######################### # Spectral peak lists # ######################### save_spectral_peak_list_1 _Spectral_peak_list.Sf_category spectral_peak_list _Spectral_peak_list.Sf_framecode spectral_peak_list_1 _Spectral_peak_list.Entry_ID 30947 _Spectral_peak_list.ID 1 _Spectral_peak_list.Name . _Spectral_peak_list.Sample_ID 1 _Spectral_peak_list.Sample_label $sample_1 _Spectral_peak_list.Sample_condition_list_ID 1 _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 _Spectral_peak_list.Chem_shift_reference_ID 1 _Spectral_peak_list.Chem_shift_reference_label $chem_shift_reference_1 _Spectral_peak_list.Experiment_ID 2 _Spectral_peak_list.Experiment_name '2D 1H-1H TOCSY' _Spectral_peak_list.Experiment_class . _Spectral_peak_list.Experiment_type . _Spectral_peak_list.Number_of_spectral_dimensions 2 _Spectral_peak_list.Chemical_shift_list . _Spectral_peak_list.Assigned_chem_shift_list_ID 1 _Spectral_peak_list.Assigned_chem_shift_list_label $assigned_chemical_shifts_1 _Spectral_peak_list.Details ; A combined overlay of 1H-1H 2D COSY, TOCSY, and ROESY experiments were used to assign the proton chemical shifts. Peaks were picked within the TOCSY spectrum as peak height maxima allowed for the most precise measurement of shifts between the experiments employed. Peaks denoted (ROE) in the list were found in the 2D 1H-1H ROESY spectrum. ; _Spectral_peak_list.Text_data_format text _Spectral_peak_list.Text_data ; Notes on peak picking and annotation: 1) Chemical shifts were calculated only from non-ROE peaks, using TOCSY maxima and in cases of overlap, the centerpoint of a phase-sensitve COSY crosspeak 2) Diastereotopic protons and methyl groups were annotate such that the more upfield of the pair was labeled 1 and the more downfield labeled 2. If superimposed and not resolvable in the f2 dimension, then the group was labeled 12. e.g. For leucine methyl groups, resolved: HD1 and HD2. For leucine beta protons, not resolved - HB12. 3) Peaks that were solely chosen from the ROESY spectrum are indicated with (ROE) in parentheses. No ROE peaks that also included a TOCSY peak were used to generate the NMR ensemble or any of the associated restraints. f2 (ppm) f1 (ppm) Annotation 1 0.89 4.30 Leu(10)HD1-HA 2 0.89 8.08 Leu(10)HD1-HN 3 0.92 8.17 Leu(4)HD1-HN 4 0.92 4.21 Leu(4)HD1-HA 5 0.92 4.29 Leu(11)HD1-HA 6 0.93 7.97 Leu(11)HD1-HN 7 0.94 4.30 Leu(10)HD2-HA 8 0.94 8.08 