data_7262 #Corrected using PDB structure: 2JM2A # #N.B. (Observed* = Observed shift + Offset correction) # #After reference correction, the following residues still #have a HA chemical shift difference (obs*-pred) greater than 0.7ppm: #NUM AA CS Observed* Predicted # 10 Q HA 4.36 5.08 # 14 A HA 4.36 5.15 # 41 R HA 4.37 3.42 # #After reference correction, the following residues still #have a N chemical shift difference (obs*-pred) greater than 10.0ppm: #NUM AA CS Observed* Predicted # 16 C N 116.00 130.14 # #The average CS difference between predicted and observed: #HA CA CB CO N HN #0.02 N/A N/A N/A -2.20 -0.40 # #bmr7262.str.corr chemical shifts have been re-referenced with the following #offsets (these values have been added to the original bmr7262.str file): #HA CA CB CO N HN #N/A N/A N/A N/A -2.20 N/A # #The 95% confidence intervals for the above recommended offsets are: # HA CA CB CO N HN #+/-0.05 N/A N/A N/A +/-0.85 +/-0.10 # #The Correlation Coefficients between predicted and observed #chemical shifts are: #HA CA CB CO N HN #0.563 N/A N/A N/A 0.706 0.529 # #The RMSD between predicted and observed* (reference #corrected) chemical shifts are: #HA CA CB CO N HN #0.155 N/A N/A N/A 2.465 0.317 # save_entry_information _Saveframe_category entry_information _Entry_title ; NMR assignments of the the N-terminal subdomain of IGFBP-6 ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Chandrashekaran Indu R. . 2 Yao Shenggen . . 3 Wang Chunxiao C. . 4 Bansal Paramjit S. . 5 Alewood Paul F. . 6 Wallace John C. . 7 Bach Leon A. . 8 Norton Raymond S. . stop_ _BMRB_accession_number 7262 _BMRB_flat_file_name bmr7262.str _Entry_type new _Submission_date 2006-08-10 _Accession_date 2006-08-11 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 199 "13C chemical shifts" 37 "15N chemical shifts" 35 "coupling constants" 15 stop_ save_ save_entry_citation _Saveframe_category entry_citation _Citation_title ; The N-Terminal Subdomain of Insulin-like Growth Factor (IGF) Binding Protein 6. Structure and Interaction with IGFs ; _Citation_status published _Citation_type journal _PubMed_ID 17305365 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Chandrashekaran Indu R. . 2 Yao Shenggen . . 3 Wang Chunxiao C. . 4 Bansal Paramjit S. . 5 Alewood Paul F. . 6 Forbes B. E. . 7 Wallace John C. . 8 Bach Leon A. . 9 Norton Raymond S. . stop_ _Journal_abbreviation Biochemistry _Journal_volume ? _Journal_issue ? _Page_first ? _Page_last ? _Year 2007 loop_ _Keyword IGFBP-6 "Insulin like growth factors" "NMR assignments" stop_ save_ save_assembly _Saveframe_category molecular_system _Mol_system_name 1-45IGFBP-6 _Abbreviation_common 1-45IGFBP-6 loop_ _Mol_system_component_name _Mol_label 1-45IGFBP-6 $1-45IGFBP-6 stop_ _System_molecular_weight 4365.7 _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state "all disulfide bound" loop_ _Biological_function "Insulin like growth factor regulation" stop_ _Details ; 1-45 of IGFBP-6 comprising the N-terminal subdomain of IGFBP-6. ; save_ save_1-45IGFBP-6 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common NN-BP-6 _Name_variant NN-BP-6 _Abbreviation_common NN-BP-6 _Mol_thiol_state "all disulfide bound" loop_ _Biological_function "IGF binding protein" stop_ _Residue_count 45 _Mol_residue_sequence ; ALARCPGCGQGVQAGCPGGC VEEEDGGSPAEGCAEAEGCL RREGQ ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 LEU 3 ALA 4 ARG 5 CYS 6 PRO 7 GLY 8 CYS 9 GLY 10 GLN 11 GLY 12 VAL 13 GLN 14 ALA 15 GLY 16 CYS 17 PRO 18 GLY 19 GLY 20 CYS 21 VAL 22 GLU 23 GLU 24 GLU 25 ASP 26 GLY 27 GLY 28 SER 29 PRO 30 ALA 31 GLU 32 GLY 33 CYS 34 ALA 35 GLU 36 ALA 37 GLU 38 GLY 39 CYS 40 LEU 41 ARG 42 ARG 43 GLU 44 GLY 45 GLN stop_ save_ save_crosslink_bonds _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single disulfide 1-45IGFBP-6 5 CYS SG 1-45IGFBP-6 8 CYS SG single disulfide 1-45IGFBP-6 16 CYS SG 1-45IGFBP-6 20 CYS SG single disulfide 1-45IGFBP-6 33 CYS SG 1-45IGFBP-6 39 CYS SG stop_ save_ save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $1-45IGFBP-6 Human 9606 Eukaryota Metazoa Homo sapiens stop_ save_ save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $1-45IGFBP-6 "chemical synthesis" ? ? ? ? ? stop_ save_ save_sample_1 _Saveframe_category sample _Sample_type solution loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $1-45IGFBP-6 1.1 mM ? "Sodium acetate" 10 mM ? "Sodium azide" 0.02 % ? D2O 5 % ? stop_ save_ save_software_1 _Saveframe_category software _Name Topspin _Version 1.3 loop_ _Vendor _Address _Electronic_address Bruker ? ? stop_ _Details "Data collection and processing" save_ save_software_2 _Saveframe_category software _Name XEASY _Version 1.3 _Details "Peak assignment" save_ save_500MHz_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 save_ save_600MHz_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 600 save_ save_NMR_experiment_list _Saveframe_category NMR_applied_experiment _Experiment_name ; 2D 1H-1H NOESY 2D 1H-1H TOCSY 2D 1H-1H DQF-COSY 1H15N_HSQC 1H-13C HMQC ; save_ save_1H-13C_HMQC _Saveframe_category NMR_applied_experiment _Experiment_name "1H-13C HMQC" _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY _Saveframe_category NMR_applied_experiment _Experiment_name "2D 1H-1H NOESY" _Sample_label $sample_1 save_ save_2D_1H-1H_DQF-COSY _Saveframe_category NMR_applied_experiment _Experiment_name "2D 1H-1H DQF-COSY" _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY _Saveframe_category NMR_applied_experiment _Experiment_name "2D 1H-1H TOCSY" _Sample_label $sample_1 save_ save_1H15N_HSQC _Saveframe_category NMR_applied_experiment _Experiment_name "1H15N HSQC" _Sample_label $sample_1 save_ save_conditions_1 _Saveframe_category sample_conditions loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 288 0.2 K pH 4.3 0.1 pH "ionic strength" 10 0.002 mM stop_ save_ save_chemical_shift_referencing _Saveframe_category chemical_shift_reference 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 ? ? ? 