data_15380 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Crystal Polymorphism of GB1 Examined by Solid-State NMR Spectroscopy and X-ray Diffraction ; _BMRB_accession_number 15380 _BMRB_flat_file_name bmr15380.str _Entry_type original _Submission_date 2007-07-16 _Accession_date 2007-07-16 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Microcrystal polymorphs of beta 1 domain of Protein G (GB1)' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Frericks-Schmidt Heather L. . 2 Sperling Lindsay J. . 3 Gao YiGui . . 4 Wylie Benjamin J. . 5 Boettcher John M. . 6 Wilson Scott R. . 7 Rienstra Chad M. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 483 "15N chemical shifts" 135 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-10-11 update author 'update chemical shifts of Form E' 2007-12-21 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 15156 'Solid-state NMR of GB1 T2Q: 13C and 15N chemical shift assignment' stop_ _Original_release_date 2016-10-11 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Crystal Polymorphism of Protein GB1 Examined by Solid-State NMR Spectroscopy and X-ray Diffraction ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18052145 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Frericks-Schmidt Heather L. . 2 Sperling Lindsay J. . 3 Gao YiGui . . 4 Wylie Benjamin J. . 5 Boettcher John M. . 6 Wilson Scott R. . 7 Rienstra Chad M. . stop_ _Journal_abbreviation 'J. Phys. Chem. B' _Journal_volume 111 _Journal_issue 51 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 14362 _Page_last 14369 _Year 2007 _Details . loop_ _Keyword 'formulation chemistry' polymorphism 'protein x-ray powder diffractio' 'single crystal diffraction' 'solid-state NMR' 'therapeutic proteins' stop_ 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 $GB1 stop_ _System_molecular_weight 6900 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'single chain polypeptide' save_ ######################## # Monomeric polymers # ######################## save_GB1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common GB1 _Molecular_mass 6900 _Mol_thiol_state 'not present' loop_ _Biological_function 'immunoglobulin binding domain' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 56 _Mol_residue_sequence ; MQYKLILNGKTLKGETTTEA VDAATAEKVFKQYANDNGVD GEWTYDDATKTFTVTE ; 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 GLU stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . 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 UNP P06654 'IgG-binding protein G' . . . . . stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Variant $GB1 'Staphylococcus sp. group G' 1320 Bacteria . Staphylococcus 'group G' 2TQ 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 'recombinant technology' . Escherichia coli BL21(DE3) 'synthetic GB1 T2Q (Smith, Withka, Regan, Biochemistry 1994, 33, 5510-5517 )' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_formulation_D _Saveframe_category sample _Sample_type 'polycrystalline powder' _Details ; Prepared using batch crystallization conditions with a protein solution of 10 mg/mL of GB1 in 50 mM sodium phosphate buffer (pH=5.5) and a reservoir solution of 55% MPD, 15% IPA and 50 mM NaCl in 7.5 mM sodium acetate buffer (pH=4.5) ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $GB1 15 mg '[U-100% 13C; U-100% 15N]' stop_ save_ save_formulation_E _Saveframe_category sample _Sample_type 'polycrystalline powder' _Details ; Prepared using batch crystallization conditions with a protein solution of 10 mg/mL of GB1 in 50 mM sodium phosphate buffer (pH=5.5) and a reservoir solution of 55% MPD, 25% IPA and 150 mM NaCl in 16.7 mM sodium acetate buffer (pH=4.5) ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $GB1 17 mg '[U-99% 13C; U-99% 15N]' stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task '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_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_ip500 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model InfinityPlus _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_N(CA)CX_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D N(CA)CX' _Sample_label $formulation_D save_ save_2D_N(CO)CX_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D N(CO)CX' _Sample_label $formulation_D save_ save_3D_NCACX_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCACX' _Sample_label $formulation_D save_ save_3D_NCOCX_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCOCX' _Sample_label $formulation_D save_ save_2D_CC_DARR_mixing_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CC DARR mixing' _Sample_label $formulation_D save_ save_2D_CC_SPC5_mixing_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CC SPC5 mixing' _Sample_label $formulation_D save_ save_2D_N(CA)CX_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D N(CA)CX' _Sample_label $formulation_E save_ save_2D_N(CO)CX_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D N(CO)CX' _Sample_label $formulation_E save_ save_3D_NCACX_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCACX' _Sample_label $formulation_E save_ save_3D_NCOCX_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCOCX' _Sample_label $formulation_E save_ save_2D_CC_DARR_mixing_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CC DARR mixing' _Sample_label $formulation_E save_ save_2D_CC_SPC5_mixing_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D CC SPC5 mixing' _Sample_label $formulation_E save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pressure 1 . atm 'temperature controller setting' 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 adamantane C 13 'alkane carbon' ppm 40.48 external direct . 'separate tube (no insert) similar to the experimental sample tube' 'magic angle' 1.0 adamantane N 15 'alkane carbon' ppm 40.48 external direct . 'separate tube (no insert) similar to the experimental sample tube' 'magic angle' 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_GB1_formulation_D_chemical_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $SPARKY $NMRPipe stop_ loop_ _Experiment_label '2D N(CA)CX' '2D N(CO)CX' '3D NCACX' '3D NCOCX' '2D CC DARR mixing' '2D CC SPC5 mixing' stop_ loop_ _Sample_label $formulation_D stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name GB1 _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 171.38 0.06 1 2 1 1 MET CA C 54.27 0.07 1 3 1 1 MET CB C 32.45 0.07 1 4 1 1 MET CE C 15.86 0.02 1 5 1 1 MET CG C 30.17 0.09 1 6 1 1 MET N N 40.04 0.06 1 7 2 2 GLN C C 174.95 0.03 1 8 2 2 GLN CA C 55.80 