Leu(10)HD2-HN 9 0.97 8.16 Leu(4)HD2-HN 10 0.97 4.21 Leu(4)HD2-HA 11 0.97 3.90 Leu(4)HD12-Ser(6)HB1(ROE) 12 0.98 7.97 Leu(11)HD2-HN 13 0.98 4.30 Leu(11)HD2-HA 14 1.16 8.04 Thr(3)HB-HN 15 1.16 4.15 Thr(3)HG-HB 16 1.16 4.31 Thr(3)HG-HA 17 1.43 3.90 Ala(7)HB-Gly(8)HA12(ROE) 18 1.44 3.95 Ala(7)HB-Ser(6)HB2(ROE) 19 1.44 4.34 Ala(7)HB-HA 20 1.44 8.31 Ala(7)HB-HN 21 1.51 4.33 Lys13/ 14 HG12-HA 22 1.51 8.08 Lys(13)HG12-HN 23 1.52 8.32 Lys(14)HG12-HN 24 1.60 4.22 Leu(4)HB12/ HG-HA 25 1.61 8.17 Leu(4)HB12/ HG-HN 26 1.61 8.37 Leu(4)HB12/ HG-Asn(5)HN(ROE) 27 1.62 8.08 Leu(10)HB12/ HG-HN 28 1.66 8.25 Leu(11)HB12/ HG-Gly(12)HN(ROE) 29 1.67 3.97 Leu(11)HB12/ HG-Gly(8)HA12(ROE) 30 1.67 7.97 Leu(11)HB12/ HG-HN 31 1.67 3.89 Leu(11)HB12/ HG-Ser(6)HB1(ROE) 32 1.68 3.91 Leu(11)HB12/ HG-Gly(8)HA12(ROE) 33 1.68 4.32 Leu(11)HB12/ HG-HA 34 1.71 8.06 Lys(13)HD12-HN 35 1.72 4.37 Lys(13)HD12-HA 36 1.72 8.32 Lys(14)HD12-hN 37 1.72 4.33 Lys(14)HD12-HA 38 1.80 4.37 Lys(13)HB1-HA 39 1.80 8.07 Lys(13)HB1-HN 40 1.81 4.32 Lys(14)HB1-HA 41 1.82 8.31 Lys(14)HB1-HN 42 1.87 4.32 Lys(14)HB2-HA 43 1.87 8.31 Lys(14)HB2-HN 44 1.88 4.36 Lys(13)HB2-HA 45 1.89 8.08 Lys(13)HB2-HN 46 2.83 6.92 Asn(5)HB12-NH1 (ROE) 47 2.83 7.58 Asn(5)HB12-NH2 (ROE) 48 2.85 8.37 Asn(5)HB12-HN 49 2.86 8.22 Asn(5)HB12-Ser(6)HN (ROE) 50 2.87 4.74 Asn(5)HB12-HA 51 3.03 4.33 Lys13/ 14 HE12/ HA 52 3.06 7.91 Tyr(9)HB12-HN 53 3.07 4.57 Tyr(9)HB12-HA 54 3.07 7.14 Tyr(9)HB12-H26 (ROE) 55 3.07 8.08 Tyr(9)HB12-Leu(10)HN (ROE) 56 3.28 7.65 Trp(2)HB1-H4 57 3.28 7.30 Trp(2)HB1-H2 (ROE/ allylic coupling) 58 3.29 8.58 Trp(2)HB1-HN 59 3.29 4.85 Trp(2)HB1-HA 60 3.31 8.05 Trp(2)HB12-Thr(3)HN (ROE) 61 3.33 7.30 Trp(2)HB2-H2 (ROE/ allylic coupling) 62 3.33 8.58 Trp(2)HB2-HN 63 3.34 7.65 Trp(2)HB2-H4 (ROE) 64 3.34 4.85 Trp(2)HB2-HA 65 3.89 4.41 Ser(6)HB1-HA 66 3.89 1.66 Ser(6)HB1-Leu(11)HB12/ HG(ROE) 67 3.89 0.95 Ser(6)HB1-Leu(4)HD12(ROE) 68 3.89 7.97 Gly(8)HA12-Leu(11)NH(ROE) 69 3.90 1.43 Gly(8)HA12-Ala(7)HB(ROE0 70 3.90 8.26 Gly(8)HA12-HN 71 3.90 7.91 Gly(8)HA12-Tyr(9)HN (ROE) 72 3.91 7.90 Gly(8)HA12-Tyr(9)HN(ROE) 73 3.92 1.67 Gly(8)HA12-Leu(11)HB12/ HG(ROE) 74 3.94 8.23 Ser(6)HB12-HN 75 3.94 4.41 Ser(6)HB2-HA 76 3.95 1.44 Ser(6)HB2-Ala(7)HB2(ROE) 77 3.95 7.90 Ser(6)HB12-Tyr(9)HN (ROE) 78 3.97 1.66 Gly(12)HA12-Leu(11)HB12/ HG(ROE) 79 3.97 8.25 Gly(12)HA12-HN 80 3.97 8.08 Gly(12)HA12-Lys(13)HN (ROE) 81 3.97 8.08 Gly(12)HA12-Leu(10)HN (ROE) 82 