data_27562 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; GB1 crystalline protein U-13C,15N ; _BMRB_accession_number 27562 _BMRB_flat_file_name bmr27562.str _Entry_type original _Submission_date 2018-07-26 _Accession_date 2018-07-26 _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 Pawlak Tomasz . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 51 "13C chemical shifts" 149 "15N chemical shifts" 51 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2018-11-15 original BMRB . stop_ _Original_release_date 2018-07-26 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Simple and Robust Study of Backbone Dynamics of Crystalline Proteins Employing 1H-15N Dipolar Coupling Dispersion ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30070484 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Paluch Piotr . . 2 Pawlak Tomasz . . 3 awniczak Karol . . 4 Trebosc Julien . . 5 Lafon Olivier . . 6 Amoreux Jean P. . 7 Potrzebowski Marek J. . stop_ _Journal_abbreviation 'J. Phys. Chem. B.' _Journal_volume 122 _Journal_issue 34 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8146 _Page_last 8156 _Year 2018 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name GB1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'GB1, 1' $GB1 'GB1, 2' $GB1 'GB1, 3' $GB1 'GB1, 4' $GB1 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_GB1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common GB1 _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 56 _Mol_residue_sequence ; MQYKLILNGKTLKGETTTEA VDAATAEKVFKQYANDNGVD GEWTYDDATKTFTVTF ; loop_ _Residue_seq_code _Residue_label 1 MET 2 GLN 3 TYR 4 LYS 5 LEU 6 ILE 7 LEU 8 ASN 9 GLY 10 LYS 11 THR 12 LEU 13 LYS 14 GLY 15 GLU 16 THR 17 THR 18 THR 19 GLU 20 ALA 21 VAL 22 ASP 23 ALA 24 ALA 25 THR 26 ALA 27 GLU 28 LYS 29 VAL 30 PHE 31 LYS 32 GLN 33 TYR 34 ALA 35 ASN 36 ASP 37 ASN 38 GLY 39 VAL 40 ASP 41 GLY 42 GLU 43 TRP 44 THR 45 TYR 46 ASP 47 ASP 48 ALA 49 THR 50 LYS 51 THR 52 PHE 53 THR 54 VAL 55 THR 56 PHE 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 $GB1 . . . . . . 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 $GB1 na . Escherichia coli . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solid _Details '13C,15N,2H-GB-1 with back exchange NH. With Na2CuEDTA as paramegnetic doping to speed up relaxation rate.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $GB1 . mM '[U-13C; U-15N; U-2H], NH back exchage' stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3 loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details 'Avance III with 1.3mm H/C/N CP-MAS prob' save_ ############################# # NMR applied experiments # ############################# save_2D_hNH_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D hNH' _Sample_label $sample_1 save_ save_2D_hNCO_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D hNCO' _Sample_label $sample_1 save_ save_2D_hNCA_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D hNCA' _Sample_label $sample_1 save_ save_3D_hCONH_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hCONH' _Sample_label $sample_1 save_ save_3D_hCANH_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hCANH' _Sample_label $sample_1 save_ save_3D_hCOcaNH_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hCOcaNH' _Sample_label $sample_1 save_ save_3D_hcoCAcoNH_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hcoCAcoNH' _Sample_label $sample_1 save_ save_3D_hcaCBcaNH_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hcaCBcaNH' _Sample_label $sample_1 save_ save_3D_hcaCBcacoNH_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D hcaCBcacoNH' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details 'Solid state sample in 1.3mm rotor spining speed 60kHz' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pressure 1 . atm temperature 273 . 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 adamantan C 13 'methyl carbons' ppm 28.8 external direct . . . 1 DSS H 1 'methyl protons' ppm 0 external direct . . . 1 'liquid anhydrous ammonia' N 15 nitrogen ppm 0 external direct . . . 1 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 '3D hcaCBcacoNH' 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 'GB1, 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 1 1 MET C C 168.854 . . 2 1 1 MET CA C 51.723 . . 3 1 1 MET CB C 29.074 . . 4 2 2 GLN H H 8.375 . . 5 2 2 GLN C C 172.424 . . 6 2 2 GLN CA C 53.152 . . 7 2 2 GLN CB C 27.568 . . 8 2 2 GLN N N 124.106 . . 9 3 3 TYR H H 9.033 . . 10 3 3 TYR C C 172.327 . . 11 3 3 TYR CA C 54.409 . . 12 3 3 TYR CB C 40.124 . . 13 3 3 TYR N N 122.307 . . 14 4 4 LYS H H 9.123 . . 15 4 4 LYS C C 170.730 . . 16 4 4 LYS CA C 52.162 . . 17 4 4 LYS CB C 32.744 . . 18 4 4 LYS N N 121.792 . . 19 5 5 LEU H H 9.121 . . 20 5 5 LEU C C 172.352 . . 21 5 5 LEU CA C 50.333 . . 22 5 5 LEU CB C 39.190 . . 23 5 5 LEU N N 125.987 . . 24 6 6 ILE H H 8.954 . . 25 6 6 ILE C C 172.725 . . 26 6 6 ILE CA C 57.228 . . 27 6 6 ILE CB C 34.502 . . 28 6 6 ILE N N 124.922 . . 29 7 7 LEU H H 9.195 . . 30 7 7 LEU C C 172.590 . . 31 7 7 LEU CA C 52.037 . . 32 7 7 LEU CB C 39.511 . . 33 7 7 LEU N N 125.579 . . 34 8 8 ASN H H 8.972 . . 35 8 8 ASN C C 173.887 . . 36 8 8 ASN CA C 48.139 . . 37 8 8 ASN CB C 35.558 . . 38 8 8 ASN N N 123.744 . . 39 9 9 GLY H H 8.112 . . 40 9 9 GLY C C 170.785 . . 41 9 9 GLY CA C 41.949 . . 42 9 9 GLY N N 108.261 . . 43 10 10 LYS H H 9.844 . . 44 10 10 LYS C C 176.525 . . 45 10 10 LYS CA C 56.484 . . 46 10 10 LYS CB C 29.578 . . 47 10 10 LYS N N 119.759 . . 48 11 11 THR H H 8.905 . . 49 11 11 THR C C 170.883 . . 50 11 11 THR CA C 59.443 . . 51 11 11 THR CB C 66.644 . . 52 11 11 THR N N 105.642 . . 53 12 12 LEU H H 7.341 . . 54 12 12 LEU C C 171.441 . . 55 12 12 LEU CA C 51.852 . . 56 12 12 LEU CB C 39.894 . . 