1.0 DSS N 15 "methyl protons" ppm 0.0 ? indirect ? ? ? 0.101329118 DSS C 13 "methyl protons" ppm 0.0 ? indirect ? ? ? 0.251449530 stop_ save_ save_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts loop_ _Experiment_label $2D_1H-1H_NOESY $2D_1H-1H_TOCSY $1H15N_HSQC $1H-13C_HMQC $2D_1H-1H_DQF-COSY stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name 1-45IGFBP-6 loop_ _Atom_shift_assign_ID _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 ALA HA H 4.09 0.02 1 2 1 ALA HB H 1.52 0.02 1 3 1 ALA CA C 51.30 0.5 1 4 1 ALA CB C 19.00 0.5 1 5 2 LEU H H 8.59 0.02 1 6 2 LEU HA H 4.33 0.02 1 7 2 LEU HB2 H 1.60 0.02 2 8 2 LEU HD1 H 0.92 0.02 2 9 2 LEU N N 122.20 0.5 1 10 3 ALA H H 8.54 0.02 1 11 3 ALA HA H 4.35 0.02 1 12 3 ALA HB H 1.38 0.02 1 13 3 ALA CA C 52.30 0.5 1 14 3 ALA N N 122.00 0.5 1 15 4 ARG H H 8.50 0.02 1 16 4 ARG HA H 4.33 0.02 1 17 4 ARG HB2 H 1.84 0.02 2 18 4 ARG HB3 H 1.76 0.02 2 19 4 ARG HG2 H 1.64 0.02 2 20 4 ARG HD2 H 3.19 0.02 2 21 4 ARG N N 118.40 0.5 1 22 5 CYS H H 8.43 0.02 1 23 5 CYS HA H 4.89 0.02 1 24 5 CYS HB2 H 3.20 0.02 2 25 5 CYS HB3 H 3.38 0.02 2 26 5 CYS N N 117.90 0.5 1 27 6 PRO HA H 4.42 0.02 1 28 6 PRO HB2 H 2.16 0.02 2 29 6 PRO HB3 H 2.31 0.02 2 30 6 PRO HG2 H 2.00 0.02 2 31 6 PRO HD2 H 3.71 0.02 2 32 6 PRO HD3 H 3.84 0.02 2 33 6 PRO CA C 64.30 0.5 1 34 7 GLY H H 8.87 0.02 1 35 7 GLY HA2 H 3.99 0.02 2 36 7 GLY HA3 H 3.92 0.02 2 37 7 GLY CA C 45.10 0.5 1 38 7 GLY N N 108.50 0.5 1 39 8 CYS H H 7.93 0.02 1 40 8 CYS HA H 4.46 0.02 1 41 8 CYS HB2 H 3.20 0.02 2 42 8 CYS HB3 H 3.42 0.02 2 43 8 CYS CA C 58.30 0.5 1 44 8 CYS CB C 38.30 0.5 1 45 8 CYS N N 117.00 0.5 1 46 9 GLY H H 8.66 0.02 1 47 9 GLY HA2 H 3.97 0.02 2 48 9 GLY N N 107.60 0.5 1 49 10 GLN H H 8.38 0.02 1 50 10 GLN HA H 4.34 0.02 1 51 10 GLN HB2 H 2.15 0.02 2 52 10 GLN HB3 H 1.98 0.02 2 53 10 GLN HG2 H 2.36 0.02 2 54 10 GLN HE21 H 7.56 0.02 2 55 11 GLY H H 8.56 0.02 1 56 11 GLY HA2 H 3.98 0.02 2 57 11 GLY N N 108.00 0.5 1 58 12 VAL H H 8.13 0.02 1 59 12 VAL HA H 4.11 0.02 1 60 12 VAL HB H 2.08 0.02 1 61 12 VAL HG1 H 0.92 0.02 2 62 12 VAL CA C 62.30 0.5 1 63 12 VAL CB C 32.50 0.5 1 64 12 VAL N N 117.40 0.5 1 65 13 GLN H H 8.55 0.02 1 66 13 GLN HA H 4.35 0.02 1 67 13 GLN HB2 H 2.11 0.02 2 68 13 GLN HB3 H 1.98 0.02 2 69 13 GLN HG2 H 2.38 0.02 2 70 13 GLN CA C 54.80 0.5 1 71 13 GLN CB C 28.90 0.5 1 72 13 GLN N N 119.70 0.5 1 73 14 ALA H H 8.40 0.02 1 74 14 ALA HA H 4.34 0.02 1 75 14 ALA HB H 1.38 0.02 1 76 14 ALA CA C 52.00 0.5 1 77 14 ALA N N 123.40 0.5 1 78 15 GLY H H 