1 3 4 4 LEU H H 8.064 . 1 4 4 4 LEU N N 121.266 . 1 5 5 5 ALA H H 8.324 . 1 6 5 5 ALA N N 124.029 . 1 7 6 6 SER H H 8.404 . 1 8 6 6 SER N N 114.967 . 1 9 7 7 ASP H H 8.606 . 1 10 7 7 ASP N N 121.633 . 1 11 8 8 GLU H H 8.481 . 1 12 8 8 GLU N N 119.129 . 1 13 9 9 GLU H H 7.970 . 1 14 9 9 GLU N N 120.181 . 1 15 10 10 ILE H H 8.019 . 1 16 10 10 ILE N N 121.323 . 1 17 13 13 VAL H H 7.676 . 1 18 13 13 VAL N N 117.169 . 1 19 14 14 SER H H 7.911 . 1 20 14 14 SER N N 115.341 . 1 21 15 15 GLY H H 9.304 . 1 22 15 15 GLY N N 111.249 . 1 23 16 16 THR H H 8.433 . 1 24 16 16 THR N N 119.188 . 1 25 17 17 TRP H H 9.077 . 1 26 17 17 TRP N N 129.279 . 1 27 18 18 TYR H H 9.285 . 1 28 18 18 TYR N N 117.301 . 1 29 19 19 LEU H H 10.292 . 1 30 19 19 LEU N N 128.509 . 1 31 20 20 LYS H H 8.671 . 1 32 20 20 LYS N N 124.390 . 1 33 21 21 ALA H H 7.428 . 1 34 21 21 ALA N N 115.811 . 1 35 22 22 MET H H 8.866 . 1 36 22 22 MET N N 115.629 . 1 37 23 23 THR H H 8.442 . 1 38 23 23 THR N N 112.193 . 1 39 24 24 VAL H H 8.356 . 1 40 24 24 VAL N N 118.096 . 1 41 25 25 ASP H H 8.413 . 1 42 25 25 ASP N N 122.887 . 1 43 27 27 GLU H H 8.642 . 1 44 27 27 GLU N N 118.052 . 1 45 28 28 PHE H H 7.911 . 1 46 28 28 PHE N N 119.670 . 1 47 30 30 GLU H H 8.958 . 1 48 30 30 GLU N N 118.852 . 1 49 31 31 MET H H 7.944 . 1 50 31 31 MET N N 119.044 . 1 51 33 33 LEU H H 7.667 . 1 52 33 33 LEU N N 122.915 . 1 53 34 34 GLU H H 9.233 . 1 54 34 34 GLU N N 126.983 . 1 55 35 35 SER H H 7.519 . 1 56 35 35 SER N N 110.189 . 1 57 36 36 VAL H H 8.512 . 1 58 36 36 VAL N N 114.484 . 1 59 37 37 THR H H 7.932 . 1 60 37 37 THR N N 114.260 . 1 61 39 39 MET H H 9.149 . 1 62 39 39 MET N N 124.924 . 1 63 40 40 THR H H 9.013 . 1 64 40 40 THR N N 118.904 . 1 65 41 41 LEU H H 9.091 . 1 66 41 41 LEU N N 128.010 . 1 67 42 42 THR H H 8.980 . 1 68 42 42 THR N N 120.288 . 1 69 43 43 THR H H 8.592 . 1 70 43 43 THR N N 121.971 . 1 71 44 44 LEU H H 8.693 . 1 72 44 44 LEU N N 127.624 . 1 73 45 45 GLU H H 8.436 . 1 74 45 45 GLU N N 121.337 . 1 75 47 47 GLY H H 8.261 . 1 76 47 47 GLY N N 106.817 . 1 77 48 48 ASN H H 7.087 . 1 78 48 48 ASN N N 118.411 . 1 79 49 49 LEU H H 8.880 . 1 80 49 49 LEU N N 120.424 . 1 81 50 50 GLU H H 9.027 . 1 82 50 50 GLU N N 123.491 . 1 83 51 51 ALA H H 9.109 . 1 84 51 51 ALA N N 131.266 . 1 85 52 52 LYS H H 8.656 . 1 86 52 52 LYS N N 122.673 . 1 87 53 53 VAL H H 8.579 . 1 88 53 53 VAL N N 123.074 . 1 89 54 54 THR H H 7.485 . 1 90 54 54 THR N N 121.844 . 1 91 55 55 MET H H 8.908 . 1 92 55 55 MET N N 124.555 . 1 93 56 56 LEU H H 8.638 . 1 94 56 56 LEU N N 126.761 . 