57 12 12 LEU N N 126.483 . . 58 13 13 LYS H H 8.819 . . 59 13 13 LYS C C 173.290 . . 60 13 13 LYS CA C 50.897 . . 61 13 13 LYS CB C 35.588 . . 62 13 13 LYS N N 121.890 . . 63 14 14 GLY H H 8.536 . . 64 14 14 GLY C C 168.856 . . 65 14 14 GLY CA C 42.085 . . 66 14 14 GLY N N 104.290 . . 67 15 15 GLU H H 8.763 . . 68 15 15 GLU C C 171.777 . . 69 15 15 GLU CA C 51.342 . . 70 15 15 GLU CB C 31.051 . . 71 15 15 GLU N N 119.789 . . 72 16 16 THR H H 8.825 . . 73 16 16 THR C C 169.519 . . 74 16 16 THR CA C 57.593 . . 75 16 16 THR CB C 67.923 . . 76 16 16 THR N N 113.472 . . 77 17 17 THR H H 8.321 . . 78 17 17 THR C C 171.918 . . 79 17 17 THR CA C 57.583 . . 80 17 17 THR CB C 69.928 . . 81 17 17 THR N N 114.711 . . 82 18 18 THR H H 9.125 . . 83 18 18 THR C C 168.853 . . 84 18 18 THR CA C 58.902 . . 85 18 18 THR CB C 68.100 . . 86 18 18 THR N N 114.655 . . 87 19 19 GLU H H 7.874 . . 88 19 19 GLU C C 173.405 . . 89 19 19 GLU CA C 51.885 . . 90 19 19 GLU CB C 28.003 . . 91 19 19 GLU N N 124.398 . . 92 20 20 ALA H H 9.331 . . 93 20 20 ALA C C 175.215 . . 94 20 20 ALA CA C 48.187 . . 95 20 20 ALA CB C 20.264 . . 96 20 20 ALA N N 123.772 . . 97 21 21 VAL H H 8.601 . . 98 21 21 VAL C C 172.599 . . 99 21 21 VAL CA C 60.951 . . 100 21 21 VAL CB C 28.844 . . 101 21 21 VAL N N 114.595 . . 102 25 25 THR C C 173.364 . . 103 25 25 THR CA C 64.754 . . 104 26 26 ALA H H 7.286 . . 105 26 26 ALA C C 174.821 . . 106 26 26 ALA CA C 52.340 . . 107 26 26 ALA CB C 14.224 . . 108 26 26 ALA N N 122.361 . . 109 27 27 GLU H H 8.599 . . 110 27 27 GLU C C 175.389 . . 111 27 27 GLU CA C 56.478 . . 112 27 27 GLU CB C 25.839 . . 113 27 27 GLU N N 115.230 . . 114 28 28 LYS H H 7.033 . . 115 28 28 LYS C C 176.469 . . 116 28 28 LYS CA C 57.566 . . 117 28 28 LYS CB C 29.490 . . 118 28 28 LYS N N 115.942 . . 119 29 29 VAL H H 7.541 . . 120 29 29 VAL C C 176.120 . . 121 29 29 VAL CA C 63.607 . . 122 29 29 VAL CB C 28.530 . . 123 29 29 VAL N N 117.564 . . 124 30 30 PHE H H 8.642 . . 125 30 30 PHE C C 176.625 . . 126 30 30 PHE CA C 54.769 . . 127 30 30 PHE CB C 34.491 . . 128 30 30 PHE N N 117.375 . . 129 31 31 LYS H H 9.008 . . 130 31 31 LYS C C 177.262 . . 131 31 31 LYS CA C 57.352 . . 132 31 31 LYS CB C 28.599 . . 133 31 31 LYS N N 119.223 . . 134 32 32 GLN H H 7.852 . . 135 32 32 GLN C C 175.080 . . 136 32 32 GLN CA C 56.191 . . 137 32 32 GLN CB C 25.738 . . 138 32 32 GLN N N 119.977 . . 139 33 33 TYR H H 8.559 . . 140 33 33 TYR C C 176.116 . . 141 33 33 TYR CA C 58.840 . . 142 33 33 TYR CB C 35.687 . . 143 33 33 TYR N N 119.575 . . 144 34 34 ALA H H 9.110 . . 145 34 34 ALA C C 177.083 . . 146 34 34 ALA CA C 53.308 . . 147 34 34 ALA CB C 14.855 . . 148 34 34 ALA N N 121.148 . . 149 35 35 ASN H H 8.434 . . 150 35 35 ASN C C 177.135 . . 151 35 35 ASN CA C 54.518 . . 152 35 35 ASN CB C 37.282 . . 153 35 35 ASN N N 117.054 . . 154 36 36 ASP H H 9.009 . . 