8.45 0.02 1 79 15 GLY HA2 H 3.97 0.02 2 80 15 GLY N N 105.50 0.5 1 81 16 CYS H H 8.20 0.02 1 82 16 CYS HA H 4.90 0.02 1 83 16 CYS HB2 H 3.26 0.02 2 84 16 CYS HB3 H 2.85 0.02 2 85 16 CYS N N 116.00 0.5 1 86 17 PRO HA H 4.40 0.02 1 87 17 PRO HB2 H 2.10 0.02 2 88 17 PRO HB3 H 2.25 0.02 2 89 17 PRO HG2 H 1.99 0.02 2 90 17 PRO HD2 H 3.67 0.02 2 91 17 PRO HD3 H 3.76 0.02 2 92 17 PRO CA C 64.10 0.5 1 93 18 GLY H H 8.79 0.02 1 94 18 GLY HA2 H 4.06 0.02 2 95 18 GLY HA3 H 3.89 0.02 2 96 18 GLY CA C 45.10 0.5 1 97 18 GLY N N 109.90 0.5 1 98 19 GLY H H 8.08 0.02 1 99 19 GLY HA2 H 3.79 0.02 2 100 19 GLY HA3 H 4.38 0.02 2 101 19 GLY CA C 43.40 0.5 1 102 19 GLY N N 107.40 0.5 1 103 20 CYS H H 8.75 0.02 1 104 20 CYS HA H 4.65 0.02 1 105 20 CYS HB2 H 2.98 0.02 2 106 20 CYS HB3 H 3.36 0.02 2 107 20 CYS CA C 55.10 0.5 1 108 20 CYS CB C 41.70 0.5 1 109 20 CYS N N 118.50 0.5 1 110 21 VAL H H 8.40 0.02 1 111 21 VAL HA H 4.10 0.02 1 112 21 VAL HB H 2.05 0.02 1 113 21 VAL HG1 H 0.92 0.02 2 114 21 VAL N N 119.10 0.5 1 115 22 GLU H H 8.58 0.02 1 116 22 GLU HA H 4.33 0.02 1 117 22 GLU HB2 H 1.96 0.02 2 118 22 GLU HB3 H 2.06 0.02 2 119 22 GLU HG2 H 2.39 0.02 2 120 23 GLU H H 8.46 0.02 1 121 23 GLU HA H 4.34 0.02 1 122 23 GLU HB2 H 1.97 0.02 2 123 23 GLU HB3 H 2.08 0.02 2 124 23 GLU HG2 H 2.40 0.02 2 125 23 GLU N N 119.80 0.5 1 126 24 GLU H H 8.54 0.02 1 127 24 GLU HA H 4.36 0.02 1 128 24 GLU HB2 H 1.98 0.02 2 129 24 GLU HB3 H 2.10 0.02 2 130 24 GLU HG2 H 2.40 0.02 2 131 24 GLU N N 123.90 0.5 1 132 25 ASP H H 8.54 0.02 1 133 25 ASP HA H 4.67 0.02 1 134 25 ASP HB2 H 2.80 0.02 2 135 25 ASP CA C 53.50 0.5 1 136 25 ASP CB C 39.60 0.5 1 137 25 ASP N N 118.80 0.5 1 138 26 GLY H H 8.46 0.02 1 139 26 GLY HA2 H 3.97 0.02 2 140 26 GLY CA C 45.00 0.5 1 141 27 GLY H H 8.29 0.02 1 142 27 GLY HA2 H 3.98 0.02 2 143 27 GLY N N 106.30 0.5 1 144 28 SER H H 8.24 0.02 1 145 28 SER HA H 4.80 0.02 1 146 28 SER HB2 H 3.85 0.02 2 147 28 SER CA C 56.20 0.5 1 148 28 SER CB C 63.20 0.5 1 149 28 SER N N 114.50 0.5 1 150 29 PRO HA H 4.43 0.02 1 151 29 PRO HB2 H 2.29 0.02 2 152 29 PRO HG2 H 1.95 0.02 2 153 29 PRO HD2 H 3.71 0.02 2 154 29 PRO CA C 63.30 0.5 1 155 29 PRO CB C 34.00 0.5 1 156 30 ALA H H 8.41 0.02 1 157 30 ALA HA H 4.28 0.02 1 158 30 ALA HB H 1.38 0.02 1 159 30 ALA CA C 52.40 0.5 1 160 30 ALA CB C 18.90 0.5 1 161 30 ALA N N 121.90 0.5 1 162 31 GLU H H 8.32 0.02 1 163 31 GLU HA H 4.33 0.02 1 164 31 GLU HB2 H 1.99 0.02 2 165 31 GLU HB3 H 2.12 0.02 2 166 31 GLU HG2 H 2.41 0.02 2 167 32 GLY H H 8.45 0.02 1 168 32 GLY HA2 H 3.96 0.02 2 169 33 CYS H H 8.32 0.02 1 170 33 CYS HA H 4.65 0.02 1 171 33 CYS HB2 H 3.12 0.02 2 172 33 CYS CA C 55.30 0.5 1 173 33 CYS CB C 41.50 0.5 1 174 33 CYS N N 116.50 0.5 1 175 34 ALA H H 8.77 0.02 1 176 34 ALA HA H 4.39 0.02 1 177 34 ALA HB H 1.42 0.02 1 178 34 ALA CA C 52.60 0.5 1 179 34 ALA CB