0.05 1 9 2 2 GLN CB C 30.43 0.05 1 10 2 2 GLN CD C 180.29 0.05 1 11 2 2 GLN CG C 35.29 0.07 1 12 2 2 GLN N N 125.29 0.07 1 13 2 2 GLN NE2 N 113.27 0.01 1 14 3 3 TYR C C 174.90 0.06 1 15 3 3 TYR CA C 56.89 0.11 1 16 3 3 TYR CB C 43.46 0.10 1 17 3 3 TYR CZ C 158.03 0.13 1 18 3 3 TYR N N 123.23 0.04 1 19 4 4 LYS C C 173.23 0.05 1 20 4 4 LYS CA C 54.81 0.05 1 21 4 4 LYS CB C 36.24 0.04 1 22 4 4 LYS CD C 28.96 0.05 1 23 4 4 LYS CE C 42.14 0.05 1 24 4 4 LYS CG C 25.46 0.17 1 25 4 4 LYS N N 122.78 0.10 1 26 4 4 LYS NZ N 33.19 0.04 1 27 5 5 LEU C C 174.78 0.05 1 28 5 5 LEU CA C 52.91 0.04 1 29 5 5 LEU CB C 42.46 0.02 1 30 5 5 LEU CD1 C 25.05 0.06 2 31 5 5 LEU CD2 C 25.71 0.05 2 32 5 5 LEU CG C 27.33 0.02 1 33 5 5 LEU N N 127.03 0.07 1 34 6 6 ILE C C 175.24 0.05 1 35 6 6 ILE CA C 59.93 0.04 1 36 6 6 ILE CB C 37.81 0.04 1 37 6 6 ILE CD1 C 12.72 0.04 1 38 6 6 ILE CG1 C 27.41 0.04 1 39 6 6 ILE CG2 C 17.57 0.04 1 40 6 6 ILE N N 126.23 0.03 1 41 7 7 LEU C C 175.13 0.06 1 42 7 7 LEU CA C 54.62 0.05 1 43 7 7 LEU CB C 42.92 0.02 1 44 7 7 LEU CD1 C 26.14 0.10 2 45 7 7 LEU CD2 C 25.08 0.03 2 46 7 7 LEU CG C 27.07 0.06 1 47 7 7 LEU N N 127.06 0.05 1 48 8 8 ASN C C 176.37 0.06 1 49 8 8 ASN CA C 50.70 0.04 1 50 8 8 ASN CB C 38.29 0.04 1 51 8 8 ASN CG C 176.51 0.07 1 52 8 8 ASN N N 125.14 0.04 1 53 8 8 ASN ND2 N 110.70 0.01 1 54 9 9 GLY C C 173.14 0.05 1 55 9 9 GLY CA C 44.60 0.07 1 56 9 9 GLY N N 109.59 0.01 1 57 10 10 LYS C C 179.12 0.06 1 58 10 10 LYS CA C 59.23 0.06 1 59 10 10 LYS CB C 32.86 0.10 1 60 10 10 LYS CD C 29.22 0.07 1 61 10 10 LYS CE C 42.21 0.02 1 62 10 10 LYS CG C 25.71 0.05 1 63 10 10 LYS N N 121.04 0.02 1 64 10 10 LYS NZ N 33.50 0.09 1 65 11 11 THR C C 173.34 0.07 1 66 11 11 THR CA C 61.89 0.04 1 67 11 11 THR CB C 69.39 0.04 1 68 11 11 THR CG2 C 22.48 0.07 1 69 11 11 THR N N 106.34 0.02 1 70 12 12 LEU C C 173.84 0.07 1 71 12 12 LEU CA C 54.39 0.04 1 72 12 12 LEU CB C 43.04 0.05 1 73 12 12 LEU CD1 C 26.02 0.02 2 74 12 12 LEU CD2 C 22.97 0.03 2 75 12 12 LEU CG C 27.86 0.03 1 76 12 12 LEU N N 127.84 0.06 1 77 13 13 LYS C C 175.72 0.03 1 78 13 13 LYS CA C 53.35 0.04 1 79 13 13 LYS CB C 38.92 0.04 1 80 13 13 LYS CD C 29.76 0.04 1 81 13 13 LYS CE C 43.02 0.07 1 82 13 13 LYS CG C 26.08 0.02 1 83 13 13 LYS N N 123.30 0.04 1 84 13 13 LYS NZ N 31.52 0.03 1 85 14 14 GLY C C 171.35 0.05 1 86 14 14 GLY CA C 44.93 0.03 1 87 14 14 GLY N N 105.56 0.02 1 88 15 15 GLU C C 174.15 0.06 1 89 15 15 GLU CA C 53.87 0.02 1 90 15 15 GLU CB C 34.25 0.08 1 91 15 15 GLU CD C 181.96 0.06 1 92 15 15 GLU CG C 35.46 0.02 1 93 15 15 GLU N N 120.98 0.04 1 94 16 16 THR C C 171.98 0.03 1 95 16 16 THR CA C 60.05 0.05 1 96 16 16 THR CB C 70.40 0.06 1 97 16 16 THR CG2 C 20.04 0.04 1 98 16 16 THR N N 115.07 0.05 1 99 17 17 THR C C 174.30 0.02 1 100 17 17 THR CA C 60.27 0.04 1 101 17 17 THR CB C 72.61 0.04 1 102 17 17 THR CG2 C 21.79 0.03 1 103 17 17 THR N N 116.03 0.01 1 104 18 18 THR C C 171.20 0.05 1 105 18 18 THR CA C 61.30 0.05 1 106 18 18 THR CB C 70.85 0.04 1 107 18 18 THR CG2 C 18.86 0.05 1 108 18 18 THR N N 116.10 0.03 1 109 19 19 GLU C C 175.83 0.05 1 110 19 19 GLU CA C 54.28 0.09 1 111 19 19 GLU CB C 30.80 0.10 1 112 19 19 GLU CD C 182.32 0.04 1 113 19 19 GLU CG C 35.92 0.09 1 114 19 19 GLU N N 125.50 0.03 1 115 20 20 ALA C C 177.71 0.06 1 116 20 