155 36 36 ASP C C 173.697 . . 156 36 36 ASP CA C 53.395 . . 157 36 36 ASP CB C 35.486 . . 158 36 36 ASP N N 120.042 . . 159 37 37 ASN H H 7.282 . . 160 37 37 ASN C C 171.820 . . 161 37 37 ASN CA C 50.982 . . 162 37 37 ASN CB C 37.791 . . 163 37 37 ASN N N 113.775 . . 164 38 38 GLY H H 7.885 . . 165 38 38 GLY C C 171.589 . . 166 38 38 GLY CA C 44.142 . . 167 38 38 GLY N N 107.187 . . 168 39 39 VAL H H 8.212 . . 169 39 39 VAL C C 172.644 . . 170 39 39 VAL CA C 59.155 . . 171 39 39 VAL CB C 28.486 . . 172 39 39 VAL N N 120.577 . . 173 40 40 ASP H H 9.038 . . 174 40 40 ASP C C 172.678 . . 175 40 40 ASP CA C 50.656 . . 176 40 40 ASP N N 129.760 . . 177 41 41 GLY H H 7.894 . . 178 41 41 GLY C C 170.233 . . 179 41 41 GLY CA C 42.503 . . 180 41 41 GLY N N 107.031 . . 181 42 42 GLU H H 8.529 . . 182 42 42 GLU C C 175.395 . . 183 42 42 GLU CA C 52.718 . . 184 42 42 GLU CB C 28.464 . . 185 42 42 GLU N N 118.492 . . 186 43 43 TRP H H 9.267 . . 187 43 43 TRP C C 174.551 . . 188 43 43 TRP CA C 54.927 . . 189 43 43 TRP CB C 30.436 . . 190 43 43 TRP N N 123.863 . . 191 44 44 THR H H 8.934 . . 192 44 44 THR C C 171.438 . . 193 44 44 THR CA C 58.296 . . 194 44 44 THR CB C 70.391 . . 195 44 44 THR N N 107.730 . . 196 45 45 TYR H H 9.248 . . 197 45 45 TYR C C 169.385 . . 198 45 45 TYR CA C 55.147 . . 199 45 45 TYR CB C 39.703 . . 200 45 45 TYR N N 117.500 . . 201 46 46 ASP H H 7.412 . . 202 46 46 ASP C C 174.088 . . 203 46 46 ASP CA C 48.407 . . 204 46 46 ASP CB C 39.965 . . 205 46 46 ASP N N 125.076 . . 206 47 47 ASP H H 8.635 . . 207 47 47 ASP C C 174.856 . . 208 47 47 ASP CA C 53.947 . . 209 47 47 ASP N N 124.009 . . 210 48 48 ALA H H 8.409 . . 211 48 48 ALA C C 176.990 . . 212 48 48 ALA CA C 51.433 . . 213 48 48 ALA CB C 15.779 . . 214 48 48 ALA N N 117.490 . . 215 49 49 THR H H 6.889 . . 216 49 49 THR C C 172.995 . . 217 49 49 THR CA C 57.905 . . 218 49 49 THR CB C 67.505 . . 219 49 49 THR N N 102.758 . . 220 50 50 LYS H H 7.866 . . 221 50 50 LYS C C 172.929 . . 222 50 50 LYS CA C 52.889 . . 223 50 50 LYS CB C 24.933 . . 224 50 50 LYS N N 118.660 . . 225 51 51 THR H H 7.385 . . 226 51 51 THR C C 171.837 . . 227 51 51 THR CA C 59.871 . . 228 51 51 THR CB C 68.834 . . 229 51 51 THR N N 111.127 . . 230 52 52 PHE H H 10.648 . . 231 52 52 PHE C C 173.189 . . 232 52 52 PHE CA C 53.940 . . 233 52 52 PHE CB C 40.165 . . 234 52 52 PHE N N 128.656 . . 235 53 53 THR H H 9.195 . . 236 53 53 THR C C 169.601 . . 237 53 53 THR CA C 57.787 . . 238 53 53 THR CB C 69.069 . . 239 53 53 THR N N 111.081 . . 240 54 54 VAL H H 8.122 . . 241 54 54 VAL C C 170.215 . . 242 54 54 VAL CA C 55.909 . . 243 54 54 VAL CB C 29.371 . . 244 54 54 VAL N N 117.069 . . 245 55 55 THR H H 8.359 . . 246 55 55 THR C C 171.586 . . 247 55 55 THR CA C 58.634 . . 248 55 55 THR CB C 69.275 . . 249 55 55 THR N N 122.695 . . 250 56 56 PHE H H 7.851 . . 251 56 56 PHE N N 129.886 . . stop_ save_