4.14 8.36 Thr(3)HB-Asn(5)HN (ROE) 83 4.15 4.31 Thr(3)HB-HA 84 4.15 8.05 Thr(3)HB-HN 85 4.15 1.16 Thr(3)HB-HG 86 4.15 8.15 Thr(3)HB-Leu(4)HN (ROE) 87 4.21 8.36 Leu(4)HA-Asn(5)HN (ROE) 88 4.21 8.16 Leu(4)HA-HN 89 4.22 1.60 Leu(4)HA-HB12/ HG 90 4.22 0.95 Leu(4)HA-HD12 91 4.30 1.85 Lys(14)HA-HD12/ HB12f 92 4.30 1.50 Lys(14)HA-HG12 93 4.31 1.16 Thr(3)HA-HG 94 4.31 4.15 Thr(3)HA-HB 95 4.31 0.94 Leu(11)HA-HD12 96 4.31 1.62 Leu(10)HA-HB12/ HG 97 4.31 0.93 Leu(10)HA-HD12 98 4.31 8.16 Thr(3)HA-Leu(4)HN (ROE) 99 4.32 1.67 Leu(11)HA-HB12/ HG 100 4.32 8.31 Ala(7)HA-HN 101 4.32 8.25 Ala(7)HA-Gly(8)HA12 (ROE) 102 4.32 8.05 Thr(3)HA-HN 103 4.33 7.97 Leu(11)HA-HN 104 4.34 1.44 Ala(7)HA-HB 105 4.35 8.31 Lys(14)HA-HN 106 4.36 8.08 Leu(10)HA-HN 107 4.36 1.85 Lys(13)HA-HD12/ HB12 108 4.36 8.08 Lys(13)HA-HN 109 4.36 1.45 Lys(13)HA-HG12 110 4.41 8.22 Ser(6)HA-HN 111 4.41 8.31 Ser(6)HA-Ala(7)HN (ROE) 112 4.41 3.92 Ser(6)HA-HB12 113 4.56 3.06 Tyr(9)HA-HB12 114 4.57 7.91 Tyr(9)HA-HN 115 6.87 4.34 Tyr(9)H35-Ala(7)HA (ROE) 116 6.87 4.57 Tyr(9)H35-HA (ROE) 117 6.87 7.16 Tyr(9)H35-H26 118 6.88 3.06 Tyr(9)H35-HB12 (ROE) 119 6.88 0.92 Tyr(9)H35-Leu(10)HD12 (ROE) 120 6.92 2.87 Asn(5)NH1-HB12(ROE) 121 6.92 7.58 Asn(5)NH1-NH2(ROE) 122 7.13 0.91 Tyr(9)H26-Leu(10)HD12 (ROE) 123 7.14 7.91 Tyr(9)H26-HN(ROE) 124 7.14 1.51 Tyr(9)H26-Lys(13)HG12(ROE) 125 7.14 6.88 Tyr(9)H26-H35 126 7.14 4.34 Tyr(9)H26-Ala(7)HA (ROE) 127 7.14 4.57 Tyr(9)H26-HA (ROE) 128 7.14 3.06 Tyr(9)H26-HB12 (ROE) 129 7.15 3.91 Tyr(9)H26-Gly(8)HA12 (ROE) 130 7.19 7.67 Trp(2)H5-H4 131 7.20 7.28 Trp(2)H5-H6 132 7.20 7.55 Trp(2)H5-H7 133 7.28 7.55 Trp(2)H6-H7 134 7.28 7.67 Trp(2)H6-H4 135 7.28 7.19 Trp(2)H6-H5 136 7.30 10.13 Trp(2)H2-NH1 137 7.30 4.78 Trp(2)H2-HA (ROE) 138 7.30 3.32 Trp(2)H2-HB12 (ROE/ allylic coupling) 139 7.53 4.31 Trp(2)H7-Thr(3)HA(ROE) 140 7.54 7.28 Trp(2)H7-H6 141 7.54 7.67 Trp(2)H7-H4 142 7.54 7.19 Trp(2)H7-H5 143 7.54 10.13 Trp(2)H7-NH1 (ROE) 144 7.58 6.92 Asn(5)NH2-NH1 (ROE) 145 7.58 2.86 Asn(5)NH2-HB12 (ROE) 146 7.58 4.31 Asn(5)NH1-Thr(3)HA(ROE) 147 7.65 7.89 Trp(2)H4-Tyr(9)HN(ROE) 148 7.66 7.19 Trp(2)H4-H5 149 7.66 7.54 Trp(2)H4-H7 150 7.66 4.31 Trp(2)H4-Thr(3)HA(ROE) 151 7.66 3.33 Trp(2)H4-HB12 (ROE) 152 7.66 7.29 Trp(2)H4-H6 153 7.88 7.64 Tyr(9)HN-Trp(2)H4(ROE) 154 7.90 4.57 Tyr(9)HN-HA 155 7.90 3.93 Tyr(9)HN-Ser(6)HB12(ROE) 156 7.90 7.14 Tyr(9)HN-H26(ROE) 157 7.90 3.06 Tyr(9)HN-HB12 158 7.90 3.90 