20 ALA CA C 50.67 0.04 1 117 20 20 ALA CB C 23.64 0.02 1 118 20 20 ALA N N 125.68 0.05 1 119 21 21 VAL C C 174.92 0.05 1 120 21 21 VAL CA C 63.51 0.04 1 121 21 21 VAL CB C 31.91 0.10 1 122 21 21 VAL CG1 C 21.01 0.03 2 123 21 21 VAL CG2 C 20.70 0.07 2 124 21 21 VAL N N 116.40 0.04 1 125 22 22 ASP C C 175.03 0.04 1 126 22 22 ASP CA C 52.48 0.02 1 127 22 22 ASP CB C 42.34 0.03 1 128 22 22 ASP CG C 179.77 0.07 1 129 22 22 ASP N N 115.45 0.03 1 130 23 23 ALA C C 179.56 0.02 1 131 23 23 ALA CA C 54.42 0.08 1 132 23 23 ALA CB C 18.24 0.04 1 133 23 23 ALA N N 122.43 0.08 1 134 24 24 ALA C C 181.40 0.05 1 135 24 24 ALA CA C 54.51 0.04 1 136 24 24 ALA CB C 18.23 0.02 1 137 24 24 ALA N N 120.77 0.04 1 138 25 25 THR C C 175.86 0.03 1 139 25 25 THR CA C 67.43 0.09 1 140 25 25 THR CB C 67.80 0.04 1 141 25 25 THR CG2 C 21.40 0.02 1 142 25 25 THR N N 117.40 0.07 1 143 26 26 ALA C C 177.23 0.04 1 144 26 26 ALA CA C 54.97 0.04 1 145 26 26 ALA CB C 17.48 0.02 1 146 26 26 ALA N N 123.77 0.07 1 147 27 27 GLU C C 177.75 0.03 1 148 27 27 GLU CA C 59.10 0.05 1 149 27 27 GLU CB C 28.99 0.05 1 150 27 27 GLU CD C 181.49 0.02 1 151 27 27 GLU CG C 35.48 0.04 1 152 27 27 GLU N N 116.31 0.04 1 153 28 28 LYS C C 179.09 0.08 1 154 28 28 LYS CA C 60.19 0.04 1 155 28 28 LYS CB C 32.77 0.06 1 156 28 28 LYS CD C 30.08 0.06 1 157 28 28 LYS CE C 42.31 0.06 1 158 28 28 LYS CG C 26.37 0.07 1 159 28 28 LYS N N 117.38 0.03 1 160 28 28 LYS NZ N 32.92 0.06 1 161 29 29 VAL C C 178.88 0.06 1 162 29 29 VAL CA C 66.26 0.04 1 163 29 29 VAL CB C 31.89 0.03 1 164 29 29 VAL CG1 C 22.21 0.05 2 165 29 29 VAL CG2 C 20.99 0.03 2 166 29 29 VAL N N 119.23 0.04 1 167 30 30 PHE C C 179.23 0.02 1 168 30 30 PHE CA C 57.42 0.08 1 169 30 30 PHE CB C 37.39 0.04 1 170 30 30 PHE N N 118.80 0.06 1 171 31 31 LYS C C 179.59 0.05 1 172 31 31 LYS CA C 60.11 0.03 1 173 31 31 LYS CB C 31.60 0.05 1 174 31 31 LYS CD C 29.40 0.07 1 175 31 31 LYS CE C 41.18 0.07 1 176 31 31 LYS CG C 27.31 0.10 1 177 31 31 LYS N N 120.59 0.07 1 178 31 31 LYS NZ N 32.21 0.04 1 179 32 32 GLN C C 177.52 0.05 1 180 32 32 GLN CA C 58.82 0.05 1 181 32 32 GLN CB C 28.89 0.04 1 182 32 32 GLN CD C 179.86 0.06 1 183 32 32 GLN CG C 34.12 0.03 1 184 32 32 GLN N N 121.29 0.04 1 185 32 32 GLN NE2 N 115.71 0.02 1 186 33 33 TYR C C 178.68 0.06 1 187 33 33 TYR CA C 61.54 0.05 1 188 33 33 TYR CB C 36.87 0.10 1 189 33 33 TYR CZ C 159.52 0.02 1 190 33 33 TYR N N 120.93 0.04 1 191 34 34 ALA C C 179.55 0.05 1 192 34 34 ALA CA C 56.05 0.02 1 193 34 34 ALA CB C 18.04 0.01 1 194 34 34 ALA N N 122.67 0.04 1 195 35 35 ASN C C 179.53 0.04 1 196 35 35 ASN CA C 57.06 0.06 1 197 35 35 ASN CB C 39.32 0.06 1 198 35 35 ASN CG C 175.96 0.04 1 199 35 35 ASN N N 118.14 0.04 1 200 35 35 ASN ND2 N 113.28 0.03 1 201 36 36 ASP C C 176.17 0.02 1 202 36 36 ASP CA C 55.90 0.03 1 203 36 36 ASP CB C 38.26 0.07 1 204 36 36 ASP CG C 177.66 0.08 1 205 36 36 ASP N N 121.15 0.06 1 206 37 37 ASN C C 174.24 0.05 1 207 37 37 ASN CA C 53.52 0.03 1 208 37 37 ASN CB C 40.29 0.06 1 209 37 37 ASN CG C 176.79 0.06 1 210 37 37 ASN N N 115.05 0.06 1 211 37 37 ASN ND2 N 114.48 0.02 1 212 38 38 GLY C C 174.00 0.02 1 213 38 38 GLY CA C 46.85 0.02 1 214 38 38 GLY N N 108.44 0.03 1 215 39 39 VAL C C 175.14 0.07 1 216 39 39 VAL CA C 61.74 0.05 1 217 39 39 VAL CB C 31.88 0.03 