1 95 57 57 ILE H H 8.839 . 1 96 57 57 ILE N N 127.214 . 1 97 58 58 SER H H 8.910 . 1 98 58 58 SER N N 123.818 . 1 99 59 59 GLY H H 8.620 . 1 100 59 59 GLY N N 103.922 . 1 101 60 60 ARG H H 7.920 . 1 102 60 60 ARG N N 120.145 . 1 103 61 61 CYS H H 8.682 . 1 104 61 61 CYS N N 121.787 . 1 105 62 62 GLN H H 9.477 . 1 106 62 62 GLN N N 126.091 . 1 107 63 63 GLU H H 8.879 . 1 108 63 63 GLU N N 128.339 . 1 109 64 64 VAL H H 9.195 . 1 110 64 64 VAL N N 129.863 . 1 111 65 65 LYS H H 8.543 . 1 112 65 65 LYS N N 128.322 . 1 113 66 66 ALA H H 8.849 . 1 114 66 66 ALA N N 128.084 . 1 115 67 67 VAL H H 8.334 . 1 116 67 67 VAL N N 122.376 . 1 117 68 68 LEU H H 9.395 . 1 118 68 68 LEU N N 129.897 . 1 119 69 69 GLU H H 9.718 . 1 120 69 69 GLU N N 124.199 . 1 121 70 70 LYS H H 8.276 . 1 122 70 70 LYS N N 124.148 . 1 123 71 71 THR H H 7.699 . 1 124 71 71 THR N N 114.037 . 1 125 72 72 ASP H H 8.393 . 1 126 72 72 ASP N N 116.574 . 1 127 73 73 GLU H H 8.128 . 1 128 73 73 GLU N N 122.537 . 1 129 75 75 GLY H H 8.660 . 1 130 75 75 GLY N N 111.302 . 1 131 76 76 LYS H H 7.491 . 1 132 76 76 LYS N N 120.164 . 1 133 77 77 TYR H H 9.468 . 1 134 77 77 TYR N N 129.434 . 1 135 78 78 THR H H 9.233 . 1 136 78 78 THR N N 109.944 . 1 137 79 79 ALA H H 8.815 . 1 138 79 79 ALA N N 121.795 . 1 139 80 80 ASP H H 9.065 . 1 140 80 80 ASP N N 119.163 . 1 141 81 81 GLY H H 9.042 . 1 142 81 81 GLY N N 108.721 . 1 143 82 82 GLY H H 7.943 . 1 144 82 82 GLY N N 106.387 . 1 145 83 83 LYS H H 7.431 . 1 146 83 83 LYS N N 119.309 . 1 147 84 84 HIS H H 7.885 . 1 148 84 84 HIS N N 116.859 . 1 149 85 85 VAL H H 8.496 . 1 150 85 85 VAL N N 122.969 . 1 151 86 86 ALA H H 8.810 . 1 152 86 86 ALA N N 127.203 . 1 153 87 87 TYR H H 9.304 . 1 154 87 87 TYR N N 118.100 . 1 155 88 88 ILE H H 9.012 . 1 156 88 88 ILE N N 122.539 . 1 157 89 89 ILE H H 9.247 . 1 158 89 89 ILE N N 128.072 . 1 159 90 90 ARG H H 8.985 . 1 160 90 90 ARG N N 127.184 . 1 161 91 91 SER H H 7.188 . 1 162 91 91 SER N N 116.951 . 1 163 92 92 HIS H H 8.565 . 1 164 92 92 HIS N N 123.788 . 1 165 93 93 VAL H H 8.406 . 1 166 93 93 VAL N N 122.065 . 1 167 94 94 LYS H H 8.263 . 1 168 94 94 LYS N N 126.608 . 1 169 95 95 ASP H H 9.220 . 1 170 95 95 ASP N N 120.639 . 1 171 96 96 HIS H H 7.753 . 1 172 96 96 HIS N N 112.882 . 1 173 97 97 TYR H H 9.358 . 1 174 97 97 TYR N N 119.544 . 1 175 98 98 ILE H H 9.521 . 1 176 98 98 ILE N N 121.123 . 1 177 99 99 PHE H H 9.555 . 1 178 99 99 PHE N N 127.273 . 1 179 100 100 TYR H H 9.436 . 1 180 100 100 TYR N N 127.986 . 1 181 101 101 SER H H 8.472 . 1 182 101 101 SER N N 121.564 . 