C 18.70 0.5 1 180 34 ALA N N 125.70 0.5 1 181 35 GLU H H 8.05 0.02 1 182 35 GLU HA H 4.32 0.02 1 183 35 GLU HB2 H 2.01 0.02 2 184 35 GLU HB3 H 2.17 0.02 2 185 35 GLU HG2 H 2.42 0.02 2 186 35 GLU N N 116.80 0.5 1 187 36 ALA H H 8.61 0.02 1 188 36 ALA HA H 4.17 0.02 1 189 36 ALA HB H 1.44 0.02 1 190 36 ALA CA C 53.80 0.5 1 191 36 ALA CB C 18.40 0.5 1 192 36 ALA N N 122.30 0.5 1 193 37 GLU H H 8.28 0.02 1 194 37 GLU HA H 4.33 0.02 1 195 37 GLU HB2 H 2.07 0.02 2 196 37 GLU HB3 H 2.19 0.02 2 197 37 GLU HG2 H 2.41 0.02 2 198 37 GLU N N 114.00 0.5 1 199 38 GLY H H 8.18 0.02 1 200 38 GLY HA2 H 4.14 0.02 2 201 38 GLY HA3 H 3.83 0.02 2 202 38 GLY CA C 45.10 0.5 1 203 38 GLY N N 106.20 0.5 1 204 39 CYS H H 8.17 0.02 1 205 39 CYS HA H 4.62 0.02 1 206 39 CYS HB2 H 3.19 0.02 2 207 39 CYS HB3 H 3.12 0.02 2 208 39 CYS CA C 56.20 0.5 1 209 39 CYS CB C 41.40 0.5 1 210 39 CYS N N 115.60 0.5 1 211 40 LEU H H 8.37 0.02 1 212 40 LEU HA H 4.34 0.02 1 213 40 LEU HB2 H 1.63 0.02 2 214 40 LEU HD1 H 0.85 0.02 2 215 40 LEU HD2 H 0.91 0.02 2 216 40 LEU N N 122.10 0.5 1 217 41 ARG H H 8.36 0.02 1 218 41 ARG HA H 4.35 0.02 1 219 41 ARG HB2 H 1.82 0.02 2 220 41 ARG HB3 H 1.75 0.02 2 221 41 ARG HG2 H 1.63 0.02 2 222 41 ARG HD2 H 3.19 0.02 2 223 41 ARG HE H 7.28 0.02 1 224 41 ARG N N 120.30 0.5 1 225 42 ARG H H 8.47 0.02 1 226 42 ARG HA H 4.34 0.02 1 227 42 ARG HB2 H 1.83 0.02 2 228 42 ARG HB3 H 1.74 0.02 2 229 42 ARG HG2 H 1.64 0.02 2 230 42 ARG HD2 H 3.19 0.02 2 231 42 ARG HE H 7.24 0.02 1 232 42 ARG N N 121.10 0.5 1 233 43 GLU H H 8.57 0.02 1 234 43 GLU HA H 4.33 0.02 1 235 43 GLU HB2 H 1.99 0.02 2 236 43 GLU HB3 H 2.09 0.02 2 237 43 GLU HG2 H 2.39 0.02 2 238 44 GLY H H 8.59 0.02 1 239 44 GLY HA2 H 4.01 0.02 2 240 44 GLY HA3 H 3.90 0.02 2 241 44 GLY N N 108.90 0.5 1 242 45 GLN H H 7.95 0.02 1 243 45 GLN HA H 4.21 0.02 1 244 45 GLN HB2 H 2.14 0.02 2 245 45 GLN HB3 H 1.94 0.02 2 246 45 GLN HG2 H 2.28 0.02 2 247 45 GLN CA C 56.70 0.5 1 248 45 GLN CB C 30.10 0.5 1 249 45 GLN N N 122.20 0.5 1 stop_ save_ save_J_coupling_list_1 _Saveframe_category coupling_constants loop_ _Experiment_label $2D_1H-1H_DQF-COSY stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name 1-45IGFBP-6 loop_ _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 3JHNHA 5 CYS H 5 CYS HA 9.8 ? ? 0.1 3JHNHA 8 CYS H 8 CYS HA 8.1 ? ? 0.1 3JHNHA 12 VAL H 12 VAL HA 8.7 ? ? 0.1 3JHNHA 16 CYS H 16 CYS HA 10.0 ? ? 0.1 3JHNHA 20 CYS H 20 CYS HA 9.35 ? ? 0.1 3JHNHA 21 VAL H 21 VAL HA 9.5 ? ? 0.1 3JHNHA 25 ASP H 25 ASP HA 9.2 ? ? 0.1 3JHNHA 28 SER H 28 SER HA 9.2 ? ? 0.1 3JHNHA 33 CYS H 33 CYS HA 8.7 ? ? 0.1 3JHNHA 34 ALA H 34 ALA HA 8.9 ? ? 0.1 3JHNHA 35 GLU H 35 GLU HA 8.9 ? ? 0.1 3JHNHA 36 ALA H 36 ALA HA 10.0 ? ? 0.1 3JHNHA 37 GLU H 37 GLU HA 7.7 ? ? 0.1 3JHNHA 39 CYS H 39 CYS HA 8.5 ? ? 0.1 3JHNHA 45 GLN H 45 GLN HA 8.6 ? ? 0.1 stop_ save_