1 218 39 39 VAL CG1 C 21.94 0.02 2 219 39 39 VAL CG2 C 21.94 0.02 2 220 39 39 VAL N N 121.77 0.04 1 221 40 40 ASP C C 174.92 0.06 1 222 40 40 ASP CA C 52.74 0.04 1 223 40 40 ASP CB C 41.70 0.02 1 224 40 40 ASP CG C 180.79 0.08 1 225 40 40 ASP N N 131.11 0.04 1 226 41 41 GLY C C 172.70 0.07 1 227 41 41 GLY CA C 45.18 0.07 1 228 41 41 GLY N N 108.23 0.01 1 229 42 42 GLU C C 177.82 0.05 1 230 42 42 GLU CA C 55.20 0.05 1 231 42 42 GLU CB C 31.57 0.07 1 232 42 42 GLU CD C 182.13 0.06 1 233 42 42 GLU CG C 35.98 0.07 1 234 42 42 GLU N N 119.21 0.03 1 235 43 43 TRP C C 177.37 0.09 1 236 43 43 TRP CA C 57.49 0.06 1 237 43 43 TRP CB C 33.90 0.10 1 238 43 43 TRP CD1 C 127.16 0.07 1 239 43 43 TRP CD2 C 130.05 0.14 1 240 43 43 TRP CE2 C 138.51 0.09 1 241 43 43 TRP CE3 C 119.64 0.09 1 242 43 43 TRP CG C 111.74 0.10 1 243 43 43 TRP CH2 C 122.95 0.22 1 244 43 43 TRP CZ2 C 114.71 0.09 1 245 43 43 TRP CZ3 C 120.92 0.04 1 246 43 43 TRP N N 125.00 0.06 1 247 43 43 TRP NE1 N 131.39 0.05 1 248 44 44 THR C C 173.94 0.06 1 249 44 44 THR CA C 60.84 0.06 1 250 44 44 THR CB C 73.04 0.03 1 251 44 44 THR CG2 C 21.00 0.05 1 252 44 44 THR N N 109.11 0.02 1 253 45 45 TYR C C 171.89 0.07 1 254 45 45 TYR CA C 57.81 0.06 1 255 45 45 TYR CB C 43.00 0.07 1 256 45 45 TYR CZ C 157.49 0.10 1 257 45 45 TYR N N 118.69 0.04 1 258 46 46 ASP C C 176.34 0.04 1 259 46 46 ASP CA C 50.86 0.04 1 260 46 46 ASP CB C 42.68 0.08 1 261 46 46 ASP CG C 180.23 0.07 1 262 46 46 ASP N N 126.38 0.04 1 263 47 47 ASP C C 177.36 0.06 1 264 47 47 ASP CA C 54.72 0.07 1 265 47 47 ASP CB C 43.02 0.01 1 266 47 47 ASP CG C 179.60 0.06 1 267 47 47 ASP N N 123.55 0.05 1 268 48 48 ALA C C 179.64 0.03 1 269 48 48 ALA CA C 54.04 0.06 1 270 48 48 ALA CB C 18.99 0.01 1 271 48 48 ALA N N 119.01 0.02 1 272 49 49 THR C C 175.68 0.05 1 273 49 49 THR CA C 60.23 0.05 1 274 49 49 THR CB C 69.91 0.06 1 275 49 49 THR CG2 C 21.57 0.04 1 276 49 49 THR N N 104.01 0.02 1 277 50 50 LYS C C 175.45 0.07 1 278 50 50 LYS CA C 55.58 0.05 1 279 50 50 LYS CB C 27.99 0.06 1 280 50 50 LYS CD C 28.22 0.05 1 281 50 50 LYS CE C 43.38 0.06 1 282 50 50 LYS CG C 24.40 0.10 1 283 50 50 LYS N N 119.96 0.03 1 284 50 50 LYS NZ N 33.95 0.03 1 285 51 51 THR C C 174.36 0.03 1 286 51 51 THR CA C 62.45 0.03 1 287 51 51 THR CB C 71.65 0.03 1 288 51 51 THR CG2 C 21.24 0.03 1 289 51 51 THR N N 112.00 0.03 1 290 52 52 PHE C C 175.71 0.07 1 291 52 52 PHE CA C 56.51 0.11 1 292 52 52 PHE CB C 42.78 0.02 1 293 52 52 PHE N N 130.31 0.07 1 294 53 53 THR C C 172.19 0.04 1 295 53 53 THR CA C 60.31 0.02 1 296 53 53 THR CB C 71.66 0.01 1 297 53 53 THR CG2 C 21.03 0.08 1 298 53 53 THR N N 112.15 0.04 1 299 54 54 VAL C C 172.59 0.03 1 300 54 54 VAL CA C 58.40 0.03 1 301 54 54 VAL CB C 32.67 0.05 1 302 54 54 VAL CG1 C 21.83 0.06 2 303 54 54 VAL CG2 C 19.68 0.02 2 304 54 54 VAL N N 118.34 0.03 1 305 55 55 THR C C 174.18 0.06 1 306 55 55 THR CA C 61.25 0.05 1 307 55 55 THR CB C 72.04 0.04 1 308 55 55 THR CG2 C 21.35 0.08 1 309 55 55 THR N N 124.11 0.04 1 310 56 56 GLU C C 180.55 0.06 1 311 56 56 GLU CA C 57.57 0.04 1 312 56 56 GLU CB C 33.24 0.05 1 313 56 56 GLU CD C 183.17 0.02 1 314 56 56 GLU CG C 38.80 0.04 1 315 56 56 GLU N N 131.06 0.03 1 stop_ save_ save_GB1_formulation_E_chemical_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $SPARKY $NMRPipe stop_ loop_ _Experiment_label '2D N(CA)CX' '2D N(CO)CX' '3D NCACX' '3D NCOCX' '2D CC DARR mixing' '2D CC SPC5 mixing' stop_ loop_ _Sample_label $formulation_E stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name GB1 _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 171.29 0.02 1 2 1 1 MET CA C 54.28 0.05 1 3 1 1 MET CB C 32.32 0.04 1 4 1 1 MET CE C 15.87 0.01 1 5 1 1 MET CG C 30.10 0.10 1 6 1 1 MET N N 39.98 0.07 1 7 2 2 GLN C C 174.89 0.06 1 8 2 2 GLN CA C 55.66 0.05 1 9 2 2 GLN CB C 30.59 0.06 1 10 2 2 GLN CD C 180.27 0.03 1 11 2 2 GLN CG C 35.35 0.09 1 12 2 2 GLN N N 125.00 0.05 1 13 2 2 GLN NE2 N 113.26 0.05 1 14 3 3 TYR C C 174.87 0.05 1 15 3 3 TYR CA C 56.99 0.06 1 16 3 3 TYR CB C 43.68 0.08 1 17 3 3 TYR N N 123.02 0.06 1 18 4 4 LYS C C 173.23 0.04 1 19 4 4 LYS CA C 54.82 0.07 1 20 4 4 LYS CB C 36.21 0.08 1 21 4 4 LYS CD C 28.98 0.10 1 22 4 4 LYS CE C 42.19 0.04 1 23 4 4 LYS CG C 25.51 0.11 1 24 4 4 LYS N N 122.55 0.08 1 25 4 4 LYS NZ N 33.54 0.06 1 26 5 5 LEU C C 174.84 0.05 1 27 5 5 LEU CA C 52.96 0.07 1 28 5 5 LEU CB C 42.57 0.04 1 29 5 5 LEU CD1 C 25.85 0.05 2 30 5 5 LEU CD2 C 25.03 0.04 2 31 5 5 LEU CG C 27.35 0.06 1 32 5 5 LEU N N 126.71 0.06 1 33 6 6 ILE C C 175.29 0.08 1 34 6 6 ILE CA C 59.89 0.05 1 35 6 6 ILE CB C 37.87 0.04 1 36 6 6 ILE CD1 C 12.70 0.04 1 37 6 6 ILE CG1 C 27.39 0.03 1 38 6 6 ILE CG2 C 17.59 0.02 1 39 6 6 ILE N N 126.05 0.06 1 40 7 7 LEU C C 175.03 0.05 1 41 7 7 LEU CA C 54.64 0.10 1 42 7 7 LEU CB C 43.03 0.06 1 43 7 7 LEU CD1 C 26.09 0.04 2 44 7 7 LEU CD2 C 25.16 0.05 2 45 7 7 LEU CG C 27.18 0.03 1 46 7 7 LEU N N 126.78 0.05 1 47 8 8 ASN C C 176.40 0.08 1 48 8 8 ASN CA C 50.64 0.05 1 49 8 8 ASN CB C 38.28 0.07 1 50 8 8 ASN CG C 176.48 0.09 1 51 8 8 ASN N N 124.80 0.05 1 52 8 8 ASN ND2 N 110.41 0.07 1 53 9 9 GLY C C 173.32 0.08 1 54 9 9 GLY CA C 44.59 0.07 1 55 9 9 GLY N N 109.30 0.04 1 56 10 10 LYS C C 179.08 0.07 1 57 10 10 LYS CA C 59.08 0.09 1 58 10 10 LYS CB C 32.79 0.04 1 59 10 10 LYS CD C 29.22 0.16 1 60 10 10 LYS CE C 42.43 0.05 1 61 10 10 LYS CG C 25.70 0.06 1 62 10 10 LYS N N 120.62 0.03 1 63 10 10 LYS NZ N 33.90 0.06 1 64 11 11 THR C C 173.21 0.04 1 65 11 11 THR CA C 61.93 0.04 1 66 11 11 THR CB C 69.56 0.05 1 67 11 11 THR CG2 C 22.65 0.07 1 68 11 11 THR N N 106.48 0.10 1 69 12 12 LEU C C 173.95 0.09 1 70 12 12 LEU CA C 54.39 0.08 1 71 12 12 LEU CB C 43.28 0.04 1 72 12 12 LEU CD1 C 26.06 0.01 2 73 12 12 LEU CD2 C 23.09 0.03 2 74 12 12 LEU CG C 27.96 0.05 1 75 12 12 LEU N N 127.19 0.10 1 76 13 13 LYS C C 175.78 0.05 1 77 13 13 LYS CA C 53.33 0.08 1 78 13 13 LYS CB C 38.89 0.02 1 79 13 13 LYS CD C 29.81 0.04 1 80 13 13 LYS CE C 42.94 0.05 1 81 13 13 LYS CG C 26.01 0.03 1 82 13 13 LYS N N 122.93 0.04 1 83 13 13 LYS NZ N 31.98 0.02 1 84 14 14 GLY C C 171.22 0.03 1 85 14 14 GLY CA C 44.98 0.05 1 86 14 14 GLY N N 105.42 0.08 1 87 15 15 GLU C C 174.17 0.05 1 88 15 15 GLU CA C 53.81 0.05 1 89 15 15 GLU CB C 33.99 0.05 1 90 15 15 GLU CD C 181.94 0.05 1 91 15 15 GLU CG C 34.81 0.11 1 92 15 15 GLU N N 120.65 0.02 1 93 16 16 THR C C 172.00 0.05 1 94 16 16 THR CA C 60.04 0.05 1 95 16 16 THR CB C 70.45 0.07 1 96 16 16 THR CG2 C 20.08 0.06 1 97 16 16 THR N N 115.05 0.08 1 98 17 17 THR C C 174.40 0.10 1 99 17 17 THR CA C 60.15 0.07 1 100 17 17 THR CB C 72.64 0.07 