1 183 102 102 GLU H H 8.350 . 1 184 102 102 GLU N N 119.552 . 1 185 103 103 GLY H H 8.324 . 1 186 103 103 GLY N N 109.872 . 1 187 104 104 GLU H H 8.154 . 1 188 104 104 GLU N N 122.347 . 1 189 105 105 LEU H H 8.913 . 1 190 105 105 LEU N N 125.377 . 1 191 107 107 GLY H H 8.723 . 1 192 107 107 GLY N N 104.048 . 1 193 108 108 LYS H H 7.845 . 1 194 108 108 LYS N N 121.623 . 1 195 110 110 VAL H H 8.351 . 1 196 110 110 VAL N N 119.533 . 1 197 112 112 GLY H H 8.282 . 1 198 112 112 GLY N N 106.712 . 1 199 113 113 VAL H H 8.163 . 1 200 113 113 VAL N N 113.869 . 1 201 114 114 LYS H H 9.045 . 1 202 114 114 LYS N N 122.288 . 1 203 115 115 LEU H H 8.707 . 1 204 115 115 LEU N N 125.479 . 1 205 116 116 VAL H H 9.253 . 1 206 116 116 VAL N N 122.724 . 1 207 117 117 GLY H H 9.171 . 1 208 117 117 GLY N N 106.890 . 1 209 118 118 ARG H H 7.648 . 1 210 118 118 ARG N N 119.322 . 1 211 119 119 ASP H H 8.058 . 1 212 119 119 ASP N N 118.425 . 1 213 125 125 GLU H H 8.295 . 1 214 125 125 GLU N N 120.592 . 1 215 126 126 ALA H H 8.379 . 1 216 126 126 ALA N N 123.383 . 1 217 127 127 LEU H H 7.859 . 1 218 127 127 LEU N N 119.401 . 1 219 128 128 GLU H H 8.159 . 1 220 128 128 GLU N N 120.554 . 1 221 129 129 ASP H H 7.724 . 1 222 129 129 ASP N N 119.793 . 1 223 130 130 PHE H H 8.443 . 1 224 130 130 PHE N N 120.239 . 1 225 131 131 GLU H H 8.698 . 1 226 131 131 GLU N N 120.617 . 1 227 132 132 LYS H H 7.960 . 1 228 132 132 LYS N N 120.201 . 1 229 133 133 ALA H H 8.174 . 1 230 133 133 ALA N N 123.394 . 1 231 134 134 ALA H H 8.304 . 1 232 134 134 ALA N N 119.496 . 1 233 135 135 GLY H H 8.278 . 1 234 135 135 GLY N N 106.317 . 1 235 136 136 ALA H H 7.942 . 1 236 136 136 ALA N N 123.935 . 1 237 137 137 ARG H H 7.096 . 1 238 137 137 ARG N N 114.886 . 1 239 138 138 GLY H H 7.756 . 1 240 138 138 GLY N N 107.254 . 1 241 139 139 LEU H H 7.755 . 1 242 139 139 LEU N N 120.691 . 1 243 143 143 SER H H 7.884 . 1 244 143 143 SER N N 114.269 . 1 245 144 144 ILE H H 7.726 . 1 246 144 144 ILE N N 121.831 . 1 247 145 145 LEU H H 8.976 . 1 248 145 145 LEU N N 129.181 . 1 249 146 146 ILE H H 8.578 . 1 250 146 146 ILE N N 127.109 . 1 251 149 149 GLN H H 8.459 . 1 252 149 149 GLN N N 121.948 . 1 253 150 150 SER H H 8.700 . 1 254 150 150 SER N N 118.590 . 1 255 151 151 GLU H H 8.772 . 1 256 151 151 GLU N N 123.214 . 1 257 152 152 THR H H 7.561 . 1 258 152 152 THR N N 107.080 . 1 259 156 156 GLY H H 8.508 . 1 260 156 156 GLY N N 109.075 . 1 261 157 157 SER H H 8.090 . 1 262 157 157 SER N N 115.393 . 1 263 158 158 ASP H H 8.016 . 1 264 158 158 ASP N N 127.590 . 1 stop_ save_