Tyr(9)HN-Gly(8)HA12 (ROE) 159 7.90 8.26 Tyr(9)HN-Gly(8)HN(ROE) 160 7.97 8.23 Leu(11)HN-Gly(12)HN(ROE) 161 7.97 3.89 Leu(11)HN-Gly(8)HA12(ROE) 162 7.97 4.33 Leu(11)HN-HA 163 7.97 1.68 Leu(11)HN-HB12/ HG 164 7.97 0.96 Leu(11)HN-HD12 165 7.97 4.57 Leu(11)HN-Tyr(9)HA (ROE) 166 8.04 1.15 Thr(3)HN-HG 167 8.04 4.32 Thr(3)HN-HA 168 8.04 4.15 Thr(3)HN-HB 169 8.04 3.31 Thr(3)HN-Trp(2)HB12 (ROE) 170 8.08 3.05 Leu(10)HN-Tyr(9)HB12 (ROE) 171 8.08 1.49 Lys(13)NH-HG12 172 8.08 0.91 Leu(10)HN-HD12 173 8.08 1.62 Leu(10)HN-HB12/ HG 174 8.08 1.82 Lys(13)HN-HB12/ HD12 175 8.08 4.56 Leu(10)HN-Tyr(9)HA (ROE) 176 8.08 4.35 Leu(10)HN-HA 177 8.08 4.37 Lys(13)HN-HA 178 8.08 3.97 Leu(10)HN-Gly(12)HA12 (ROE) 179 8.08 3.98 Lys(13)HN-Gly(12)HA12 (ROE) 180 8.15 4.22 Leu(4)HN-HA 181 8.15 4.33 Leu(4)HN-Thr(3)HA (ROE) 182 8.15 1.16 Leu(4)HN-Thr(3)HG (ROE) 183 8.15 0.95 Leu(4)HN-HD12 184 8.15 4.14 Leu(4)HN-Thr(3)HB (ROE) 185 8.16 1.61 Leu(4)HN-HB12/ HG 186 8.22 3.93 Ser(6)HN-HB12 187 8.22 4.41 Ser(6)HN-HA 188 8.22 2.86 Ser(6)HN-Asn(5)HB12 (ROE) 189 8.24 7.98 Gly(12)HN-Leu(11)HN(ROE) 190 8.24 1.66 Gly(12)HN-Leu(11)HB12/ HG(ROE) 191 8.25 3.89 Gly(8)HN-HA12 192 8.25 4.34 Gly(8)HN-Ala(7)HA (ROE) 193 8.25 3.97 Gly(12)HN-HA12 194 8.26 7.91 Gly(8)HN-Tyr(9)HN(ROE) 195 8.31 1.43 Ala(7)HN-HB 196 8.31 4.33 Lys(14)NH-HA 197 8.31 4.33 Ala(7)HN-HA 198 8.31 4.42 Ala(7)HN-Ser(6)HA (ROE) 199 8.31 1.45 Lys(14)HN-HG12 200 8.32 1.83 Lys(14)HN-HB12/ HD12 201 8.36 4.74 Asn(5)HN-HA 202 8.37 4.22 Asn(5)HN-Leu(4)HA (ROE) 203 8.37 1.61 Asn(5)HN-Leu(4)HB12/ HG (ROE) 204 8.37 0.95 Asn(5)HN-Leu(4)HD12 (ROE) 205 8.38 2.85 Asn(5)HN-HB12 206 8.56 3.33 Trp(2)HN-HB12 207 8.57 4.78 Trp(2)HN-HA 208 10.12 7.31 Trp(2)NH1-H2 209 10.12 7.54 Trp(2)NH1-H7 (ROE) ; loop_ _Spectral_dim.ID _Spectral_dim.Axis_code _Spectral_dim.Spectrometer_frequency _Spectral_dim.Atom_type _Spectral_dim.Atom_isotope_number _Spectral_dim.Spectral_region _Spectral_dim.Magnetization_linkage_ID _Spectral_dim.Under_sampling_type _Spectral_dim.Sweep_width _Spectral_dim.Sweep_width_units _Spectral_dim.Value_first_point _Spectral_dim.Absolute_peak_positions _Spectral_dim.Acquisition _Spectral_dim.Center_frequency_offset _Spectral_dim.Encoding_code _Spectral_dim.Encoded_reduced_dimension_ID _Spectral_dim.Entry_ID _Spectral_dim.Spectral_peak_list_ID 1 . . H 1 H . . 4761.9 Hz . . . 4.69 . . 30947 1 2 . . H 1 H . . 4761.9 Hz . . . 4.69 . . 30947 1 stop_ save_