1 101 17 17 THR CG2 C 21.81 0.04 1 102 17 17 THR N N 115.37 0.08 1 103 18 18 THR C C 171.39 0.09 1 104 18 18 THR CA C 61.43 0.05 1 105 18 18 THR CB C 70.81 0.04 1 106 18 18 THR CG2 C 18.87 0.05 1 107 18 18 THR N N 115.61 0.08 1 108 19 19 GLU C C 175.89 0.09 1 109 19 19 GLU CA C 54.50 0.06 1 110 19 19 GLU CB C 30.88 0.03 1 111 19 19 GLU CD C 182.44 0.03 1 112 19 19 GLU CG C 36.04 0.07 1 113 19 19 GLU N N 125.07 0.06 1 114 20 20 ALA C C 177.74 0.01 1 115 20 20 ALA CA C 50.74 0.04 1 116 20 20 ALA CB C 23.51 0.01 1 117 20 20 ALA N N 124.73 0.05 1 118 21 21 VAL C C 175.00 0.06 1 119 21 21 VAL CA C 63.61 0.07 1 120 21 21 VAL CB C 32.00 0.08 1 121 21 21 VAL CG1 C 20.24 0.08 2 122 21 21 VAL CG2 C 21.41 0.04 2 123 21 21 VAL N N 115.80 0.06 1 124 22 22 ASP C C 175.03 0.06 1 125 22 22 ASP CA C 52.65 0.09 1 126 22 22 ASP CB C 42.37 0.03 1 127 22 22 ASP CG C 179.79 0.08 1 128 22 22 ASP N N 115.04 0.05 1 129 23 23 ALA C C 179.55 0.05 1 130 23 23 ALA CA C 54.49 0.09 1 131 23 23 ALA CB C 18.29 0.04 1 132 23 23 ALA N N 122.40 0.06 1 133 24 24 ALA C C 181.40 0.04 1 134 24 24 ALA CA C 54.55 0.05 1 135 24 24 ALA CB C 18.33 0.03 1 136 24 24 ALA N N 120.64 0.02 1 137 25 25 THR C C 175.84 0.07 1 138 25 25 THR CA C 67.41 0.14 1 139 25 25 THR CB C 67.79 0.07 1 140 25 25 THR CG2 C 21.51 0.04 1 141 25 25 THR N N 116.95 0.09 1 142 26 26 ALA C C 177.34 0.07 1 143 26 26 ALA CA C 54.99 0.07 1 144 26 26 ALA CB C 17.45 0.04 1 145 26 26 ALA N N 123.63 0.04 1 146 27 27 GLU C C 177.82 0.06 1 147 27 27 GLU CA C 59.17 0.06 1 148 27 27 GLU CB C 29.05 0.07 1 149 27 27 GLU CD C 181.52 0.02 1 150 27 27 GLU CG C 35.53 0.06 1 151 27 27 GLU N N 116.11 0.09 1 152 28 28 LYS C C 179.11 0.03 1 153 28 28 LYS CA C 60.23 0.06 1 154 28 28 LYS CB C 32.76 0.05 1 155 28 28 LYS CD C 29.99 0.05 1 156 28 28 LYS CE C 42.36 0.03 1 157 28 28 LYS CG C 26.47 0.08 1 158 28 28 LYS N N 117.06 0.08 1 159 28 28 LYS NZ N 33.37 0.03 1 160 29 29 VAL C C 178.81 0.07 1 161 29 29 VAL CA C 66.30 0.05 1 162 29 29 VAL CB C 31.90 0.04 1 163 29 29 VAL CG1 C 22.29 0.05 2 164 29 29 VAL CG2 C 21.03 0.05 2 165 29 29 VAL N N 118.96 0.07 1 166 30 30 PHE C C 179.10 0.08 1 167 30 30 PHE CA C 57.47 0.05 1 168 30 30 PHE CB C 37.38 0.04 1 169 30 30 PHE N N 118.44 0.09 1 170 31 31 LYS C C 179.64 0.05 1 171 31 31 LYS CA C 60.13 0.07 1 172 31 31 LYS CB C 31.69 0.06 1 173 31 31 LYS CD C 29.39 0.08 1 174 31 31 LYS CE C 41.24 0.07 1 175 31 31 LYS CG C 27.17 0.09 1 176 31 31 LYS N N 120.51 0.04 1 177 31 31 LYS NZ N 32.33 0.04 1 178 32 32 GLN C C 177.55 0.06 1 179 32 32 GLN CA C 58.87 0.09 1 180 32 32 GLN CB C 28.93 0.03 1 181 32 32 GLN CD C 179.83 0.07 1 182 32 32 GLN CG C 34.15 0.05 1 183 32 32 GLN N N 121.00 0.08 1 184 32 32 GLN NE2 N 115.58 0.07 1 185 33 33 TYR C C 178.66 0.04 1 186 33 33 TYR CA C 61.51 0.09 1 187 33 33 TYR CB C 37.62 0.15 1 188 33 33 TYR N N 120.70 0.07 1 189 34 34 ALA C C 179.64 0.03 1 190 34 34 ALA CA C 56.08 0.07 1 191 34 34 ALA CB C 18.14 0.02 1 192 34 34 ALA N N 122.45 0.03 1 193 35 35 ASN C C 179.57 0.08 1 194 35 35 ASN CA C 57.04 0.07 1 195 35 35 ASN CB C 39.30 0.08 1 196 35 35 ASN CG C 176.05 0.06 1 197 35 35 ASN N N 118.07 0.03 1 198 35 35 ASN ND2 N 113.38 0.06 1 199 36 36 ASP C C 176.24 0.07 1 200 36 36 ASP CA C 55.94 0.10 1 201 36 36 ASP CB C 38.30 0.07 1 202 36 36 ASP CG C 177.71 0.04 1 203 36 36 ASP N N 121.10 0.08 1 204 37 37 ASN C C 174.33 0.04 1 205 37 37 ASN CA C 53.53 0.04 1 206 37 37 ASN CB C 40.33 0.06 1 207 37 37 ASN CG C 176.80 0.06 1 208 37 37 ASN N N 114.83 0.05 1 209 37 37 ASN ND2 N 114.27 0.04 1 210 38 38 GLY C C 174.07 0.09 1 211 38 38 GLY CA C 46.90 0.03 1 212 38 38 GLY N N 108.37 0.08 1 213 39 39 VAL C C 175.15 0.02 1 214 39 39 VAL CA C 61.71 0.07 1 215 39 39 VAL CB C 31.87 0.06 1 216 39 39 VAL CG1 C 21.98 0.04 2 217 39 39 VAL CG2 C 21.98 0.04 2 218 39 39 VAL N N 121.47 0.07 1 219 40 40 ASP C C 175.07 0.06 1 220 40 40 ASP CA C 52.77 0.04 1 221 40 40 ASP CB C 41.78 0.09 1 222 40 40 ASP CG C 180.89 0.05 1 223 40 40 ASP N N 130.70 0.07 1 224 41 41 GLY C C 172.70 0.05 1 225 41 41 GLY CA C 45.14 0.04 1 226 41 41 GLY N N 108.30 0.11 1 227 42 42 GLU C C 177.85 0.08 1 228 42 42 GLU CA C 55.25 0.05 1 229 42 42 GLU CB C 31.53 0.05 1 230 42 42 GLU CD C 181.95 0.07 1 231 42 42 GLU CG C 36.12 0.11 1 232 42 42 GLU N N 119.03 0.02 1 233 43 43 TRP C C 177.32 0.03 1 234 43 43 TRP CA C 57.52 0.06 1 235 43 43 TRP CB C 33.74 0.03 1 236 43 43 TRP N N 112.01 0.13 1 237 44 44 THR C C 173.93 0.08 1 238 44 44 THR CA C 60.89 0.09 1 239 44 44 THR CB C 73.03 0.07 1 240 44 44 THR CG2 C 21.01 0.05 1 241 44 44 THR N N 108.98 0.09 1 242 45 45 TYR C C 171.89 0.06 1 243 45 45 TYR CA C 57.87 0.07 1 244 45 45 TYR CB C 42.96 0.08 1 245 45 45 TYR N N 118.42 0.04 1 246 46 46 ASP C C 176.26 0.08 1 247 46 46 ASP CA C 50.84 0.05 1 248 46 46 ASP CB C 42.63 0.12 1 249 46 46 ASP CG C 180.12 0.08 1 250 46 46 ASP N N 126.05 0.03 1 251 47 47 ASP C C 177.41 0.07 1 252 47 47 ASP CA C 54.83 0.06 1 253 47 47 ASP CB C 43.11 0.04 1 254 47 47 ASP CG C 176.63 0.06 1 255 47 47 ASP N N 123.42 0.10 1 256 48 48 ALA C C 179.63 0.04 1 257 48 48 ALA CA C 54.13 0.06 1 258 48 48 ALA CB C 18.99 0.04 1 259 48 48 ALA N N 118.77 0.01 1 260 49 49 THR C C 175.70 0.09 1 261 49 49 THR CA C 60.22 0.09 1 262 49 49 THR CB C 69.97 0.07 1 263 49 49 THR CG2 C 21.67 0.02 1 264 49 49 THR N N 103.68 0.10 1 265 50 50 LYS C C 175.47 0.10 1 266 50 50 LYS CA C 55.63 0.09 1 267 50 50 LYS CB C 28.10 0.12 1 268 50 50 LYS CD C 28.22 0.08 1 269 50 50 LYS CE C 43.38 0.06 1 270 50 50 LYS CG C 24.43 0.04 1 271 50 50 LYS N N 119.88 0.03 1 272 50 50 LYS NZ N 34.36 0.08 1 273 51 51 THR C C 174.42 0.06 1 274 51 51 THR CA C 62.45 0.05 1 275 51 51 THR CB C 71.67 0.04 1 276 51 51 THR CG2 C 21.32 0.05 1 277 51 51 THR N N 111.87 0.08 1 278 52 52 PHE C C 175.79 0.06 1 279 52 52 PHE CA C 56.59 0.08 1 280 52 52 PHE CB C 43.30 0.13 1 281 52 52 PHE N N 129.94 0.08 1 282 53 53 THR C C 172.26 0.04 1 283 53 53 THR CA C 60.25 0.11 1 284 53 53 THR CB C 71.88 0.08 1 285 53 53 THR CG2 C 21.17 0.10 1 286 53 53 THR N N 111.87 0.04 1 287 54 54 VAL C C 172.60 0.05 1 288 54 54 VAL CA C 58.46 0.05 1 289 54 54 VAL CB C 32.69 0.05 1 290 54 54 VAL CG1 C 21.84 0.03 2 291 54 54 VAL CG2 C 19.69 0.03 2 292 54 54 VAL N N 118.00 0.06 1 293 55 55 THR C C 174.23 0.07 1 294 55 55 THR CA C 61.27 0.09 1 295 55 55 THR CB C 72.02 0.05 1 296 55 55 THR CG2 C 21.45 0.06 1 297 55 55 THR N N 123.84 0.03 1 298 56 56 GLU C C 180.63 0.02 1 299 56 56 GLU CA C 57.62 0.06 1 300 56 56 GLU CB C 33.17 0.06 1 301 56 56 GLU CD C 183.22 0.02 1 302 56 56 GLU CG C 38.72 0.05 1 303 56 56 GLU N N 130.79 0.10 1 stop_ save_